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APPLICATIONS

GC Applications by Column Phase . . . . . . . . . . . . .462463 EPA Method Chart . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .463 HPLC Applications . . . . . . . . . . . . . . . . . . . . . . . . .464-527 Biochemical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .465-469
Nucleosides, Nucleotides, Nucleic Acid Bases, Aromatic Amino Acids, Carboxylic Acids

Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .470-488
Aldehydes & Ketones, Herbicides, Aromatics, Explosives, Pesticides, Phenols, Phthalate Esters, Polynuclear Aromatic Hydrocarbons

General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .488-496
Test Mixes

Dietary Supplements / Plant Extracts . . . . . . . . . . .497-500


Extracts, Vitamins

Foods & Flavors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .501-508


Antimicrobial Agents, Carboxylic Acids, Sugars, Seasonings, Flavorings

Pharmaceutical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .509-527
Analgesics, Antiarrhythmics, Antiasthmatics, Antibiotics, Antidepressants, Anti-Diabetics, Anti-Inflammatories, Anti-Ulceratives, Bronchodilators, Corticosteroids, Steroid Hormones, Mixed Drugs, Sedatives, Xanthenes

GC Applications . . . . . . . . . . . . . . . . . . . . . . . . . . .528-737 Environmental . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .529-623


Volatiles, Semivolatiles, Pesticides, Herbicides, PCBs, Chlorinated Disinfection Byproducts, Dioxins, Endocrine Disruptors, Explosives, Gasoline Range Organics (GRO), Diesel Range Organics (DRO), Glycols, Haloacetic Acids, Air Analysis

Foods, Flavors, & Fragrances . . . . . . . . . . . . . . . . . . . .624-653


Chiral Separations, Fatty Acids, FAMEs, Essential Oils, Flavors & Fragrances, Food Contaminants, Sterols, Triglycerides, Sugars/Sugar Alcohols

Forensics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .654-660
Blood Alcohol, Drugs of Abuse, Anesthetics, Solvents, Inhalants, Arson Accelerants

Personal Care & Cleaning Products . . . . . . . . . . . . .661-662


Solvents, Fragrances

Petroleum & Petrochemicals . . . . . . . . . . . . . . . . . . .663-689


Permanent Gases, Fluorocarbon Gases, Hydrocarbon Gases, Hydrocarbons, Sulfur Compounds

Pharmaceutical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .690-704
Antidepressants, Antihistamines, Antiepileptics, Barbiturates, Basic Drugs, Chiral Analyses, Pharmaceutical Solvents, Steroids, Sympathomimetic Amines

Solvents & Chemicals . . . . . . . . . . . . . . . . . . . . . . . . . .705-737


Solvents, Alcohols, Aldehydes, Acrylates, Amines, Aromatics, Chlorofluorocarbons, Cresylic Acids, Esters, Glycols, Ketones, Silanes, Styrene, Siloxanes

Compound Index . . . . . . . . . . . . . . . . . . . . . . . . . .738-745

462

GC Applications by Phase
GC Applications by Phase
Rtx-1 air samples . . . . . . . . . . . . . . . . . . . . 619, 621, 622, 623 aromatics (gasoline) . . . . . . . . . . . . . . . . . . . . . . . . 673 chlorofluorocarbons. . . . . . . . . . . . . . . . . 730, 731, 732 essential oils . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 642 fatty acids (free). . . . . . . . . . . . . . . . . . . . . . . . . . . . 630 flavor volatiles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 643 fragrances . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 647, 662 hydrocarbons (accelerants) . . . . . . . . . . . . . . . 659, 660 hydrocarbons (C7-C42) . . . . . . . . . . . . . . . . . . . . . 678 hydrocarbons (crude oil). . . . . . . . . . . . . . . . . . . . . 681 hydrocarbons (detailed reformate analysis) . . . . . . 680 hydrocarbons (gases) . . . . . . . . . . . . . . . . . . . . 671, 672 hydrocarbons (waxes) . . . . . . . . . . . . . . . . . . . 682, 683 organophosphorus pesticides . . . . . . . . . . . . . . . . . 582 oxygenates . . . . . . . . . . . . . . . . . . . . . . . . . . . . 674, 675 ozone precursors . . . . . . . . . . . . . . . . . . . . . . . . . . . 619 solvents . . . . . . . . . . . . . . . . . . . 705, 706, 708, 711, 717 solvents (pharmaceutical) . . . . . . . . . . . . . . . . 699, 715 sulfur compounds . . . . . . . . . . . . . . . . . . . . . . . . . . 688 Rtx-1PONA hydrocarbons (detailed gasoline analysis) . . . . . . . 679 MXT-1HT Sim Dist hydrocarbons (crude oil). . . . . . . . . . . . . . . . . . . . . 682 hydrocarbons (high temp.) . . . . . . . . . . . . . . . 684, 685 MXT-1 Sim Dist hydrocarbons (high temp.) . . . . . . . . . . . . . . . . . . . 685 MXT-500 Sim Dist hydrocarbons (high temp.) . . . . . . . . . . . . . . . . . . . 685 Rtx-2887 simulated distillation . . . . . . . . . . . . . . . . . . . . . . . . 686 Rtx-XLB organochlorine pesticides . . . . . . . . . . . . . . . . 574, 575 PCBs. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 598 Rtx-5 / MXT-5 alcohols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 721 benzidines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 546 chlorinated disinfection byproducts . . . . . . . . . . . . 599 chlorinated hydrocarbons . . . . . . . . . . . . . . . . . . . . 553 chlorophenoxyacid herbicides. . . . . . . . . . . . . . . . . 587 Diesel range organics (DRO). . . . . . . . . . 612, 613, 614 drugs of abuse . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 656 endocrine disruptors . . . . . . . . . . . . . . . . . . . . . . . . 601 essential oils . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 639 gasoline range organics (GRO) . . . . . . . . 606, 607, 611 haloacetic acids . . . . . . . . . . . . . . . . . . . . . . . . . . . . 617 haloethers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 552 hazardous substances . . . . . . . . . . . . . . . . . . . . . . . 553 hydrocarbons (accelerants) . . . . . . . . . . . . . . . . . . . 659 nitrosamines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548 nitroaromatics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548 nitrogen herbicides . . . . . . . . . . . . . . . . . . . . . . . . . 590 nitrogen/phosphorus pesticides & herbicides. . . . . 586 organochlorine pesticides . . . . . . . . . . . . 568, 569, 577 PCBs. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 592, 593 pharmaceuticals (basic) . . . . . . . . . . . . . . 694, 695, 704 phenols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 545, 546 polynuclar aromatic hydrocarbons . . . . . 550, 551, 552 phthalate esters . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547 siloxane . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 737 solvents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 712 steroids. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 701 sterols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 651 XTI-5 glycols / alcohols . . . . . . . . . . . . . . . . . . . . . . . . . . . 735 phenols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 546 sterols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 651 Rtx-5MS endocrine disruptors . . . . . . . . . . . . . . . . . . . . . . . . 601 semivolatiles. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 555 volatiles (food packaging) . . . . . . . . . . . . . . . . . . . . 650 Rtx-5Sil MS aromatics (GRO) . . . . . . . . . . . . . . . . . . . . . . . . . . . 604 polynuclear aromatic hydrocarbons . . . . . . . . . . . . 549 phenols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 554 semivolatiles . . . . . . . . . . . . . . . . . . . . . . . 554, 556-565 Rtx-5 Amine amines / phenols . . . . . . . . . . . . . . . . . . . . . . . . . . . 725 ethanolamines / ethyleneamines . . . . . . . . . . . . . . . 724 pharmaceuticals (basic) . . . . . . . . . . . . . . 690, 696, 703 Rtx-20 antioxidants . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 624 essential oils . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 641 pharmaceuticals (acid/neutral) . . . . . . . . . . . . . . . . 691 Rtx-1301 flavor volatiles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 645 solvents (pharmacutical) . . . . . . . . . . . . . . . . . 699, 701 Rtx-1701 acrylates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 723 aldehydes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 723 fragrances. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 647 organochlorine pesticides . . . . . . . . . . . . . . . . . . . . 577 organophosphorus pesticides . . . . . . . . . . . . . . . . . 580 pharmaceuticals (acid/neutral) . . . . . . . . . . . . 691, 692 pharmaceuticals (basic). . . . . . . . . . . . . . . . . . . . . . 690 solvents . . . . . . . . . . . . . . . . . . . . . . . . . . . 710, 717, 718 styrene . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 736 Rtx-200 aromatics (BTEX) . . . . . . . . . . . . . . . . . . . . . . . . . . 676 chlorofluorocarbons . . . . . . . . . . . . . . . . . . . . 731, 732 chlorinated disinfection byproducts . . . . . . . . . . . . 599 chlorinated hydrocarbons . . . . . . . . . . . . . . . . . . . . 552 explosives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 602 fatty acids (free). . . . . . . . . . . . . . . . . . . . . . . . . . . . 630 glycols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 615, 735 haloacetic acids . . . . . . . . . . . . . . . . . . . . . . . . . . . . 617 nitrosamines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548 pharmaceuticals (basic) . . . . . . . . . . . . . . 693, 695, 703 phenols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 545 silanes. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 736 siloxane . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 737 solvents . . . . . . . . . . . . . . . . . . . . . . . 705, 707, 708, 710 solvents (pharmaceutical) . . . . . . . . . . . . . . . . . . . . 716 triazine herbicides . . . . . . . . . . . . . . . . . . . . . . . . . . 588 Rtx-35 chlorinated hydrocarbons . . . . . . . . . . . . . . . . . . . . 553 chlorophenoxyacid herbicides. . . . . . . . . . . . . . . . . 587 endocrine disruptors . . . . . . . . . . . . . . . . . . . . . . . . 601 nitrogen herbicides . . . . . . . . . . . . . . . . . . . . . . . . . 590 organochlorine pesticides . . . . . . . . . . . . . . . . . . . . 576 organophosphorus pesticides . . . . . . . . . . . . . . . . . 580 pharmaceuticals (acid/neutral) . . . . . . . . . . . . 692, 693 pharmaceuticals (basic) . . . . . . . . . . . . . . . . . . 694, 696 Rtx-35 Amine amines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 736 pharmaceuticals (basic) . . . . . . . . . . . . . . . . . . 702, 703 Rtx-50 antioxidants . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 624 chlorophenoxy herbicides . . . . . . . . . . . . . . . . . . . . 589 organochlorine pesticides . . . . . . . . . . . . . . . . . . . . 577 phenols. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 545 phthalate esters . . . . . . . . . . . . . . . . . . . . . . . . . . . . 547 triazine herbicides . . . . . . . . . . . . . . . . . . . . . . . . . . 588 Rtx-65TG triglycerides . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 652 Rtx-225 sugars . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 653 Rtx-440 organochlorine pesticides . . . . . . . . . . . . . . . . . . . . 569 polynuclear aromatic hydrocarbons . . . . . . . . . . . . 551 Stabilwax acrylamide . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 649 alcohols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 720 alcohols / aldehydes . . . . . . . . . . . . . . . . . . . . . . . . . 722 aldehydes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 722 amines / alcohols / chlorides . . . . . . . . . . . . . . . . . . 727 aromatics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 728, 729 essential oils . . . . . . . . . . . . . . . . . . . . . . . 639, 641, 642 esters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 733 ethers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 734 FAMEs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 635 flavor volatiles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 643 glycols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 616 hydrocarbons (synthetic lubricant) . . . . . . . . . . . . 682 ketones . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 735 nitrosamines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 548 oxygenates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 675 solvents . . . . . . . . . . . . . . . 706, 707, 709, 711, 713, 718 styrene . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 736 Rtx-WAX / MXT-WAX aldehydes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 723 aromatics (BTEX) . . . . . . . . . . . . . . . . . . . . . . . . . . 676 essential oils . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 640 FAMEs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 635 FAMEs (cis/trans) . . . . . . . . . . . . . . . . . . . . . . . . . . 634 glycols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 615 solvents . . . . . . . . . . . . . . . . . . . . . . . . . . . 661, 712, 713 FAMEWAX FAMEs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 636, 638 RT-CW20M F&F flavors / fragrances. . . . . . . . . . . . . . . . . . . . . . . . . . 648 Stabilwax-DA cresylic acids . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 732 fatty acids (free) . . . . . . . . . . . . . . . . . . . . . . . . 630, 631 flavor volatiles . . . . . . . . . . . . . . . . . . . . . . . . . 644, 646 solvents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 713 Stabilwax-DB amines . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 725, 727 Rtx-2330 Dioxins (TCDD) . . . . . . . . . . . . . . . . . . . . . . . . . . . 600 FAMEs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 635, 637 sugars . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 652 Rt-2560 FAMEs (cis/trans) . . . . . . . . . . . . . . . . . . 632, 633, 634 Stx-CLPesticides/Stx-CLPesticides2 organochlorine pesticides . . . . . . . . . . . . . . . . . . . . 572 Rtx-CLPesticides/Rtx-CLPesticides2 chlorophenoxyacid herbicides. . . . . . . . . . . . . . . . . 589 EDB / DBCP . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 566 haloacetic acids . . . . . . . . . . . . . . . . . . . . . . . . . . . . 618 nitrogen/phosphorus herbicides . . . . . . . . . . . . . . . 585 organochlorine pesticides 567, 570, 571, 573, 576, 583, 584 organophosphorus pesticides . . . . . . . . . . . . . . . . . 581 polynuclear aromatic hydrocarbons . . . . . . . . . . . . 549 PCBs . . . . . . . . . . . . . . . . . . . . . . . . . 594, 595, 596, 597 Rtx-OPPesticides/Rtx-OPPesticides2 organophosphorus pesticides . . . . . . . . . . . . . 578, 579 triazine herbicides . . . . . . . . . . . . . . . . . . . . . . . . . . 591 Rtx-VMS solvents. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 661, 662 volatiles. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 537-543 Rtx-VGC aromatics (BTEX) . . . . . . . . . . . . . . . . . . . . . . . . . . 608 oxygenates . . . . . . . . . . . . . . . . . . . . . . . . . . . . 608, 610 volatiles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 530, 532 Rtx-VRX volatiles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 531, 536

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GC Applications by Phase, EPA Methods Chart


GC Applications by Phase (cont.)
Rtx-502.2 air toxins . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 620 alcohols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 719 alcohols / aldehydes . . . . . . . . . . . . . . . . . . . . . . . . . 721 aromatics . . . . . . . . . . . . . . . . . . . . . . . . . 676, 728, 729 aromatics (BTEX) . . . . . . . . . . . . . . . . . . . . . . . . . . 609 aromatics / aliphatics (GRO). . . . . . . . . . . . . . 605, 607 ethers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 734 volatiles . . . . . . . . . . . . . . . . . . . . . . . 533, 534, 535, 544 Rtx-Volatiles alcohols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 721 solvents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 713 Rtx-TNT/Rtx-TNT2 explosives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 603 Rtx-BAC1/Rtx-BAC2 anesthetics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 657 blood alcohol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 654 glycols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 616 inhalants . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 658 solvents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 657 Rtx-G27 & Rtx-G43 solvents (pharmaceutical) . . . . . . . . . . . . . . . . . . . . 700 Rt-TCEP aromatics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 677 oxygenates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 674 Chiral Columns flavors / fragrances . . . . . . . . . . . . . . . . . . . . . . 625-629 pharmaceuticals . . . . . . . . . . . . . . . . . . . . . . . . 697, 698 di-isodecyl phthalate cresylic acids . . . . . . . . . . . . . 733 Micropacked & PLOT HayeSep S hydrocarbon gases . . . . . . . . . . . . . . . . . . . . . . . . . . 671 Rt-Alumina PLOT hydrocarbon gases . . . . . . . . . . . . . . . . . . 670, 671, 672 Rt-Msieve 13X PLOT hydrocarbon gases . . . . . . . . . . . . . . . . . . . . . . . . . . 666 permanent gases. . . . . . . . . . . . . . . . . . . . . . . . 663, 664 Rt-Msieve 5A PLOT permanent gases. . . . . . . . . . . . . . . . . . . . . . . . 664, 665 Rt-QPLOT alcohols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 720 fatty acids (free). . . . . . . . . . . . . . . . . . . . . . . . . . . . 630 hydrocarbon gases . . . . . . . . . . . . . . 666, 667, 668, 669 permanent gases. . . . . . . . . . . . . . . . . . . . . . . . 664, 665 solvents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 714 Rt-SPLOT hydrocarbon gases . . . . . . . . . . . . . . . . . . . . . . . . . . 669 Rt-UPLOT hydrocarbon gases . . . . . . . . . . . . . . . . . . . . . . 666, 669 solvents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 714 Rt-XLSulfur sulfurs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 689 sulfurs in beverages . . . . . . . . . . . . . . . . . . . . . . . . . 649 Rt-Sulfur sulfurs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 689 ShinCarbon ST fluorocarbons . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 666 natural gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 668 permanent gases . . . . . . . . . . . . . . . . . . . . . . . . . . . 663 sulfur dioxide. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 688 TCEP oxygenates . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 674 Packed CarboBlack B flavor volatiles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 645 5% Carbowax 20M blood alcohol . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 655 HayeSep Q solvents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 714 5% Krytox/CarboBlack B chlorofluorocarbons . . . . . . . . . . . . . . . . . . . . . . . . 731 3% Rt-101 sugars . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 653 sugar alcohols . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 653 5% Rt-1200/1.75% Bentone 34 aromatics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 677 Rtx-1 Sim Dist 2887 simulated distillation . . . . . . . . . . . . . . . . . . . . 686, 687 10% TCEP aromatics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 678 20% TCEP aromatics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 674

463

A P P L I C AT I O N S

EPA Methods Chart


EPA 500 Series Methods
Method # Method Title ..................................................................Page # 502.2 Volatile Organic Compounds ..............................................534 504.1 1,2-dibromoethane & 1,2-dibromo-3-chloropropane ........566 508 Chlorinated Pesticides ................................................................567, 568 515.1 Chlorophenoxyacid Herbicides ............................................589 524.1/.2 Volatile Organics....................................................................543, 544 525 Semivolatile Organics............................................................563 526 Semivolatile Organics (screening) ........................................554 528 Phenols ..................................................................................554 551.1 Chlorinated Disinfection Byproducts ..................................599 552.2 Haloacetic Acids ....................................................................617, 618

E PA 8 0 0 0 S e r i e s M e t h o d s
Method # 8021 8060 8081 8090 8095 8100 8140/8141/ 8141A 8151 8240 8260B 8270 8330 8095 Method Title ..................................................................Page # Volatile Organics....................................................................530-533, 536 Phthalate Esters......................................................................547 Chlorinated Pesticides ..........................................................569-577 Nitroaromatics & Cyclic Ketones ........................................547 Explosives ..............................................................................603 Polynuclear Aromatic Hydrocarbons ..................................552 Organophosphorus Pesticides ..............................................578-582 Chlorophenoxyacid Herbicides ............................................589 Volatile Organics (8260 short list)........................................539 Volatile Organics....................................................................538, 540-542 Semivolatile Organics............................................................556-560 Explosives by HPLC ..............................................................474, 475 Explosives by GC ..................................................................603

E PA 6 0 0 S e r i e s M e t h o d s
Method # Method Title ..................................................................Page # 601 Purgeable Halocarbons ........................................................535 602 Purgeable Aromatics..............................................................535 604 Phenols ..................................................................................545, 546 605 Benzidines ..............................................................................546 606 Phthalate Esters......................................................................547 607 Nitrosamines..........................................................................548 609 Nitroaromatics & Isophorone ..............................................547 610 Polynuclear Aromatic Hydrocarbons (HPLC/GC)..............549, 550, 551 611 Haloethers ..............................................................................552 612 Chlorinated Hydrocarbons ..................................................552, 553 615 Chlorophenoxyacid Herbicides ............................................587 619 Nitrogen/Phosphorus Herbicides & Pesticides ..................585, 588 625 Base/Neutrals, Acids, & Pesticides ........................................564

CLP Methods
Method # OLC 03.2 CLP Appendix IX Skinner List Method Title ..................................................................Page # Volatile Organics....................................................................537, 562 Semivolatile Organics............................................................555 Semivolatile Organics ....................................................................561 Semivolatile Organics ....................................................................565

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HPLC & GC Applications

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Compound Index
starting on page 738

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Larry Peters
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HPLC Applications
Restek chromatograms are time-saving starting points for a new application, or for improving an analysis that is giving unsatisfactory results. The following pages include HPLC chromatograms for a wide range of samples, including environmental contaminants, biochemicals, pharmaceuticals, nutraceuticals, foods, flavors & fragrances, and forensic materials. To keep up with frequent new additions to our library of chromatograms, subscribe to the Restek Advantage, and regularly visit our web site at www.restek.com.

Biochemical
Adenine, Adenosine, ATP, ADP, and AMP on Ultra IBD
Peak List: 1. ATP 2. ADP 3. AMP 4. adenine 5. adenosine Conc. (g/mL) g 258 320 274 84 254 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
3

465

Cytosine, Cytidine, CTP, CDP, and CMP on Ultra IBD


Peak List: 1. CTP 2. CDP 3. CMP 4. cytosine 5. cytidine Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Conc. (g/mL): g 248 322 248 100 340 20L 20mM ammonium acetate, pH 5.8 Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM ammonium acetate,pH 5.8: methanol (97.5:2.5) 1.0mL/min. 35C UV @ 260nm

20L 20mM ammonium acetate, pH 5.8 Ultra IBD 9175565 150 x 4.6mm 5m 100

Flow: Temp.: Det.:

20mM ammonium acetate, pH 5.8: methanol (97.5:2.5) 1.0mL/min 35C UV @ 260nm

H P LC A P P L I C AT I O N S

1 5 4

10
LC_0129

12

14

16

18 min.
LC_0130

Nucleotides, Nucleosides, and Nitrogenous Bases on Ultra IBD


Peak List: Conc. (g/mL) g 1. CDP 146 2. CMP 113 3. ATP 117 5 4. ADP 145 5. cytidine 155 6. TMP 157 7. AMP 125 8. guanine 36 9. guanosine 103 10. adenine 38 11. adenosine 115 Sample: Inj.: Solvent: 20L 20mM ammonium acetate, pH 5.8 Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM ammonium acetate, pH 5.8:methanol (97.5:2.5) 1.0mL/min. 35C UV @ 260nm

Uracil, Uridine, UTP, UDP, and UMP on Ultra IBD

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

5 2 4

Peak List: 1. UTP 2. UDP 3. UMP 4. uracil 5. uridine Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

Conc. (g/mL) g 360 360 284 90 230

20L 90-360g/mL each component 20mM ammonium acetate, pH 5.8 Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM ammonium acetate, pH 5.8: methanol (97.5:2.5) 1.0mL/min. 35C UV @ 260nm

1 2 1 3 11 10 8 9

Flow: Temp.: Det.:

10
LC_0128

12

14

16

18

min.

4
LC_0133

6 min.

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466

Biochemical
Guanine, Guanosine, GTP, GDP, and GMP on Ultra IBD
Peak List: Conc. (g/mL) g 1. GTP 212 2. GDP 260 3. GMP 362 4. guanine 80 5. guanosine 226 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
1 1 4 5

Thymine, Thymidine, TTP, TDP, and TMP on Ultra IBD

20L 20mM ammonium acetate, pH 5.8 Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM ammonium acetate, pH 5.8:methanol (97.5:2.5) 1.0mL/min. 35C UV @ 260nm
2 4 5

Peak List: Conc. (g/mL) g 1. TTP 224 2. TDP 152 3. TMP 346 4. thymine 88 5. thymidine 318 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 20L 20mM ammonium acetate, pH 5.8 Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM ammonium acetate, pH 5.8: methanol (97.5:2.5) 1.0mL/min. 35C UV @ 260nm

H P LC A P P L I C AT I O N S

2.5

7.5
LC_0131

10

12.5

15 min.

10
LC_0132

12

14

16 min.

Nucleic Acid Bases on Allure PFP Propyl

Peak List: 1. cytosine 2. uracil 3. guanine 4. thymine 5. adenine

Sample: Inj.: Conc. Solvent:

1.0L 100g/mL each 20 mM ammonium acetate, pH 5.0 Note: 1-3 drops of ammonium hydroxide added to keep guanine in solution Allure PFP Propyl 9169565 150 x 4.6mm 5m 60 20mM ammonium acetate, pH 5.0: methanol (85:15, v/v) 1.0mL/min. ambient UV @ 260nm

2 3

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
4

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5
LC_0137

9 min.

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Biochemical
Purines/Pyrimidines on Ultra PFP

467

5 6 7 2 8

Peak List: 1. cytosine 2. 5-methylcytosine 3. uracil 4. uric acid 5. hypoxanthine 6. xanthine 7. thymine 8. purine 9. theobromine 10. ethyluracil 11. 6-methylpurine 12. 1,7-dimethylxanthine 13. theophylline 14. propyluracil Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size:
9 10

H P LC A P P L I C AT I O N S

10L 100mg/mL each mobile phase Ultra PFP 9176575 250 x 4.6mm 5m 100 0.001% formic acid in water: methanol (50:50, v/v) 1.0mL/min. ambient UV @ 260nm

Conditions: Mobile phase:


11 12 13 14

Flow: Temp.: Det.:

10

15
LC_0136

20

25 min.

Aromatic Amino Acids on Ultra Aqueous C18 (Fast Analysis)


Conc. (mg/mL) 1.25 0.55 0.035

Aromatic Amino Acids on Ultra Aqueous C18

Peak List: 1. tyrosine 2. phenylalanine 3. tryptophan Sample: Inj.: Diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

Peak List: Conc. (mg/mL) 1. tyrosine 0.2 2. phenylalanine 1.6 3. tryptophan 0.4 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: 20L mobile phase A Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100

10L 50mM potassium phosphate, pH 2.5 Ultra Aqueous C18 9178535 30 x 4.0mm 5m 100 A: 50mM potassium phosphate, pH 2.5 B: acetonitrile Time (min.) 0.0 1.0 1.2 5.0 %B 0 40 0 0

Conditions: Mobile phases: A: 50mM potassium phosphate, pH 2.5 B: acetonitrile 5% - 20% B: 0-5 min. 20% - 5% B: 5-6 min. Hold at 5% B: 6-13 min. Flow: 1.0mL/min. Temp.: 30C Det.: UV @ 254nm

Flow: Temp.: Det.:

1.0mL/min. 50C UV @ 254nm


1

0
LC_0307

4
LC_0146

10

min.

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468

Biochemical
Carboxylic Acids on Ultra Aqueous C18 Carboxylic Acids in 100% Aqueous Mobile Phase on Ultra Aqueous C18
Peak List: 1. glycolic acid 2. malonic acid 3. acetic acid 4. maleic acid Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conc. (mg/mL) 5.4 4.2 7.8 0.06 10L mobile phase Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100
4

Peak List: Conc. (mg/mL) 1. glycolic acid 5.4 2. malonic acid 4.2 3. acetic acid 7.8 4. maleic acid 0.060 Sample: Inj.: Solvent: 10L 50mM potassium phosphate, pH 2.5 Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100 50mM potassium phosphate, pH 2.5 1.0mL/min. 25C (or ambient) UV @ 210nm

Stable retention times, even with 100% aqueous mobile phase!

H P LC A P P L I C AT I O N S

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Conditions: Mobile phase: 50mM potassium phosphate, pH 2.5 Flow rate: 1.0mL/min. Temp.: 25C Det.: UV @ 210nm 1

A. initial B. after 3 Days

0
LC_0168

4
LC_0142

7 min.

Carboxylic Acids on Ultra Aqueous C18

Carboxylic Acids on Ultra Aqueous C18

Peak List: 1. malonic acid 2. lactic acid 3. acetic acid 4. citric acid 5. succinic acid 6. fumaric acid Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 10L water

Conc. (g/mL): g 500 500 1000 1000 2000 10


1

5 3

Peak List: 1. glycolic acid 2. malonic acid 3. lactic acid 4. acetic acid Sample: Inj.: Solvent:
6

Conc. (mg/mL) 2.0 1.8 3.3 2.1 10L mobile phase Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100

Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100 50mM potassium phosphate, pH 2.5: acetonitrile (99:1) 1.5mL/min. 25C UV @ 210nm
2

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

50mM potassium phosphate, pH 2.5 1.0mL/min. ambient UV @ 210nm

4 min.

LC_0140

LC_0228

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Biochemical
Carboxylic Acids on Ultra Aqueous C18 (Fast Analysis) Carboxylic Acids on Ultra IBD
Peak List: 1. glycolic acid 2. lactic acid 3. acetic acid 4. malonic acid Conc. (mg/ml) 2.6 2.8 4.9 0.0125 10L 50mM potassium phosphate, pH 2.5 Ultra Aqueous C18 Fast LC Cartridge (91783340) and holder (25298) 30 x 4.0mm 5m 100 50mM potassium phosphate, pH 2.5 2.0mL/min. ambient UV @ 210nm Conc. (mg/mL) 2.0 3.3 2.1 1.8

469

Peak List: 1. glycolic acid 2. malonic acid 3. acetic acid 4. maleic acid Sample: Inj.: Diluent: Column: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

10L mobile phase Ultra IBD 9175565 150 x 4.6mm 5m 100

H P LC A P P L I C AT I O N S

50mM potassium phosphate, pH 2.5 1.0mL/min. ambient UV @ 210nm

LC_0306

LC_0229

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470

Environmental
Aldehydes and Ketones (DNPH derivatives) on Ultra C18 (40C) Peak List:
1

H P LC A P P L I C AT I O N S

DNPH derivatives of: 1. formaldehyde 2. acetaldehyde 3. acetone 4. acrolein 5. propionaldehyde 6. crotonaldehyde 7. MEK 8. methacrolein 9. butyraldehyde 10. benzaldehyde 11. valeraldehyde 12. m-tolualdehyde 13. hexanaldehyde
4 3 5 6 7 8 9

Sample: Inj.: Conc.: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

10L 3.0g/mL each, as derivative Ultra C18 9174565 150 x 4.6mm 5m 100

Flow rate: Wavelength: Temp.:

Solvent A: water Solvent B: acetonitrile Solvent C: tetrahydrofuran 50-30% A/30-65% B/20-5% C, 0-15 min. 1.5mL/min. 365nm 40C

10

11 12 13

6
LC_0036

10

12

14 min.

Aldehydes and Ketones (DNPH derivatives) on Ultra C18 (60C)


1

Peak List DNPH derivatives of: 1. formaldehyde 2. acetaldehyde 3. acrolein 4. acetone 5. propionaldehyde 6. crotonaldehyde 7. methacrolein 8. butyraldehyde 9. methyl ethyl ketone (MEK) 10. benzaldehyde 11. valeraldehyde 12. m-tolualdehyde 13. hexanaldehyde

Sample: Inj. Conc. Column: Catalog #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

10L 3g/mL as DNPH derivative Ultra C18 9174565 150 x 4.6mm 5m 100 Solvent A: water Solvent B: methanol Mode : gradient 70-76% B: 0-18 min. 1.0mL/min. 60C UV @ 360nm

Flow: Temp.: Det.:

3 45

7 8 9 10 11 12 13

8
LC_0052

10

12

14

16 min.

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Environmental
Aldehydes and Ketones (DNPH derivatives) on Allure C18 (15C)
Peak List: DNPH derivatives of: 1. formaldehyde 2. acetaldehyde 3. acrolein 4. acetone 5. propionaldehyde 6. crotonaldehyde 7. n-butyraldehyde 8. benzaldehyde 9. isovaleraldehyde 10. valeraldehyde 11. o-tolualdehyde 12. m-tolualdehyde 13. p-tolualdehyde 14. hexaldehyde 15. dimethylbenzaldehyde Ret. time (min.) 3.03 3.80 4.77 4.93 5.29 6.50 7.30 8.24 9.72 10.40 11.40 11.83 12.33 15.28 16.43 Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pressure:

471

5L Aldehydes/Ketones DNPH Standard (Cat.# 31808) 15g/mL each component acetonitrile Allure C18 9164565 150 x 4.6mm 5m 60 water:acetonitrile (30:70 v/v) 1.0mL/min. 15C UV @ 365nm 85 bar

H P LC A P P L I C AT I O N S

EPA TO-11A and 8315

LC_0298

Aldehydes and Ketones (DNPH derivatives) on Allure C18 (25C)


1

Peak List: DNPH derivatives of: 1. formaldehyde 2 acetaldehyde 3. acrolein 4. acetone 5. propionaldehyde 6. crotonaldehyde 7. butyraldehyde 8. benzaldehyde 9. isovaleraldehyde 10. valeraldehyde 11. o-tolualdehyde 12. m-tolualdehyde 13. p-tolualdehyde 14. hexanaldehyde 15. dimethylbenzaldehyde

Ret. Time (min.) 2.84 3.53 4.35 4.53 4.85 5.81 6.63 7.24 8.77 9.33 9.85 10.20 10.50 13.50 13.95

Sample: Inj.: Conc.: Solvent:


2

10L Aldehydes/Ketones DNPH Standard (cat.# 31808) 15g/mL each acetonitrile Allure C18 9164565 150 x 4.6 mm 5m 60 water:acetonitrile (30:70 v/v) 1.0mL/min. 25C UV @ 365 nm

Column: Cat.# Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
6 7 8

4 5

EPA TO-11A and 8315

10 11 12 13 14 15

LC_0294

10

12

14

min.

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472

Environmental
Herbicides (Phenylurea) on Ultra C18
Peak List: 1. tebuthiuron 2. thidiazuron 3. monuron 4. fluometuron 5. diuron 6. propanil 7. siduron 8. linuron 9. carbazole 10. diflubenzuron Conc. (g/mL or ppm) 2 2 5 2 2 2 2 2 5 2 Sample: Inj.: Conc.: Sample diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

20L see peak list acetonitrile Ultra C18 9174565 150 x 4.6mm 5m 100 A: 25mM phosphate buffer, pH 2.5 B: acetonitrile Time (min.) %B 0 40 8 40 14 55 18 55 19 40 1.5 mL/min. ambient UV @ 245nm

H P LC A P P L I C AT I O N S

Flow: Temp.: Det.:

LC_0319

Phenylurea Herbicides on Ultra Cyano


Peak List: Conc. (g/mL or ppm) 1. tebuthiuron 2 2. monuron 5 3. thidiazuron 2 4. fluometuron 2 5. diuron 2 6. propanil 2 7. siduron 2 8. linuron 2 9. carbazole 5 10. diflubenzuron 2 Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile Phase: Ultra Cyano 9106575 250 x 4.6mm 5m 100 A: 25mM phosphate buffer, pH 2.5 B: acetonitrile Time (min.) %B 0 30 8 30 14 50 21 50 21.1 30 1.5mL/min ambient UV @ 245nm 20L see peak list acetonitrile

Flow: Temp.: Det.: Sample: Inj.: Conc.: Sample diluent:

LC_0320

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Environmental
Aromatics on Pinnacle II C18 Aromatics on Pinnacle DB C18
5 Peak List: 1. propylbenzene 2. butylbenzene 3. o-terphenyl 4. amylbenzene 5. triphenylene Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Conc. 15mg/mL 15mg/mL 0.2mg/mL 15mg/mL 0.1mg/mL 1

473

Peak List: 1. propylbenzene 2. butylbenzene 3. o-terphenyl 4. amylbenzene 5. triphenylene Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Conc. (g/mL) g 15000 15000 200 15000 100

5L methanol Pinnacle DB C18 9414565 150 x 4.6mm 5m 140 water:methanol (20:80) 1.0mL/min. ambient UV @ 254nm 2

5L methanol Pinnacle II C18 9214565 150 x 4.6mm 5m 110 water:methanol (20:80 v/v) 1.0mL/min. ambient UV @ 254nm
5 1

H P LC A P P L I C AT I O N S

3
2

10

12

14

16

0
LC_0258

8
LC_0256

10

12

14

min.

BTEX Mix on Pinnacle II C18


Peak List: 1. benzene 2. toluene 3. o-xylene 4. ethylbenzene 5. m-xylene & p-xylene Sample: Inj.: Conc.: Solvent: 10L 200g/mL each methanol Column: Catalog #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pinnacle II C18 9214565 150 x 4.6mm 5m 110 water:acetonitrile (50:50, v/v) 1.0mL/min. ambient UV @ 254nm

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LC_0161

Phone: 800-356-1688 or 814-353-1300 www.restek.com

474

Environmental
Explosives by EPA Method 8330 on Pinnacle II C18
Peak List: 1. HMX 2. RDX 3. 1,3,5-trinitrobenzene 4. 1,3-dinitrobenzene 5. tetryl 6. nitrobenzene 7. 2,4,6-trinitrotoluene 8. 2-amino-4,6-dinitrotoluene 9. 4-amino-2,6-dinitrotoluene 10. 2,6-dinitrotoluene 11. 2,4-dinitrotoluene 12. 2-nitrotoluene 13. 4-nitrotoluene 14. 3-nitrotoluene Sample: Inj.: Conc.: Solvent: 3L* 500g/mL each component acetonitrile Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pinnacle II C18 9214575 250 x 4.6mm 5m 110 water:methanol (50:50, v/v) 1.5 mL/min. 27C UV @ 254nm

Explosives by EPA Method 8330 on Pinnacle II Cyano


Peak List: 1. nitrobenzene 2. 2-nitrotoluene 3. 4-nitrotoluene 4. 3-nitrotoluene 5. 1,3-dinitrobenzene 6. 1,3,5-trinitrobenzene 7. 2,6 dinitrotoluene 8. 2,4-dinitrotoluene 9. 2,4,6-trinitrotoluene 10. 4-amino-2,6-dinitrotoluene 11. 2-amino-4,6-dinitrotoluene 12. RDX 13. tetryl 14. HMX Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 3L 500g/mL each acetonitrile Pinnacle II Cyano 9216575 250 x 4.6mm 5m 110 water:methanol (50:50, v/v) 1.5mL/min. 27C UV @ 254nm

H P LC A P P L I C AT I O N S

*Equal amounts of 8330 Calibration Mix #1 (cat.# 31450) 8330 Calibration Mix #2 (cat.# 31451)

LC_0189

LC_0188

Explosives by EPA Method 8330 on Ultra C18


5

7 13

3 6 1 2

11

Peak List: 1. HMX 2. RDX 3. 1,2-dinitrobenzene (SS) 4. 1,3,5-trinitrobenzene 5. 1,3-dinitrobenzene 6. tetryl 7. nitrobenzene 8. 3,4-dinitrobenzene (IS) 9. 2,4,6-trinitrotoluene 10. 4-amino-2,6-dinitrotoluene 11. 2-amino-4,6-dinitrotoluene 12. 2,6-dinitrotoluene 13. 2,4-dinitrotoluene 14. 2-nitrotoluene 15. 4-nitrotoluene 16. 3-nitrotoluene Sample: Inj.: 5L Conc.: 30g/mL (30ppm) each Sample diluent: acetonitrile Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Ultra C18 9174575 250 x 4.6mm 5m 100 water:methanol (44:56, v/v) 1.0mL/min. 30C UV @ 254nm

10

12

14 15

16

10
LC_0254

12

14

16

18

min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Environmental
Explosives by EPA Method 8330 on Ultra Cyano
5

475

Peak List: 1. nitrobenzene 2. 2-nitrotoluene 3. 3-nitrotoluene 4. 4-nitrotoluene 5. 1,3,5-trinitrotoluene 6. 1,3-dinitrobenzene 7. 2,6-dinitrotoluene 8. 2,4-dinitrotoluene 9. 2,4,6-trinitrotoluene 10. 4-amino-2,6-dinitrotoluene 11. 2-amino-4,6-dinitrotoluene 12. RDX 13. tetryl 14. HMX

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size:

5L 100g/mL each water:methanol (50:50, v/v) Ultra Cyano 9106575 250 x 4.6mm 5m 100 water:methanol (50:50, v/v) 1.0mL/min. ambient UV @ 254nm

1 8 6 4 4 3 2 2, 3 7 6

Conditions: Mobile phase: Flow: Temp.: Det.:

H P LC A P P L I C AT I O N S

7 9

11

10

13

8
12

10 min.

14

10

20

30
LC_0109

40

50

60 min.

Explosives by EPA Method 8330 on Allure C18


3 4

2 5 6 8

Peak List: 1. HMX 2. RDX 3. 1,3,5-trinitrobenzene 4. 1,3-dinitrobenzene 5. nitrobenzene 6. tetryl 7. 3,4-dinitrotoluene (IS) 8. 2,4,6-trinitrotoluene 9. 4-amino-dinitrotoluene 10. 2-amino-dinitrotoluene 11. 2,6-dinitrotoluene 12. 2,4-dinitrotoluene 13. 2-nitrotoluene 14. 4-nitrotoluene 15. 3-nitrotoluene
12

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

5L 100g/mL each mobile phase Allure C18 9164575 250 x 4.6mm 5m 60 water:methanol (50:50 v/v) 1.0mL/min. ambient UV @ 254nm

10 11 9

13 14

15

10

15

20
LC_0055

25

30

35

40 min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

476

Environmental
Herbicides (Phenoxyacid Mix B) on Ultra Aqueous C18

H P LC A P P L I C AT I O N S

Peak List: 1. 4-nitrophenol 2. MCPA 3. 3,5-dichlorobenzoic acid 4. MCPP 5. 2,4,5-T 6. 2,4-DB 7. 1,4-dichlorobenzene (IS) 8. dinoseb 9. pentachlorophenol

Sample: Inj.: Conc.: Sample diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

10L 10 ppm each herbicide acetonitrile Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100 A: 0.05% H3PO4 B: acetonitrile Time (min.) 0 10 16 22 24 25 1.0mL/min ambient UV @ 225nm %B 10 45 45 90 90 10

Flow: Temp.: Det.:

LC_0314

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Environmental
Herbicides (Phenoxyacid Mix A) on Ultra Aqueous C18

477

Peak List: 1. picloram 2. chloramben 3. dicamba 4. bentazon 5. 2,4-D 6. dichlorprop 7. 2,4,5-TP 8. acifluorfen 9. 1,4-dichlorobenzene (IS)

Sample: Inj.: Conc.: Sample diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

10L 10ppm each herbicide acetonitrile Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100 A:0.05% H3PO4 B:acetonitrile Time (min.) %B 0 20 15 80 20 80 21 20 1.0mL/min. ambient UV @ 225nm

H P LC A P P L I C AT I O N S

Flow: Temp.: Det.:

LC_0313

Herbicides on Ultra Aqueous C18


Peak List: 1. 2,4-D 2. Silvex (2,4,5-TP) 3. 1,4-dichlorobenzene (IS)
1

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

10L 10ppm each 0.05% phosphoric acid : acetonitrile, 50:50 Ultra Aqueous C18 9178355 50 x 4.6mm 3m 100 0.05% phosphoric acid : acetonitrile, 60:40 1.0mL/min. ambient UV @ 225nm

6
LC_0304

10

12

14

min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

478

Environmental
Herbicides (Uron) on Pinnacle II C8

Peak List: 1. fenuron 2. monuron 3. chlorotoluron 4. isoproturon 5. diuron 6. linuron 7. neburon Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 10L uron herbicide mix 35.7g/mL each acetonitrile Pinnacle II C8 9213565 150 x 4.6mm 5m 110 A: water B: acetonitrile Time (min.) 0 8 10 15 1.0mL/min. ambient UV @ 240nm

H P LC A P P L I C AT I O N S

%B 40 40 90 90

Flow: Temp.: Det.:

LC_0190

Herbicides on Allure C18

Peak List: 1. cyanazine 2. methabenzthiazuron 3. chlortoluron 4. secbumeton 5. isoproturon 6. diuron 7. linuron 8. flusilazole 9. ethofumesate 10. neburon 11. pendimethalin

Ret. Time (min.) 12.04 13.88 14.59 15.74 16.18 16.78 22.48 24.29 24.53 25.74 31.46

Sample: Inj.: Conc.: Diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

5L custom mix approx. 20g/mL each acetonitrile Allure C18 9164565 150 x 4.6mm 5m 60 A: water B: acetonitrile Time (min.) 0 10 15 26 34 34.1 %B 20 40 40 80 80 20

Flow: Temp.: Det.:

1.2mL/min. ambient UV @ 220nm

LC_0309

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Environmental
Herbicides (Uron) on Allure C18
Peak List: 1. methomyl 2. carbendazim 3. aldicarb 4. chlortoluron 5. isoproturon 6. diuron 7. monolinuron 8. linuron Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Ret. time (min.) 3.80 4.93 6.53 8.65 9.45 9.90 10.43 15.36 5L 500g/mL each N,N-dimethylacetamide:acetonitrile (28:72 v/v) Allure C18 9164565 150 x 4.6mm 5m 60 A: 20mM potassium phosphate, pH 7.0 B: acetonitrile Time (min.) 0.0 3.0 12.0 13.0 14.0 24.0 Flow: Temp.: Det.: %B 20 45 45 80 20 20

479

H P LC A P P L I C AT I O N S

1.0mL/min. 25C UV @ 220nm and 254nm


254nm 220nm

LC_0305

Pesticide (Diflubenzuron) on Ultra IBD


1

Peak List: 1. diflubenzuron 2. N,N'-bis-(chlorobenzyl)urea Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Solvent A: Flow rate: Temp.: Det.: 10L 1mg/mL water:acetonitrile (1:1, v/v) Ultra IBD 9175365 150 x 4.6mm 3m 100 water:acetonitrile (45:55, v/v) 65% 0.1M ammonium acetate pH 6.0 1.0mL/min. ambient UV @ 260nm

free literature
Environmental HPLC: Applications-Columns-Reference Materials (lit. cat.# 59741) Save time, improve separations, using these columns and conditions.
Restek HPLC columns support environmental HPLC applications with rapid analysis times and effective analyte resolution. Sample turn-around can be 50% faster, or more, than with alternative columns. In addition, we prepare analytical reference materials and solid phase extraction products for these methods. Applications described in this 8-page publication include polyaromatic hydrocarbons, carbamates, phenoxyacid herbicides, explosives, and carbonyls. Request from your Restek representative, or visit our website.

8
LC_0081

10

12

14 min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

480

Environmental
Pesticides (Carbamates) on Ultra Carbamate
Compound 1. aldicarb sulfone 2. aldicarb sulfoxide 3. oxamyl 4. methomyl 5. 3-hydroxycarbofuran Ion 223.3 207.3 237.2* 163.2 238.3 Cone V 25V 18V 10V 15V 15V Compound 6. aldicarb 7. propoxur 8. carbofuran 9. carbaryl 10. methiocarb Ion 191.2 210.2 222.3 202.2 226.3 Cone V 8V 18V 22V 18V 19V Sample: Inj.: Conc.: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 10L 100g/mL each component Ultra Carbamate 9177315 100 x 4.6mm 3m 100 A: 90% water: 10% methanol with 10mM ammonium formate B: 90% acetonitrile: 10% methanol with 10 mM ammonium formate Time (min.) %B 0.0 10% 15 90% 20 90% Flow:
methiocarb aldicarb sulfone carbofuran propoxur aldicarb sulfoxide carbaryl aldicarb methomyl UV @220nm

*Ammonium adduct (all other are [M+H]+ ions)

H P LC A P P L I C AT I O N S

3-hydroxycarbofuran oxamyl

Temp.: Det.: MSD Conditions: Detector: Mode: Capillary V: Extractor: Ion energy: Multiplier: Source temp: Desolv. temp: Gas flow:

1.0mL/min. (approx. 0.75mL/min. to UV detector, 0.25mL/min. to MSD) ambient UV @ 220nm; MSD Micromass ZMD ESI+ 3.50 4.0 0.4 650 100C 250C 490 L/hr.

LC_0308

Pesticides (Carbamates) on Ultra Carbamate (Fast LC)


Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

Peak List: 1. aldicarb 2. aldicarb sulfoxide 3. oxamyl 4. methomyl 5. 3-hydroxycarbofuran 6. aldicarb 7. propoxur 8. carbofuran 9. carbaryl 10. methiocarb 11. 4-bromo-3,5-dimethylcarbamate

5L cat. # 32274 and cat. # 32273 mixed 50:50 50g/mL each methanol Ultra Carbamate 9177355 50 x 4.6mm 3m 100 A: 90:10 water:methanol B: 90:10 methanol: acetonitrile Time (min.) 0 10 %B 10 90

Flow: Temp.: Det.:

1.5mL/min. 27C UV @ 220nm

LC_0225

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Environmental
Pesticides on Allure C18
Peak List: 1. desisopropyl atrazine 2. desethyl atrazine 3. simazine 4. terbuthylazine desethyl 5. cyanazine 6. methabenzthiazuron 7. chlortoluron 8. atrazine 9. secbumeton 10. isoproturon 11. diuron 12. terbumeton 13. terbuthylazine 14. linuron 15. flusilazole 16. ethofumerate 17. neburon Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase

481

5L approx. 10ppm each pesticide acetonitrile Allure C18 9164565 150 x 4.6mm 5m 60 A: 20mM K2HPO4, pH 7.0 B: acetonitrile

H P LC A P P L I C AT I O N S

Time (min.) 0 10 15 30 30.1 Flow: Temp.: Det.:

%B 20 40 40 70 20

1.2mL/min. ambient UV @ 220nm

LC_0310

Pesticides on Allure PFP Propyl


Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase 5L approx. 10ppm each pesticide acetonitrile Allure PFP Propyl 9169355 50 x 4.6mm 3m 60 A: 20mM K2HPO4, pH 7.0 B: acetonitrile Time (min.) 0 10 12 18 26 26.1 Flow: Temp.: Det.: %B 20 30 30 50 50 20

Peak List: 1. desisopropyl atrazine 2. desethyl atrazine 3. simazine 4. terbuthylazine desethyl 5. cyanazine 6. atrazine 7. methabenzthiazuron 8. secbumeton 9. chlortoluron 10. isoproturon 11. terbumeton 12. diuron 13. terbuthylazine 14. linuron 15. ethofumerate 16. flusilazole 17. neburon

1.0 mL/min. ambient UV @ 220nm

LC_0312

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482

Environmental
Phenols on Pinnacle DB C18
1

Phenols on Pinnacle II C18

Peak List: 1. phenol 2. 2,6-dinitrophenol 3. 3,5-dinitrophenol Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Conc. 0.6mg/mL 1.4mg/mL 1.5mg/mL

Peak List: 1. phenol 2. 2,6-dinitrophenol 3. 3,5-dinitrophenol Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

conc. (mg/mL) 0.6 1.4 1.5

5L methanol Pinnacle DB C18 9414565 150mm x 4.6mm 5m 140 0.7% acetic acid:methanol (60:40 v/v) 1.0mL/min. ambient 2 UV @ 254nm

5L methanol Pinnacle II C18 9214565 150 x 4.6mm 5m 110 0.7%acetic acid:methanol (60:40 v/v) 1.0mL/min. ambient UV @ 254nm

H P LC A P P L I C AT I O N S

10
LC_0272

12

14

16

min.
LC_0274

Paraquat and Diquat on Ultra Quat Column


1

Peak List: 1. diquat 2. paraquat

Peak time (min.) 7.5 8.8

min.

diquat 308nm
100g/mL

Column: Cat. #: Dimensions: Particle size: Conditions: Mobile phase: Flow: Temp.: Det.: Sample: Inj.: Conc.:
40g/mL

Ultra Quat 9181565 150 x 4.6mm 5m


100g/mL

paraquat 257nm

Ultra Quat Reagent Solution (cat.# 32441): acetonitrile, 95:5 (v/v) 1.0 mL/min. 27C UV @ 257nm (paraquat) UV @ 308nm (diquat)

20L 20ppm each component (above); 20g/mL, 40g/mL, and 100g/mL each component at 308nm (left) and at 257nm (right) Sample diluent: water

40g/mL

20g/mL

20g/mL LC_0321

min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Environmental
Phthalate Esters on Pinnacle II Phenyl (Isocratic Elution)
Peak List: 1. dimethyl phthalate 2. diethyl phthalate 3. di-n-butyl phthalate 4. butyl benzyl phthalate 5. bis(2-ethylhexyl)phthalate 6. di-n-octyl phthalate

483

Phthalate Esters on Pinnacle II Phenyl (Gradient Elution)


Conditions: Mobile phase: A: water B: acetonitrile Time (min.) %B 0 60 5 60 10 80 15 80 1.0mL/min. ambient UV @ 254nm

Sample: Inj.: Conc.:


4 3

5L Method 606-phthalate esters calibration mix (cat.# 31031) 2,000g/mL each in methanol Pinnacle II Phenyl 9199565 150 x 4.6mm 5m 110 water:acetonitrile (30:70 v/v) 1.0mL/min. ambient UV @ 254 nm
5 6

Flow: Temp.: Det.:


2

Column and sample information same as for isocratic elution (LC_0178).

H P LC A P P L I C AT I O N S

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

34

5 6

4
LC_0178

10 min.

10

15 min.

LC_0180

Phthalate Esters on Pinnacle II C8 (Isocratic Elution)


Peak List: 1. dimethyl phthalate 2. diethyl phthalate 3. butyl benzyl phthalate 4. di-n-butyl phthalate 5. bis(2-ethylhexyl)phthalate 6. di-n-octyl phthalate
2

Searching for a chromatogram?

Sample: Inj.:
1

Conc.:

5L Method 606-phthalate esters calibration mix (cat.# 31031) 2,000g/mL each in methanol Pinnacle II C8 9213565 150 x 4.6mm 5m 110 water:acetonitrile (20:80 v/v) 1.0mL/min. ambient UV @ 254nm

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3 4

Column: Cat #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

2.5

7.5

10

12.5
LC_0179

15

17.5

20

22.5 min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

484

Environmental
Polynuclear Aromatic Hydrocarbons on Pinnacle II PAH
Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
10

5L 1:9 methylene chloride:acetonitrile Pinnacle IIPAH 9219563 150 x 3.2mm 5m 110


4 6

H P LC A P P L I C AT I O N S

Flow: Temp.: Det.:

A: purified water, B: acetonitrile Time (min.) %B 0 40 7 60 11 100 17.9 100 18 40 1.2 mL/min. ambient UV @ 254nm

5 11 9

Peak List: 1. naphthalene 2. acenaphthylene 3. acenaphthene 4. fluorene 5. phenanthrene 6. anthracene 7. fluoranthene 8. pyrene 9. benzo(a)anthracene 10. chrysene 11. benzo(b)fluoranthene 12. benzo(k)fluoranthene 13. benzo(a)pyrene 14. dibenzo(a,h)anthracene 15. benzo(ghi)perylene 16. indeno(1,2,3-cd)pyrene

Conc. (g/mL) g 100 100 100 100 50 100 50 50 50 50 50 50 50 50 50 50

13

12 7 8 1 15 2 3 14 16

10
LC_0303

12

14

16

18

min.

Reproducibility for Column Lots: EPA Method 610 PAHs on Pinnacle II PAH
Peak List: 1. naphthalene 2. acenaphthylene 3. acenaphthene 4. fluorene 5. phenanthrene 6. anthracene 7. fluoranthene 8. pyrene 9. benzo(a)anthracene 10. chrysene 11. benzo(b)fluoranthene 12. benzo(k)fluoranthene 13. benzo(a)pyrene 14. dibenzo(a,h)anthracene 15. benzo(ghi)perylene 16. indeno(1,2,3-cd)pyrene Sample: Inj.: Sample diluent: Column: Catalog #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Ret. Time (min.) Lot 1 Lot 2 Lot 3 11.95 12.17 11.80 13.41 13.65 13.26 15.61 15.89 15.45 16.09 16.31 15.92 17.41 17.61 17.23 18.80 18.92 18.61 20.23 20.39 20.03 21.31 21.46 21.11 24.88 24.87 24.65 25.64 25.54 25.40 28.62 28.53 28.35 29.97 29.74 29.70 31.26 31.02 30.97 33.09 32.74 32.81 34.46 34.24 34.16 35.19 34.85 34.91 Conc. (g/mL) g 100 100 100 100 50 100 50 50 50 50 50 50 50 50 50 50

610 PAH Calibration Mix A (cat.# 31264), 5L methylene chloride:acetonitrile (1:9, v/v) 9219563 150 x 3.2mm 5m 110 A: water; B: acetonitrile Time (min.) %B 0 40 30 100 40 100 41 40 51 40 0.5mL/min 30C (or ambient) UV @ 254nm
LC_0243

Flow: Temp.: Det.:

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Environmental
Polynuclear Aromatic Hydrocarbons on Pinnacle II PAH EPA 8310-18 Component Standard
Peak List: 1. naphthalene 2. acenaphthylene 3. 1-methylnaphthalene 4. 2-methylnaphthalene 5. acenaphthene 6. fluorene 7. phenanthrene 8. anthracene 9. fluoranthene 10. pyrene 11. benzo(a)anthracene 12. chrysene 13. benzo(b)fluoranthene 14. benzo(k)fluoranthene 15. benzo(a)pyrene 16. dibenzo(a,h)anthracene 17. benzo(ghi)perylene 18. indeno(1,2,3-cd)pyrene Conc. (g/mL or ppm) 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 5 Sample: Inj.: Conc.: Sample diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 5L cat.# 31841 see peak list acetonitrile Pinnacle II PAH 9219563 150 x 3.2mm 5m 110 A: purified water B: acetonitrile Time (min.) %B 0 40 7 60 11 100 17.9 100 18 40 1.2mL/min. ambient UV @ 254nm

485

H P LC A P P L I C AT I O N S

Flow: Temp.: Det.:

LC_0317

Polynuclear Aromatic Hydrocarbons on Pinnacle II PAH EPA 8310 - 20 Component Standard


Peak List: 1. naphthalene 2. acenaphthylene 3. 1-methylnaphthalene 4. 2-methylnaphthalene 5. acenaphthene 6. fluorene 7. phenanthrene 8. anthracene 9. o-terphenyl 10. fluoranthene 11. pyrene 12. p-terphenyl 13. benzo(a)anthracene 14. chrysene 15. benzo(b)fluoranthene 16. benzo(k)fluoranthene 17. benzo(a)pyrene 18. dibenzo(a,h)anthracene 19. benzo(ghi)perylene 20. indeno(1,2,3-cd)pyrene Conc. (g/mL or ppm) 100 100 100 100 100 100 50 100 100 50 50 50 50 50 50 50 50 50 50 50

Great resolution in less than 18 minutes!

Sample: Inj.: Conc.: Sample diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

5L see peak list acetonitrile Pinnacle II PAH 9219563 150 x 3.2mm 5m 110 A: purified water B: acetonitrile Time (min.) %B 0 40 7 60 11 100 17.9 100 18 40 1.2mL/min. ambient UV @ 254nm

Flow: Temp.: Det.:

LC_0318

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486

Environmental
Polynuclear Aromatic Hydrocarbons on Pinnacle II PAH (Fast LC)
Sample: Inj.: Conc.: Sample diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Peak List: 1. naphthalene 2. acenaphthylene 3. acenaphthene 4. fluorene 5. phenanthrene 6. anthracene 7. fluoranthene 8. pyrene 9. benzo(a)anthracene 10. chrysene 11. benzo(b)fluoranthene 12. benzo(k)fluoranthene 13. benzo(a)pyrene 14. dibenzo(a,h)anthracene 15. benzo(ghi)perylene 16. indeno(1,2,3-cd)pyrene

5L 5-10 ppm each methylene chloride:acetonitrile (1:9 v/v) Pinnacle II PAH 9219555 50 x 4.6mm 5m 110 A: water B: acetonitrile Time (min.) 0 1.5 4.0 5.5 5.6 3.0mL/min. ambient UV @ 254nm

H P LC A P P L I C AT I O N S

Conditions: Mobile phase:

%B 50 60 100 100 50

Flow: Temp.: Det.:

LC_0315

Polynuclear Aromatic Hydrocarbons on Pinnacle II PAH (Fast LC)


Sample: Inj.: Conc.: Sample diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 5L 5-10ppm each methylene chloride:acetonitrile (1:9 v/v) Pinnacle II PAH 9219555 50 x 4.6mm 5m 110 A: water B: acetonitrile Time (min.) 0 1.5 4.0 5.5 5.6 3.0mL/min. ambient UV @ 254nm

%B 50 60 100 100 50

Peak List: 1. naphthalene 2. acenaphthylene 3. 1-methylnaphthalene 4. 2-methylnaphthalene 5. acenaphthene 6. fluorene 7. phenanthrene 8. anthracene 9. o-terphenyl 10. fluoranthene 11. pyrene 12. p-terphenyl 13. benzo(a)anthracene 14. chrysene 15. benzo(b)fluoranthene 16. benzo(k)fluoranthene 17. benzo(a)pyrene 18. dibenzo(a,h)anthracene 19. benzo(ghi)perylene 20. indeno(1,2,3-cd)pyrene

Flow: Temp.: Det.:

LC_0316

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Environmental
Polynuclear Aromatic Hydrocarbons on Allure C18
Peak List: 1. naphthalene 2. acenaphthylene 3. acenaphthene 4. fluorene 5. phenanthrene 6. anthracene 7. fluoranthene 8. pyrene 9. benzo(a)anthracene 10. chrysene 11. benzo(b)fluoranthene 12. benzo(k)fluoranthene 13. benzo(a)pyrene 14. dibenzo(a,h)anthracene 15. indeno(1,2,3-c,d)pyrene 16. benzo(ghi)perylene Ret. time (min.) 15.06 16.53 19.12 19.12 20.19 21.05 22.58 23.56 25.81 25.81 28.31 28.72 29.62 30.45 32.07 32.33 Conc. (g/mL) g 500 1000 500 100 50 50 100 50 50 50 100 50 50 100 50 100 Sample: Inj.: Sample diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 5L 610 PAH Calibration Mix B (cat.#31455), diluted 1:1 with acetonitrile methylene chloride:methanol:acetonitrile (25:25:50 v/v/v) Allure C18 9164565 150 x 4.6mm 5m 60 A: water B: acetonitrile Time (min.) %B 0.0 40 30 100 40 100 41 40 51 40 1.0mL/min. 30C (or ambient) UV @ 254nm

487

H P LC A P P L I C AT I O N S

Flow: Temp.: Det.:

LC_0295

Polynuclear Aromatic Hydrocarbons on Pinnacle II C18

Polynuclear Aromatic Hydrocarbons on Hypersil ODS

Peak List: 1. naphthalene 2. fluorene 3. phenanthrene 4. anthracene 5. pyrene 6. chrysene Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L 100g/mL each acetonitrile Pinnacle II C18 9214565 150 x 4.6mm 5m 110 water:acetonitrile (25:75 v/v) 1.0mL/min. ambient UV @ 254nm

Peak List: 1. naphthalene 2. fluorene 3. phenanthrene 4. anthracene 5. pyrene 6. chrysene Sample: Inj.: Conc.: Sample diluent: Column: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L 100g/mL each acetonitrile Hypersil ODS 150 x 4.6mm 5m 120 water:acetonitrile (25:75 v/v) 1.0mL/min. ambient UV @ 254nm

Compare to the performance on a Hypersil ODS column.

LC_0270

LC_0269

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488

Environmental / General (Test Mixes)


Polynuclear Aromatic Hydrocarbons on Pinnacle DB C18
3 4

Neutral/Base Mix on Pinnacle DB C18


Peak List: 1. uracil 2. aniline 3. 2-nitroaniline 4. 2,4-nitroaniline 5. 3,5-xylenol 6. anisole 7. toluene Conc. 0.05mg/mL 0.75mg/mL 0.35mg/mL 0.35mg/mL 2.5mg/mL 2.5mg/mL 3.5mg/mL

Peak List: 1. naphthalene 2. fluorene 3. phenanthrene 4. anthracene 5. pyrene 6. chrysene Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

H P LC A P P L I C AT I O N S

5L 100g/mL each acetonitrile Pinnacle DB C18 9414565 150 x 4.6mm 5m 140 water:acetonitrile 2 (25:75 v/v) 1.0mL/min ambient UV @ 254nm
6

Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

2L methanol:water (50:50 v/v) Pinnacle DB C18 9414565 150 x 4.6mm 5m 140 50mM KH2PO4, pH 3.5:methanol (35:65 v/v) 1.0mL/min. ambient UV @ 254nm

5 1

6
LC_0268

10

min.
LC_0264

Acids and Bases on Ultra IBD (pH 3)


Peak List: 1. uracil 2. unknown 3. maleate 4. benzoic acid 5. nortriptyline 6. amitriptyline 7. trimipramine Conc. (g/mL) g 5 5 50 50 50 50 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.:
1 4

Acid/Base Mix on Ultra IBD (pH 7)


10L mobile phase Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM KH2PO4 pH 3: acetonitrile (70:30, v/v) 1.0mL/min. 30C UV @ 254nm

Peak List: Conc. (g/mL) g 1. uracil 5 2. benzoic acid 50 3. maleate 5 4. trimipramine 50 5. nortriptyline 50 6. amitriptyline 50 Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
2

Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM KxHyPO4, pH 7: acetonitrile (65:35, v/v) 1.0mL/min. 30C UV @ 254nm

6 5 7

Flow: Temp.: Det.:

6 1 4 5 3

4
LC_0057

8 min.

10

15
LC_0056

20

25 min.

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General (Test Mixes)


Neutral/Base Mix on Pinnacle II C18
Peak List: 1. uracil 2. aniline 3. 2-nitroaniline 4. 2,4-dinitroaniline 5. 3,5-xylenol 6. anisole 7. toluene Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Ret. time (min.) 1.642 2.100 2.758 3.109 3.972 4.577 7.853 conc. 0.05mg/mL 0.75mg/mL 0.35mg/mL 0.35mg/mL 2.5mg/mL 2.5mg/mL 3.5mg/mL

489

Acid/Base Mix on Pinnacle II C18

Peak List: Ret. time (min.) 1. caffeine 2.733 2. acetylsalicylic acid 4.588 3. benzoic acid 7.738

Conc. 0.5mg/mL 3.5mg/mL 2.8mg/mL

Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

2L methanol:water (50:50 v/v) Pinnacle II C18 9214565 150 x 4.6mm 5m 110 50mM KH2PO4 pH 3.5: methanol (35:65 v/v) 1.0mL/min. ambient UV @ 254nm

2L methanol:water (50:50 v/v) Pinnacle II C18 9214565 150 x 4.6mm 5m 110 50 mM KH2PO4 pH 3.5:methanol (40:60 v/v) 1.0 mL/min. ambient UV @ 254nm

H P LC A P P L I C AT I O N S

LC_0266

LC_0262

Acid/Base Mix on Pinnacle DB C18

Peak List: Ret. Time (min.) 1. caffeine 2.525 2. acetylsalicylic acid 4.088 3. benzoic acid 6.733 Sample: Inj.: Solvent: Column: Cat #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Conc. 0.5mg/mL 3.5mg/mL 2.8mg/mL

2L methanol:water (50:50 v/v) Pinnacle DB C18 9414565 150 x 4.6mm 5m 140 5 mM KH2PO4, pH 3.5:methanol (40:60 v/v) 1.0mL/min. ambient UV @ 254nm

LC_0260
0 1 2 3 4 5 6 7 min.

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490

General (Test Mixes)


Column Performance Test Mix (NIST SRM870) on Pinnacle II C18
Peak List: 1. uracil 2. toluene 3. ethylbenzene 4. quinizarin 5. amitriptyline Sample: Inj.: Solvent: Conc. (g/mL) g 28 1400 1700 94 2800

Pyridine on Ultra Aqueous C18

Peak List: 1. pyridine Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Ret. Time (min.) 9.717 5L mobile phase Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100

Conc. (L/mL) L 0.1

HPLC Performance Test Mix (cat.# 31699) 5.0L methanol Pinnacle II C18 9214565 150 x 4.6mm 5m 110 5mM potassium phosphate, pH 7.0: methanol (20:80 v/v) 2.0mL/min. 23C UV @ 254nm

H P LC A P P L I C AT I O N S

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

20mM potassium phosphate, pH 7.0: acetonitrile (80:20 v/v) 1.0mL/min. ambient UV @ 254nm

2 1

4
LC_0242

min.
LC_0230

Pyridine/Phenol Test Mix on Ultra C18

Pyridine/Phenol Test Mix on Pinnacle II C18


Peak List: 1. uracil 2. pyridine 3. phenol Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Conc. 5.0g/mL 0.1L/mL 1.86mg/mL

Peak List: 1. uracil 2. pyridine 3. phenol Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Conc. 5.0g/mL 0.1L/mL 1.86mg/mL 5.0L mobile phase Ultra C18 9174565 150 x 4.6mm 5m 100 20mM potassium phosphate, pH 7.0: acetonitrile (80:20 v/v) 1.0mL/min. ambient UV @ 254nm

5.0L mobile phase Pinnacle II C18 9214565 150 x 4.6mm 5m 110 20mM potassium phosphate, pH 7.0: acetonitrile (80:20 v/v) 1.0mL/min. ambient UV @ 254nm

LC_0245

LC_0247

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General (Test Mixes)


Pyridine/Phenol Test Mix on Pinnacle DB C18
Peak List: 1. uracil 2. pyridine 3. phenol Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Ret. Time (min.) 1.643 3.119 6.969 Conc. 5.0g/mL 0.1L/mL 1.86mg/mL Peak List: 1. uracil 2 pyridine 3. phenol Ret. Time (min.) 1.812 4.528 8.576 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Conc. 50g/mL 0.1L/mL 1.86mg/mL

491

Pyridine/Phenol Test Mix on Ultra IBD

5.0L mobile phase Pinnacle DB C18 9414565 150 x 4.6mm 5m 140 20mM potassium phosphate, pH 7.0: acetonitrile (80:20 v/v) 1.0mL/min. ambient UV @ 254nm

5L mobile phase Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM potassium phosphate, pH 7.0: acetonitrile (80:20 v/v) 1.0mL/min. ambient UV @ 254nm

H P LC A P P L I C AT I O N S

LC_0248

LC_0232

Reversed Phase Test Mix on Pinnacle DB C18


Peak List: 1. uracil 2. benzene 3. naphthalene 4. biphenyl Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Run Time: Flow: Temp.: Det.: Conc. 0.02mg/mL 3.0mg/mL 0.5mg/mL 0.06mg/mL 5L reversed phase test mix water:methanol (25:75 v/v) Pinnacle DB C18 9414565 150 x 4.6mm 5m 140 water:methanol (20:80 v/v) 8 min. 1.0mL/min. ambient UV @ 254nm

free literature
For more information about Pinnacle DB columns, request applications note #59742.

LC_0249

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492

General (Test Mixes)


Reversed Phase Test Mix on Ultra Aqueous C18
Peak List: Conc. (mg/mL) 1. uracil 0.02 2 benzene 3.00 3. naphthalene 0.50 4. biphenyl 0.06 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 1.3L methanol:water (75:25, v/v) Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100 water:methanol (20:80 v/v) 1.0mL/min. ambient UV @ 254nm

Reversed Phase Test Mix on Ultra IBD


Peak List: Conc. (mg/mL) 1. uracil 0.02 2 benzene 3.00 3. naphthalene 0.50 4. biphenyl 0.06 Sample: Inj.: Solvent: Column: Cat #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 1.3L methanol:water (75:25, v/v) Ultra IBD 9175565 150 x 4.6mm 5m 100 water:methanol (20:80 v/v) 1.0mL/min. ambient UV @ 254nm

H P LC A P P L I C AT I O N S

LC_0233

LC_0234

Reversed Phase Test Mix on Pinnacle II C18 (3m)

Reversed Phase Test Mix on Pinnacle DB C18


Peak List: 1. uracil 2. benzene 3. naphthalene 4. biphenyl Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Conc. 0.02mg/mL 3mg/mL 0.5mg/mL 0.06mg/mL

Peak List: conc.: (mg/mL) 1. uracil 0.02 2. benzene 3.0 3. napthalene 0.5 4. biphenyl 0.06 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L methanol:water (75:25, v/v) Pinnacle II C18 9214365 150 x 4.6mm 3m 110 water:methanol (20:80) 1.0mL/min. ambient UV @ 254nm
2 4

5L methanol Pinnacle DB C18 9414565 150 x 4.6mm 5m 140 water:methanol (20:80 v/v) 1.0mL/min. ambient UV @ 254nm

4 2

1
1

4
LC_0201

7 min.

min

LC_0280

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General (Test Mixes)


Reversed Phase Test Mix on Pinnacle II C18
Peak List: Conc. (mg/mL) 1. uracil 0.02 2. benzene 3.00 3. naphthalene 0.50 4. biphenyl 0.06 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L water:methanl (25:75, v/v) Pinnacle II C18 9214565 150 x 4.6mm 5m 110 water:methanol (20:80 v/v) 1.0mL/min. ambient UV @ 254nm

493

Searching for a chromatogram?

www.restek.com

H P LC A P P L I C AT I O N S

LC_0162

Pyridine, N,N-Dimethylaniline, Benzophenone on Pinnacle II C18


Peak List: 1. uracil 2. pyridine 3. n,n-dimethylaniline 4. benzophenone Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Conc. 1g/mL 0.64mg/mL 0.45mg/mL 0.59mg.mL 5L water:methanol (50:50 v/v) Pinnacle II C18 9214565 150 x 4.6mm 5m 110 water: methanol (40:60 v/v) 1.0 mL/min. ambient UV @ 254nm

SRM 870 Mix on Pinnacle II C18


Peak List: 1. uracil 2. toluene 3. ethylbenzene 4. quinizarin 5. amitriptyline Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Conc. 28g/mL 1.4mg/mL 1.7mg/mL 94g/mL 2.8mg/mL 5L methanol Pinnacle II C18 9214565 150 x 4.6mm 5m 110 5mM potassium phosphate pH 7:methanol (20:80 v/v) 2.0mL/min. ambient UV @ 254nm

LC_0278

LC_0286

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494

General (Test Mixes)


SRM 870 Mix on Pinnacle DB C18
Peak List: 1. uracil 2. toluene 3. ethylbenzene 4. amitriptyline 5. quinizarin Sample: Inj.: Solvent: Column: Pinnacle DB C18 Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Conc. 28g/mL 1.4mg/mL 1.7mg/mL 2.8mg/mL 94g/mL

SRM 870 mix on BDS Hypersil BDS C18


Peak List: 1. uracil 2. toluene 3. ethylbenzene 4. quinizarin 5. amitriptyline Conc. 28 g/mL 1.4 mg/mL 1.7 mg/mL 94 g/mL 2.8mg/mL

5L methanol

Same performance as Hypersil BDS

Sample: Inj.: 5L Sample diluent: methanol Column: Hypersil BDS C18 Dimensions: 150 x 4.6mm Particle size: 5m Pore size: 130 Conditions: Mobile phase: 5 mM potassium phosphate pH 7:methanol (20:80 v/v) 2.0 mL/min. ambient UV @ 254nm

H P LC A P P L I C AT I O N S

9414565 150 x 4.6mm 5m 140 5 mM potassium phosphate pH 7: methanol (20:80 v/v) 2.0 mL/min. ambient UV @ 254nm

Flow: Temp.: Det.:

Flow: Temp.: Det.:

480nm 254nm 210nm

480nm 254nm 210nm

LC_0284

LC_0283

Pyridine/Phenol on Ultra IBD (pH7)


Peak List: 1. uracil 2. pyridine 3. phenol Conc. (g/mL) g 5 50 300 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size:
2

10L mobile phase Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM KxHy PO4 pH 7:acetonitrile (80:20, v/v) 1.2mL/min. 30C UV @ 254nm

Searching for a chromatogram?

Conditions: Mobile phase: Flow rate: Temp.: Det.:

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1

4
LC_0058

8 min.

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General (Test Mixes)


Uracil, Pyridine, N,N-Dimethylaniline, Benzophenone Test Mix on Pinnacle DB C18
4

495

Peak List: 1. uracil 2. pyridine 3. N,N-dimethylaniline 4. benzophenone Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Conc. 1g/mL 0.64mg/mL 0.45mg/mL 0.59mg/mL

H P LC A P P L I C AT I O N S

5L water:methanol (50:50 v/v) Pinnacle DB C18 9414565 150 x 4.6mm 5m 140 water:methanol (40:60 v/v) 1.0mL/min. ambient UV @ 254nm
1

0
LC_0276

10

min.

Normal Phase Test Mix #1 on Pinnacle II 5m Silica


Peak List: Conc. (mg/mL) 1. benzene 1.0 2 benzaldehyde 0.04 3. benzyl alcohol 3.0 4. 4-methoxybenzylalcohol 2.0 Sample: Inj.: Solvent: 5L hexane Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pinnacle II Silica 9210565 150 x 4.6mm 5m 110 hexane:isopropanol (96:4, v/v) 1.0mL/min. ambient UV @ 254nm

Normal Phase Test Mix on Pinnacle II 3m Silica


Peak List: 1. benzene 2. benzaldehyde 3. benzyl alcohol 4. 4-methoxybenzyl alcohol Sample: Inj.: Conc.: Solvent: Column: Catalog #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L see peak list hexane Pinnacle II Silica 9210365 150 x 4.6mm 3m 110 hexane:isopropyl alcohol (96:4) 1.0mL/min. ambient UV @ 254nm
2 4

conc.: (mg/mL) 1.0 0.04 3.0 2.0

0
LC_0163

3
LC_0200

6 min.

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496

General (Test Mixes)


Normal Phase Test Mix on Pinnacle II Cyano
Peak List: 1. benzene 2 benzaldehyde 3. benzyl alcohol 4. 4-methoxybenzyl alcohol Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pressure: 5L hexane Pinnacle II Cyano 9216565 150 x 4.6mm 5m 110 hexane:isopropyl alcohol (96:4, v/v) 1.0mL/min. 1 ambient UV @ 254nm 28 bar Conc. (mg/mL) 1.0 0.04 3.0 2.0
3

Test Mix on Pinnacle II Phenyl


Peak List: 1. uracil 2 benzene 3. naphthalene 4. biphenyl Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pressure: Conc. (mg/mL) 0.02 3.0 0.5 0.06 1.3L methanol:water (75:25, v/v) Pinnacle II Phenyl 9215565 150 x 4.6mm 5m 110 : methanol:water (65:35, v/v) 1.0mL/min. ambient UV @ 254nm 130 bar

4 2

H P LC A P P L I C AT I O N S

min.

LC_0184

LC_0187

Reversed Phase Test Mix on Pinnacle II C8


Peak List: 1. uracil 2 benzene 3. naphthalene 4. biphenyl Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pressure: Conc. (mg/mL) 0.02 3.0 0.5 0.06 1.3L methanol:water (75:25 v/v) Pinnacle II C8 9213565 150 x 4.6mm 5m 110 methanol:water (80:20 v/v) 1.0 mL/min. ambient UV @ 254nm 116 bar
2
3

PCMX in Hand Soap on Pinnacle DB C18

Peak List: 1. PCMX (4-chloro-3,5-dimethylphenol) Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

10L of 5% solution of hand soap methanol Pinnacle DB C18 9414565 150 x 4.6mm 5m 140 water:methanol (35:65 v/v) 1.0mL/min. ambient UV @ 280nm

min. 0 2 4 6 8 min.

LC_0183

LC_0293

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Dietary Supplements / Plant Extracts


Allicin in Garlic Tablets on Pinnacle II C18
Peak List: 1. allicin Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 20L 1.2mg/mL garlic tablet in water deionized water Pinnacle II C18 9214565 150 x 4.6mm 5m 110 water:methanol (50:50 v/v) 0.8 mL/min. 30C UV @ 240nm

497

Cabbage Extract on Ultra Aqueous C18


Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

Peak List: 1. phenethyl glucosinolate

20L water Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100 A: 50mM potassium phosphate, pH 2.5 B: acetonitrile Time (min.) %B 0 0 10 75 11 0 16 0 1.0mL/min. ambient UV @ 210nm

H P LC A P P L I C AT I O N S

Flow: Temp.: Det.:

4
LC_0174

min.
LC_0165

Phenethyl Glucosinolate on Ultra Aqueous C18

Hyperforin in St. Johns Wort on Pinnacle II C18

Peak List: 1. phenethyl glucosinolate Sample: Inj.: Conc.: Solvent: 10L 1000g/mL water

Column: Ultra Aqueous C18 Cat. #: 9178565 Dimensions: 150 x 4.6mm Particle size: 5m Pore size: 100 Conditions: Mobile phase: A: 50mM potassium phosphate, pH 2.5 B: acetonitrile Time (min.): 0.0 10 11 16 1.0mL/min. ambient UV @ 210nm

Peak List: 1. hyperforin 2. adhyperforin Sample: Inj.: Conc.: Solvent: Autosampler: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: St. Johns wort capsule 20L 4.17mg/mL methanol 15C Pinnacle II C18 9214565 150 x 4.6mm 5m 110 0.01N phosphate buffer, pH 2.5: acetonitrile (15:85, v/v) 1.2mL/min. 30C UV @ 270nm

%B 0 75 0 0

Flow: Temp.: Det.:

LC_0166

LC_0175

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498

Dietary Supplements / Plant Extracts


Phenolic Antioxidants on Pinnacle II C18
Peak List: conc. (ppm) 1. propyl gallate 168 2. TBHQ 182 3. 2-BHA + 3-BHA 197 4. BHT 193 Sample: Inj.: Solvent:
1

Phenolics in Echinacea on Pinnacle II C18


Pinnacle II C18 9214565 150 x 4.6mm 5m 110 A = 1% acetic acid B = methanol Time B (min.) (%) 0 50 4 50 10 90 25 90 26 50 1.0mL/min. 30C UV @ 280nm Sample: Inj.: Conc.: Solvent: Sample temp.: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

Echinacea capsule 10L 6.7 mg/mL capsule contents in sample diluent ethanol:water (70:30, v/v) 25C
Pinnacle II C18 9214565 150 x 4.6mm 5m 110 A = 0.1% phosphoric acid B = acetonitrile Time (min.) %B 0 10 13 22 14 40 14.5 40 15 10 20 10 1.5mL/min. 35C UV @ 330nm

Peak List: 1. caftaric acid 2. chlorogenic acid 3. echinacoside 4. cichoric acid

10L methanol

H P LC A P P L I C AT I O N S

Flow: Temp.: 3 Det.:

Flow: Temp.: Det.:


2 4

10
LC_0198

12

14

16

18 min.
LC_0195

Tobacco Extract on Ultra Aqueous C18


1

Peak List: 1. oxalic acid 2. pyruvic acid 3. malic acid 4. citric acid Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Ret. Time (min.) 2.898 3.968 4.070 7.644 20L 0.4N sulfuric acid Ultra Aqueous C18 9178575 250 x 4.6mm 5m 100 50mM potassium phosphate, pH 2.5 1.0mL/min. ambient UV @ 210nm

10

12

14 min.

LC_0172

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Dietary Supplements / Plant Extracts


Tocopherols in Soy Oil on Pinnacle II Silica
Peak List: 1. -tocopherol 2. -tocopherol 3. -tocopherol 4. -tocopherol Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 10L approx. 1.25% soy oil hexane Pinnacle II Silica 9210565 150 x 4.6mm 5m 110 isopropyl alcohol:hexane (0.5:99.5) 0.6 mL/min. 30C UV @ 295nm

499

free literature
H P LC A P P L I C AT I O N S
For more information about dietary supplement analysis, request applications note lit. cat.# 59364, Analyzing Nutraceutical Products by Liquid & Gas Chromatography.

4 1 2

8
LC_0197

10

12

14 min.

Vitamins (Water Soluble) on Ultra Aqueous C18

Peak List: 1. thiamin (B1) 2. ascorbic acid (C) 3. unknown 4. nicotinic acid (B3) 5. unknown 6. pantothenic acid (B5) 7. folic acid (B9) 8. riboflavin (B2) 9. methyl paraben

Conc.: (mg/mL) 250 1000 n/a 1000 n/a 1000 500 250 0.2

Sample: Initial dilutions of B1 and B2 basified with ammonium hydroxide Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile Phase: Ultra Aqueous C18 9178575 250 x 4.6mm 5m 100 A: 25mM potassium phosphate, pH 2.00:methanol (95:5, v/v) B: methanol:25mM potassium phosphate, pH 3.5 (60:40, v/v) Time (min.) 0-6 6.01 11 16 Flow: Temp.: Det.: 1.0mL/min. 27C UV @ 254nm %B 0 25 100 100

7 8 1

5 6

8
LC_0141

10

12

14

min.

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500

Dietary Supplements / Plant Extracts


Vitamins (Fat Soluble) on Ultra C18
Peak List: 1. solvent front 2. menadione (vitamin K3) 3. all-trans-retinol (vitamin A) 4. vitamin D3 5. unknown 6. tocopherol (vitamin E) 7. tocopherol acetate (vitamin E acetate) 8. unknown 9. phylloquinone (vitamin K1) Conc.. (mg/mL) n/a 0.45 0.34 0.4 Sample: n/a Solvent: 2.4 Column: 2.4 Cat. #: n/a Dimensions: 0.84 Particle size: Pore size: Conditions: Mobile phase:

Vitamins Thiamin (Vitamin B1) and Ascorbic Acid (Vitamin C) on Ultra Aqueous C18

diethyl ether Ultra C18 9174575 250 x 4.6mm 5m 100 acetonitrile:methanol (90:10, v/v) Time (min.) Flow (mL/min.) 1.00 1.00 5.00 1.00 5.01 2.00 50.0 2.00 30C UV @ 280nm

Peak List: Conc. (mg/mL) 1. ascorbic acid 2.5 2. thiamin 2.5 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle Size: Pore Size: Conditions: Mobile phase: Flow: Temp.: Det.:

1.0L mobile phase Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100

H P LC A P P L I C AT I O N S

Temp.: Det.:

50mM potassium phosphate, pH 2.5 1.0 mL/min. ambient UV @ 254nm

6 7 9

1 5 8

10

20
LC_0144

30

40

min.
LC_0226

Vitamins Thiamin (Vitamin B1) and Ascorbic Acid (Vitamin C) on Ultra IBD

Watercress Extract on Ultra Aqueous C18


Peak List: 1. phenethyl glucosinolate Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: watercress extract 100L water Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100 A: 50mM potassium phosphate, pH 2.5 B: acetonitrile Time (min.) %B 0.0 0 10 75 11 0 16 0 1.0mL/min. ambient UV @ 210nm

Peak List: Conc. (mg/mL) 1. thiamin 2.5 2. ascorbic acid 2.5

Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

1.0L mobile phase Ultra IBD 9175565 150 x 4.6mm 5m 100 50mM potassium phosphate, pH 2.5 1.0mL/min. ambient UV @ 254nm

Flow: Temp.: Det.:

LC_0227

LC_0167

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Foods & Flavors


Capsaicinoids: Heat Level Standard on Ultra C18
Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Ultra C18 9174565 150 x 4.6mm 5m 100 A: 1% acetic acid in water B: acetonitrile Time (min.) %B 0 50 2 50 9 80 12 80 13 50 1.0mL/min. ambient UV @ 280nm Peak List: 1. capsaicin Sample: Inj.: Conc.: Solvent: 10L 110ppm capsaicin ethanol

501

Black Pepper: Piperine on Pinnacle II Cyano


Peak List: 1. piperine Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L 100g/mL methanol Pinnacle II Cyano 9216565 150 x 4.6mm 5m 110 water:acetonitrile (50:50 v/v) 1.0mL/min. ambient UV/Vis @ 345nm
1

H P LC A P P L I C AT I O N S

Flow: Temp.: Det.:

4
LC_0155

10 min.

4
LC_0181

7 min.

Capsaicinoids: Heat Level Assay for Habeero Nuggets on Ultra C18


Peak List: 1. unknown 2. capsaicin 3. dihydrocapsaicin Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 10L habaero nugget extract 0.8g sample in 200mL ethanol Ultra C18 9174565 150 x 4.6mm 5m 100 A: 1% acetic acid in water B: acetonitrile Time (min.) %B 0 50 2 50 9 80 12 80 13 50 1.0mL/min. ambient UV @ 280nm
3

Capsaicinoids: Heat Level Assay for Habeero Nuggets on Pinnacle II C18


Peak List: 1. unknown 2. capsaicin 3. dihydrocapsaicin Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 10L habaero nugget extract 4000g/mL ethanol Pinnacle II C18 9214565 150 x 4.6mm 5m 110 A: 1% acetic acid in water (v/v) B: acetonitrile Time (min.) %B 0 50 2 50 9 80 12 80 13 50 1.0mL/min. ambient UV @ 280nm

Flow: Temp.: Det.:

Flow: Temp.: Det.:

4
LC_0156

10 min.
LC_0160

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502

Foods & Flavors/Antimicrobial Agents


Sorbic and Benzoic Acids on Ultra Phenyl Sorbic and Benzoic Acids on Pinnacle II Phenyl

Peak List: 1. sorbic acid 2. benzoic acid Sample: Inj.: Conc.: Solvent:

Column: Cat. #: Dimensions: Particle size: Pore size: 10L 100 ppm sorbic acid, 200 ppm benzoic acid mobile phase Ultra Phenyl 9105565 150 x 4.6mm 5m 100 1% acetic acid:methanol (80:20, v/v) 1.2 mL/min. ambient UV @ 245nm Conditions: Mobile phase: Flow: Temp.: Det.:

Pinnacle II Phenyl 9215565 150 x 4.6mm 5m 110 1% acetic acid:methanol (80:20) 1.0 mL/min. 25C UV @ 230nm
1

Peak List: 1. sorbic acid 2. benzoic acid Sample: Inj.: Conc.: Solvent:
2

10L 100ppm each methanol

H P LC A P P L I C AT I O N S

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

10
LC_0150

12

14

16

18 min.

10
LC_0199

12

14

16

18 min.

Parabens on Pinnacle II C8
Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pinnacle II C8 9213565 150 x 4.6mm 5m 110 0.1% acetic acid in water: acetonitrile (50:50, v/v) 1.0mL/min. ambient UV @ 254nm

Parabens on Pinnacle II Phenyl


Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pinnacle II Phenyl 9215565 150 x 4.6mm 5m 110 0.1% acetic acid in water: acetonitrile (50:50, v/v) 1 1.0 mL/min. ambient UV @ 254nm

Peak List: 1. methyl paraben 2. ethyl paraben 3. propyl paraben 4. butyl paraben Sample: Inj.: Solvent:

Conc. (g/mL) g 10 20 30 40

5L methanol:water (50:50 v/v)

0
LC_0176

3
LC_0177

min.

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Foods & Flavors


Carboxylic Acids on Ultra Aqueous C18 Carboxylic Acids in 100% Aqueous Mobile Phase on Ultra Aqueous C18
Peak List: 1. glycolic acid 2. malonic acid 3. acetic acid 4. maleic acid Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conc. (mg/mL) 5.4 4.2 7.8 0.06 10L mobile phase Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100

503

Peak List: 1. malonic acid 2. lactic acid 3. acetic acid 4. citric acid 5. succinic acid 6. fumaric acid Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 10L water

Conc. (g/mL): g 500 500 1000 1000 2000 10


1

5 3

restek innovation!
Excellent peak symmetry even with a 100% aqueous mobile phase!

Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100 50mM potassium phosphate, pH 2.5: acetonitrile (99:1) 1.5mL/min. 25C UV @ 210nm
2

H P LC A P P L I C AT I O N S

Conditions: 1 Mobile phase: 50mM potassium phosphate, pH 2.5 Flow rate: 1.0mL/min. Temp.: 25C Det.: UV @ 210nm

A. initial B. after 3 Days 0 1 2 3 4 min. 0


LC_0140

3
LC_0142

6 min.

Organic Acids (Isocitric and Malic) on Allure Organic Acids

Organic Acids in Cranberry Juice on Allure Organic Acids


Peak List: 1. quinic acid 2. malic acid 3. citric acid Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Peak List: 1. malic acid 2. isocitric acid Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L approx. 0.2 mg/mL malic acid; 0.02 mg/mL isocitric acid water Allure Organic Acids 9165575 250 x 4.6mm 5m 60 100mM KH2PO4, pH 2.5 0.5mL/min. ambient UV @ 226nm

10L cranberry juice:water (50:50, v/v) water Allure Organic Acids 9165585 300 x 4.6mm 5m 60 100mM phosphate buffer, pH 2.5 0.5mL/min. ambient UV @ 226nm

restek innovation!
Excellent peak symmetry even with a 100% aqueous mobile phase!

LC_0311

LC_0236

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504

Foods & Flavors


Organic Acids in Grape Juice on Allure Organic Acids Organic Acids Standard on Allure Organic Acids

restek innovation!
Excellent peak symmetry in 100% aqueous mobile phase!

restek innovation!
Baseline resolution of tartaric and quinic acids in 100% aqueous mobile phases!
Peak List: 1. tartaric acid 2. quinic acid 3. malic acid 4. citric acid 5. fumaric acid Sample: Inj.: Solvent: Conc. (mg/mL) 1 1 1 1 0.005 10L standard solution water Allure Organic Acids 9165585 300 x 4.6mm 5m 60 100mM phosphate buffer, pH 2.5 0.5mL/min. ambient UV @ 226nm

H P LC A P P L I C AT I O N S

Peak List: 1. tartaric acid 2. malic acid Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 10L grape juice:water (50:50, v/v) purified water Allure Organic Acids 9165585 300 x 4.6mm 5m 60 100mM phosphate buffer, pH 2.5 0.5mL/min. ambient UV @ 226nm

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

LC_0237

LC_0238

Carboxylic Acids (Pyruvic and Lactic) on Ultra Aqueous C18


Peak List: 1. pyruvic acid 2. lactic acid Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Conc. (mg/mL) 5 50 5L 50mM potassium phosphate, pH 2.5 Ultra Aqueous C18 9178565 150 x 4.6mm 5m 100 50mM potassium phosphate, pH 2.5 1.0mL/min. 26C UV @ 210nm

Diet Cola on Pinnacle II C18


Peak List: 1. citric acid 2. caffeine 3. aspartame 4. benzoic acid and other components Sample: Inj.: Solvent: Column: Cat.#: Dimensions: Particle size: Pore size: Pinnacle II C18 9214565 150 x 4.6mm 5m 110 A: 10mM potassium phosphate monobasic with 0.1% v/v TEA, pH 2.9 B: acetonitrile Time (min.) %B 0.00 20 4.99 20 5.00 75 9.99 75 10.00 20 1.0mL/min. 27C UV @ 210nm

restek innovation!
Excellent peak symmetry in 100% aqueous mobile phase!

Conditions: Mobile phase: 5.0L raw sample diluted (50:50, v/v) with mobile phase A, filtered, and injected.
2

Flow: Temp.: Det.:

0
LC_0297

6
LC_0153

9 min.

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Foods & Flavors


Sugars on Pinnacle II Amino
Peak List: 1. fructose 2 glucose 3. sucrose 4. maltose 5. lactose Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5.0L 15mg/mL each methanol:water (10:90, v/v) Pinnacle II Amino 9217565 150 x 4.6mm 5m 110 water:acetonitrile (25:75, v/v) 1.0mL/min. 35C refractive index @ 35C

505

Sugars on Pinnacle II Amino (3m)

Peak List: 1. fructose 2. glucose 3. sucrose 4. maltose 5. lactose

Conc. (mg/mL) 2.0 2.1 4.0 4.5 4.4

Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

5L mobile phase Pinnacle II Amino 9217365 150 x 4.6mm 3m 110 water:acetonitrile (25:75, v/v) 1.5 mL/min. 35C refractive index @ 35C

H P LC A P P L I C AT I O N S

1 3

4
LC_0202

10 min.
LC_0223

Sugars: Maple Flavored Syrup on Ultra Amino


Peak List: 1. fructose 2. glucose 3. sucrose Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 20L 10% solution of maple syrup acetonitrile:water (70:30, v/v) Ultra Amino 9107365 150 x 4.6mm 3m 100 water:acetonitrile (25:75, v/v) 0.8mL/min. 35C refractive index @ 35C

Sugars on Ultra Amino


Peak List: 1. fructose 2. glucose 3. sucrose 4. maltose 5. lactose Sample: Inj.: Solvent: Conc.(mg/mL) 2.0 2.1 4.0 4.5 4.4 20L mobile phase Ultra Amino 9107365 150 x 4.6mm 3m 100 water:acetonitrile (25:75, v/v) 0.8mL/min. 35C refractive index @ 35C

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

1 2

4 5

8
LC_0159

10

12

14 min.

8
LC_0154

10

12

14 min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

506

Foods & Flavors


Sugars: 100% Maple Syrup on Pinnacle II Amino (high sensitivity)
Peak List: 1. fructose 2. glucose 3. sucrose Sample: Inj.: Conc.: Solvent: 100.0L 1% maple syrup in solvent acetonitrile:water (70:30, v/v)
3

Sugars: 100% Maple Syrup on Pinnacle II Amino (low sensitivity)


Pinnacle II Amino 9217565 150 x 4.6mm 5m 110 water:acetonitrile 1.0mL/min. 35C refractive index @ 35C Peak List: 1. fructose 2. glucose 3. sucrose Sample: Inj.: 50.0L Conc.: 1% maple syrup in solvent Solvent: acetonitrile:water (70:30, v/v) Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pinnacle II Amino 9217565 150 x 4.6mm 5m 110 water:acetonitrile (25:75) 1.0mL/min. 35C refractive index @ 35C

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: (25:75, v/v) Flow: Temp.: Det.:

H P LC A P P L I C AT I O N S

1 2 1 2

8
LC_0204

10

12

14 min.

8
LC_0205

10

12

14 min.

Sugars: Skim Milk on Pinnacle II Amino


Peak List: 1. lactose Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 10.0L 10% skim milk in solvent acetonitrile:water (70:30, v/v) Pinnacle II Amino 9217565 150 x 4.6mm 5m 110 water:acetonitrile (25:75, v/v) 1.0mL/min. 35C refractive index @ 35C

Laxative Lactulose Concentrate by USP 25: Resolution Solution on Pinnacle II Amino


Peak List: Conc. (mg/mL) 1. fructose 0.4 2. galactose 6.4 3. epi-lactose unknown 4. lactulose 40 5. lactose 4.8 Ret. Time (min.) 4.6 6.1 10.0 10.5 12.7 RRT 0.44 0.58 0.95 1.00 1.21 Res. Inj. % RSD (n=5) 1.1 0.3% 2.9

Sample: Inj.: 20L resolution standard Solvent: acetonitrile:water (50:50) Column: Cat. #: Dimensions: Particle size: Pore size: Pinnacle II Amino 9217365 150 x 4.6mm 3m 110 Conditions: Mobile phase: Flow: Temp.: Det.: A: 10mM sodium phosphate monobasic in water, pH 4.8 B: acetonitrile (22A:78B, v/v) 1.3mL/min. 40C refractive index @ 40C

4
LC_0206

10 min.
LC_0222

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Foods & Flavors


Sugars: Cola on Pinnacle II Amino Sugars: Orange Soda on Pinnacle II Amino
Peak List: 1. fructose 2. glucose Sample: Inj.: Solvent: Conditions: Mobile phase: Flow: Temp.: Det.: water:acetonitrile (25:75, v/v) 1.0mL/min. 35C refractive index @ 35C 20.0L 10% orange soda in solvent acetonitrile/water (70:30, v/v) Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 1 Pinnacle II Amino 9217565 150 x 4.6mm 5m 110 water:acetonitrile (25:75) 1.0mL/min. 35C (or ambient) refractive index @ 35C

507

Peak List: 1. fructose 2. glucose Sample: Inj.: Solvent: 10.0L 10% cola in solvent acetonitrile:water (70:30, v/v)

Column: Cat. #: Dimensions: Particle size: Pore size:

Pinnacle II Amino 9217565 150 x 4.6mm 5m 110

H P LC A P P L I C AT I O N S

2
1

4
LC_0203

7 min.

4
LC_0207

min.

Vanillin and Ethyl Vanillin on Ultra C8


Peak List: 1. vanillin 2. ethyl vanillin Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conc. (mg/mL) 0.12 0.04

Vanillin and Ethyl Vanillin on Pinnacle DB C18 (Fast LC)


Peak List: 1. vanillin 2. ethyl vanilling/mL each component Sample Diluent: 4% v/v ethanol in water Sample: Inj.: Conc.: Sample Diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 5L 200g/mL each 4% v/v ethanol in water Pinnacle DB C18 9414555 50 x 4.6mm 5m 140 0.2% v/v phosphoric acid in water:methanol (80:20 v/v) 2mL/min. 27C UV @ 254nm

10L 40% ethanol Ultra C8 9103565 150 x 4.6mm 5m 100

Conditions: Mobile phases: A: 1.2% acetic acid B: methanol Time (min.) %B 0.0 20.0 5.0 20.0 15.0 40.0 20.0 40.0 25.0 20.0 Flow: 1.0mL/min. Temp.: 28C Det.: UV @ 254nm

Flow: Temp.: Det.:

10
LC_0148

12

14

16

18 min.
LC_0251

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508

Foods & Flavors


Vanilla Bean Extract on Pinnacle DB C18 (Fast LC)
Peak List Sample: Inj.: Diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 5L 20% v/v commercial extract in water Pinnacle DB C18 9414555 50 x 4.6mm 5m 140 0.2% v/v phosphoric acid in water:methanol (80:20 v/v) 2mL/min. 27C UV @ 254nm 1. vanillin Ret. Time (min.) 2.00

Vanilla Flavoring (Imitation) on Pinnacle DB C18 (Fast LC)


Peak List: 1. Vanillin Sample: Inj.: Diluent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Ret. Time (min.) 2.00 5L 20% v/v commercial flavoring in water Pinnacle DB C18 9414554 50 x 4.0mm 5m 140 0.2% v/v phosphoric acid in water:methanol (80:20 v/v) 1.5mL/min. 27C UV @ 254nm

H P LC A P P L I C AT I O N S

Flow: Temp.: Det.:

LC_0252

LC_0253

a plus 1 story
When first seeking help with application issues it was suggested to me from a friend that I call Restek. His experience was that the support group from Restek was very willing to assist and that they might possibly ship me some phase to try out as opposed to spending a large sum of money on a new column phase that was no better then what I already had been using. After giving Restek a call, the customer support person sent me some CarboFrits free of charge to see if it would benefit my chromatography. I have since experienced many hours of useful consultation that has benefited my organization in numerous ways. On every occasion where I called for assistance it was always followed by a call later to check and see if things were going as planned. Thank you Restek for your caring support group of personnel. R. Frank Hart III, Lab Tech, GenApps research facility

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Pharmaceutical
Analgesic Acetaminophen on Pinnacle II C18
1

509

Analgesic Acetaminophen and Narcotic Analgesic Codeine Phosphate on Pinnacle II C18


Peak List: 1. acetaminophen 2. codeine phosphate Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Conc. (g/mL) g 1200 246

Peak List: 1. acetaminophen Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 1.0L 1.2 mg/mL mobile phase Pinnacle II C18 9214565 150 x 4.6mm 5m 110 10mM potassium phosphate monobasic, pH 3.0: acetonitrile (90:10) 1.0mL/min. 27C UV @ 210nm

1.0L mobile phase Pinnacle II C18 9214565 150 x 4.6mm 5m 110

H P LC A P P L I C AT I O N S

10mM potassium phosphate monobasic with 0.1% v/v TEA, pH 3.0:acetonitrile (90:10, v/v) 1.0mL/min. 27C UV @ 210nm

0.5

1.5

2.5

3.5

4 min.

LC_0151

LC_0152

Analgesic Acetaminophen and Narcotic Analgesics on Allure Basix


Peak List: 1. acetaminophen 2. codeine 3. oxycodone 4. hydroxycodone Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.:
2

Analgesic Acetaminophen and Narcotic Analgesics on Ultra C18


Peak List: Conc. (g/mL) U. unknown unknown 1. morphine sulfate 204 2. acetaminophen 92 3. codeine phosphate 216 4. oxycodone HCl 206 5. hydrocodone bitartrate 218 Ret. Time (min.) 3.1 3.3 5.0 5.5 7.5 8.9 Sample: Inj.: Sample: Solvent: Column: Catalog #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Tailing NA 1.0 1.1 1.4 1.4 1.4 Resolution NA 1.8 14.1 2.6 8.5 5.0 4.0L raw material mix mobile phase Ultra C18 9174575 250 x 4.6mm 5m 100 A: 10mm potassium phosphate, pH 2.8 B: acetonitrile: methanol (90:10 v/v) (85A:15B, v/v) 1.0mL/min. 27C UV @ 235nm

5L 100g/mL mobile phase Allure Basix 9161565 150 x 4.6mm 5m 60

20mM ammonium acetate, pH 4.5: acetonitrile (85:15, v/v) 1.0mL/min. 30C UV @ 280nm

Flow: Temp.: Det.:

3 4

min.

LC_0082

LC_0218

Phone: 800-356-1688 or 814-353-1300 www.restek.com

510

Pharmaceutical
Analgesic Acetaminophen and Narcotic Analgesics on Ultra C18
Peak List: Conc. (g/mL) 1. morphine sulfate 204 2. acetaminophen 92 3. codeine phosphate 216 4. oxycodone HCl 206 5. hydrocodone bitartrate 218 Sample: Inj.: Sample: Solvent:

Analgesic Acetaminophen and Narcotic Analgesics on Ultra C18


Peak List: Conc. (g/mL) U. unknown unknown 1. morphine sulfate 204 2. acetaminophen 92 3. codeine phosphate 216 4. oxycodone HCl 206 5. hydrocodone bitartrate 218

4.0L raw material mix mobile phase Ultra C18 9174575 250 x 4.6mm 5m 100 A: 10mm potassium phosphate, pH 2.8 B: acetonitrile (90A:10B, v/v) 1.0mL/min. 27C UV @ 235nm Sample: Inj.: Sample: Solvent: Column: Catalog #: Dimensions: Particle size: Pore size: 4.0L raw material mix mobile phase Ultra C18 9174575 250 x 4.6mm 5m 100 Conditions: Mobile phase: A: pH 2.8 10mm potassium phosphate B: acetonitrile:methanol, (90:10, v/v) (85A:15B, v/v) 1.0mL/min. 35C UV @ 235nm

H P LC A P P L I C AT I O N S

Column: Catalog #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

Flow: Temp.: Det.:

Flow: Temp.: Det.:

LC_0220

LC_0221

Narcotic Analgesic Morphine Sulfate Raw Material USP 25: Resolution Solution on Pinnacle II C18
Peak List: Conc. (g/mL) g 1. unknown unknown 2. phenol 0.15 3. morphine sulfate 0.24 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 20.0L mobile phase Pinnacle II C18 9214575-700 250 x 4.6mm 5m 110 A: 0.73g 1-heptane sulfonic acid and 10mL glacial acetic acid, diluted to 720mL with water, pH=2.33 B: methanol (72A:28B, v/v) 1.00mL/min, 26.5C UV @ 284nm

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Flow: Temp.: Det.:

LC_0209

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Pharmaceutical
Narcotic Analgesic Hydrocodone Bitartrate by USP 25 on Pinnacle II Silica

511

Peak List: 1. hydrocodone bitartrate Sample: Inj.: Conc.: Sample: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 20L 1g/mL assay standard mobile phase

Ret. Time (min.) 3.1

Inj. % RSD (n=5) 0.37%

Pinnacle II Silica 9210575 250 x 4.6mm 5m 110 A: 800mL acetonitrile; 4mL water; 1mL diethylamine B: methanol (55A:45B, v/v) 1.5mL/min. 27C UV @ 280nm

H P LC A P P L I C AT I O N S

Impurities resolved from primary peak.

min.

LC_0211

Narcotic Analgesic Oxycodone HCl Raw Material by USP 25 (modified): Resolution Solution on Ultra C8
Peak List: Conc. (g/mL) g 1. codeine phosphate 13 2. oxycodone HCl 9 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Ret. Time (min.) 5.7 7.6 RRT 0.8 1.0 Tailing 1.4 1.2 Res. 5.9

10L resolution solution mobile phase Ultra C8 9103564 150 x 4.0mm 5m 100 A: 20mM potassium phosphate monobasic pH=2.5 B: methanol (90A:10B, v/v) 1.5mL/min. 27C UV @ 206nm and 284nm

206nm

284nm

LC_0215

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512

Pharmaceutical
Narcotic Analgesic Oxycodone HCl Raw Material by USP 25: Resolution Solution on Ultra C8
Peak List: Conc. (g/mL) g 1. codeine phosphate 13 2. oxycodone HCl 9 Sample: Inj.: Sample: Solvent: 10L resolution solution mobile phase 9103564 150 x 4.0mm 5m 100 A: 5mM hexane sulfonic acid with 2mL TEA and 3mL of phosphoric acid per liter. pH adjusted to 2.5 B: methanol (90A:10B, v/v) 1.5mL/min. 40C UV @ 206nm Ret. Time (min.) 19.3 26.8 RRT 0.7 1.0 Tailing 1.1 0.99 Res. 3.3

Narcotic Analgesic Oxycodone HCI Raw Material by USP 25 (modified): Resolution Solution on Pinnacle II C8
Peak List: Conc. (g/mL) g 1. codeine phosphate 13 2. oxycodone HCl 9 Ret. Time (min.) 4.3 6.2 Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: RRT 0.8 1.0 Tailing 1.5 1.1 Res. 4.5

10L resolution solution mobile phase Pinnacle II C8 9213564 150 x 4.0mm 5m 110

H P LC A P P L I C AT I O N S

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

Flow: Temp.: Det.:

Flow: Temp.: Det.:

A: 20mM potassium phosphate monobasic pH=2.5 B: methanol (90A:10B, v/v) 1.5mL/min. 27C UV @ 284nm

LC_0213

LC_0210

Antiarrhythmic Atenolol on Allure Basix

Antiarrhythmic Digoxin on Ultra IBD


Peak List: 1. unknown 2. unknown 3. digoxin Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 10L 1000g/mL water:methanol (1:1, v/v) Ultra IBD 9175565 150 x 4.6mm 5m 100 water with 0.1% (v/v) acetic acid: acetonitrile (65:35, v/v) 1.0mL/min. 27C UV @ 220nm

Peak List: 1. uracil (marker) 2. atenolol Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 1L 1mg/mL water:methanol (7:3, v/v) Allure Basix 9161565 150 x 4.6mm 5m 60 acetonitrile:20mM ammonium acetate, pH 4.5 (80:20, v/v) 1.2mL/min. 25C UV @ 225nm

10

12 min.

LC_0072

LC_0068

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Pharmaceutical
Antiarrhythmic Calcium Channel Blockers on Ultra Cyano Digitalis Extracts/Derivatives on Ultra PFP Propyl Cartridge Column (Fast LC)
Peak List: Conc. 1. digoxigenin 100g/mL 2. gitoxigenin 100g/mL 3. digoxin 100g/mL 4. gitoxin ~10g/mL 5. digitoxin 100g/mL Sample: Inj.: Solvent: Column: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
4 5 3

513

Peak List: 1. diltiazem 2. nifedipine impurity 3. verapamil 4. nifedipine 5. nicardipine

Sample: Inj.: Conc.: Solvent:

5L 100mg/mL acetonitrile:water (1:1) Ultra Cyano 9106565 150 x 4.6mm 5m 100 20mM potassium phosphate monobasic, pH 3.0:acetonitrile (70:30, v/v) 1.2mL/min. 30C (1C) 235nm

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
1

Ret. Time (min.) 0.40 0.80 1.10 2.20 2.60

10L water:acetonitrile (80:20 v/v)

H P LC A P P L I C AT I O N S

Flow rate: Temp.: Det.:

Custom Fast LC Cartridge 30 x 4.0mm 3m 100 A: water B: acetonitrile Time (min.) 0.0 1.5 1.51 3.0 3.1 %B 20 20 35 35 20

Flow: Temp.: Det.:

2.0mL/min. 27C UV @ 230nm

5
LC_0062

9 min.
LC_0250

Antiarrhythmic Enalapril Maleate on Allure Basix

Antiarrhythmic Furosemide on Ultra IBD

Peak List: 1. maleate 2. enalapril Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 2.5L 1.1mg/mL methanol:water (30:70) Allure Basix 9161565 150 x 4.6mm 5m 60 10mM ammonium formate, pH 2.5: acetonitrile (20:80, v/v) 1.2mL/min. 25C UV @ 225nm

Peak List: 1. uracil (marker) 2. furosemide Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 5L 1000g/mL acetonitrile:water (60:40, v/v) Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM ammonium acetate, pH 4.5: acetonitrile (70:30, v/v) 2.0mL/min. 27C UV @ 280nm

Impurities in Furosemide
(enlargement of baseline)

Flow rate: Temp.: Det.:

LC_0091

LC_0071

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514

Pharmaceutical
Antiarrhythmic Metoprolol on Allure Basix
Peak List: 1. unknown 2. metoprolol Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 2.5L 1.5mg/mL methanol:water (30:70) Allure Basix 9161565 150 x 4.6mm 5m 60 10mM ammonium formate, pH 2.5: acetonitrile (10:90, v/v) 1.2mL/min. 25C UV @ 225nm

Antiarrhythmic Timolol Maleate on Allure Basix


Peak List: 1. maleate 2. timolol Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 2.5L 1.2mg/mL methanol:water (30:70) Allure Basix 9161565 150 x 4.6mm 5m 60 10mM ammonium formate, pH 2.5: acetonitrile (20:80, v/v) 1.2mL/min. 25C UV @ 290nm

H P LC A P P L I C AT I O N S

LC_0090

LC_0092

Antiarrhythmic Triamterene and Hydrochlorothiazide on Allure Basix


Peak List: 1. hydrochlorothiazide 2. triamterene Sample: Inj.: Conc.: Solvent: 1L 500g/mL methanol:water: tetrahydrofuran (30:35:35) Allure Basix 9161565 150 x 4.6mm 5m 60 20mM ammonium acetate, pH 4.5:acetonitrile (65:35,v/v) 1.2mL/min. 25C UV @ 225nm

Antiarrhythmic Triamterene on Allure Basix


Peak List: 1. uracil (marker) 2. triamterene Sample: Inj.: Conc.: Solvent: 1L 1mg/mL methanol: tetrahydrofuran (7:3,v/v) Allure Basix 9161565 150 x 4.6mm 5m 60 20mM ammonium acetate, pH 4.5: acetonitrile (65:35,v/v) 1.2mL/min. 25C UV @ 225nm

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.:

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

Flow rate: Temp.: Det.:

LC_0086

LC_0074

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Pharmaceutical
Antiarrhythmic Verapamil HCl on Allure Basix
Peak List: 1. toluene (marker) 2. verapamil HCl
2

515

Antiarrhythmic Verapamil HCl Raw Material on Ultra IBD (EP 2002 modified)
Peak List: 1. verapamil
1

Ret. time (min.) 15.0 20L 25g/mL initial mobile phase Ultra IBD 9175575 250 x 4.6mm 5m 100

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

1L 1mg/mL water:acetonitrile (70:30, v/v) Allure Basix 9161565 150 x 4.6mm 5m 60 acetonitrile: 20mM ammonium acetate, pH 4.5 (65:35,v/v) 1.2mL/min. 25C UV @ 230nm

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size:

H P LC A P P L I C AT I O N S

Flow rate: Temp.: Det.:

Conditions: Mobile phase: A: 40 mM potassium phosphate monobasic pH 6.25 B: acetonitrile Time (min.) %B 0.0 37 22.0 37 27.0 65 35.0 65 36.0 37 46.0 37 Flow: 1.5 mL/min. Temp.: 25C Det.: UV @ 278nm

min.
0 5 10 15 20 25 30 35 min.

LC_0077

LC_0208

Antiasthmatic Beclomethasone on Ultra Cyano


Peak List: 1. deschlorobeclomethasone 2. beclomethasone Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 10L 100g/mL beclomethasone water:acetonitrile (9:1, v/v) Ultra Cyano 9106565 150 x 4.6mm 5m 100 water:acetonitrile (70:30, v/v) 1.0mL/min. ambient UV @ 238nm

Antiasthmatic Beclomethasone on Ultra C18

Peak List: 1. beclomethasone 2. deschlorobeclomethasone


2

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

10L 79.5g/mL (beclomethasone) water:acetonitrile (10:90, v/v) Ultra C18 9174565 150 x 4.6mm 5m 100 water:acetonitrile (70:30, v/v) 1.0mL/min. 25C UV @ 238nm

6
LC_0070

9 min.

10
LC_0120

15

20 min.

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516

Pharmaceutical
Antiasthmatic Beclomethasone on Ultra C18
1 1

Antibiotic Amoxicillin on Ultra IBD

Peak List: 1. beclomethasone 2. deschlorobeclomethasone Sample: Inj.: Conc.: Solvent: 10L 79.5g/mL (beclomethasone) water:acetonitrile (10:90, v/v) Ultra C18 9174565 150 x 4.6mm 5m 100 water:acetonitrile (30:70, v/v) 1.0mL/min. 25C UV @ 238nm

Peak List: 1. amoxicillin Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 5L 1.5mg/mL acetonitrile:water (10:90, v/v) Ultra IBD 9175565 150 x 4.6mm 5m 100 10mM ammonium formate, pH 2.5: acetonitrile (95:5, v/v) 1.2mL/min. 30C UV @ 270nm

H P LC A P P L I C AT I O N S

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

0.5

1.5

2 min.

min.

LC_0121

LC_0095

Antibiotic Cephaloridine on Ultra IBD (LC/MS)


Peak List: 1. cephaloridine Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 5L 5g/mL mobile phase Ultra IBD 9175552 50 x 2.1mm 5m 100
1

Antibiotic Cephaloridine on Ultra IBD (Normal Phase)


Peak List: 1. cephaloridine
1

Sample: Inj.: Conc: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

5L 1mg/mL acetonitrile:water (50:50, v/v) Ultra IBD 9175565 150 x 4.6mm 5m 100 acetonitrile: 20mM ammonium phosphate, pH 4.0 (80:20,v/v) 1.2mL/min. 27C UV @ 254nm

5mM ammonium acetate, pH 7.4: acetonitrile (20:80, v/v) Flow: 0.2mL/min. Temp.: ambient Det.: PE/Sciex API 150 EX Interface: turbo ion spray Ion mode: positive Nebulizer: 8L/hour Curtain gas: 12L/Hour Ion spray voltage: 4700.0 V Temp.: 350C Orifice: + 10.0 V Ring: + 25.0 V SIM monitoring: 416 3 Daltons

Flow: Temp.: Det.:

1.0

2.0 min.

5
LC_0101

9 min.

LC_0124

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Pharmaceutical
Antibiotic Cephaloridine on Ultra IBD (Reversed Phase)
1

517

Antibiotic Cephalexin on Ultra IBD


1

Peak List: 1. cephaloridine Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L 1mg/mL acetonitrile:water (50:50, v/v) Ultra IBD 9175565 150 x 4.6mm 5m 100 20mM:acetonitrile ammonium phosphate, pH 4.0 (20:80,v/v) 1.2mL/min. 27C UV @ 254nm

Peak List: 1. cephalexin 2. cephradine Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 10L 500g/mL acetonitrile:water (10:90, v/v) Ultra IBD 9175565 150 x 4.6mm 5m 100 10mM ammonium formate, pH 2.5: acetonitrile (90:10, v/v) 1.2mL/min. 30C UV @ 270nm

H P LC A P P L I C AT I O N S

Flow rate: Temp.: Det.:

min.

10 min.

LC_0102

LC_0094

Antibiotic Cephradine on Ultra IBD (LC/MS)


Peak List: 1. cephradine Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: 5L 5g/mL mobile phase Ultra IBD 9175552 50 x 2.1mm 5m 100
1

Antibiotic Penicillin V on Ultra IBD (LC/MS)


Peak List: 1. penicillin V Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Interface: Ion mode: Nebulizer: Curtain gas: Ion spray voltage: Temp.: Orifice: Ring: SIM monitoring:

Conditions: Mobile phase: Flow: Temp.: Det.: Interface: Ion mode: Nebulizer: Curtain gas: Ion spray voltage: Temp.: Orifice: Ring: SIM monitoring:

5mM ammonium acetate, pH 7.4: acetonitrile (20:80, v/v) 0.2mL/min. ambient PE/Sciex API 150 EX turbo ion spray positive 8L/hour 12L/Hour 4700.0 V 350C + 10.0 V + 25.0 V 349 3dal.

5L 5g/mL mobile phase Ultra IBD 9175552 50 x 2.1mm 5m 100 5mM ammonium acetate pH 7.4: acetonitrile (20:80, v/v) 0.2mL/min. ambient PE/Sciex API 150 EX turbo ion spray positive 8L/hour 12L/hour 4700.0 v 350C + 10.0 V + 25.0 V 349 3dal.

1.0

2.0 min.

1.0

2.0

min.

LC_0125

LC_0127

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518

Pharmaceutical
Antibiotic Penicillin V on Ultra IBD
1

Antibiotic Sulfamethoxazole on Allure Basix


1

Peak List: 1. penicillin V Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 2.5L 1.2mg/mL acetonitrile:water (10:90,v/v) Ultra IBD 9175565 150 x 4.6mm 5m 100 10mM ammonium formate, pH 2.5: acetonitrile (95:5, v/v) 1.2mL/min. 30C UV @ 270nm

Peak List: 1. sulfamethoxazole Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 10L 100g/mL water:methanol (1:1, v/v) Allure Basix 9161565 150 x 4.6mm 5m 60 water:methanol (70:30, v/v) 1.0mL/min. ambient UV @ 254nm

H P LC A P P L I C AT I O N S
0

min. 0 2.5 5 7.5


LC_0066

10

12.5

15

17.5 min.

LC_0096

Antibiotic Sulfamethoxazole, Trimethoprim, and Naphthoate on Allure C18


1

Antidepressants (Tricyclic) on Allure Basix

Peak List: 1. trimethoprim 2. sulfamethoxazole 3. naphthoate


2

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

10L 100g/mL water:methanol (1:1, v/v) Allure C18 9164565 150 x 4.6mm 5m 60 10mM ammonium formate, pH to 3.0 with formic acid: methanol (50:50, v/v) 1.0mL/min. ambient UV @ 220nm

Peak List: 1. doxepin 2. nordoxepin 3. amitriptyline 4. imipramine 5. desimipramine 6. nortriptyline 7. protriptyline

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size:
1 2 3

10L 100g/mL each mobile phase Allure Basix 9161565 150 x 4.6mm 5m 60

Conditions: Mobile phase: acetonitrile: 50mM KH2PO4 pH3:methanol (60:25:15, v/v) Flow rate: 1.2mL/min. Temp.: 30C Det.: UV @ 254nm
4 6 5

Flow rate: Temp.: Det.:


3

0 0 2 4 6 8
LC_0067

5
LC_0053

9 min.

10

12

14 min.

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Pharmaceutical
Antidepressants (Tricyclic) on Allure Basix (LC/MS)
Peak List: 1. desipramine 2. trimipramine Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Split ratio: Column temp.: Det.: Interface: Ion mode: Ion spray voltage: Temp.: Orifice: Ring: Auxiliary gas: 10L 10g/mL water:methanol (1:1, v/v) Allure Basix 9161565 150 x 4.6mm 5m 60
2

519

Antidepressant Sertraline HCl on Allure Basix

Peak List: 1. toluene (marker) 2. sertraline HCl Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 1L 1mg/mL water:acetonitrile (7:3, v/v)

H P LC A P P L I C AT I O N S

5mM ammonium formate, pH 3:methanol (25:75, v/v) 1.0mL/min. 1:1 ambient PE/Sciex API 150 EX heated nebulizer negative 3000V 400C -40V -100V 6000cc/min.

Allure Basix 9161565 150 x 4.6mm 5m 60 acetonitrile: 20mM ammonium acetate, pH 4.5 (40:60, v/v) 2.0mL/min. 25C UV @ 230nm

Flow rate: Temp.: Det.:

9 min. 0

8
LC_0079

10

12

14 min.

LC_0112

Anti-Diabetic Glyburide (Glybenclamide) on Ultra IBD


2

Peak List: 1. unknown 2. glyburide Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 1L 500mg/mL water:methanol:acetone (1:1:2, v/v) Ultra IBD 9175565 150 x 4.6mm 5m 100 water with 0.1% (v/v) acetic acid: acetonitrile (95:05, v/v) 1.0mL/min. 27C UV @ 254nm

Searching for a chromatogram?

www.restek.com

3
LC_0069

min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

520

Pharmaceutical
Anti-inflammatory Naproxen on Pinnacle DB Cyano
1

Anti-inflammatory Naproxen on Pinnacle DB C8


1

Peak List: 1. naproxen Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 2L 550g/mL mobile phase Pinnacle DB Cyano 9416565 150 x 4.6mm 5m 140 20mM KH2PO4, pH 3.0:acetonitrile (90:10 v/v) 1.0mL/min. 27C UV @ 254nm

Peak List: 1. naproxen Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 2L 550g/mL mobile phase Pinnacle DB C8 9413565 150 x 4.6mm 5m 140 20mM KH2PO4, pH 3.0:acetonitrile (90:10 v/v) 1.0mL/min 27C UV @ 254nm

H P LC A P P L I C AT I O N S

0.5

1.5

2
LC_0239

2.5

3.5

min.

0.5

1.5

2.5
LC_0240

3.5

4.5 min.

Anti-ulcerative Cimetidine on Ultra IBD (LC/MS)


Peak List: 1. cimetidine Sample: Inj.: Conc.: Solvent: 5L 10g/mL mobile phase Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Column temp.: Det.: Interface: Ion mode: Ion spray voltage: Temp.: Orifice: Ring: Auxiliary gas: Ultra IBD 9175552 50 x 2.1mm 5m 100 water:acetonitrile (20:80, v/v) 0.2 mL/min. ambient PE/Sciex API 150 EX turbo ion spray positive 4800V 350C 10V 100V 6000cc/min.

Bronchodilator Albuterol on Allure Basix


1

Peak List: 1. albuterol Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 2.5L 1.1mg/mL methanol:water (30:70) Allure Basix 9161565 150 x 4.6mm 5m 60 10mM ammonium formate, pH 2.5: acetonitrile (20:80, v/v) 1.2mL/min. 25C UV @ 225nm

Flow rate: Temp.: Det.:

0.2

0.4

0.6

0.8

1.0
LC_0115

1.2

1.4

1.6

1.8

min.

3
LC_0089

5 min.

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Pharmaceutical
Corticosteroids on Allure C18 Corticosteroids on Ultra C18
Peak List: 1. uracil 2. triamcinolone 3. hydrocortisone 4. dexamethasone 5. corticosterone 6. deoxycorticosterone Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L 100g/mL mobile phase
5

521

Peak List: 1. uracil 2. corticosterone 3. deoxycorticosterone Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 5L 100g/mL each water:acetonitrile (1:1) Allure C18 9164565 150 x 4.6mm 5m 60 water:methanol (50:50, v/v) 1.0mL/min. ambient UV @ 254nm

H P LC A P P L I C AT I O N S

Ultra C18 9174565 150 x 4.6mm 5m 100 water:methanol (30:70, v/v) 1.0mL/min. 30C UV @ 220nm

4 min. 0 1 2
LC_0108

6 min.

LC_0054

Corticosteroids on Allure C18 vs. Conventional C18 (LC/MS)


12% increase in organic = 26% increase in LC/MS sensitivity

Conventional C18
water:methanol (40:60, v/v) 3324.0 cps

Allure C18
water:methanol (33:67, v/v) 4191.1 cps Peak List: 1. deoxycorticosterone (DCC) acetate 2. DCC glucoside 3. DCC
2 3

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Scan range: Flow rate: LC/MS Interface: Voltage: Nozzle temp.: Nozzle volt.:

9164552 50 x 2.1mm 5m 60 320-520amu 0.4mL/min. positive ion ESI-TOF 3800V 160V 190V

4 min.
LC_0111

4 min.

Data Courtesy of Pfizer Inc

Phone: 800-356-1688 or 814-353-1300 www.restek.com

522

Pharmaceutical
Corticosteroids on Pinnacle II Phenyl
Pinnacle II Phenyl 9215565 150 x 4.6mm 5m 110 water:methanol (60:40 v/v) 1.0mL/min. ambient UV @ 254nm

Corticosteroids on Pinnacle II Cyano (Normal Phase Separation)

Peak List: 1. hydrocortisone 2. cortisone 3. corticosterone 4. cortisone acetate Sample: Inj.: Conc.: Solvent:
1

Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

Peak List: 1. corticosterone 2 cortisone acetate 3. cortisone Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pressure: 10L ethanol

Conc. (mg/mL) 0.7 0.4 0.4

5L 200g/mL each methanol

H P LC A P P L I C AT I O N S

Pinnacle II Cyano 9216565 150 x 4.6mm 5m 110 hexane:ethanol (90:10, v/v) 1.0mL/min. 30C UV @ 254nm 29 bar

2 3

4
LC_0182

8 min.

6
LC_0185

10

12

Corticosteroids on Pinnacle II Cyano (Reversed Phase Separation)


Peak List: 1. cortisone 2. corticosterone 3. cortisone acetate Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: Pressure: 5.0L methanol Pinnacle II Cyano 9216565 150 x 4.6mm 5m 110

Conc. (mg/mL) 0.1 0.5 0.7

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1 3

water:methanol (65:35, v/v) 1.0mL/min. 30C UV @ 254nm 133 bar

5
LC_0186

9 min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Pharmaceutical
Hormones -Estradiol, Norethindrone and Ethynyl Estradiol on Ultra C18
3

523

Hormones -Estradiol, Norethindrone and Ethynyl Estradiol on Ultra C18

Peak List: 1. -estradiol 2. ethynyl estradiol 3. norethindrone Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 10L 333g/mL water:acetonitrile (20:80, v/v) Ultra C18 9174565 150 x 4.6mm 5m 100
1

Peak List: 1. -estradiol 2. norethindrone 3. ethynyl estradiol Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:
2

10L 333g/mL acetonitrile:water (80:20, v/v)

H P LC A P P L I C AT I O N S

Ultra C18 9174565 150 x 4.6mm 5m 100 10mM ammonium formate, pH 3.0: acetonitrile (60:40, v/v) 1.0 mL/min. 30C UV @ 230nm

10mM ammonium formate, pH 3.0: acetonitrile (40:60, v/v) 1.0 mL/min. 30C UV @ 230nm

2
LC_0122

4min.

8
LC_0118

10

12

14

min.

Hormones -Estradiol, Norethindrone and Ethynyl Estradiol on Ultra C4


Peak List: 1. -estradiol 2. norethindrone 3. 17--ethynyl estradiol Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: 15L 333g/mL acetonitrile:water (70:30) Ultra C4 9102365 150 x 4.6mm 3m 100 10mM ammonium formate, pH 3.0: acetonitrile (60:40, v/v) 1.2mL/min. 30C UV @ 230nm
3

Hormones Norethindrone and Ethynyl Estradiol on Allure Basix


3

Peak List: 1. uracil (marker) 2. norethindrone 3. ethynyl estradiol


1

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.:

5L 200g/mL mobile phase Allure Basix 9161565 150 x 4.6mm 5m 60 water:methanol (35:65, v/v) 1.0mL/min. 25C UV @ 220nm
2

Flow rate: Temp.: Det.:

6 min.

6 min.

LC_0085

LC_0099

Phone: 800-356-1688 or 814-353-1300 www.restek.com

524

Pharmaceutical
Hormones Norgestrel and Ethynyl Estradiol on Allure Basix
Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size:

Hormones Norgestrel and Ethynyl Estradiol on Ultra C18

Peak List: 1. uracil (marker) 2. norgestrel 3. ethynyl estradiol

5L 100g/mL mobile phase Allure Basix 9161565 150 x 4.6mm 5m 60 water:methanol (40:60, v/v) 1.0mL/min. 25C UV @ 220nm
1

Peak List: 1. uracil (marker) 2. ethynyl estradiol 3. norgestrel Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L 100g/mL mobile phase Ultra C18 9174565 150 x 4.6mm 5m 100 water:methanol (40:60, v/v) 1.0mL/min. 25C UV @ 220nm
3

H P LC A P P L I C AT I O N S

Conditions: Mobile phase: Flow rate: Temp.: Det.:


2

6
LC_0100

min.

2.5

7.5

10

12.5
LC_0116

15

17.5

20

22.5 min.

Hormones Norgestrel and Ethynyl Estradiol on Allure C18


1

Hormones Norgestrel and Ethynyl Estradiol on Allure C18


Peak List: 1. uracil (marker) 2. ethynyl estradiol 3. norgestrel
1

Peak List: 1. uracil (marker) 2. ethynyl estradiol 3. norgestrel Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 5L 100g/mL mobile phase Allure C18 9164565 150 x 4.6mm 5m 60 water:methanol (40:60, v/v) 1.0mL/min. 25C UV @ 220nm

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

5L 100g/mL mobile phase Allure C18 9164565 150 x 4.6mm 5m 60 water:methanol (25:75, v/v) 1.0mL/min. 25C UV @ 220nm

10

15
LC_0117

20

25 min.

3
LC_0123

min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Pharmaceutical
Hormones Norethindrone and Medroxyprogesterone Acetate on Allure Basix
Peak List: 1. uracil (marker) 2. norethindrone 3. medroxyprogesterone Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 10L 100g/mL mobile phase Allure Basix 9161565 150 x 4.6mm 5m 60
3

525

Hormone Medroxyprogesterone Acetate on Ultra C4


Peak List: 1. unknown 2. medroxyprogesterone

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.:

1L 1mg/mL acetonitrile:water (70:30) Ultra C4 9102365 150 x 4.6mm 3m 100 10mM ammonium formate, pH 3.0: acetonitrile (40:60, v/v) 1.2mL/min. 30C UV @ 240nm

H P LC A P P L I C AT I O N S

water:acetonitrile (40:60, v/v) 1.0mL/min. 30C UV @ 220nm

0.5

1.5

2
LC_0083

2.5

3.5

min.

5
LC_0084

9 min.

Hormone Levothyroxine on Ultra PFP


2

Peak List: 1. unknown 2. levothyroxine Sample: Inj.: Conc.: Solvent: 20L 1.1mg/mL water:methanol (70:30) Add 3 drops of concentrated ammonium hydroxide to each 10mL of solvent. Levothyroxine will not dissolve unless the pH is basic. Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: Ultra PFP 9176565 150 x 4.6mm 5m 100 10mM ammonium formate, pH 2.5: methanol (60:40, v/v) 1.2mL/min. 25C UV @ 254nm

Laxative Lactulose Concentrate by USP 25: Resolution Solution on Pinnacle II Amino


Peak List: Conc. (mg/mL) 1. fructose 0.4 2. galactose 6.4 3. epi-lactose unknown 4. lactulose 40 5. lactose 4.8 Ret. Time (min.) 4.6 6.1 10.0 10.5 12.7 RRT 0.44 0.58 0.95 1.00 1.21 Res. Inj. % RSD (n=5) 1.1 0.3% 2.9

Sample: Inj.: 20L resolution standard Solvent: acetonitrile:water (50:50) Column: Cat. #: Dimensions: Particle size: Pore size: Pinnacle II Amino 9217365 150 x 4.6mm 3m 110 Conditions: Mobile phase: Flow: Temp.: Det.: A: 10mM sodium phosphate monobasic in water, pH 4.8 B: acetonitrile (22A:78B, v/v) 1.3mL/min. 40C refractive index @ 40C

10
LC_0093

12

14

16

18 min.
LC_0222

Phone: 800-356-1688 or 814-353-1300 www.restek.com

526

Pharmaceutical
Mixed Drugs: Analgesic Ibuprofen and Decongestant Pseudoephedrine on Allure Basix
Peak List: 1. uracil 2. ibuprofen 3. pseudoephedrine

Mixed Drugs: Analgesic Acetaminophen, Decongestant Pseudoephedrine and Stimulant Caffeine on Allure Basix
Peak List: 1. sample solvent 2. caffeine 3. acetaminophen 4. pseudoephedrine

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

5L 200g/mL mobile phase Allure Basix 9161565 150 x 4.6mm 5m 60

Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.:

5L 100g/mL mobile phase Allure Basix 9161565 150 x 4.6mm 5m 60

H P LC A P P L I C AT I O N S

10mM ammonium acetate, pH 6.9: methanol (75:25, v/v) 1.0mL/min. 25C UV @ 210nm

10mM ammonium acetate, pH 6.9: methanol (75:25, v/v) 1.0mL/min. 25C UV @ 210nm

10
LC_0098

12

14 min.

6
LC_0097

10

12 min.

Mixed Drugs: Hydrocodone Bitartrate/Acetaminophen by USP 25 on Ultra C18


Peak List: Conc. (g/mL) g 1. acetaminophen 0.76 2. hydrocodone bitartrate 0.0076 Ret. Time (min.) 3.304 6.664 RRT 1.0 2.0 Tailing Resolution Inj. %RSD (n=5) 1.1 1.1 1.1 17.0 0.9

Mixed Drugs: Expectorant/Antitussive Guaifenesin and Narcotic Analgesic Codeine on Ultra Phenyl
2 1

Sample: Inj.: Sample: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

25L 500mg acetaminophen with 5mg hydrocodone bitartrate (tablet) mobile phase Ultra C18 9174575 250 x 4.6mm 5m 100 A: 6.8 g potassium monobasic with 0.2mL of TEA per liter B: acetonitrile (85A:15B, v/v) 1.5mL/min. 27C UV @ 210nm (hydrocodone bitartrate) and 295nm (acetaminophen).

Peak List: 1. codeine 2. guaifenesin Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:

Conc. (g/mL) g 825 375 5L methanol:water (50:50) Ultra Phenyl 9105565 150 x 4.6mm 5m 100 10mM ammonium formate, pH 2.5: acetonitrile (80:20, v/v) 1.2mL/min. 25C UV @ 280nm

Flow: Temp.: Det.:

Flow rate: Temp.: Det.:

0
LC_0212

min.

LC_0088

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Pharmaceutical
Sedatives Alprazolam and Lorazepam on Allure Basix Sedative Cyclobenzaprine on Allure Basix

527

Peak List: 1. toluene (marker) 2. lorazepam 3. alprazolam Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 10L 500g/mL water:acetonitrile (7:3, v/v) Allure Basix 9161565 150 x 4.6mm 5m 60 10mM ammonium formate, pH 3.0:acetonitrile (70:30, v/v) 2.0mL/min. 25C UV @ 230nm

Peak List: 1. toluene (marker) 2. cyclobenzaprine HCl Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.: 1L 1.5g/mL 100% water Allure Basix 9161565 150 x 4.6mm 5m 60 10mM ammonium formate, pH 3.0 acetonitrile (25:75, v/v) 1.2mL/min. 30C UV @ 230nm

H P LC A P P L I C AT I O N S

3
LC_0078

min.

3
LC_0087

6 min.

Xanthenes on Pinnacle DB C18


Sample: Inj.: Solvent:
1 2

Xanthenes on Pinnacle DB C18


Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
1

Xanthenes on Pinnacle II C18


Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow: Temp.: Det.: 2L water:methanol (75:25 v/v) Pinnacle II C18 9214565 150 x 4.6mm 5m 110 20mM KH2PO4 pH 3: methanol (80:20 v/v) 1.0mL/min. ambient UV @ 254nm

2L mobile phase Pinnacle DB C18 9414565 150 x 4.6 mm 5m 140

2L water:methanol (75:25 v/v) Pinnacle DB C18 9414565 150 x 4.6mm 5m 140 20mM KH2PO4, pH 3:methanol (80:20 v/v) 1.0mL/min. ambient UV @ 254nm

Column: Cat. #: Dimensions: Particle size: Pore size:

Conditions: Mobile phase: 20mM KH2PO4, pH 3.0: acetonitrile (90:10 v/v) Flow: 1.0 mL/min. Temp.: 27C Det.: UV @ 254nm
3 4

Flow: Temp.: Det.:


3 4

min.

min.

Peak List: Conc. ( g/mL) 1. theobromine 225 2. theophylline 418 3. -hydroxyethyltheophylline 418 4. caffeine 400
LC_0241

Peak List: Conc. (g/mL) 1. theobromine 200 2. theophylline 390 3. -hydroxytheophylline 390 4. caffeine 390
LC_0288

Peak List: Conc. (g/mL) g 1. theobromine 200 2. theophylline 390 3. -hydroxytheophylline 390 4. caffeine 390
LC_0290

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Chris English
Innovations Group Leader

GC Applications
Our library of chromatograms will save you time when you are researching a new application or attempting to improve on current results. This selection includes representative GC chromatograms for environmental contaminants, petrochemicals, industrial chemicals, biochemicals, pharmaceuticals, nutraceuticals, foods, flavors & fragrances, and forensics. To see our newest chromatograms, subscribe to the Restek Advantage, and regularly visit our web site at www.restek.com.

Volatiles Choosing a Volatiles GC Column for PID/ELCD


Restek Phase Rtx-VGC Coelutions by Peak #s (Coelutions by PID/ELCD are indicated in BOLD) Close Pairs by PID/ELCD 7/8, 32/33 Suggested Confirmation Column Poor Choice for Confirmation Column Recomended Thick Phase High Temp. Stable Temp. for VOA Work Advantages Page # for Chromatogram2

529

28/29 1, 53/54

Rtx-502.2, Rtx-VRX, Rtx-VMS, Rtx-1 Rtx-DX1 Rtx-VGC, Rtx-VRX, Rtx-1 Rtx-VGC, Rtx-1, Rtx-624 Rtx-VGC, Rtx-502.2 Rtx- VGC, Rtx-502.2 Rtx-Volatiles, Vocol, Rtx-35, Rtx-20 Rtx-502.2, Vocol, Rtx-20, Rtx-35

260

230

fast runtime

530, 532 533, 534, 535, 544

Rtx-502.2

14/15, 33/34, 39/40

4/5, 44/45, 56/57, 52/55, 64/65 56/57, 68/69

270

240

low bleed

Rtx-Volatiles

14/15, 21/22, 38/40, 44/45, 53/55 7/8, 10/11, 52/53, 31/34, 53/55, 59/60
11/13, 39/43, 46/50, 40/44

270

240

low bleed

no

Rtx-624

32/33, 44/45, 51/54 8/9, 15/17, 24/27, 58/60

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Rtx-1701

280

240

no

Rtx-VRX

Rtx-1

260

230

531, 536

Rtx-1

9/12, 15/17, 25/26, 24/27, 33/36, 38/40, 40/44, 45/50, 56/57

7/12, 49/55

Rtx-502

Rtx-VRX

320

260

no

Rtx-1701

9/10, 18/19, 16/20, 50/53, 51/55, 54/56 2/3, 5/6, 11/12, 14/16, 22/24, 28/35, 32/33/37, 43/44, 50/55/56, 57/58 4/5, 16/19, 18/20, 21/22, 34/31, 39/38/41/42/40, 46/51/49, 53/54, 48/52/55, 61/62, 66/67 4/5/6, 8/7/12, 25/28, 32/33, 37/41/42, 38/40, 45/47, 46/54/52, 56/55/48, 57/58 4/5, 9/10, 25/27, 38/39, 47/50, 49/46/48, 52/54, 53/55

5/6, 29/30, 32/33

Rtx-502.2

Rtx-624

270

240

no

Rtx-200

13/17,36/37

Rtx-VGC Rtx-VGC, Rtx-624 Rtx-502.2, Rtx-Volatiles, Rtx-20

320

240

m/p xylene separation

no

Rtx-35

2/3,

270

240

no

Rtx-50

2/3, 20/18, 31/32, 39/41/42 27/28, 32/36/31, 65/67

Rtx-VGC, Rtx-624

Rtx-35

280

240

no

Rtx-DX1 (custom)
1

Rtx-502.2

Rtx-VGC

220

200

no

Can be resolved under different conditions. See application showing method 601/602 with the Rtx -VGC column on www.restek.com/chromatograms (search for chromatogram number GC_EV00420). pages listed include GC/MS analyses.

Volatile Analytes:
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane 1,1-dichloroethene Freon 113 methylene chloride trans-1,2-dichloroethene methyl tert-butyl ether tert-butyl alcohol 1,1-dichloroethane cis-1,2-dichloroethene 2,2-dichloropropane bromochloromethane chloroform carbon tetrachloride 1,1,1-trichloroethane 1,1-dichloropropene benzene 1,2-dichloroethane fluorobenzene trichloroethene dibromomethane 1,2-dichloropropane bromodichloromethane 2-chloroethyl vinyl ether cis-1,3-dichloropropene toluene tetrachloroethene trans-1,3-dichloropropene 2-bromo-1-chloropropane 1,1,2-trichloroethane dibromochloromethane 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 1,3-dichloropropane 1,2-dibromoethane chlorobenzene ethyl benzene 1,1,1,2-tetrachloroethane m-xylene p-xylene 1-chloro-2-fluorobenzene o-xylene styrene bromoform isopropyl benzene bromobenzene n-propylbenzene 1,4-dichlorobutane 1,1,2,2-tetrachloroethane 2-chlorotoluene 1,3,5-trimethylbenzene 1,2,3-trichloropropane 4-chlorotoluene tert-butylbenzene 1,2,4-trimethylbenzene sec-butylbenzene p-isopropyl toluene 1,3-dichlorobenzene 1,4-dichlorobenzene n-butylbenzene 1,2-dichlorobenzene 4-bromo-1-chlorobenzene 1,2-bromo-3-chloropropane hexachlorobutadiene 1,2,4-trichlorobenzene naphthalene 1,2,3-trichlorobenzene

Conditions for Rtx-VGC, Rtx-502.2, Rtx-Volatiles, Rtx-VRX and Rtx-1: optimum conditions on 75 m, 0.45mm ID, 2.55m columns. Conditions for all other columns: Column: 60m, 0.53mm ID, 3.0m column flow 10mL/min., GC Program: 35C (hold 9 min.) to 220C @ 11 min. (hold 10 min.) Analytes identified using HP5971a mass selective detector with splitless injection or using Finnigan PID/ELCD Please see chromatograms on pages 530544 for more details, or call technical service at 800-356-1688 (ext. 4), or your Restek representative.

for more info


For GC/MS analyses, see Rtx-VMS applications on pages 537543.

Compounds listed in US EPA Methods 502.2, 8021, 8010, 8020, 601 & 602, plus commonly added compounds.

m/p xylene coelute on all phases listed above except Rtx-200 in 60m, 0.25mm ID, 1.0m under optimized conditions. See 8260 application, using the Rtx-200 column, www.restek.com/chromatograms (search for chromatogram number GC_EV00429).

Phone: 800-356-1688 or 814-353-1300 www.restek.com

530

Volatiles
Volatile Organics US EPA Method 8021 Rtx-VGC
Primary column, dual-column analysis. Polymer specially designed for volatiles analysis by PID/ELCD. Confirmation analysis shown on page 531. Rtx-VGC 75m, 0.45mm ID, 2.55m (cat.# 19409)

restek innovation!
35C starting temperature for better resolution of early-eluting compounds. Excellent resolution of trihalomethanes.
47

49

ELCD
51

41,42

PID

50 53 40 63

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

44

47 52 53 50

55

58 59 61

38 39

48 43 46 54

57 56

60

Freon 113 included (peak 8)

59

64 58

24
10

24.5

25

61

37 66 3 11 17 33 35 7 6 65 5 12 16 15 20 13 14 18 19 22 26 27 29 24 3132 34 38 37 9 30 23 14 12 3 7 20 29 63 24 3132 4 8 25 62 28 36 45

22

23

24

25

26
64 37 66

11

21

PID
min. 5 10 15 20 25

ELCD
min.
GC_EV00416

23

10

15

20

25

20ppb in 5mL of RO water. Column: Confirmation column: Concentrator: Trap: Purge: Dry purge: Desorb preheat: Desorb: Bake: Interface: Transfer line: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane 1,1-dichloroethene Freon 113 allyl chloride methylene chloride trans-1,2-dichloroethene methyl tert-butyl ether 1,1-dichloroethane cis-1,2-dichloroethene

75m, 0.45mm ID, 2.55m Rtx-VGC (cat.# 19409) 75m, 0.45mm ID, 2.55m Rtx-VRX (cat.# 19309) Tekmar LSC-3000 Purge and Trap Vocarb 3000 11 min. @ 40mL/min. 1 min. @ 40mL/min. (MCS by-passed with Silcosteel tubing [cat.# 21035]) 245C 250C for 2 min. 260C for 8 min. direct 0.32mm ID Siltek tubing 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 2,2-dichloropropane bromochloromethane chloroform carbon tetrachloride 1,1,1-trichloroethane 1,1-dichloropropene benzene 1,2-dichloroethane fluorobenzene (SS) trichloroethene dibromomethane 1,2-dichloropropane bromodichloromethane 1-bromo-2-chloroethane (SS) 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42.

GC: Oven temp.: Carrier gas: Detectors:

Finnigan 9001 35C (hold 4 min.) to 75C @ 3C/min. (hold 2 min.) to 175C @ 21C/min. to 205C @ 35C/min. (hold 5 min.) helium 11mL/min., constant pressure Adjust dichlorodifluoromethane to a retention time of 2.28 min. @ 35C on the Rtx-VGC column. Gold Tandem PID/HALL 2000 PID: makeup 7mL/min., purge 7mL/min., set @ 0.35mV, base temp. 200C. ELCD Hall 2000: RxnGas 25mL/min., RxnTemp. 940C, propanol flow 470L/min. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56.

cis-1,3-dichloropropene toluene tetrachloroethene trans-1,3-dichloropropene 1,1,2-trichloroethane dibromochloromethane 1,3-dichloropropane 1,2-dibromoethane 1-chloro-3-fluorobenzene (SS) chlorobenzene ethylbenzene 1,1,1,2-tetrachloroethane m-xylene p-xylene

o-xylene styrene bromoform isopropylbenzene bromobenzene n-propylbenzene 1,1,2,2-tetrachloroethane 2-chlorotoluene 1,2,3-trichloropropane 1,3,5-trimethylbenzene 4-chlorotoluene tert-butylbenzene 1,2,4-trimethylbenzene sec-butylbenzene

57. 58. 59. 60. 61. 62. 63. 64. 65. 66.

p-isopropyltoluene 1,3-dichlorobenzene 1,4-dichlorobenzene n-butylbenzene 1,2-dichlorobenzene 1,2-dibromo-3-chloropropane hexachlorobutadiene 1,2,4-trichlorobenzene naphthalene 1,2,3-trichlorobenzene

Acknowledgement: Finnigan 9001 GC, Gold Tandem Photoionization/HALL 2000 Electrolytic Conductivity Detector provided courtesy of Thermo Finnigan GC & GC/MS Division, 2215 Grand Avenue Pkwy, Austin, Texas 78728

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Volatiles
Volatile Organics US EPA Method 8021 Rtx-VRX
Excellent confirmation column to Rtx-VGC. Primary analysis shown on page 530. Rtx-VRX 75m, 0.45mm ID, 2.55m (cat.# 19309)

531

restek innovation!
41 42

PID

41 42 52 56,58 47 53 50 44 48 55 61 57 60 54 39 46 43 59

35C starting temperature for better resolution of earlyeluting compounds.


10

63 40 59

Freon 113 included (peak 8)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

49 58 31

61

3 24,27 44 5 17 8,9 51 64 66

38

37

43 38 6 1 39 65 2 13 16 7 11 14 15 20 28 63 4 25 30 23 24 7 12 14 20 29 32 31 34 36 62 37 22 33 19 18 26 29 32 35 53 45 50 38

31

20.0

22.5

25.0

64 66 37

47

11

21

PID
3 9

ELCD

23

min.

10

15

20

25

min. GC_EV00417

10

15

20

25

30

20ppb in 5mL of RO water. Column: Primary column: Concentrator: Trap: Purge: Dry purge: Desorb preheat: Desorb: Bake: Interface: Transfer line: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane 1,1-dichloroethene Freon 113 allyl chloride methylene chloride trans-1,2-dichloroethene methyl tert-butyl ether 1,1-dichloroethane cis-1,2-dichloroethene 2,2-dichloropropane bromochloromethane chloroform

75m, 0.45mm ID, 2.55m Rtx-VRX (cat.# 19309) 75m, 0.45mm ID, 2.55m Rtx-VGC (cat.# 19409) Tekmar LSC-3000 Purge and Trap Vocarb 3000 11 min. @ 40mL/min. 1 min. @ 40mL/min. (MCS by-passed with Silcosteel tubing [cat.# 21035]) 245C 250C for 2 min. 260C for 8 min. direct 0.32mm ID Siltek tubing 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. carbon tetrachloride 1,1,1-trichloroethane 1,1-dichloropropene benzene 1,2-dichloroethane fluorobenzene (SS) trichloroethene dibromomethane 1,2-dichloropropane bromodichloromethane 1-bromo-2-chloroethane (SS) cis-1,3-dichloropropene toluene tetrachloroethene trans-1,3-dichloropropene 1,1,2-trichloroethane dibromochloromethane

GC: Oven temp.: Carrier: Detectors:

Finnigan 9001 35C (hold 4 min.) to 75C @ 3C/min. (hold 2 min.) to 175C @ 21C/min. to 205C @ 35C/min. (hold 5 min.) helium 11mL/min., constant pressure Adjust dichlorodifluoromethane to a retention time of 2.28 min. @ 35C on the Rtx-VGC column. Gold Tandem PID/HALL 2000 PID: makeup 7mL/min., purge 7mL/min., set @ 0.35mV, base temp. 200C. ELCD Hall 2000: RxnGas 25mL/min., RxnTemp. 940C, propanol flow 470L/min.

35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51.

1,3-dichloropropane 1,2-dibromoethane 1-chloro-3-fluorobenzene (SS) chlorobenzene ethylbenzene 1,1,1,2-tetrachloroethane m-xylene p-xylene o-xylene styrene bromoform isopropylbenzene bromobenzene n-propylbenzene 1,1,2,2-tetrachloroethane 2-chlorotoluene 1,2,3-trichloropropane

52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66.

1,3,5-trimethylbenzene 4-chlorotoluene tert-butylbenzene 1,2,4-trimethylbenzene sec-butylbenzene p-isopropyltoluene 1,3-dichlorobenzene 1,4-dichlorobenzene n-butylbenzene 1,2-dichlorobenzene 1,2-dibromo-3-chloropropane hexachlorobutadiene 1,2,4-trichlorobenzene naphthalene 1,2,3-trichlorobenzene

Acknowledgement: Finnigan 9001 GC, Gold Tandem Photoionization/HALL 2000 Electrolytic Conductivity Detector provided courtesy of Thermo Finnigan GC & GC/MS Division, 2215 Grand Avenue Pkwy, Austin, Texas 78728

Phone: 800-356-1688 or 814-353-1300 www.restek.com

532

Volatiles
Volatile Organics US EPA Method 8021B Expanded List Rtx-VGC
Primary column, dual-column analysis. Confirmation analysis shown on page 533.
45 46

PID
66,67

Column: Confirmation column: Conc.: Concentrator: Trap: Purge: Dry purge: Desorb preheat: Desorb: Bake: Interface: GC: Carrier gas: Oven temp.:

57

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

49 52 55 53 48 51 47 58 61

64

65

68 63 59 62

Detectors:

42 43

75m, 0.45mm ID, 2.55m Rtx-VGC (cat.# 19409) 75m, 0.45mm ID, 2.55m Rtx-502.2 (cat.# 10986) 10ppb in 5mL of RO water Tekmar LSC-3000 Purge and Trap Vocarb 3000 11 min. @ 40mL/min. 1 min. @ 40mL/min. (MCS bypassed using Silcosteel tubing) 245C, Flow 10mL/min. 250C for 2 min. 260C for 8 min. direct using 0.32mm ID Siltek transfer line Finnigan 9001 helium @ ~10mL/min. constant pressure Adjust dichlorodifluoromethane to a retention time of 2.40 min. @ 45C on the Rtx-VGC column. 45C (hold 4 min.) to 70C @ 2C/min. to 210C @ 20C/min. (hold 10 min.) Gold Tandem PID/HALL 2000 PID: makeup 7mL/min., purge 7mL/min., set @ 0.35mV base temp. 200C. Hall 2000: RxnGas 25mL/min., RxnTemp. 940C, propanol flow 470L/min.

54 56

please note
see page 533 for peak identifications.
20.0 20.5 21.0 21.5 22.0 22.5 23.0 23.5 24.0
52 55

ELCD

58

Rtx-VGC 75m, 0.45mm ID, 2.55m (cat.# 19409)

22.1 22.2 22.3 22.4 22.5 22.6 22.7 22.8

44

72 target compounds
16 17 73 3 6 16 13 70 72 74 75 71 76 25 27 18 24 3 10 7 15 33,34 9 28 35 36 37 1 4 11 29 69 2 5 22 18 7,8 20 19 24 30 31 33,34 32 50 41 42 47 70 66 23 26 9 13 28 39 21 37 12 36 40 38 65 68 64 74 60 71

72

14

PID
min.

ELCD
10 15 20 25
GC_EV00421

27

min.

10

15

20

25

Acknowledgement: Finnigan 9001 GC, Gold Tandem Photoionization/HALL 2000 Electrolytic Conductivity Detector provided courtesy of Thermo Finnigan GC & GC/MS Division, 2215 Grand Avenue Pkwy, Austin, Texas 78728

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Volatiles
Volatile Organics US EPA Method 8021B Expanded List Rtx-502.2
Confirmation column to Rtx-VGC. Primary analysis shown on page 532.
Column: Primary column: Conc.: Concentrator: Trap: Purge: Dry purge: Desorb preheat: Desorb: Bake: Interface: GC: Carrier gas: Oven temp.: Detectors: 75m, 0.45mm ID, 2.55m Rtx-502.2 (cat.# 10986) 75m, 0.45mm ID, 2.55m Rtx-VGC (cat.# 19409) 10 ppb in 5mL of RO water Tekmar LSC-3000 Purge and Trap Vocarb 3000 11 min. @ 40mL/min. 1 min. @ 40mL/min. (MCS bypassed using Silcosteel tubing) 245C, Flow 10mL/min. 250C for 2 min. 260C for 8 min. direct using 0.32 mm ID Siltek transfer line Finnigan 9001 helium @ ~10mL/min. constant pressure Adjust dichlorodifluoromethane to a retention time of 2.40 min. @ 45C on the Rtx-VGC column. 45C (hold 4 min.) to 70C @ 2C/min. to 210C @ 20C/min. (hold 10 min.) Gold Tandem PID/HALL 2000 PID: makeup 7mL/min., purge 7mL/min., set @ 0.35mV base temp. 200C. Hall 2000: RxnGas 25mL/min., RxnTemp. 940C, propanol flow 470L/min.

533

45 46

55,57

PID

48,49 52

59,61 58 64 65

43 42 51 47

53 63 62 67

68

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

66

min.

22.5

25.0

54 44

restek innovation!
Rtx-502.2 75m, 0.45mm ID, 2.55m (cat.# 10986)

36,40

Acknowledgement: Finnigan 9001 GC, Gold Tandem Photoionization/HALL 2000 Electrolytic Conductivity Detector provided courtesy of Thermo Finnigan GC & GC/MS Division, 2215 Grand Avenue Pkwy, Austin, Texas 78728
38 3

56

71 64 65 60 68

5 12 2 73 10,11 26 1 70 16 35 13 25 14 7,9 18 24 3 15 27 37 28 34 33 36 72 74 71 75 76 4
10, 11

6 13 19,18 21 34 28

37 39 42

58 55 50

72

74

7,9 17

16 23 20

22 24 32 30 31

41 47 52 66

70

69 29

PID

ELCD
20 25 30 GC_EV00422 min. 5 10

27

33

min.

10

15

15

20

25

30

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane 1,1-dichloroethene Freon 113 chloromethyl methyl ether iodomethane (40ppb) allyl chloride methylene chloride trans-1,2-dichloroethene methyl tert-butyl ether tert-butyl alcohol (40ppb) chloroprene 1,1-dichloroethane cis-1,2-dichloroethene 2,2-dichloropropane

20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

bromochloromethane chloroform carbon tetrachloride 1,1,1-trichloroethane 1,1-dichloropropene benzene 1,2-dichloroethane fluorobenzene (SS) trichloroethene dibromomethane 1,2-dichloropropane bromodichloromethane 1-bromo-2-chloroethane (SS) 2-chloroethyl vinyl ether cis-1,3-dichloropropene toluene tetrachloroethene trans-1,3-dichloropropene 1,1,2-trichloroethane

39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57.

dibromochloromethane 1,3-dichloropropane 1,2-dibromoethane chlorobenzene ethylbenzene 1,1,1,2-tetrachloroethane m-xylene p-xylene 1-chloro-2-fluorobenzene (SS) o-xylene styrene bromoform isopropylbenzene bromobenzene n-propylbenzene 1,1,2,2-tetrachloroethane 2-chlorotoluene 1,2,3-trichloropropane 1,3,5-trimethylbenzene

58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76.

4-chlorotoluene tert-butylbenzene pentachloroethane 1,2,4-trimethylbenzene sec-butylbenzene p-isopropyltoluene 1,3-dichlorobenzene 1,4-dichlorobenzene benzyl chloride n-butylbenzene 1,2-dichlorobenzene 1,2-dibromo-3-chloropropane 2-bromo-1-chlorobenzene (SS) hexachlorobutadiene 1,2,4-trichlorobenzene naphthalene 1,2,3-trichlorobenzene 2-methylnaphthalene (40ppb) 1-methylnaphthalene (40ppb)

Phone: 800-356-1688 or 814-353-1300 www.restek.com

534

Volatiles
Volatile Organics US EPA Method 502.2 Rtx-502.2

for more info


A confirmational analysis can be found on www.restek.com/chromatograms Search for chromatogram number GC_EV00006
54/55 69 17

14

16

25

Rtx-502.2 75m, 0.45mm ID, 2.55m (cat.# 10986)


14 67 42/43 10 61 53 23 46 31 39 52 41 45 48 59 71 57 69 70 63 53 38 2 4 7 24 9 29 66 44 47 63 5 6 8 16 20 32 30 36 44 60 24 25 56 58 65 64 68 1 3 50 28 37 39 56 49 51 54 67 62 12 15 13 18 22 21 26 19 20 32 35 36 27 33,34 30 40 68 62 61 65 71

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

12

11 3

PID
min. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 5

ELCD
10 15 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 20 25 30 min.
GC_EV00005

10

15

20

25

30

dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane Freon 113 1,1-dichloroethene allyl chloride methylene chloride methyl tert-butyl ether trans-1,2-dichloroethene 1,1-dichloroethane chloroproprene (40ppb) 2,2-dichloropropane cis-1,2-dichloroethene chloroform bromochloromethane 1,1,1-trichloroethane 1,1-dichloropropene carbon tetrachloride 1,2-dichloroethane benzene fluorobenzene (SS) trichloroethene 1,2-dichloropropane bromodichloromethane dibromomethane 2-chloroethyl vinyl ether cis-1,3-dichloropropene toluene trans-1,3-dichloropropene 1,1,2-trichloroethane 2-bromo-1-chloropropane (IS) 1,3-dichloropropane tetrachloroethene

dibromochloromethane 1,2-dibromoethane chlorobenzene 1,1,1,2-tetrachloroethane ethyl benzene m-xylene p-xylene 1-chloro-2-fluorobenzene (IS) o-xylene styrene bromoform isopropyl benzene 1,4-dichlorobutane (SS) 1,1,2,2-tetrachloroethane 1,2,3-trichloropropane n-propylbenzene bromobenzene 2-chlorotoluene 1,3,5-trimethylbenzene 4-chlorotoluene tert-butylbenzene 1,2,4-trimethylbenzene sec-butylbenzene p-isopropyltoluene 1,3-dichlorobenzene 1,4-dichlorobenzene benzyl chloride n-butylbenzene 1,2-dichlorobenzene 1,2-bromo-3-chloropropane 4-bromo-1-chlorobenzene (SS) 1,2,4-trichlorobenzene hexachlorobutadiene naphthalene 1,2,3-trichlorobenzene

Column: Conc.: Inj.:

75m, 0.45mm ID, 2.55m Rtx-502.2 (cat.# 10986). 20ppb in 5mL of RO water (unless otherwise noted, peak 14). a combination of the following reference materials was used: 502.2 Cal2000 MegaMix (cat.# 30431) 502.2 Calibration Mix #1A (cat.# 30439) 502.2 Internal Standard Mix #2 (cat.# 30041) 1-chloro-2-fluorobenzene (cat.# 30040) 4-bromochlorobenzene (cat.# 30230) 2-chlorethyl vinyl ether (cat.# 30265) 1,4-dichlorobutane (cat.# 30227) MTBE (cat.# 30402) and custom mixtures of Freon 113, allyl chloride, chloroprene, and benzyl choride. Tekmar LSC-3000 Purge and Trap Vocarb 3000 11 min. @ 40mL/min. 1 min. @ 40mL/min. (MCS off) 245C 250C for 2 min. 260C for 8 min. Finnigan 9001 helium, 9mL/min. constant pressure 35C (hold 6 min.) to 115C @ 11C/min. (hold 7 min.) to 130C @ 7C/min. (no hold), to 220C @ 9.2C/min. (hold 4 min.) Gold Tandem PID/HALL 2000 PID: makeup 7mL/min., purge 7mL/min. set @ 0.35mV, base temp. 200C Hall 2000: Rxn gas 25mL/min., Rxn temp. 940C propanol flow 470L/min.

Concentrator: Trap: Purge: Dry purge: Desorb preheat: Desorb: Bake: GC: Carrier gas: Oven temp.: Detectors:

Acknowledgement: Finnigan 9001 GC, Gold Tandem Photoionization/HALL 2000 Electrolytic Conductivity Detector provided courtesy of Thermo Finnigan GC & GC/MS Division, 2215 Grand Avenue Pkwy, Austin, Texas 78728

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Volatiles
Volatile Organics US EPA Method 601/602 Rtx-502.2
Confirmation column to Rtx-VGC.

535

for more info


The primary analysis (Rtx-VGC) can be found on www.restek.com/chromatograms Search for chromatogram number GC_EV00420
38 34

36 35

Rtx-502.2 75m, 0.45mm ID, 2.55m (cat.# 10986)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

29 30

37

33

Best resolution for Method 601 / 602

3 13 8 6 9 15 11 20 21 12 23 26 17 27 14 19

25 36

31 2 1

35 37

16

28 32 31 29

9 7 18 19 22 7 10 23 26 24 25 4

38

22

PID
min.

18

ELCD
5 10 15 20 min.
GC_EV00540

10

15

20

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15 16. 17. 18. 19. 20.

dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane 1,1-dichloroethene methylene chloride trans-1,2-dichloroethene methyl tert-butyl ether 1,1-dichloroethane bromochloromethane chloroform carbon tetrachloride 1,1,1-trichloroethane benzene 1,2-dichloroethane fluorobenzene trichloroethene 1,2-dichloropropane

21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

bromodichloromethane 2-chloroethyl vinyl ether cis-1,3-dichloropropene toluene tetrachloroethene trans-1,3-dichloropropene 1,1,2-trichloroethane dibromochloromethane chlorobenzene ethylbenzene 1-chloro-2-fluorobenzene bromoform 1,4-dichlorobutane 1,1,2,2-tetrachloroethane 1,3-dichlorobenzene 1,4-dichlorobenzene 1,2-dichlorobenzene 4-bromo-1-chlorobenzene

Column: Primary column: Conc.: Concentrator: Trap: Purge: Dry purge: Desorb preheat: Desorb: Bake: Interface: Transfer line: Gas chromatograph: Carrier gas: Dead time: Oven temp.: Detectors:

Acknowledgement: Finnigan 9001 GC, Gold Tandem Photoionization/HALL 2000 Electrolytic Conductivity Detector provided courtesy of Thermo Finnigan GC & GC/MS Division, 2215 Grand Avenue Pkwy, Austin, Texas 78728

75m, 0.45mm ID, 2.55m Rtx-502.2 (cat.# 10986) 75m, 0.45mm ID, 2.55m Rtx-VGC (cat.# 19409) 10ppb in 5mL of RO water (see below) Tekmar LSC3100 Purge and Trap Vocarb 3000 11 min. @ 40mL/min. 1 min. @ 40mL/min. 245C 250C for 2 min. 260C for 8 min. direct connection from concentrator to column Silcosteel Tubing Finnigan 9001 helium @ ~10mL/min. constant pressure 2.04 min. Adjust dichlorodifluoromethane to a retention time of 2.47 min. @ 40C on the Rtx-VGC column. 40C (hold 2 min.) to 58C @ 4C/min. to 90C @ 10C/min. (hold 5 min.) to 220C @ 40C/min. (hold 5 min.) Gold Tandem PID/Hall 2000 PID: makeup 7mL/min., purge 7mL/min., set @ 0.35mV base temp.: 200C. Hall 2000: RxnGas 25mL/min., Rxn Temp. 940C, propanol flow 470L/min. cat.# 30042 30021 30022 30402 30227 30030 30040 30230 30225

Reference Standard 502.2 mix#1 624 cal mix #2 624 cal mix #3 MTBE 1,4-dichlorobutane fluorobenzene 1-chloro-2-fluorobenzene 4-bromo-1-chlorobenzene bromochloromethane

Phone: 800-356-1688 or 814-353-1300 www.restek.com

536

Volatiles
Volatile Organics US EPA Method 8021 Rtx-VRX
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66.
39/40

PID
55 56

Good choice for waste water analysis.

dichlorodifluoromethane See page 530 for recommended chloromethane drinking water analysis. vinyl chloride bromomethane 52 chloroethane trichlorofluoromethane 62 1,1-dichloroethene methylene chloride 48 51 42 Freon113 54 57 50 trans-1,2-dichloroethene 75m, 0.45mm ID, 2.55m Rtx -VRX (cat.# 19309) methyl tert-butyl ether 45 Conc.: 20ppb in 5mL of RO water (see below) 49 59 37 1,1-dichloroethane 58 60 Concentrator: Tekmar LSC-3000 Purge and Trap cis-1,2-dichloroethene Trap: Vocarb 3000 38 bromochloromethane Purge: 11 min. @ 40mL/min. 47 53 chloroform Dry purge: 1 min. @ 40mL/min. (MCS by2,2-dichloropropane passed with Silcosteel tubing) 1,2-dichloroethane Desorb preheat: 245C 1,1,1-trichloroethane Desorb: 250C for 2 min. Bake: 260C for 8 min. 1,1-dichloropropene Interface: direct carbon tetrachloride Transfer line: 0.32mm ID Siltek tubing benzene GC: Finnigan 9001 fluorobenzene (SS) GC program: 35C (hold 12 min.) to 60C dibromomethane @ 5C/min. (hold 1 min.) to 1,2-dichloropropane 220C @ 17C/min. (hold 3 min.) trichloroethene Carrier gas: helium 9mL/min. bromodichloromethane Detectors: Gold Tandem PID/HALL 2000 2-chloroethyl vinyl ether PID: makeup 7mL/min., purge cis-1,3-dichloropropene 7mL/min, set @ 0.35mV base trans-1,3-dichloropropene temp. 200C. 22.5 25.0 27.5 1,1,2-trichloroethane ELCD Hall 2000: RxnGas 25mL/min., toluene RxnTemp.: 940C, 1,3-dichloropropane propanol flow 470L/min. dibromochloromethane Reference Standard cat.# 1,2-dibromoethane 30431 502.2 Cal2000 MegaMix tetrachloroethene 502.2 Calibration Mix#1A 30439 1,1,1,2-tetrachloroethane 4-bromochlorobenzene 30230 chlorobenzene 2-chloroethyl vinyl ether 30265 ethyl benzene 1,4-dichlorobutane 30227 m-xylene fluorobenzene 30030 p-xylene methyl-tert-butyl-ether 30402 bromoform Freon 113 custom styrene 1,4-dichlorobutane (SS) 1,1,2,2-tetrachloroethane 65 35 36 o-xylene 1,2,3-trichloropropane isopropyl benzene bromobenzene n-propylbenzene 2-chlorotoluene 4-chlorotoluene 1,3,5-trimethylbenzene 57 63 8 tert-butylbenzene 66 1,2,4-trimethylbenzene 56 sec-butylbenzene 59 1,3-dichlorobenzene 30 1,4-dichlorobenzene 7 3 10 p-isopropyltoluene 37 44 15 25 5 32 1,2-dichlorobenzene 2 12 n-butylbenzene 29 1 13 6 62 28 1,2-bromo-3-chloropropane 33 4-bromo-1-chlorobenzene (SS) 51 26 50 24 20 1,2,4-trichlorobenzene 46 naphthalene 31 63 14 16 18 64 hexachlorobutadiene 43 34 17 19 66 9 1,2,3-trichlorobenzene 41 48
65 10 21 35 4 23 22 19 25 29 27 28

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

PID
3 7 11

13

ELCD
22

27

61

min.

10

15

20

25
GC_EV00001

min.

10

15

20

25

Acknowledgement: Finnigan 9001 GC, Gold Tandem Photoionization/HALL 2000 Electrolytic Conductivity Detector provided courtesy of Thermo Finnigan GC & GC/MS Division, 2215 Grand Avenue Pkwy, Austin, Texas 78728

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Volatiles
Volatile Organics US EPA Method OLC 03.2 Rtx-VMS

537

Fast analysis time

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00681

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.

dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane 1,1-dichloroethene carbon disulfide Freon 113 methylene chloride acetone trans-1,2-dichloroethene methyl acetate methyl tert-butyl ether

15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

1,1-dichloroethane cis-1,2-dichloroethene cyclohexane bromochloromethane chloroform carbon tetrachloride 1,1,1-trichloroethane 2-butanone benzene 1,2-dichloroethane methyl cyclohexane trichloroethene 1,4-difluorobenzene 1,2-dichloropropane

29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42.

bromodichloromethane cis-1,3-dichloropropene toluene tetrachloroethene 4-methyl-2-pentanone trans-1,3-dichloropropene 1,1,2-trichloroethane dibromochloromethane 1,2-dibromoethane 2-hexanone chlorobenzene-d5 chlorobenzene ethylbenzene m-xylene

43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55.

p-xylene o-xylene styrene bromoform isopropylbenzene 1,1,2,2-tetrachloroethane 1,3-dichlorobenzene 1,4-dichlorobenzene-d4 1,4-dichlorobenzene 1,2-dichlorobenzene 1,2-dibromo-3-chloropropane 1,2,4-trichlorobenzene 1,2,3-trichlorobenzene

Rtx-VMS 20m, 0.18mm ID, 1.0m (cat.# 49915) Sample: Components at 10ppb (50ppb ketones) in 5mL RO water OLC 03.2 VOA MegaMix, cat.# 30492 502.2 Calibration Mix #1 (gases), cat.# 30042 VOA Calibration Mix #1 (ketones), cat.# 30006 L/C VOA Internal Standard Mix, cat.# 30091 Concentrator: Tekmar 3100 Purge and Trap Trap: Vocarb 3000 Purge: 11 min. @ 40mL/min. (ambient temperature) Dry purge: 1 min. @ 40mL/min. (MCS bypassed) Desorb preheat: 245C Desorb: 250C for 1 min. @ 40mL/min.

Bake: Interface:

260C for 8 min. 30:1 split using 1/16" Silcosteel tee (cat.# 20513) & 0.3m of 0.25mm ID fused silica tubing for split line Carrier gas: 24psi helium, constant pressure Flow rate: 1.3 mL/min. @ 45C Dead time: 0.77 min. @ 45C Oven temp.: 45C (hold 4 min.) to 225C @ 32C/min. (hold 2 min.) Det: Agilent 5971A GC/MS w/ K&M electron multiplier Transfer line temp.: 280C Scan range: 35260 amu Tune: PFTBA/BFB Ionization: EI

Phone: 800-356-1688 or 814-353-1300 www.restek.com

538

Volatiles
Volatile Organics US EPA Method 8260 (80ppb Standard) Rtx-VMS

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00686

GC_EV00685

Rtx-VMS, 30m, 0.25mm ID, 1.4m (cat.# 19915) Calibration, internal standard, surrogate standard mixes (cat.# 30475B, 30465, 30006, 30240, 30074) Purge and trap conditions: Trap: #10 (Tenax/silica gel/carbon molecular sieve) Purge Time: 11 min. Purge Flow Rate: 38mL/min. Desorb Flow Rate: 32mL/min. Desorb Time: 1.0 min. Bake Time: 10 min. Sample Size: 10mL Water Management: 110C purge, 0C desorb, 240C bake Split Ratio: 1:25 Temperatures: Sample: 40C Trap: 20C purge, 190C desorb, 210C bake 6-Port Valve: 110C

Column: Sample:

Transfer Line: Sparge Mount: Desorb Preheat: Valve Manifold: Other Conditions: Chromatography: Inj. temp.: Carrier gas: Flow rate: Dead Time: Oven temp.:

110C 45C 150C 50C pre-purge, pre-heat, dry purge OFF

250C helium, constant flow 1.3 mL/min. 1.47 min. @ 35C 35C (hold 7 min.) to 90C @ 4C/min.(no hold) to 220C @ 45C/min. (hold 1 min.). Det.: Agilent 5971A GC/MS Transfer line temp.: 280C Scan range: 35-260 amu Tune: PFTBA/BFB

*carbon dioxide 1. dichlorodifluoromethane 2. chloromethane 3. vinyl chloride 4. bromomethane 5. chloroethane 6. trichlorofluoromethane 7. diethylether 8. 1,1-dichloroethene 9. carbon disulfide 10. Freon 113 11. iodomethane 12. allyl chloride 13. methylene chloride 14. acetone 15. trans-1,2-dichloroethene 16. methyl-d3-tert-butyl-ether 17. methyl acetate 18. methyl-tert-butyl-ether 19. tert-butyl alcohol 20. acetonitrile 21. diisopropyl ether 22. chloroprene 23. 1,1-dichloroethane 24. acrylonitrile 25. ethyl-tert-butyl ether

26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51.

cis-1,2-dichloroethene 2,2-dichloropropane bromochloromethane chloroform carbon tetrachloride tetrahydrofuran methyl acrylate 1,1,1-trichloroethane dibromofluoromethane 1,1-dichloropropene 2-butanone benzene propionitrile methacrylonitrile 1,2-dichloroethane-d4 pentafluorobenzene tert-amyl-methyl ether 1,2-dichloroethane isobutyl alcohol trichloroethene 1,4-difluorobenzene dibromomethane 1,2-dichloropropane bromodichloromethane methyl methacrylate cis-1,3-dichloropropene

52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77.

2-chloroethyl vinyl ether toluene-d8 toluene 2-nitropropane tetrachloroethene 2-bromo-1-chloropropane 4-methyl-2-pentanone trans-1,3-dichloropropene 1,1,2-trichloroethane ethyl methacrylate dibromochloromethane 1,3-dichloropropane 1,2-dibromoethane 2-hexanone chlorobenzene-d5 chlorobenzene ethylbenzene 1,1,1,2-tetrachloroethane m-xylene p-xylene o-xylene bromoform stryrene isopropylbenzene 4-bromo-1-fluorobenzene (SS) bromobenzene

78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 88. 89. 90. 91. 92. 93. 94. 95. 96. 97. 98. 99. 100. 101. 102.

cis-1,4-dichloro-2-butene 1,4-dichlorobutane n-propylbenzene 1,1,2,2-tetrachloroethane 2-chlorotoluene 1,2,3-trichloropropane 1,3,5-trimethylbenzene trans-1,4-dichloro-2-butene 4-chlorotoluene tert-butylbenzene pentachloroethane 1,2,4-trimethylbenzene sec-butylbenzene p-isopropyltoluene 1,3-dichlorobenzene 1,4-dichlorobenzene-d4 1,4-dichlorobenzene n-butylbenzene 1,2-dichlorobenzene 1,2-dibromo-3-chloropropane nitrobenzene hexachlorobutadiene 1,2,4-trichlorobenzene naphthalene 1,2,3-trichlorobenzene

Acknowledgments: Purge & trap courtesy of O.I. Analytical.

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Volatiles
Volatile Organics US EPA Method 8240 (8260 Short List) Rtx-VMS
Instrumentation & Conditions Common to BOTH RUNS Carrier gas: 1.3mL/min. @ constant flow Concentrator: Tekmar LSC-3000 Purge and Trap Trap: Vocarb 3000 (type K) Purge: 11 min. @ 40mL/min. (ambient temp.) Dry purge: 1 min. @ 40mL/min. (MCS bypass) Desorb preheat: 245C Desorb: 250C for 2 min., flow 26mL/min. Bake: 260C for 8 min. Interface to GC: transfer line 0.32mm ID Siltek fused silica 1:20 split at injection port w/ 1mm ID liner. GC: HP 6890 Detector: HP 5973 MSD
8-9 12 11 14 3 1 min. 2.00 3.00 4 5 6 7 4.00 5.00 6.00 10 13 17 7.00 8.00 9.00 15 16 53-56

539

Rtx-VMS 30m, 0.25mm ID, 1.40m (cat.# 19915)

restek innovation!
Standard wastewater analysis (35300amu)

44-46

57,58

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

18 21,22

25 26-27 28,29

31,32

36,37 41 42

47 51 59,60 64 65,66 62,63 69 70 68 72 67 61 71 73 11.00 12.00 13.00 14.00 15.00

19 20

23 24

34 33

35 39 38 40 43

30

48 49 52 50

10.00

Top chromatogram: Oven temp.: 40C (hold 4 min.) to 90C @ 16C/min. (no hold) to 210C @ 32C/min. (hold 5 min.) Adjust dichlorodifluoromethane to a retention time of 2.27 min. @ 40C. MS Scan Range: 35-300amu compound concentrations, by mix: (in 5mL of RO water) Compounds at 100ppb (cat.# 30213, 30004, 30006, 30011, 30042) Alcohols at 1ppm (cat.# 30214) except 2-chloroethanol at 10ppm vinyl acetate at 500ppb (cat.#30216) 8240 Nitrile Mix at 200ppb (cat.# 30215) 8240 Mix 1A at 300ppb (cat.# 30217) 8240 Mix 2A at 500ppb (cat.# 30218)
methanol 8,9 3 25-27 31,32

Bottom chromatogram: Oven temp.: 45C (hold 4 min.) to 110C @ 19C/min. (hold 5 min.) to 220C @ 32C/min. (hold 5 min.) Adjust dichlorodifluoromethane to 2.23 min. @ 45C. MS Scan Range: 29-260amu, for 2-chloroethanol response compound concentrations, by mix: (in 5mL of RO water) Compounds at 100ppb (cat.# 30213, 30004, 30006, 30011, 30042) Alcohols at 1ppm (cat.# 30214) (see MS scan) vinyl acetate at 100ppb (cat.# 30216) 8240 Nitrile Mix at 400ppb (cat.# 30215) 8240 Mix 1A at 300ppb (cat.# 30217) 8240 Mix 2A at 500ppb (cat.# 30218)

Scan range 29260amu, for detecting 2-chloroethanol


57,58

47 4 2 11 6 1 17,18 28, 29 41 42 45,46 44 5 36

53-55 60,61

slower run resolves these

67

70

59 56

69 68 72

38 34 39 33 48 62 63 40 50 51

65 66

12 14 10 13

16 15

22, 20 19 23 21 24

30 35

64 49 71 73 52 43

37

min. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

2.00

3.00

4.00 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30.

5.00

6.00

7.00

8.00 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45.

dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane ethanol 1,1-dichloroethene carbon disulfide iodomethane allyl chloride methylene chloride acetone trans-1,2-dichloroethene 1,1-dichloroethane

acrylonitrile allyl alcohol vinyl acetate bromochloromethane chloroform carbon tetrachloride propargyl alcohol 1,1,1-trichloroethane 2-butanone benzene propionitrile methacrylonitrile 1,2-dichloroethane-d4 isobutyl alcohol 1,2-dichloroethane

9.00 10.00 GC_EV00426 trichloroethene 1,4-difluorobenzene dibromomethane 1,2-dichloropropane bromodichloromethane methyl methacrylate 1,4-dioxane 2-chloroethanol 2-chloroethyl vinyl ether cis-1,3-dichloropropene toluene-d8 toluene pyridine 4-methyl-2-pentanone tetrachloroethene

11.00 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60.

12.00

13.00

14.00

15.00 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73.

16.00

17.00

trans-1,3-dichloropropene ethyl methacrylate 1,1,2-trichloroethane dibromochloromethane 1,2-dibromoethane 2-hexanone 2-picoline chlorobenzene-D5 ethylbenzene chlorobenzene 1,1,1,2-tetrachloroethane m-xylene p-xylene o-xylene styrene

bromoform 4-bromo-1-fluorobenzene cis-1,4-dichloro-2-butene 1,1,2,2-tetrachloroethane 1,2,3-trichloropropane trans-1,4-dichloro-2-butene pentachloroethane 1,3-dichlorobenzene 1,4-dichlorobenzene benzyl chloride malononitrile 1,2-dichlorobenzene 1,2-dibromo-3-chloropropane

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540

Volatiles
Volatile Organics US EPA Method 8260B Rtx-VMS
60m, 0.25 mm ID, 1.40m Rtx-VMS (cat.# 19916) Conc.: 10ppb in 5mL of RO water (unless noted); ketones 2.5X Concentrator: Tekmar LSC-3100 Purge and Trap Trap: Vocarb 3000 (type K) Purge: 11 min. @ 40mL/min. (ambient temperature) Dry purge: 1 min. @ 40mL/min. Desorb preheat: 245C Desorb: 250C for 2 min., flow 26mL/min. Bake: 260C for 8 min. Interface: 0.53mm ID Silcosteel tubing transfer line 1:20 split at injection port. 1mm ID liner. Oven temp.: 60C (hold 2 min.) to 180C @ 12C/min. (hold 0 min.) to 225C @ 45C/min. (hold 6 min.) Carrier gas: helium @ ~1.3mL/min. constant flow Adjust dichlorodifluoromethane to a retention time of 4.03 min. @ 60C. Detector: Agilent 5973 MSD Scan range: 35-300amu 44-46
36-38 24,25 51 95 97

68,69

restek innovation!
60C starting temperature fast analyses fast cycles
79,80 83,84 86 82 85

64-67 73 75 76, 78 77 71 70 81 87

90

Reduce starting temperature to best focus the gases

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

88,89

96 91

41,42 13-15 11,12 23 22 29-33 34 39,40 28 49

55-56 57 59 54

93,94

17,18 19-21 7,8 27 26 16 1 3 2 45 9 6 10 35 47 43

50

58 72 74 61 60 52, 53 92

62

48

63

min. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25.

6 dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane ethanol (2500ppb) 1,1-dichloroethene carbon disulfide (40ppb) allyl chloride methylene chloride acetone trans-1,2-dichloroethene tert-butyl alcohol (100ppb) methyl tert-butyl ether diisopropyl ether 1,1-dichloroethane acrylonitrile vinyl acetate* allyl alcohol (250ppb) ethyl-tert-butyl ether* cis-1,2-dichloroethene 2,2-dichloropropane bromochloromethane chloroform 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50.

10
GC_EV00427

12 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75.

14 76. 77. 78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 88. 89. 90. 91. 92. 93. 94. 95. 96. 97.

16 1,1,2,2-tetrachloroethane bromobenzene 1,3,5-trimethylbenzene 2-chlorotoluene 1,2,3-trichloropropane 4-chlorotoluene tert-butylbenzene 1,2,4-trimethylbenzene pentachloroethane sec-butylbenzene p-isopropyltoluene 1,3-dichlorobenzene 1,4-dichlorobenzene-d4 (IS) 1,4-dichlorobenzene n-butylbenzene 1,2-dichlorobenzene 1,2-dibromo-3-chloropropane nitrobenzene (250ppb) hexachlorobutadiene 1,2,4-trichlorobenzene naphthalene 1,2,3-trichlorobenzene

ethyl acetate methyl acrylate propargyl alcohol (500ppb) dibromofluoromethane (SMC) tetrahydrofuran carbon tetrachloride 2-butanone 1,1,1-trichloroethane 1,1-dichloropropene pentafluorobenzene (IS) tert-amyl methyl ether benzene isobutyl alcohol (500ppb) 1,2-dichloroethane isopropyl acetate 1,4-difluorobenzene (SMC) trichloroethene dibromomethane bromodichloromethane 1,2-dichloropropane methyl methacrylate n-propyl acetate 2-chloroethanol (2500ppb) cis-1,3-dichloropropene toluene-d8 (SMC)

toluene 4-methyl-2-pentanone pyridine (250ppb) trans-1,3-dichloropropene ethyl methacrylate tetrachloroethene 1,1,2-trichloroethane dibromochloromethane 1,3-dichloropropane n-butyl acetate 1,2-dibromoethane 2-hexanone 2-picoline (250ppb) ethylbenzene chlorobenzene-D5 (IS) chlorobenzene 1,1,1,2-tetrachloroethane m-xylene p-xylene o-xylene styrene bromoform isopropylbenzene 4-bromo-1-fluorobenzene (SMC) n-propylbenzene

*Peaks 19 & 21 share an ion (43).

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Volatiles
Volatile Organics US EPA Method 8260B Rtx-VMS
79,80

541

restek innovation!
First choice for use with dual purge & traps1 EPA recommended surrogate used.

82,83 68,69 84 73 66,67 64,65 70 78 76 81

88,89 86 90

96

85 71,72 91 87 95 94 97

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

75 77

54,55 29-32 26-28 25 36 35 33,34 38 37 39 4 GC_EV00428 40 42 41 43 44 45 50 46 47 48 6 52 8 49 51 53 56 59 92 58 60


57

8 1

11 13 9 10

24 12 17

3 2 45

6 7

23 22 19-21 14 16 18 15

74 61
62, 63

93 10

min.

20m, 0.18 mm ID, 1.00m Rtx-VMS (cat.# 49914) Conc.: 10ppb in 5mL of RO water unless otherwise noted; ketones at 2.5X Concentrator: Tekmar LSC-3100 Purge and Trap Trap: Vocarb 3000 (type K) Purge: 11 min. @ 40mL/min. (ambient temperature) Dry purge: 1 min. @ 40mL/min. Desorb preheat: 245C Desorb: 250C for 2 min., flow 40mL/min. Bake: 260C for 8 min. Interface: 0.53mm ID Silcosteel tubing transfer line 1:40 split at injection port. 1mm ID liner. Oven temp.: 50C (hold 4 min.) to 100C @ 18C/min. (hold 0 min.) to 230C @ 40C/min. (hold 3 min.) Carrier gas: helium @ ~1.0mL/min. constant flow Adjust dichlorodifluoromethane to a retention time of 1.03 min. @ 50C. Detector: Agilent 5973 MSD Scan range: 35-300amu

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25.
1

dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane ethanol (2500ppb) 1,1-dichloroethene carbon disulfide (40ppb) allyl chloride methylene chloride acetone trans-1,2-dichloroethene methyl tert-butyl ether tert-butyl alcohol (100ppb) diisopropyl ether 1,1-dichloroethane acrylonitrile vinyl acetate allyl alcohol (250ppb) ethyl-tert-buyl ether cis-1,2-dichloroethene 2,2-dichloropropane bromochloromethane chloroform

26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50.

ethyl acetate carbon tetrachloride methyl acrylate propargyl alcohol (500ppb) dibromofluoromethane (SMC) tetrahydrofuran 1,1,1-trichloroethane 2-butanone 1,1-dichloropropene benzene pentafluorobenzene (IS) tert-amyl-methyl ether 1,2-dichloroethane isobutyl alcohol (500ppb) isopropyl acetate trichloroethene 1,4-difluorobenzene (SMC) dibromomethane 1,2-dichloropropane bromodichloromethane methyl methacrylate n-propyl acetate 2-chloroethanol (2500ppb) cis-1,3-dichloropropene toluene-d8 (SMC)

51. toluene 52. pyridine (250ppb) 53. tetrachloroethene 54. 4-methyl-2-pentanone 55. trans-1,3-dichloropropene 56. 1,1,2-trichloroethane 57. ethyl methacrylate 58. dibromochloromethane 59. 1,3-dichloropropane 60. 1,2-dibromoethane 61. n-butyl acetate 62. 2-hexanone 63. 2-picoline (250ppb) 64. chlorobenzene-D5 (IS) 65. chlorobenzene 66. ethylbenzene 67. 1,1,1,2-tetrachloroethane 68. m-xylene 69. p-xylene 70. o-xylene 71. stryrene 72. bromoform 73. isopropylbenzene 74. 4-bromo-1-fluorobenzene (SMC)

75. 76. 77. 78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 88. 89. 90. 91. 92. 93. 94. 95. 96. 97.

bromobenzene n-propylbenzene 1,1,2,2-tetrachloroethane 2-chlorotoluene 1,3,5-trimethylbenzene 1,2,3-trichloropropane 4-chlorotoluene tert-butylbenzene pentachloroethane 1,2,4-trimethylbenzene sec-butylbenzene p-isopropyltoluene 1,3-dichlorobenzene 1,4-dichlorobenzene-d4 (IS) 1,4-dichlorobenzene n-butylbenzene 1,2-dichlorobenzene 1,2-dibromo-3-chloropropane nitrobenzene (250ppb) hexachlorobutadiene 1,2,4-trichlorobenzene naphthalene 1,2,3-trichlorobenzene

A.L. Hilling and G. Smith, Environmental Testing & Analysis, 10(3), 15-19, 2001.

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542

Volatiles
Volatile Organics US EPA Method 8260B Rtx-VMS

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Reference Standard 8260B Calibration Mix #1* 502.2 Calibration Mix #1 (gases) VOA Calibration Mix #1 (ketones) 8260 Internal Standard Mix 8260 Surrogate Mix 8260 Acetate Mix California Oxygenates Mix Acrolein Mix Ethanol Mix Freon 114

cat.# 30475 30042 30006 30074 30073 30489 30465 30478 30466 30476

GC_EV00641

Rtx-VMS 40m, 0.18mm ID, 1.0m (cat.# 49915) Conc.: 5ppb each in 25mL of RO water Concentrator: Tekmar LSC-3100 Purge and Trap Trap: Vocarb 3000 Purge: 11 min. @ 40mL/min. Dry purge: 1 min. @ 40mL/min. (MCS by-passed with Silcosteel tubing, cat.# 21035) Desorb preheat: 245C Desorb: 2 min. @ 250C Desorb flow rate: 45mL/min. helium Bake: 8 min. @ 260C Interface: plumbed through injection port Transfer line: Silcosteel transfer line (cat.# 20591) Mount Temp: 40C

Column:

Split ratio: Inlet liner: Inj. temp.: Carrier gas: Linear velocity: Oven temp.: Detector: Source Temp.: Scan range: Ionization:

1:40 split Agilent Split 1mm Liner (cat.# 20972) 250C 1.1mL/min. helium, constant flow 32cm/sec. @ 40C 35C (hold 2 min.) to 60C @ 4C/min. (hold 0 min.) to 225C @ 40C/min. (hold 5 min.) 5973 GC/MS w/ turbomolecular pump 280C 35260amu EI

GC_EV00640

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23.

carbon dioxide dichlorodifluoromethane Freon 114 chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane ethanol diethyl ether 1,1-dichloroethene iodomethane carbon disulfide Freon 113 acrolein allyl chloride methylene chloride acetone trans-1,2-dichloroethene methyl acetate methyl tert-butyl ether tert-butyl alcohol acetonitrile

24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46.

diisopropyl ether chloroprene 1,1-dichloroethane acrylonitrile vinyl acetate** ethyl-tert-butyl ether** cis-1,2-dichloroethene 2,2-dichloropropane bromochloromethane chloroform carbon tetrachloride ethyl acetate methyl acrylate dibromofluoromethane tetrahydrofuran 1,1,1-trichloroethane 2-butanone 1,1-dichloropropene benzene propionitrile methacrylonitrile pentafluorobenzene tert-amyl-methyl ether

47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69.

1,2-dichloroethane isobutyl alcohol isopropyl acetate trichloroethene 1,4-difluorobenzene dibromomethane 1,2-dichloropropane bromodichloromethane methyl methacrylate n-propyl acetate 2-chloroethyl vinyl ether cis-1,3-dichloropropene toluene-d8 toluene 2-nitropropane tetrachloroethene 4-methyl-2-pentanone trans-1,3-dichloropropene 2-bromo-1-chloropropane 1,1,2-trichloroethane ethyl methacrylate dibromochloromethane 1,3-dichloropropane

70. 71. 72. 73. 74. 75. 76. 77. 78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 88. 89. 90. 91. 92.

1,2-dibromoethane n-butyl acetate 2-hexanone chlorobenzene-d5 chlorobenzene ethylbenzene 1,1,1,2-tetrachloroethane m-xylene p-xylene o-xylene styrene bromoform isopropylbenzene n-amyl acetate 4-bromo-1-fluorobenzene (ss) cis-1,4-dichloro-2-butene n-propylbenzene bromobenzene 1,4-dichlorobutane 1,1,2,2-tetrachloroethane 2-chlorotoluene 1,3,5-trimethylbenzene 1,2,3-trichloropropane

93. trans-1,4-dichloro-2-butene 94. 4-chlorotoluene 95. tert-butylbenzene 96. pentachloroethane 97. 1,2,4-trimethylbenzene 98. sec-butylbenzene 99. p-isopropyltoluene 100. 1,3-dichlorobenzene 101. 1,4-dichlorobenzene-d4 102. 1,4-dichlorobenzene 103. n-butylbenzene 104. 1,2-dichlorobenzene 105. 1,2-dibromo-3-chloropropane 106. nitrobenzene 107. hexachlorobutadiene 108. 1,2,3-trichlorobenzene 109. naphthalene 110. 1,2,4-trichlorobenzene

*2-Chloroethanol in 8260B mix requires lower scan range for identification; 1,4-dioxane requires fortification or identification using single point high calibration standard. **Peaks 28 & 29 share ion (43).

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Volatiles
Volatile Organics US EPA Method 524.2 Revision IV Rtx-VMS

543

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00718

Purge and Trap Conditions: Concentrator: Tekmar LSC-3100 purge and trap Trap: Vocarb 3000 (type K) Purge: 11 min. @ 40 mL/min. @ ambient temperature. Dry purge: 1 min. @ 40mL/min. (MCS bypassed using Silcosteel tubing) Desorb preheat: 245C Desorb: 250C for 2 min., flow 10mL/min. Bake: 260C for 8 min. Interface: Silcosteel transfer line 1:30 split at injection port. 1mm ID split injection sleeve (cat.# 20972).

Column: Sample:

Rtx-VMS, 30m, 0.25mm ID, 1.4m (cat.# 19915) 502.2 Calibration Mix #1 (cat.# 30042) Drinking Water VOA MegaMix, 524.2 Rev 4 (cat.# 30601) 524 Internal Standard/Surrogate Mix (cat.# 30201) Ketone Mix, EPA Method 524.2 Rev 4.1 (cat.# 30602) Compounds at 20 ppb each in 5mL RO water (ketones at 50ppb; internal standards at 40ppb) Inj. temp.: 250C Carrier gas: helium, constant flow Flow rate: 1.1mL/min. Dead time: 1.48 min. @ 40C Oven temp.: 40C (hold 2 min.) to 85C @ 14C/min. (hold 2 min.) to 220C @ 30C/min. (hold 4 min.). Det: Agilent 5971A GC/MS Transfer line temp.: 280C Scan range: 35-300 amu Tune PFTBA/BFB Ionization: EI 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. chlorobenzene ethylbenzene 1,1,1,2-tetrachloroethane o-xylene styrrene bromoform isopropylbenzene 4-bromofluorobenzene bromobenzene n-propylbenzene 1,1,2,2-tetrachloroethane 2-chlorotoluene 1,2,3-trichloropropane 1,3,5-trimethylbenzene trans-1,4-dichloro-2-butene 4-chlorotoluene tert-butylbenzene pentachloroethane 73. 74. 75. 76. 77. 78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 1,2,4-trimethylbenzene sec-butylbenzene p-isopropyltoluene 1,3-dichlorobenzene 1,4-dichlorobenzene n-butylbenzene hexachloroethane 1,2-dichlorobenzene-d4 1,2-dichlorobenzene 1,2-dibromo-3-chloropropane nitrobenzene hexachlorobutadiene 1,2,4-trichlorobenzene naphthalene 1,2,3-trichlorobenzene

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18.

dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane diethyl ether 1,1-dichloroethene carbon disulfide iodomethane allyl chloride methylene chloride acetone trans-1,2-dichloroethene methyl tert-butyl ether 1,1-dichloroethane acrylonitrile cis-1,2-dichloroethene

19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36.

2,2-dichloropropane bromochloromethane chloroform methyl acrylate carbon tetrachloride tetrahydrofuran 1,1,1-trichloroethane 2-butanone 1,1-dichloropropene 1-chlorobutane propionitrile methacrylonitrile benzene 1,2-dichloroethane fluorobenzene trichloroethene dibromomethane 1,2-dichloropropane

37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54.

bromodichloromethane methyl methacrylate cis-1,3-dichloropropene toluene chloroacetonitrile 2-nitropropane 1,1-dichloropropanone 4-methyl-2-pentanone tetrachloroethene trans-1,3-dichloropropene 1,1,2-trichloroethane ethyl methacrylate dibromochloromethane 1,3-dichloropropane 1,2-dibromoethane 2-hexanone m-xylene p-xylene

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544

Volatiles
Volatile Organics US EPA Method 524.2 Rtx-502.2
35,36 33,34

18,19 8 20 13 21 22 24 15 14 16 17 23

25 32 27 29 26 28 30 31

54 43 48 50 51 45 49 37 38 52 53 44 46 47 55 42 39 41 40 56 58 57 59 60

9 3 6 45 7 12

12 10 11

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

min.

10

15

20 GC_EV00010

25

30

35

40m, 0.18mm ID, 1.0m Rtx -502.2 (cat.# 40915) Conc.: Reference Standard 524 Volatiles Kit (cat. # 30052) 200ppb VOA standards in 5mL RO water. Purge & trap: Tekmar LCS 2000 Trap: Vocarb 4000 Purge: 11 min. Desorb preheat: 250C Desorb time: 2 min. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. dichlorodifluoromethane chloromethane vinyl chloride bromomethane chloroethane trichlorofluoromethane 1,1-dichloroethene methylene chloride trans-1,2-dichloroethene 1,1-dichloroethane 2,2-dichloropropane cis-1,2-dichloroethene bromochloromethane 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. chloroform 1,1,1-trichloroethane 1,1-dichloropropene carbon tetrachloride benzene 1,2-dichloroethane trichloroethene 1,2-dichloropropane bromodichloromethane dibromomethane cis-1,3-dichloropropene toluene trans-1,3-dichloropropene 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39.

Desorb flow rate: Oven temp.: Inj. / det. temp.: Detector: Linear velocity: Split ratio: 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52.

30mL/min. 35C (hold 4 min.) to 150C @ 6C/min. to 220C @ 8C/min. (hold 8 min.). 200C / 250C MS 21cm/sec. set @ 35C 30:1 53. 54. 55. 56. 57. 58. 59. 60. 1,4-dichlorobenzene n-butylbenzene 1,2-dichlorobenzene 1,2-dibromo-3-chloropropane 1,2,4-trichlorobenzene hexachlorobutadiene naphthalene 1,2,3-trichlorobenzene

1,1,2-trichloroethane 1,3-dichloropropane tetrachloroethene dibromochloromethane ethylene dibromide chlorobenzene ethylbenzene 1,1,1,2-tetrachloroethane m-xylene p-xylene o-xylene styrene isopropylbenzene

bromoform 1,1,2,2-tetrachloroethane 1,2,3-trichloropropane propylbenzene bromobenzene 1,3,5-trimethylbenzene 2-chlorotoluene 4-chlorotoluene tert-butylbenzene 1,2,4-trimethylbenzene sec-butylbenzene p-isopropyltoluene 1,3-dichlorobenzene

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Semivolatiles
Phenols US EPA Method 604 MXT-5
Reference Standard 604 Phenols Mix (cat. # 31029): 1. phenol 2. 2-chlorophenol 3. 2-nitrophenol 4. 2,4-dimethylphenol 5. 2,4-dichlorophenol 6. 4-chloro-3-methylphenol 7. 2,4,6-trichlorophenol 8. 2,4-dinitrophenol 9. 4-nitrophenol 10. 2-methyl-4,6-dinitrophenol 11. pentachlorophenol
7 9 10 8 11

545

Phenols US EPA Method 604 Rtx-200


1 3

6 2

1 6

5 4 7

Reference Standard 604 Phenols Mix (cat. # 31029): 1. phenol 2. 2-chlorophenol 3. 2,4-dimethylphenol 4. 2,4-dichlorophenol 5. 2-nitrophenol 6. 4-chloro-3-methylphenol 7. 2,4,6-trichlorophenol 8. 4-nitrophenol 9. pentachlorophenol 10. 2,4-dinitrophenol 11. 2-methyl-4,6-dinitrophenol
8

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

11 9 10

5 2 3

min.

8 12 GC_EV00027

16

min.

12

16 GC_EV00028

20

24

28

30m, 0.28mm ID, 0.25m MXT-5 (cat.# 70224) 1.0L splitless injection of phenols. Concentration 25ng/L per component. Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C to 250C @ 10C/min. 280C / 300C hydrogen 50cm/sec. set @ 40C 2.56 x 10-10 AFS

30m, 0.32mm ID, 0.25m Rtx-200 (cat.# 15024) 1.0L split injection of a 200ng standard. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 50C (hold 4 min.) to 250C @ 6C/min. 250C helium 20cm/sec. 4 x 10-11 AFS 40:1

Phenols US EPA Method 604 Rtx-50


2 1 4 5 7 3 6

Reference Standard 604 Phenols Mix (cat. # 31029): 1. phenol 2. 2-chlorophenol 3. 2,4-dimethylphenol 4. 2-nitrophenol 5. 2,4-dichlorophenol 6. 4-chloro-3-methylphenol 7. 2,4,6-trichlorophenol 8. 2,4-dinitrophenol 9. 4-nitrophenol 10. 2-methyl-4,6-dinitrophenol 11. pentachlorophenol
10 9 8 11

Phenols US EPA Method 604 Rtx-5

4 6 9 1 3

Reference Standard 604 Phenols Mix (cat. # 31029): 1. phenol 2. 2-chlorophenol 3. 2-nitrophenol 4. 2,4-dimethylphenol 5. 2,4-dichlorophenol 6. 4-chloro-3-methylphenol 7. 2,4,6-trichlorophenol 8. 2,4-dinitrophenol 9. 4-nitrophenol 10. 2-methyl-4,6-dinitrophenol 11. pentachlorophenol
10

8 11

min.

12 16 GC_EV00029

20

24

28

min.

12 16 GC_EV00030

20

24

30m, 0.25mm ID, 0.25m Rtx-50 (cat.# 10523) 1.0L split injection of phenols. Concentration 35ng/L per component. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split vent: 50C (hold 10 min.) to 250C @ 15C/min. (hold 15 min.) 280C helium 20cm/sec. (flow rate: 0.7cc/min.) 32 x 10-11 AFS 40cc/min.

30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 1.0L split injection of phenols. Concentration 3-5ng/L per component. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 50C (hold 4 min.) to 250C @ 8C/min. 250C hydrogen 40cm/sec. set @ 110C 8 x 10-11 AFS 40:1

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546

Semivolatiles
Phenols XTI-5
IS2 IS3

30m, 0.25mm ID, 0.25m XTI-5 (cat.# 12223) 1.0L splitless injection. 40ng of phenols and IS mix. Oven temp.: Inj. temp.: Detector: Scan rate: Scan range: 40C to 350C @ 15C/min. (hold 15 min.) 350C MS 1.5 scan/sec. 35-400AMU
6 8 4 10 3 9 IS1 11

IS4

IS5

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Reference Standard SV Calibration Mix #2 (cat.# 31008) 1. phenol 2. 2-chlorophenol 3. 2-methylphenol 4. 4-methylphenol 5. 2-nitrophenol 6. 2,4-dimethylphenol 7. benzoic acid 8. 2,4-dichlorophenol 9. 4-chloro-3-methylphenol 10. 2,4,6-trichlorophenol 11. 2,4,5-trichlorophenol 12. 2,4-dinitrophenol 13. 4-nitrophenol 14. 2-methyl-4,6-dinitrophenol 15. pentachlorophenol

IS6

SV Internal Std. Mix (cat.# 31006): IS1. dichlorobenzene-d4 IS2. naphthalene-d8 IS3. acenaphthene-d10 IS4. phenanthrene-d10 IS5. chrysene-d12 IS6. perylene-d12

15 2 1 5 12 13 14

min.

10

15

20 GC_EV00031

25

30

35

Phenols & Benzidines US EPA Methods 604 & 605 Rtx-5

Phenols & Benzidines US EPA Methods 604 & 605 Rtx-5

1 2 3

6 9 5 7 12 13 10 11

Reference Standard 604 Phenols Mix (cat. # 31029) 605 Benzidines Mix (cat.# 31030): 1. phenol 2. 2-chlorophenol 3. 2-nitrophenol 4. 2,4-dimethylphenol 5. 2,4-dichlorophenol 6. 4-chloro-3-methylphenol 7. 2,4,6-trichlorophenol 8. 2,4-dinitrophenol 9. 4-nitrophenol 10. 2-methyl-4,6-dinitrophenol 11. pentachlorophenol 12. benzidine 13. 3,3'-dichlorobenzidine

2 3

4 6 7 5 9 10 12 13

11 8

min.

12

16

20

24

28

32

min.

12

16

20

24

28

32

GC_EV00032

GC_EV00033

30m, 0.32mm ID, 1.0m Rtx-5 (cat.# 10254) 1.5L split injection of benzidines and phenols. Concentration 13ng per component on-column. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 110C to 290C @ 8C/min. 310C hydrogen 40cm/sec. 2 x 10-11 AFS 100:1

30m, 0.53mm ID, 1.5m Rtx-5 (cat.# 10270) 2.5L direct injection of benzidines and phenols. Concentration approximately 25ng per component. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C (hold 6 min.) to 300C @ 10C/min. (hold 15 min.) 300C hydrogen 80cm/sec. (flow rate: 10cc/min.) 8 x 10-11 AFS

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Semivolatiles
Phthalate Esters US EPA Method 606 Rtx-5
2 2

547

Phthalate Esters US EPA Method 606 MXT-5


3 4 5

Reference Standard 606 Phthalate Esters Mix (cat.# 31031): 1. dimethyl phthalate 2. diethyl phthalate 3. di-n-butyl phthalate 4. butyl benzyl phthalate 5. bis(2-ethylhexyl)phthalate 6. di-n-octyl phthalate 1

3 4

Reference Standard 606 Phthalate Esters Mix (cat.# 31031): 1 1. dimethyl phthalate 2. diethyl phthalate 3. di-n-butyl phthalate 4. butyl benzyl phthalate 5. bis(2-ethylhexyl)phthalate 6. di-n-octyl phthalate
6

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

min. 4

12

16

20 GC_EV00034

24

28

32

min.

12

16

20 GC_EV00035

24

28

32

36

30m, 0.53mm ID, 1.5m Rtx-5 (cat.# 10270) 2.5L direct injection of phthalate esters. Concentration approximately 25ng per component. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C (hold 6 min.) to 300C @ 10C/min. (hold 15 min.) 300C hydrogen 80cm/sec. (flow rate: 10cc/min.) 8 x 10-11 AFS

30m, 0.53mm ID, 1.0m MXT-5 (cat.# 70255) 0.5L split injection of phthalate esters. Concentration 50ng per component. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 40C (hold 6 min.) to 300C @ 10C/min. (hold 15 min.) 300C hydrogen 50cm/sec. 8 x 10-11 AFS 50:1

Phthalate Esters US EPA Method 8060 Rtx-50


1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. dimethyl phthalate diethyl phthalate diisobutyl phthalate di-n-butyl phthalate bis(methoxyethyl) phthalate bis(4-methyl,2-pentyl) phthalate bis(ethoxyethyl) phthalate di-amyl phthalate hexyl-2-ethylhexyl phthalate di-n-hexyl phthalate butyl benzyl phthalate bis(2-n-butoxyethyl) phthalate dicyclohexyl phthalate bis(2-ethylhexyl)phthalate di-n-octyl phthalate di-nonyl phthalate
min. 4 8

12

3 4

8 6 10 79 5

12 13 14 11 15 16

30m, 0.53mm ID, 0.50m Rtx-50 (cat.# 10540) 1.5L direct injection of phthalate esters using a Uniliner direct injection liner. Concentration approximately 60g/mL per component. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 100C to 275C @ 15C/min. (hold 10 min.) 275C helium 20cm/sec. 64 x 10-11 AFS

12

16

20

24

GC_EV00037

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548

Semivolatiles
Nitrosamines US EPA Method 607 Rtx-5 3
2 3

Nitrosamines US EPA Method 607 Stabilwax

1. 2. 3. 4.
1

N-nitrosodimethylamine N-nitrosodiethylamine N-nitroso-di-n-propylamine diphenylamine (breakdown product of N-nitrosodiphenylamine)


1

1. 2. 3. 4.

N-nitrosodimethylamine N-nitrosodiethylamine N-nitroso-di-n-propylamine diphenylamine (breakdown product of N-nitrosodiphenylamine)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

min.

12 GC_EV00038

16

20

min.

12

16

GC_EV00039

15m, 0.53mm ID, 1.50m Rtx-5 (cat.# 10267) 1.0L direct injection of nitrosamines using a Unilinerinlet liner. Concentration approximately 50ng/L in methanol. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C (hold 4 min.) to 240C @ 20C/min. 240C hydrogen 80cm/sec. (flow rate: 10cc/min.) 128 x 10-11 AFS

30m, 0.32mm ID, 1.0m Stabilwax (cat.# 10654) 1.0L split injection of nitrosamines. Concentration approximately 50ng/L in methanol. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 40C (hold 4 min.) to 240C @ 20C/min. 240C hydrogen 80cm/sec. (flow rate: 10cc/min.) 128 x 10-11 AFS 40:1

Nitrosamines Rtx-200

Nitroaromatics US EPA Method 609 Rtx-5


1. 2. 3. 4. 5. 6. 7. 8.
3 2 1 6 4 5 7 8 3 4

N-nitrosodimethylamine N-nitrosomethylethylamine N-nitrosodiethylamine N-nitrosoazetidine N-nitrosopiperidine N-nitrosomorpholine N-nitrosopyrrolidine N-nitrosohexamethyleneimine

Reference Standard 609 Nitroaromatics/Isophorone Mix (cat.# 31033): 1. nitrobenzene 2. isophorone 3. 2,6-dinitrotoluene 4. 2,4-dinitrotoluene

min.

4 6 GC_EV00040

min.

12

16

GC_EV00041

30m, 0.53mm ID, 0.50m Rtx-200 (cat.# 15040) 1.0L split injection of nitrosamines. Concentration 10g/mL. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split vent: 100C (hold 1 min.) to 200C @ 5C/min. 250C hydrogen 40cm/sec. (flow rate: 5.2cc/min.) 16 x 10-12 AFS 40cc/min.

15m, 0.53mm ID, 1.50m Rtx-5 (cat.# 10267) 0.25L split injection of nitroaromatics. On-column concentration 28ng/component. Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: 100C to 300C @ 15C/min. (hold 10 min.) 250C / 300C helium 23cm/sec. set @ 40C range = 4, atten. = 3

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Semivolatiles
Polynuclear Aromatic Hydrocarbons US EPA Method 610 Rtx-CLPesticides2
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. naphthalene acenaphthylene acenaphthene fluorene phenanthrene anthracene fluoranthene pyrene benzo(a)anthracene chrysene benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene indeno(1,2,3-cd)pyrene dibenzo(a,h)anthracene benzo(ghi)perylene

549

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00596

Column: Sample: Inj.: Inj. temp.: Carrier gas: Oven temp.: Det.:

Rtx-CLPesticides2 30m, 0.25mm ID, 0.20m (cat.# 11323) 50g/mL 610 PAH Mix (cat.# 31011) in methylene chloride 1.0L splitless (hold 2 min.), 2mm splitless inlet liner w/ wool (cat.# 20829) 330C hydrogen, 4mL/min. constant flow 40C (hold 2 min.) to 250C @ 25C/min. to 265C @ 5C/min. to 300C (hold 4 min.) @25C/min. FID @ 350C

Polynuclear Aromatic Hydrocarbons US EPA Method 610 Rtx-5Sil MS

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.

naphthalene acenaphthylene acenaphthene fluorene phenanthrene anthracene fluoranthene pyrene benzo(a)anthracene chrysene benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene indeno(1,2,3-cd)pyrene dibenzo(a,h)anthracene benzo(ghi)perylene

GC_EV00595

Column: Sample: Inj.: Inj. temp.: Carrier gas: Oven temp.: Det.:

Rtx-5Sil MS 30m, 0.25mm ID, 0.25m (cat.# 12723) 50g/mL 610 PAH Mix (cat.# 31011) in methylene chloride 1.0L splitless (hold 2 min.), 2mm splitless inlet liner w/ wool (cat.# 20829) 330C hydrogen, 4mL/min. constant flow 40C (hold 2 min.) to 250C @ 25C/min. to 265C @ 5C/min. to 300C (hold 4 min.) @ 25C/min. FID @ 350C

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550

Semivolatiles
Polynuclear Aromatic Hydrocarbons US EPA Method 610 Rtx-5
0.53mm ID (direct injection)

3 4

5 6

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

7 8 9 10 12 11 13 15 14 16

min.

12

16

20

24

28

32

36

40

44

GC_EV00043

30m, 0.53mm ID, 1.50m Rtx-5 (cat.# 10270) 2.5L direct injection of PAHs using a Uniliner. Concentration approximately 25ng per component. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C (hold 6 min.) to 300C @ 10C/min. (hold 15 min.) 300C hydrogen 80cm/sec. (flow rate: 10cc/min.) 8 x 10-11 AFS

0.32mm ID (cold on-column injection)

Reference Standard SV Calibration Mix #5 (cat.# 31011): 1. naphthalene 2. acenaphthylene 3. acenapthene 4. fluorene 5. phenanthrene 6. anthracene 7. fluoranthene 8. pyrene 9. benzo(a)anthracene 10. chrysene 11. benzo(b)fluoranthene 12. benzo(k)fluoranthene 13. benzo(a)pyrene 14. indeno(1,2,3-cd)pyrene 15. dibenzo(a,h)anthracene 16. benzo(ghi)perylene

1 2 3 4 5 6 78 10 9 11 13 15 14 16 12

min.

12

16

20

24

28

32

GC_EV00376

30m, 0.32mm ID, 0.25m Rtx-5 (cat.# 10224) 0.5L cold on-column injection of PAHs. Concentration approximately 10ng per component. Oven temp.: Det. temp.: Carrier gas: Linear velocity: FID sensitivity: 35C (hold 4 min.) to 325C @ 10C/min. (hold) 325C hydrogen 40cm/sec. 8 x 10-11 AFS

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Semivolatiles
Polynuclear Aromatic Hydrocarbons US EPA Method 610 Rtx-440
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. naphthalene acenaphthylene acenaphthene fluorene phenanthrene anthracene fluoranthene pyrene benzo(a)anthracene chrysene benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene indeno(1,2,3-cd)pyrene dibenzo(a,h)anthracene benzo(ghi)perylene

551

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00732

Column: Sample: Inj.: Inj. temp.: Carrier gas: Flow: Oven temp.: Det.:

Rtx-440 30m, 0.25mm ID, 0.25m (cat.# 12923) 610 PAH Mix (cat.# 31011) diluted to 20ppm each compound in methylene chloride 1.0L splitless (hold 0.4 min.), 4mm splitless liner (cat.# 20772) 320C hydrogen, constant flow 3.6mL/min. 40C (hold 2 min.) to 240C @ 30C/min., to 320C @ 8C/min. (hold 5 min.) FID @ 320C

Polynuclear Aromatic Hydrocarbons US EPA Method 610 Rtx-5

2 3 4 1 5 6

Fast GC using microbore column

7 8 9 10 12 11

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.

naphthalene acenaphthylene acenaphthene fluorene phenanthrene anthracene fluoranthene pyrene chrysene benzo(a)anthracene benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene indeno(1,2,3-cd)pyrene dibenzo(a,h)anthracene benzo(ghi)perylene

13

14,15 16

10m, 0.10mm ID, 0.10m Rtx-5 (cat.# 41201) 0.5L splitless injection. 41psi initial pressure, hold 2 min. 8 psi/min. to 99psi (hold 1.87 min.). 275C, vent open @ 1 min. Oven temp.: 40C (hold 0.5 min.) to 90C @ 70C/min. then to 100C @ 5C/min., to 310C @ 30C/min. (hold 2 min.).

min.

7 GC_EV00045

10

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552

Semivolatiles
Polynuclear Aromatic Hydrocarbons US EPA Method 8100 MXT-5
Reference Standards SV Calibration Mix #5 (cat.# 31011): 1. naphthalene 2. acenaphthylene 3. acenaphthene 4. fluorene 5. phenanthrene 6. anthracene 7. fluoranthene 8. pyrene 9. benzo(a)anthracene 10. chrysene 11. benzo(b)fluoranthene 12. benzo(k)fluoranthene 13. benzo(a)pyrene 14. indeno(1,2,3-cd)pyrene 15. dibenzo(a,h)anthracene 16. benzo(ghi)perylene
3 2 4 6 1 5 7 9 10 11 13 16 14 15 8 12

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

min.

10

12

14

16

18 GC_EV00042

20

22

24

26

28

30m, 0.28mm ID, 0.25m MXT-5 (cat.# 70224) 1.0L splitless injection of PAHs. Concentration 20ng/L. Oven temp.: Inj. / det. temp.: Detector: Carrier gas: Linear velocity: Splitless hold time: 40C to 325C @ 10C/min. (hold 10 min.) 280C / 325C MS helium 50cm/sec. set @ 325C 1 min.

Haloethers US EPA Method 611 Rtx-5

Reference Standard 611 Haloethers Mix (cat.# 31034): 1. bis(2-chloroethyl)ether 2. bis(2-chloroisopropyl)ether 3. bis(2-chloroethoxy)methane 4. 4-chlorophenyl phenyl ether 5. 4-bromophenyl phenyl ether

Chlorinated Hydrocarbons US EPA Method 612 Rtx-200 Reference Standard


2,4

612 Chlorinated Hydrocarbons Mix (cat.# 31035): 1. 1,3-dichlorobenzene (0.2mg/mL) 2. 1,4-dichlorobenzene (0.3mg/mL) 3. 1,2-dichlorobenzene (0.3mg/mL) 4. hexachloroethane (0.02mg/mL) 5. 1,2,4-trichlorobenzene (0.2mg/mL) 6. hexachlorobutadiene (0.02mg/mL) 7. hexachlorocyclopentadiene (0.02mg/mL) 8. 2-chloronaphthalene (0.3mg/mL) 9. hexachlorobenzene (0.02mg/mL)

5 6 1 2 3 7 9

3 1 8

min.

8 12 GC_EV00050

16

min.

8 GC_EV00051

12

16

15m, 0.53mm ID, 1.50m Rtx-5 (cat.# 10267) 0.25L split injection of EPA Method 611 haloethers. On-column concentration 28ng/component. Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: 100C to 300C @ 15C/min. (hold 10 min.) 200C / 300C helium 23cm/sec. set @ 40C

30m, 0.53mm ID, 0.50m Rtx-200 (cat.# 15040) 0.5L direct injection of chlorinated hydrocarbons. Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: 40C to 280C @ 8C/min. (hold 5 min.) 275C / 220C helium 40cm/sec. set @ 40C

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Semivolatiles
Chlorinated Hydrocarbons US EPA Method 612 Rtx-35 Chlorinated Hydrocarbons US EPA Method 612 Rtx-5

553

5,6

Reference Standard 612 Chlorinated Hydrocarbons Mix (cat.# 31035): 1. 1,3-dichlorobenzene (0.2mg/mL) 2. 1,4-dichlorobenzene (0.3mg/mL) 3. 1,2-dichlorobenzene (0.3mg/mL) 4. hexachloroethane (0.02mg/mL) 5. 1,2,4-trichlorobenzene (0.2mg/mL) 6. hexachlorobutadiene (0.02mg/mL) 7. hexachlorocyclopentadiene (0.02mg/mL) 8. 2-chloronaphthalene (0.3mg/mL) 9. hexachlorobenzene (0.02mg/mL)
1 3 2

5 6

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

1 2

3 8

min.

10

15 GC_EV00052

20

min.

10 GC_EV00053

15

20

30m, 0.53mm ID, 0.50m Rtx-35 (cat.# 10440) 0.1L direct injection of chlorinated hydrocarbons. Concentration: 4ng/L Oven temp.: 40C to 250C @ 8C/min. (hold 5 min.) Inj. / det. temp.: 250C / 300C Carrier gas: helium Linear velocity: 35cm/sec. set @ 40C

30m, 0.53mm ID, 0.50m Rtx-5 (cat.# 10240) 0.1L direct injection of chlorinated hydrocarbons. Concentration: 4ng/L Oven temp.: 40C to 250C @ 8C/min. (hold 5 min.) Inj. / det. temp.: 250C / 300C Carrier gas: helium Linear velocity: 35cm/sec. set @ 40C

Chlorinated Hydrocarbons US EPA Method 612 MXT-5


4 5 6 7 9

US EPA Hazardous Substances Rtx-5


3 1 2 4 6 7 11

3 1

1. 2. 3. 4. 5. 6. 7. 8. 9.

1,3-dichlorobenzene 1,4-dichlorobenzene 1,2-dichlorobenzene hexachloroethane 1,2,4-trichlorobenzene hexachlorobutadiene hexachlorocyclopentadiene 2-chloronaphthalene hexachlorobenzene


5

10

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.


12

aniline benzyl alcohol 2-methylphenol 4-methylphenol benzoic acid 4-chloroaniline 2-methylnaphthalene 2,4,5-trichlorophenol 2-nitroaniline dibenzofuran 3-nitroaniline 4-nitroaniline

min. min. 4 8 12 GC_EV00054 16 20

12

16

20

24

28

32

36

GC_EV00055

30m, 0.53mm ID, 0.50m MXT -5 (cat.# 70240) 0.2L direct injection of chlorinated hydrocarbons.

30m, 0.53mm ID, 1.50m Rtx-5 (cat.# 10270) 2.5L direct injection of hazardous substances using a Uniliner liner. Concentration approximately 25ng per component. Oven temp.: 40C (hold 6 min.) to 300C @ 10C/min. (hold 15 min.) 300C hydrogen 80cm/sec. (flow rate: 10cc/min.) set @ 40C

Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity:

40C to 280C @ 8C/min. (hold 15 min.) 200C / 300C helium 20cm/sec. (flow rate: 2.5cc/min.)

Inj. & det. temp.: Carrier gas: Linear velocity:

Phone: 800-356-1688 or 814-353-1300 www.restek.com

554

Semivolatiles
Semivolatile Organics US EPA Method 526 (Screening) Rtx-5Sil MS

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

nitrobenzene 2,4-dichlorophenol 1,3-dimethyl-2-nitrobenzene (ss) 2,4,6-trichlorophenol acenaphthene-d10 (IS#1) azobenzene* prometon terbufos diazinon fonofos

11. phenanthrene-d10 (IS#2) 12. disulfoton 13. acetochlor 14. cyanazine 15. triphenylphosphate (ss) 16. chrysene-d12 * Compound listed in method, 1,2-diphenylhydrazine, decomposes to azobenzene.

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Optimized resolution!

Rtx-5Sil MS, 30m, 0.25mm ID, 0.25m (cat.# 12723) US EPA Method 526 Mix 1L 10ppm (20ppm IS) Primary Dilution Standard / Semivolatiles/ EPA 526 cat.# 31691 Surrogate Standard / Method 526 cat.# 31693 Internal Standard / Method 526 cat.# 31692 1.0L splitless (hold 0.3 min.), 4mm Drilled Uniliner (cat.# 21055) Agilent 6890 300C helium, constant flow 0.8 mL/min. 50C (hold 1 min.) to 200C @ 20C/min. (hold 5 min.) to 310C @ 30C/min. (hold 3 min.) Det: Agilent 5973 GC/MS Transfer line temp.: 280C Scan range: 35-550 amu Solvent delay: 5.5 min. Tune: DFTPP Ionization: EI GC Inj. temp.: Carrier gas: Flow rate: Oven temp.: Inj.:

GC_EV00656

Phenols US EPA Method 528 Rtx-5Sil MS


Excellent sensitivity and peak shape at 5ng on-column

1. 2. 3. 4. 5. 6. 7. 8. 9.

phenol 2-chlorophenol-3,4,5,6-d4 (SS) 2-chlorophenol 2-methylphenol 2-nitrophenol 2,4-dimethylphenol-3,5,6-d3 (SS) 2,4-dimethylphenol 2,4-dichlorophenol 4-chloro-3-methylphenol

10. 11. 12. 13. 14. 15. 16. 17.

1,2-dimethyl-3-nitrobenzene (IS#1) 2,4,6-trichlorophenol 2,4-dinitrophenol 4-nitrophenol 2,3,4,5-tetrachlorophenol (IS#2) 2-methyl-4,6-dinitrophenol 2,4,6-tribromophenol (SS) pentachlorophenol

Rtx-5Sil MS 30m, 0.25mm ID, 0.25m (cat.# 12723) US EPA Method 528 Mix 1L 5ppm standard Phenol Stock Calibration Solution Internal Standard Phenols Method 528 Surrogate Fortification Standard/Phenols 5ng each analyte on-column Inj.:

cat.# 31694 cat.# 31696 cat.# 31692

1.0L pulsed splitless (hold 0.5 min.), 4mm Drilled Uniliner (cat.# 21055), pulsed pressure 50psi for 0.5 min. GC: Agilent 6890 Inj. temp.: 220C Carrier gas: helium, constant flow Flow rate: 1.3 mL/min. Oven temp.: 40C (hold 1 min.) to 220C @ 12C/min. (hold 0 min.) to 300C @ 30C/min (hold 1 min.) Det: Agilent 5973 GC/MS Transfer line temp.: 280C Scan range: 35-550 amu Solvent delay: 5.5 min. Tune: DFTPP Ionization: EI

GC_EV00664

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Semivolatiles
Semivolatiles CLP Method Rtx-5MS
80ng splitless 0.25m film thickness 5% diphenyl phase

555

30m, 0.25 mm ID, 0.25m Rtx-5MS (cat.# 12623) 80ng splitless injection of CLP standard Oven temp.: Carrier gas: Inj. temp.: Det. temp.: Scan range: 40C (hold 2 min.) to 245C @ 25C/min.to 330C @ 6C/min. (hold 5 min.) helium @ 1.0 mL/min. constant flow 300C 280C 35-550 amu

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00544

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27.

2-fluorophenol (SS) phenol-d6 (SS) phenol bis(2-chloroethyl)ether 2-chlorophenol-d4 (SS) 2-chlorophenol 1,3-dichlorobenzene 1,4-dichlorobenzene-d4 (IS) 1,4-dichlorobenzene 1,2-dichlorobenzene-d4 (IS) benzyl alcohol 1,2-dichlorobenzene 2-methylphenol bis(2-chloroisopropyl)ether 4-methylphenol/3-methylphenol N-nitroso-di-n-propylamine hexachloroethane nitrobenzene-d5 (SS) nitrobenzene isophorone 2-nitrophenol 2,4-dimethylphenol bis(2-chloroethoxy)methane benzoic acid 2,4-dichlorophenol 1,2,4-trichlorobenzene naphthalene-d8 (IS)

RT 4.65 5.53 5.55 5.64 5.66 5.67 5.81 5.86 5.87 6.01 6.01 6.03 6.10 6.13 6.25 6.28 6.33 6.41 6.43 6.66 6.73 6.75 6.85 6.91 6.95 7.03 7.08

28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55.

naphthalene 4-chloroaniline hexachlorobutadiene 4-chloro-3-methylphenol 2-methylnaphthalene hexachlorocyclopentadiene 2,4,6-trichlorophenol 2,4,5-trichlorophenol 2-fluorobiphenyl (SS) 2-chloronaphthalene 2-nitroaniline dimethylphthalate 2,6-dinitrotoluene acenaphthylene acenaphthene-d10 (IS) acenaphthene 3-nitroaniline 2,4-dinitrophenol 4-nitrophenol dibenzofuran 2,4-dinitrotoluene diethyl phthalate 4-chlorophenyl phenyl ether fluorene 4-nitroaniline 2-methyl-4,6-dinitrophenol diphenylamine 2,4,6-tribromophenol (SS)

7.10 7.20 7.21 7.62 7.77 7.92 8.05 8.08 8.13 8.25 8.38 8.54 8.62 8.66 8.79 8.83 8.88 8.88 8.92 8.99 9.01 9.22 9.32 9.33 9.39 9.40 9.44 9.57

56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77. 78. 79. 80.

4-bromophenyl phenyl ether hexachlorobenzene pentachlorophenol phenanthrene-d10 (IS) phenanthrene anthracene carbazole di-n-butylphthalate fluoranthene pyrene p-terphenyl-d14 (SS) butyl benzyl phthalate benzo(a)anthracene 3,3'-dichlorobenzidine chrysene-d12 (IS) chrysene bis(2-ethylhexyl)phthalate di-n-octyl phthalate benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene perylene-d12 (IS) indeno(1,2,3-cd)pyrene dibenzo(a,h)anthracene benzo(ghi)perylene

9.80 9.88 10.07 10.24 10.27 10.32 10.49 10.84 11.62 11.94 12.16 13.01 14.05 14.06 14.08 14.14 14.2 15.77 16.57 16.64 17.38 17.52 20.18 20.26 20.81

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556

Semivolatiles
Semivolatiles US EPA Method 8270 Rtx-5Sil MS
80ng splitless 0.25m film thickness Silarylene phase

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

30m, 0.25 mm ID, 0.25m Rtx-5Sil MS (cat.# 12723) 80ng splitless injection of 8270 standard Oven temp.: Carrier gas: Inj. temp.: Det. temp.: Scan range: 40C (hold 2 min.) to 245C @ 25C/min. to 330C @ 6C/min. (hold 5 min.) helium @ 1.0mL/min. constant flow 300C 280C 35-550amu

GC_EV00545

1. N-nitrosodimethylamine 2. pyridine 3. methyl methanesulfonate 4. 2-fluorophenol (SS) 5. ethyl methanesulfonate 6. phenol 7. phenol-d6 (SS) 8. aniline 9. bis(2-chloroethyl)ether 10. 2-chlorophenol-d4 (SS) 11. 2-chlorophenol 12. 1,3-dichlorobenzene 13. 1,4-dichlorobenzene-d4 (IS) 14. 1,4-dichlorobenzene 15. benzyl alcohol 16. 1,2-dichlorobenzene-d4 (SS) 17. 1,2-dichlorobenzene 18. 2-methylphenol 19. bis(2-chloroisopropyl)ether 20a. 4-methylphenol 20b. 3-methylphenol 21. N-nitroso-di-n-propylamine 22. acetophenone 23. hexachloroethane 24. nitrobenzene-d5 (SS) 25. nitrobenzene 26. isophorone 27. 2,4-dimethylphenol 28. 2-nitrophenol 29. benzoic acid 30. bis(2-chloroethoxy)methane 31. 2,4-dichlorophenol 32. 1,2,4-trichlorobenzene 33. naphthalene-d8 (IS) 34. naphthalene

RT 3.38 3.37 4.53 4.61 5.16 5.51 5.50 5.52 5.58 5.60 5.61 5.73 5.79 5.80 5.96 5.94 5.96 6.06 6.06 6.22 6.22 6.24 6.20 6.25 6.35 6.37 6.59 6.70 6.66 6.87 6.79 6.89 6.95 7.00 7.03

35. 2,6-dichlorophenol 36. 4-chloroaniline 37. hexachloropropene 38. hexachlorobutadiene 39. 4-chloro-3-methylphenol 40. isosafrole 41. 2-methylnaphthalene 42. 1-methylnaphthalene 43. hexachlorocyclopentadiene 44. 1,2,4,5-tetrachlorobenzene 45. 2,4,6-trichlorophenol 46. 2,4,5-trichlorophenol 47. 2-fluorobiphenyl (SS) 48. safrole 49. 2-chloronaphthalene 50. 2-nitroaniline 51. 1,4-naphthoquinone 52. dimethylphthalate 53. 1,3-dinitrobenzene 54. 2,6-dinitrotoluene 55. acenaphthylene 56. 3-nitroaniline 57. acenaphthene-d10 (IS) 58. acenaphthene 59. 2,4-dinitrophenol 60. 4-nitrophenol 61. pentachlorobenzene 62. 2,4-dinitrotoluene 63. dibenzofuran 64. 2,3,4,6-tetrachlorophenol 65. diethyl phthalate 66. 4-chlorophenyl phenyl ether 67. fluorene 68. 4-nitroaniline 69. 4,6-dinitro-2-methylphenol 70. diphenylamine

7.10 7.12 7.10 7.14 7.57 7.61 7.69 7.79 7.85 7.86 7.98 8.02 8.05 8.11 8.17 8.32 8.37 8.48 8.54 8.56 8.57 8.68 8.71 8.74 8.82 8.91 8.89 8.94 8.91 9.05 9.15 9.24 9.24 9.30 9.33 9.37

71. azobenzene 72. 2,4,6-tribromophenol (SS) 73. phenacetin 74. 4-bromophenyl phenyl ether 75. hexachlorobenzene 76. pentachlorophenol 77. pentachloronitrobenzene 78. dinoseb 79. phenanthrene-d10 (IS) 80. phenanthrene 81. anthracene 82. di-n-butylphthalate 83. 4-nitroquinoline-1-oxide 84. isodrin 85. fluoranthene 86. benzidine 87. pyrene 88. Aramite 89. p-terphenyl-d14 (SS) 90. chlorbenzilate 91. butyl benzyl phthalate 92. Kepone 93. bis(2-ethylhexyl)phthalate 94. chrysene-d12 (IS) 95. 3,3'-dichlorobenzidine 96. benzo(a)anthracene (IS) 97. chrysene 98. di-n-octyl phthalate 99. benzo(b)fluoranthene 100. benzo(k)fluoranthene 101. benzo(a)pyrene 102. perylene-d12 (IS) 103. 3-methylcholanthrene 104. indeno(1,2,3-cd)pyrene 105. dibenzo(a,h)anthracene 106. benzo(ghi)perylene

9.39 9.49 9.70 9.71 9.80 9.99 10.02 10.16 10.16 10.18 10.23 10.75 11.04 11.29 11.50 11.71 11.80 12.10 12.02 12.31 12.84 12.81 13.99 13.87 13.87 13.84 13.93 15.51 16.29 16.35 17.07 17.22 17.98 19.82 19.91 20.44

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Semivolatiles
Semivolatile Organics US EPA Method 8270 Rtx-5Sil MS
Excellent benzo(b) & benzo(k) fluoranthene separation!
30m, 0.25mm ID, 0.5m Rtx-5Sil MS (cat# 12738) 80ng splitless injection of 8270 standard GC: Agilent 6890 Det.: MSD Oven temp.: 40C (hold 2 min) to 290C @ 20C/min. (hold 0 min.) to 303C @ 2C/min. (hold 0 min.) to 330C @ 6C/min. (hold 1 min.) Carrier gas: helium @ 1.0mL/min. constant flow Inj. temp.: 300C Det. temp.: 280C, scan range 35-550 AMU
93 84 90 91 1,2 5 3 83 86 92 102 103 94 98 100 99 101 104,105 106 95,96 97

557

47

10,11 34 4 6,7 58 89 67 81 85 82 87,88

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

min.

10

11

12

13

14

15

16

17

18

19

20

21

22

23

24

47

10,11 16,17 34 20 21,22 6,7 13,14 49 12 32 35,36 18 9 15 19 2324 25 26 29,30 46 31 33 37 43 54 50 8 53 59 60 39 48 45 51 52 57 61 38 40 44 27,28 41 42 58 55

80ng splitless 0.5m film thickness Silarylene phase

62,63 67 68,69 72 66 65 70 71 74 75 80 81

64 73 76 77 79 78

min.

7.0

7.5

8.0

8.5

9.0

9.5

10.0 GC_EV00532

10.5

11.0

11.5

12.0

12.5

1. N-nitrosodimethylamine 2. pyridine 3. methyl methanesulfonate 4. 2-fluorophenol 5. ethyl methanesulfonate 6. phenol-d6 7. phenol 8. aniline 9. bis(2-chloroethyl)ether 10. 2-chlorophenol-d4 11. 2-chlorophenol 12. 1,3-dichlorobenzene 13. 1,4-dichlorobenzene-d4 14. 1,4-dichlorobenzene 15. benzyl alcohol 16. 1,2-dichlorobenzene-d4 17. 1,2-dichlorobenzene 18. 2-methylphenol 19. bis(2-chloroisopropyl)ether 20a. 4-methylphenol 20b. 3-methylphenol 21. N-nitroso-di-n-propylamine

22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39 40. 41. 42. 43.

acetophenone hexachloroethane nitrobenzene-d5 nitrobenzene isophorone 2,4-dimethylphenol 2-nitrophenol benzoic acid bis(2-chloroethoxy)methane 2,4-dichlorophenol 1,2,4-trichlorobenzene naphthalene-d8 naphthalene 2,6-dichlorophenol 4-chloroaniline hexachloropropene hexachlorobutadiene 4-chloro-3-methylphenol isosafrole 2-methylnaphthalene 1-methylnaphthalene hexachlorocyclopentadiene

44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65.

1,2,4,5-tetrachlorobenzene 2,4,6-trichlorophenol 2,4,5-trichlorophenol 2-fluorobiphenyl safrole 2-chloronaphthalene 2-nitroaniline 1,4-naphthoquinone dimethylphthalate 1,3-dinitrobenzene 2,6-dinitrotoluene acenaphthylene 3-nitroaniline acenaphthene-d10 acenaphthene 2,4-dinitrophenol 4-nitrophenol pentachlorobenzene 2,4-dinitrotoluene dibenzofuran 2,3,4,6-tetrachlorophenol diethyl phthalate

66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77. 78 79. 80. 81. 82. 83. 84. 85. 86. 87.

4-chlorophenyl phenyl ether fluorene 4-nitroaniline 4,6-dinitro-2-methylphenol diphenylamine azobenzene 2,4,6-tribromophenol phenacetin 4-bromophenyl phenyl ether hexachlorobenzene pentachlorophenol pentachloronitrobenzene dinoseb phenanthrene-d10 phenanthrene anthracene di-n-butylphthalate 4-nitroquinoline-1-oxide isodrin fluoranthene benzidine pyrene

88. Aramite 89. p-terphenyl-d14 90. chlorbenzilate 91. butyl benzyl phthalate 92. Kepone 93. bis(2-ethylhexyl)phthalate 94. 3,3'-dichlorobenzidine 95. benzo(a)anthracene 96. chrysene-d12 97. chrysene 98. di-n-octyl phthalate 99. benzo(b)fluoranthene 100. benzo(k)fluoranthene 101. benzo(a)pyrene 102. perylene-d12 103. 3-methylcholanthrene 104. indeno(1,2,3-cd)pyrene 105. dibenzo(a,h)anthracene 106. benzo(ghi)perylene

Phone: 800-356-1688 or 814-353-1300 www.restek.com

558

Semivolatiles
Semivolatile Organics US EPA Method 8270 Rtx-5Sil MS
16ng on-column Drilled Uniliner inlet liner 0.25m film thickness Silarylene phase

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00561

Rtx -5Sil MS, 30m, 0.25mm ID, 0.25m (cat.# 12723) Sample: 16g/mL in methylene chloride Inj.: 1L splitless (hold 0.4 min.), Drilled Uniliner liner (cat.# 21054) Inj. temp.: 300C Carrier gas: helium, constant flow Flow rate: 1mL/min. Oven temp.: 35C (hold 2 min.) to 260C @ 20C/min., to 330C @ 6C/min. (hold 1 min.) Det.: MS Transfer line temp.: 280C Scan range: 35550amu Ionization: EI Mode: full scan

Analytical Reference Materials used: cat.# 31618, 31619, 31620, 31621, 31622, 31206, 31062, 31063

1. N-nitrosodimethylamine 2. pyridine 3. methyl methanesulfonate 4. 2-fluorophenol 5. ethyl methanesulfonate 6. phenol-d6 7. phenol 8. aniline 9. bis(2-chloroethyl)ether 10. 2-chlorophenol 11. 1,3-dichlorobenzene 12. 1,4-dichlorobenzene-d4 13. 1,4-dichlorobenzene 14. 1,2-dichlorobenzene 15. benzyl alcohol 16. 2-methylphenol 17. bis(2-chloroisopropyl)ether 18. acetophenone 19a. 4-methylphenol 19b. 3-methylphenol 20. N-nitroso-di-n-propylamine 21. hexachloroethane 22. nitrobenzene-d5 23. nitrobenzene 24. isophorone 25. 2-nitrophenol 26. 2,4-dimethylphenol

27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53.

bis(2-chloroethoxy)methane benzoic acid 2,4-dichlorophenol 1,2,4-trichlorobenzene naphthalene-d8 naphthalene 2,6-dichlorophenol 4-chloroaniline hexachloropropene hexachlorobutadiene 4-chloro-3-methylphenol isosafrole 2-methylnaphthalene 1-methylnaphthalene hexachlorocyclopentadiene 1,2,4,5-tetrachlorobenzene 2,4,6-trichlorophenol 2,4,5-trichlorophenol 2-fluorobiphenyl safrole 2-chloronaphthalene 2-nitroaniline 1,4-naphthoquinone dimethyl phthalate 1,3-dinitrobenzene 2,6-dinitrotoluene acenaphthylene

54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77. 78. 79. 80.

acenaphthene-d10 3-nitroaniline acenaphthene 2,4-dinitrophenol pentachlorobenzene 4-nitrophenol dibenzofuran 2,4-dinitrotoluene 2,3,4,6-tetrachlorophenol diethyl phthalate fluorene 4-chlorophenyl phenyl ether 4-nitroaniline 4,6-dinitro-2-methylphenol diphenylamine azobenzene 2,4,6-tribromophenol phenacetin 4-bromophenyl phenyl ether hexachlorobenzene pentachlorophenol pentachloronitrobenzene phenanthrene-d10 dinoseb phenanthrene anthracene di-n-butylphthalate

81. 4-nitroquinoline-1-oxide 82. isodrin 83. fluoranthene 84. benzidine 85. pyrene 86. p-terphenyl-d14 87. Aramite 88. chlorbenzilate 89. Kepone 90. butyl benzyl phthalate 91. benzo(a)anthracene 92. 3,3'-dichlorobenzidine 93. chrysene-d12 94. chrysene 95. bis(2-ethylhexyl)phthalate 96. di-n-octyl phthalate 97. benzo(b)fluoranthene 98. benzo(k)fluoranthene 99. benzo(a)pyrene 100. perylene-d12 101. 3-methylcholanthrene 102. indeno(1,2,3-cd)pyrene 103. dibenzo(a,h)anthracene 104. benzo(ghi)perylene

See page 559 for resolution of close eluting compounds.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Semivolatiles
Semivolatile Organics US EPA Method 8270 Rtx-5Sil MS

559

please note
highlighted regions from c-grams on page 558.

1. phenol (m/z 94) 2. aniline (m/z 93) 3. bis(2-chloroethyl)ether (m/z 93)

1. 1,3-dichlorobenzene (m/z 146) 2. 1,4-dichlorobenzene (m/z 146) 3. 1,2-dichlorobenzene (m/z 146)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00562

GC_EV00563

1. benzo(b)fluoranthene (m/z 252) 2. benzo(k)fluoranthene (m/z 252)

1. indeno(1,2,3-cd)pyrene (m/z 276) 2. dibenzo(a,h)anthracene (m/z 278)

GC_EV00564

GC_EV00565

Rtx-5Sil MS, 30m, 0.25mm ID, 0.25m (cat.# 12723) Sample: 16g/mL in methylene chloride Inj.: 1L splitless (hold 0.4 min.), Drilled Uniliner liner (cat.# 21054) Inj. temp.: 300C Carrier gas: 1mL/min., constant flow Linear velocity: 34cm/sec. Oven temp.: 35C (hold 2 min.) to 260C @ 20C/min., to 330C @ 6C/min. (hold 1 min.) Det.: MS Transfer line temp.: 280C Scan range: 35550amu Ionization: EI Mode: full scan

Phone: 800-356-1688 or 814-353-1300 www.restek.com

560

Semivolatiles
Semivolatile Organics US EPA Method 8270 Rtx-5Sil MS (Integra-Guard)
Rtx-5Sil MS with 5 meter Integra-Guardintegral guard column, 30m, 0.25mm ID, 0.25m (cat.# 12723-127) Sample: US EPA Method 8270 Mix 1L 10 ppm (10ng on column) 8270 Calibration Mix #1, cat.# 31618 8270 Calibration Mix #2, cat.# 31619 8270 Calibration Mix #3, cat.# 31620 8270 Calibration Mix #4, cat.# 31621 8270 Calibration Mix #5, cat.# 31622 SV Internal Standard Mix, cat.# 31206 Acid Surrogate Mix (4/89), cat.# 31063 B/N Surrogate Standard Mix (4/89), cat.# 31062 Inj.: 1.0L splitless (hold 0.3 min.), 4mm Drilled Uniliner (cat.# 21055) Inj. temp.: 300C Carrier gas: helium, constant flow Flow rate: 1.1mL/min. Dead Time: 1.8 minutes @ 35C

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

10ng on-column Drilled Uniliner inlet liner 0.25m film thickness Silarylene phase Integra-Guard column

GC_EV00611

Oven temp.: Det: Transfer line temp.: Scan range: Solvent delay: Tune: Ionization:

35C (hold 4 min.) to 245C @ 25C/min.(no hold) to 330C @ 6C/min. (hold 3 min.) Agilent 5973 GC/MS 280C 35550 amu 5 min. DFTPP EI

GC_EV00612

1. N-nitrosodimethylamine 2. pyridine 3. methyl methanesulfonate 4. 2-fluorophenol 5. ethyl methanesulfonate 6. phenol-d6 7. phenol 8. aniline 9. bis(2-chloroethyl)ether 10. 2-chlorophenol-d4 11. 1,3-dichlorobenzene 12. 1,4-dichlorobenzene-d4 13. 1,4-dichlorobenzene 14. benzyl alcohol 15. 1,2-dichlorobenzene 16. 2-methylphenol 17. bis(2-chloroisopropyl)ether 18. 4-methylphenol/3-methylphenol 19. acetophenone 20. N-nitroso-di-n-propylamine 21. hexachloroethane 22. nitrobenzene-d5

23. nitrobenzene 24. isophorone 25. 2-nitrophenol 26. 2,4-dimethylphenol 27. benzoic acid 28. bis(2-chloroethoxy)methane 29. 2,4-dichlorophenol 30. 1,2,4-trichlorobenzene 31. naphthalene-d8 32. naphthalene 33. 2,6-dichlorophenol 34. 4-chloroaniline 35. hexachloropropene 36. hexachlorobutadiene 37. 4-chloro-3-methylphenol 38. isosafrole 39. 2-methylnaphthalene 40. 1-methylnaphthalene 41. hexachlorocyclopentadiene 42. 1,2,4,5-tetrachlorobenzene 43. 2,4,6-trichlorophenol 44. 2,4,5-trichlorophenol

45. 2-fluorobiphenyl 46. safrole 47. 2-chloronaphthalene 48. 2-nitroaniline 49. 1,4-naphthoquinone 50. dimethyl phthalate 51. 1,3-dinitrobenzene 52. 2,6-dinitrotoluene 53. acenaphthylene 54. 3-nitroaniline 55. acenaphthene-d10 56. acenaphthene 57. 2,4-dinitrophenol 58. 4-nitrophenol 59. pentachlorobenzene 60. dibenzofuran 61. 2,4-dinitrotoluene 62. 2,3,4,6-tetrachlorophenol 63. diethyl phthalate 64. 4-chlorophenyl phenyl ether 65. fluorene 66. 4-nitroaniline

67. 4,6-dinitro-2-methylphenol 68. diphenylamine 69. azobenzene 70. 2,4,6-tribromophenol 71. phenacetin 72. 4-bromophenyl phenyl ether 73. hexachlorobenzene 74. pentachlorophenol 75. pentachloronitrobenzene 76. dinoseb 77. phenanthrene-d10 78. phenanthrene 79. anthracene 80. di-n-butyl phthalate 81. 4-nitroquinoline-1-oxide 82. isodrin 83. fluoranthene 84. benzidine 85. pyrene 86. aramite 87. p-terphenyl-d14 88. aramite isomer

89. chlorbenzilate 90. butyl benzyl phthalate 91. kepone 92. benzo(a)anthracene 93. 3,3'-dichlorobenzidine 94. chrysene-d12 95. chrysene 96. bis(2-ethylhexyl) phthalate 97. di-n-octyl phthalate 98. benzo(b)fluoranthene 99. benzo(k)fluoranthene 100. benzo(a)pyrene 101. perylene-d12 102. 3-methylcholanthrene 103. indeno(1,2,3-cd)pyrene 104. dibenzo(a,h)anthracene 105. benzo(ghi)perylene

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Semivolatiles
Semivolatile Organics US EPA Appendix IX Rtx-5Sil MS
50ng each on-column 0.25m film thickness Silarylene phase
Column: Rtx-5Sil MS, 30m, 0.25mm ID, 0.25m (cat.# 12723) Sample: 8270 MegaMix (cat.# 31686) Appendix IX Mix #1 (cat#31625) Appendix IX Mix #2 (cat#31806) SV Internal Standard Mix (cat#31206) B/N Surrogate Mix (4/89 SOW) (cat#31062) Acid Surrogate Mix (4/89 SOW) (cat#31063) 50ng each analyte on-column

561

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00682

Inj.: Inj. temp.: Carrier gas: Column flow: Oven temp.: Det.: Transfer line temp.: Scan range: Ionization: Mode:

1.0L splitless, double gooseneck inlet liner (cat.# 20784) pressure pulse injection, 30psig (0.5min) 275C helium, constant flow 1mL/min 35C (hold 1 min.) to 260C @ 20C/min. to 330C @ 6C/min (hold 1 min.) 5973 MS 280C 35-550amu EI TIC

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23.

24. bis(2-chloroisopropyl)ether 1,4-dioxane 25. acetophenone pyridine N-nitrosodimethylamine 26a. 4-methylphenol 26b. 3-methylphenol ethyl methacrylate 27. N-nitroso-di-n-propylamine 2-picoline N-nitrosomethylethylamine 28. nitrosopyrrolydine methyl methanesulfonate 29. o-toluidine 2-fluorophenol 30. 4-nitrosomorpholine N-nitrosodiethylamine 31. hexachloroethane ethyl methanesulfonate 32. nitrobenzene-d5 (SS) benzaldehyde 33. nitrobenzene phenol-d6 (SS) 34. N-nitrosopiperidine phenol 35. isophorone aniline 36. 2-nitrophenol pentachloroethane 37. 2,4-dimethylphenol bis(2-chloroethyl)ether 38. bis(2-chloroethoxy)methane 2-chlorophenol 39. 2,4-dichlorophenol 1,3-dichlorobenzene 40. 1,2,4-trichlorobenzene 1,4-dichlorobenzene-d4 41. ,-dimethylphenylamine (IS) 42. naphthalene-d8 (IS) 1,4-dichlorobenzene 43. naphthalene benzyl alcohol 44. 2,6-dichlorophenol 1,2-dichlorobenzene 45. 4-chloroaniline 2-methylphenol 46. hexachloropropene

47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70.

hexachlorobutadiene N-nitroso-n-butylamine 1,4-phenylenediamine caprolactam 4-chloro-3-methylphenol isosafrole 2-methylnaphthalene 1-methylnaphthalene hexachlorocyclopentadiene 1,2,4,5-tetrachlorobenzene isosafrole 2,4,6-trichlorophenol 2,4,5-trichlorophenol 2-fluorobiphenyl (SS) safrole biphenyl 2-chloronaphthalene 1-chloronaphthalene diphenyl ether 2-nitroaniline 1,4-naphthoquinone 1,4-dinitrobenzene dimethylphthalate 1,3-dinitrobenzene

71. 72. 73. 74. 75. 76. 77. 78. 79. 80. 81. 82. 83. 84. 85. 86. 87. 88. 89. 90. 91. 92. 93. 94.

2,6-dinitrotoluene acenaphthylene 1,2-dinitrobenzene 3-nitroaniline acenaphthene-d10 (IS) acenaphthene 2,4-dinitrophenol pentachlorobenzene 4-nitrophenol dibenzofuran 2,4-dinitrotoluene 1-naphthalamine 2,3,4,6-tetrachlorophenol 2,3,5,6-tetrachlorophenol 2-naphthylamine diethyl phthalate fluorene 4-chlorophenyl phenyl ether 2-methyl-5-nitroaniline 4-nitroaniline 4,6-dinitro-2-methylphenol diphenylamine azobenzene 2,4,6-tribromophenol (SS)

95. diallate 96. 1,3,5-trinitrobenzene 97. phenacetin 98. 4-bromophenyl phenyl ether 99. hexachlorobenzene 100. atrazine 101. 4-aminobiphenyl 102. pentachlorophenol 103. pentachloronitrobenzene 104. propyzamide 105. phenanthrene-d10 (IS) 106. phenanthrene 107. anthracene 108. carbazole 109. di-n-butylphthalate 110. 4-nitroquinoline-1-oxide 111. methapyriline 112. isodrin 113. fluoranthene 114. pyrene 115. Aramite (isomer) 116. p-terphenyl-d14 (SS) 117. Aramite (isomer) 118. dimethylaminoazobenzene

119. dichlorobenzilate 120. 3,3-dimethylbenzidine 121. butyl benzyl phthalate 122. Kepone 123. bis(2-ethylhexyl)adipate 124. 2-acetylaminofluorene 125. benz(a)anthracene 126. chrysene-d12 (IS) 127. chrysene 128. bis(2-ethylhexyl)phthalate 129. di-n-octyl phthalate 130. benzo(b)fluoranthene 131. 7,12dimethylbenzo(a)anthracene 132. benzo(k)fluoranthene 133. benzo(a)pyrene 134. perylene-d12 (IS) 135. 3-methylcholanthrene 136. dibenzo(a,j)acridine 137. indeno(1,2,3-cd)pyrene 138. dibenzo(a,h)anthracene 139. benzo(ghi)perylene

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562

Semivolatiles
Semivolatile Organics US EPA OLC 03.2 Rtx-5Sil MS

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00683

Rtx-5Sil MS 30m, 0.25mm ID, 0.25m (cat.# 12723) Sample: 1L. standards (component concentrations): cat.# 31812 (10g/mL), cat.# 31813 (50g/mL), cat.# 31026 (50g/mL), cat.# 31206 (20g/mL). 10ppm each component on-column, except as noted. Inj.: splitless (hold 0.4 min.), Drilled Uniliner (cat.# 20756) Inj. temp.: 275C Carrier gas: helium, constant flow Flow rate: 1mL/min. Oven temp.: 35C (hold 1 min.) to 260C @ 20C/min. to 330C @ 6C/min. (hold 1 min.) Det: MS Transfer line temp.: 280C Scan range: 35550amu Ionization: EI Mode: scan 1. 2. 3. 4. 5. 6. 7. 8a. 8b. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22 23. 24. benzaldehyde phenol bis(2-chloroethyl)ether 2-chlorophenol 1,2-dichlorobenzene-d4 (IS)* 2-methylphenol bis(2-chloroisopropyl)ether 4-methylphenol 3-methylphenol acetophenone N-nitroso-di-n-propylamine hexachloroethane nitrobenzene isophorone 2-nitrophenol 2,4-dimethylphenol bis(2-chloroethoxy)methane 2,4-dichlorophenol naphthalene-d8 (IS)* naphthalene 4-chloroaniline hexachlorobutadiene caprolactam 4-chloro-3-methylphenol 2-methylnaphthalene 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. hexachlorocyclopentadiene 1,2,4,5-tetrachlorobenzene 2,4,6-trichlorophenol 2,4,5-trichlorophenol** biphenyl 2-chloronaphthalene 2-nitroaniline** dimethylphthalate 2,6-dinitrotoluene acenaphthylene 3-nitroaniline** acenaphthene-d10 (IS) acenaphthene 2,4-dinitrophenol** 4-nitrophenol** dibenzofuran 2,4-dinitrotoluene diethyl phthalate fluorene 4-chlorophenyl phenyl ether 4-nitroaniline** 4,6-dinitro-2-methylphenol** diphenylamine 4-bromophenyl phenyl ether hexachlorobenzene 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. atrazine pentachlorophenol phenanthrene-d10 (IS)* phenanthrene anthracene di-n-butylphthalate fluoranthene pyrene butyl benzyl phthalate benzo(a)anthracene 3,3'-dichlorobenzidine** chrysene-d12 (IS)* chrysene bis(2-ethylhexyl)phthalate di-n-octyl phthalate benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene perylene-d12 (IS)* indeno(1,2,3-cd)pyrene dibenz(a,h)anthracene benzo(ghi)perylene

*20ppm **50ppm

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Semivolatiles
Semivolatile Organics US EPA Method 525.2 Rtx-5Sil MS

563

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00698

Rtx-5Sil MS 30m, 0.25mm ID, 0.25m (cat.# 12723) Sample: US EPA Method 525.2 Mix 1L 10ppm (20ppm IS) Standards used: 31824, 32420, 32421, 32422, 32423, 31825, 31826, 31828, 32291 Inj.: 1.0L 30psi 0.4min pulsed splitless (hold 0.4 min.), 4mm Drilled Uniliner inlet liner (cat.# 21055) Inj. temp.: 300C Carrier gas: helium, constant flow Flow rate: 0.8 mL/min. Oven temp.: 35C (hold 1 min.) to 270C @ 18C/min. (hold 0 min.) to 330C @ 5C/min. (hold 1 min.) Det: Agilent 5973 GC/MS Transfer line temp.: 280C Scan range: 40550 amu Solvent Delay 4.0 min. Tune DFTPP Ionization: EI

GC_EV00699

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26.

isophorone 2-nitro-m-xylene dichlorvos hexachlorocyclopentadiene EPTC mevinphos butylate vernolate dimethylphthalate etridiazole (Terrazole) 2,6-dinitrotoluene pebulate acenaphthylene acenaphthylene-d10 chloroneb 2-chlorobiphenyl (BZ#1) tebuthiuron 2,4-dinitrotoluene molinate diethyl phthalate fluorene propachlor ethoprop cycloate trifluralin chlorpropham

-BHC 2,3-dichlorobiphenyl (BZ#5) hexachlorobenzene atraton prometon simazine atrazine propazine -BHC pentachlorophenol -BHC (lindane) terbufos diazinon pronamide phenanthrene-d10 chlorothalonil phenanthrene methyl parathion OA disulfoton terbacil anthracene -BHC 2,4,5-trichlorobipenyl (BZ#29) 50. metribuzin 51. alachlor 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49.

52. 53. 54. 55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74.

simetryn ametryn prometryne heptachlor terbutryn di-n-butylphthalate bromacil 2,2',4,4'-tetrachlorobiphenyl (BZ#47) metolachlor chlorpyrifos cyanazine (Bladex) DCPA methyl ester (Dacthal) aldrin triadimefon diphenamid MGK-264 merphos heptachlor epoxide (isomer B) 2,2',3',4,6-pentachlorobiphenyl (BZ#98) heptachlor epoxide (isomer A) stirofos (tetrachlorvinphos) butachlor -chlordane

75. fenamiphos 76. pyrene-d10 77. -chlordane 78. endosulfan I 79. pyrene 80. trans-nonachlor 81. napropamide 82. 4,4'-DDE 83. tricyclazole 84. p-terphenyl-d14 85. 2,2',4,4',5,6'-hexachlorobiphenyl (BZ#154) 86. carboxin 87. dieldrin 88. chlorbenzilate 89. endrin 90. 4,4'-DDD 91. endosulfan II 92. endrin aldehyde 93. norflurazon 94. butyl benzyl phthalate 95. 4,4'-DDT 96. bis(2-ethylhexyl)adipate 97. endosulfan sulfate 98. hexazinone 99. triphenylphosphate

100. endrin ketone 101. 2,2',3,3',4,4',6-heptachlorobiphenyl (BZ#171) 102. methoxychlor 103. 2,2',3,3',4,5',6,6'-octachlorobiphenyl (BZ#207) 104. benzo(a)anthracene 105. chrysene-d12 106. chrysene 107. bis(2-ethylhexyl)phthalate 108. fenarimol 109. cis-permethrin 110. trans-permethrin 111. benzo(b)fluoranthene 112. benzo(k)fluoranthene 113. fluridone (Sonar) 114. benzo(a)pyrene 115. perylene-d12 116. dibenzo(a,h)anthracene 117. indeno(1,2,3-cd)pyrene 118. benzo(ghi)perylene

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564

Semivolatiles
Semivolatile Organics US EPA Method 625 Rtx-5Sil MS

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00700

Rtx -5Sil MS 30m, 0.25mm ID, 0.25m (cat.# 12723) Sample: US EPA Method 625 Mix 1L 10ppm (20ppm IS) Standards used: 31048, 31044, 31039, 31047, 31046, 31040, 31829 Inj.: 1.0L 20psi 0.3 min. pulsed splitless (hold 0.3 min.), 4mm Drilled Uniliner inlet liner (cat.# 21055) Inj. temp.: 300C Carrier gas: helium, constant flow Flow rate: 1.0mL/min. Oven temp.: 35C (hold 1 min.) to 270C @ 18C/min.(hold 0 min.) to 305C @ 5C/min. (hold 0 min.) To 330 @ 30C (hold 1 min.) Det: Agilent 5973 GC/MS Transfer line temp.: 280C Scan range: 35-450 amu Solvent Delay 3.0 min. Tune DFTPP Ionization: EI

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

N-nitrosodimethylamine pyridine-d5 (SS) 2-fluorophenol (SS) pentafluorophenol (IS) phenol bis(2-chloroethyl)ether 2-chlorophenol 1,3-dichlorobenzene 1,4-dichlorobenzene 1,2-dichlorobenzene bis(2-chloroisopropyl)ether N-nitroso-di-n-propylamine hexachloroethane nitrobenzene-d5 (IS) nitrobenzene isophorone 2-nitrophenol 2,4-dimethylphenol bis(2-chloroethoxy)methane 2,4-dichlorophenol 1,2,4-trichlorobenzene

22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42.

naphthalene hexachlorobutadiene 4-chloro-3-methylphenol hexachlorocyclopentadiene 2,4,6-trichlorophenol 2-chloronaphthalene dimethylphthalate 2,6-dinitrotoluene acenaphthylene acenaphthene 2,4-dinitrophenol 4-nitrophenol 2,4-dinitrotoluene diethyl phthalate fluorene 4-chlorophenyl phenyl ether 4,6-dinitro-2-methylphenol diphenylamine 4,4'-dibromooctafluorophenol (SS) 4-bromophenyl phenyl ether hexachlorobenzene

43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60.

pentachlorophenol phenanthrene anthracene di-n-butylphthalate 4,4'-dibromobiphenyl (IS) fluoranthene pyrene butyl benzyl phthalate benzo(a)anthracene chrysene bis(2-ethylhexyl)phthalate di-n-octyl phthalate benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene indeno(1,2,3,-cd)pyrene dibenzo(a,h)anthracene benzo(ghi)perylene

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Semivolatiles
Semivolatile Organics US EPA Skinner List Rtx-5Sil MS

565

Screening Method

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00684

Rtx-5Sil MS 30m, 0.25mm ID, 0.25m (cat.# 12723) Sample: Skinner SV MegaMix (cat.# 31690) B/N Surrogate Mix (cat.# 31024) Acid Surrogate Mix (cat.# 31025) SV Internal Standard Mix (cat.# 31206) Inj.: 1.0L splitless (hold 0.4 min.), Drilled Uniliner (cat.# 20756) Inj. temp.: 275C Carrier gas: helium, constant flow Flow rate: 1mL/min. Oven temp.: 35C (hold 1 min.) to 260C @ 20C/min. to 300C @ 6C/min. (hold 1 min.) Det: MS Transfer line temp.: 280C Scan range: 35-550amu Ionization: EI Mode: scan 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. pyridine 2-fluorophenol phenol-d6 (SS) phenol 1,3-dichlorobenzene 1,4-dichlorobenzene-d4 (IS) 1,4-dichlorobenzene 1,2-dichlorobenzene 2-methylphenol indene 4-methylphenol 3-methylphenol 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. nitrobenzene-d5 (SS) 2,4-dimethylphenol naphthalene-d8 (IS) naphthalene quinoline 1-methylnaphthalene 2-fluorobiphenyl (SS) dimethylphthalate acenaphthene-d10 (IS) acenaphthene 2,4-dinitrophenol 4-nitrophenol 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. diethyl phthalate fluorene 2,4,6-tribromophenol (SS) phenanthrene-d10 (IS) phenanthrene anthracene di-n-butylphthalate fluoranthene pyrene p-terphenyl-d14 (SS) benzo(a)anthracene chrysene-d12 (IS) 37. 38. 39. 40. 41. 42. 43. 44. 45. chrysene bis(2-ethylhexyl)phthalate benzo(b)fluoranthene benzo(k)fluoranthene benzo(a)pyrene perylene-d12 (IS) dibenzo(a,h)acridine indeno(1,2,3-cd)pyrene dibenzo(a,h)anthracene

a plus 1 story
Restek offers a wide range of columns and accessories for the environmental analyses performed in my lab. I am satisfied with the Restek products I have been using for several years-particularly the Rtx-5Sil MS and Rtx-CLPesticides columns and the deactivated inlet sleeves. The quality of the technical support provided by Restek is a plus. Michel Letort, Veolia Environnement (Paris, France)

Phone: 800-356-1688 or 814-353-1300 www.restek.com

566

Pesticides
EDB / DBCP US EPA Method 504.1 Rtx-CLPesticides & Rtx-CLPesticides2
Rtx-CLPesticides
5

free literature
Dual-column analysis

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

8 6

1 7

min.

10

GC Analysis of US EPA Method 504.1 Organochlorine Pesticides, Using the Rtx-CLPesticides and Rtx-CLPesticides2 Columns (lit. cat.# 59539) A versatile column pair for analyzing organochlorine pesticides, herbicides, or PCBs Analysts following Method 504.1 in monitoring 1,2-dibromoethane (EDB), 1,2-dibromo-3-chloropropane (DBCP), and 1,2,3-trichloropropane (TCP) in drinking water will value Rtx-CLPesticides and Rtx-CLPesticides2 columns because this same primary column/confirmation column pair can be used to perform numerous related analyses: organochlorine pesticides (e.g., by EPA Method 608 or 8081), herbicides, or polychlorinated biphenyls (PCBs). Details in this 2-page note show EDB, DBCP and TCP are fully resolved from , common interference compounds, per requirements of Method 504.1.

Rtx-CLPesticides2
5

2 3

4 1

Rtx-CLPesticides and Rtx-CLPesticides2 columns also are ideal for:


7

min.

6 GC_EV00020

10

Triazine herbicides (lit. cat.# 59101) PCBs (lit. cat.# 59120) Haloacetic acids (lit. cat.# 59175) Polynuclear aromatic hydrocarbons (lit. cat.# 59196A)

1. chloroform 2. bromodichloromethane 3. chlorodibromomethane 4. 1,2-dibromoethane (EDB) 5. 1,1,1,2-tetrachloroethane 6. bromoform 7. 1,2,3-trichloropropane 8. 1,2-dibromo-3-chloropropane (DBCP)

30m, 0.32mm ID, 0.50m Rtx-CLPesticides (cat.# 11139) and 30m, 0.32mm ID, 0.25m Rtx-CLPesticides2 (cat.# 11324), 0.32mm ID guard column (cat.# 10044), universal angled Y Press-Tight connector (cat.# 20403). Direct injection using a Uniliner liner (cat.#20335). On-column conc.: 10pg each compound. Oven temp.: 35C (hold 2 min.) to 300C @ 12C/min. Inj./det. temp.: 200C/300C Carrier gas: helium, 12psi constant pressure.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Pesticides
Organochlorine Pesticides US EPA Method 508 Rtx-CLPesticides & Rtx-CLPesticides2
14 1 5,6 18,19

567

13

RtxCLPesticides
4 8,9

16, 17

15

24,25 22 26 28 23 27 32

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

10,11,12

31 20,21 36 33

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

hexachloropentadiene etridiazole chlorneb hexachlorobenzene propachlor -BHC simazine -BHC atrazine trifluralin pentachloronitrobenzene -BHC -BHC metribuzin heptachlor aldrin chlorothalonil 4,4'-dibromobiphenyl alachlor metalachlor

21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

DCPA (Dacthal) heptachlor epoxide -chlordane cyanazine -chlordane 4,4'-DDE endosulfan I dieldrin endrin chlorobenzilate 4,4'-DDD endosulfan II 4,4'-DDT endrin aldehyde methoxychlor endosulfan sulfate cis-permethrin trans-permethrin

34 3 2

29 38 35 37 7

min. 6

10
4 6

12
17

14

16

18

20

14 11,8 1 16 13

22

Rtx-CLPesticides2

26 15 23 25 27 28

21,18 3 12

32 36 31 33 34

24

30m, 0.32mm ID, 0.50m Rtx -CLPesticides (cat.# 11139) 30m, 0.32mm ID, 0.25m Rtx-CLPesticides2 (cat.# 11324) EPA 508.1 list w/ added compounds.

19 10 2 20

29, 30 38 35

Oven temp.: Inj.: Dead time: Head pressure: Carrier gas: Flow:

120C (hold 1 min.) to 300C @ 9C/min. (hold 10 min.) direct, Uniliner inlet liner, 200C 1.797 (Rtx-CLPesticides), 1.663 (Rtx-CLPesticides2) 12 psi (constant) helium 2.1mL/min. @ 120C

9 37 5 7

min. 6

10

12

14
GC_EV00082

16

18

20

Phone: 800-356-1688 or 814-353-1300 www.restek.com

568

Pesticides
Organochlorine Pesticides US EPA Method 508 Rtx-5
Peak 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. etridiazole chlorneb propachlor trifluralin -BHC hexachlorobenzene -BHC -BHC PCNB (impurity) PCNB (IS) -BHC chlorothalonil heptachlor aldrin DCPA DCB (SS) heptachlor epoxide -chlordane endosulfan I -chlordane dieldrin endrin endosulfan II chlorobenzilate 4,4'-DDD endrin aldehyde endosulfan sulfate 4,4'-DDT methoxychlor cis-permethrin trans-permethrin Conc. (pg/L) L 50 1000 1000 50 20 10 20 30 100 100 20 50 20 30 50 5000 30 30 30 30 40 30 30 1000 50 50 30 120 100 1000 1000
2 3 9 30 10 16 21 28 31

12

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

8 14 5 1 11 13 4 6 7 15 17 19 18 20 23 22

26 24 25 29

27

min.

12

16

20

24

28 GC_EV00083

32

36

40

44

48

52

30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 2.0L splitless injection Splitless hold: Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: 0.75 min. 60C to 300C @ 4C/min. (hold 10 min.) 250C / 320C helium 30cm/sec. (flow rate: 1.4cc/min.)

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Pesticides
Organochlorine Pesticides US EPA Method 8081 Rtx-CLPesticides2
Compound 1. 2,4,5,6-tetrachloro-m-xylene (ss) 2. -BHC 3. -BHC 4. -BHC 5. -BHC 6. heptachlor 7. aldrin 8. heptachlor epoxide 9. -chlordane 10. -chlordane 11. endosulfan I 12. 4,4'-DDE 13. dieldrin 14. endrin 15. 4,4'-DDD 16. endosulfan II 17. endrin aldehyde 18. 4,4'-DDT 19. endosulfan sulfate 20. methoxychlor 21. endrin ketone 22. decachlorobiphenyl (ss) Conc. (ppb) 80 80 80 80 80 80 80 80 80 80 80 160 160 160 160 160 160 160 160 800 160 160 RT (min.) 2.415 2.916 3.192 3.260 3.476 3.518 3.749 4.149 4.277 4.376 4.412 4.489 4.594 4.794 4.866 4.934 5.167 5.078 5.368 5.582 5.790 6.940

569

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Rtx-CLPesticides2 30m, 0.32mm ID, 0.25m (cat.# 11324), intermediate-polarity deactivated guard column, 5m x 0.32mm ID (cat.# 10044) Sample: Organochlorine Pesticide Mix AB #2 (cat.# 32292), 2,4,5,6-tetrachloro-m-xylene (ss) (cat.# 32027), decachlorobiphenyl (ss) (cat.# 32029), diluted in hexane, on-column amounts listed on figure Inj.: 1.0L splitless (hold 0.75 min.), 4mm Drilled Uniliner inlet liner (cat.# 21055) Inj. temp.: 225C Carrier gas: hydrogen, constant pressure Linear velocity: 77cm/sec. @ 140C Oven temp.: 140C (hold 0.5 min.) to 268C @ 30C/min., to 290C @ 11C/min., to 330C @ 25C/min. (hold 5 min.) Det.: ECD @ 320C

GC_EV00734

Organochlorine Pesticides US EPA Method 8081 Rtx-440

Rtx-440 30m, 0.32mm ID, 0.50m (cat.# 12939), intermediate-polarity deactivated guard column, 5m x 0.32mm ID (cat.# 10044) Sample: Organochlorine Pesticide Mix AB #2 (cat.# 32292), 2,4,5,6-tetrachlorom-xylene (ss) (cat.# 32027), decachlorobiphenyl (ss) (cat.# 32029), diluted in hexane, on-column amounts listed on figure Inj.: 1.0L splitless (hold 0.75 min.), 4mm Drilled Uniliner inlet liner (cat.# 21055) Inj. temp.: 225C Carrier gas: hydrogen, constant pressure Linear velocity: 73cm/sec. @ 140C Oven temp.: 140C (hold 0.5 min.) to 268C @ 30C/min., to 290C @ 11C/min., to 330C @ 25C/min. (hold 5 min.) Det.: ECD @ 320C Compound Conc. (ppb) RT (min.) 1. 2,4,5,6-tetrachloro-m-xylene (ss) 80 3.538 2. -BHC 80 3.931 3. -BHC 80 4.211 4. -BHC 80 4.356 5. -BHC 80 4.560 6. heptachlor 80 4.715 7. aldrin 80 4.995 8. heptachlor epoxide 80 5.346 9. -chlordane 80 5.576 10. -chlordane 80 5.653 11. endosulfan I 80 5.698 12. 4,4-DDE 160 5.800 13. dieldrin 160 5.959 14. endrin 160 6.190 15. 4,4-DDD 160 6.309 16. endosulfan II 160 6.404 17. endrin aldehyde 160 6.543 18. 4,4-DDT 160 6.662 19. endosulfan sulfate 160 6.810 20. methoxychlor 800 7.198 21. endrin ketone 160 7.355 22. decachlorobiphenyl (ss) 160 8.813

GC_EV00733

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570

Pesticides
Organochlorine Pesticides US EPA Method 8081 Rtx-CLPesticides & Rtx-CLPesticides2 (0.32mm ID)
Rtx-CLPesticides 30m, 0.32mm ID, 0.50m (cat.# 11139)
19

22

Rtx-CLPesticides2 30m, 0.32mm ID, 0.25m (cat.# 11324)

19

22

11 13 11 13 15 17 2 3 5 14 6 7 8 9 12 4 10 4 10 12 18 20 3 5 7 6 8 9 1 16 21 1 2 16 17

15 14 18 20

21

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

min. 10

12

14

16

18

20

22

min. 10 GC_EV00075

12

14

16

18

20

22

24

16160pg Organochlorine Pesticide Mix AB#2 (cat.# 32292), Pesticide Surrogate Mix (cat. # 32000) Oven temp.: 120C (hold 1 min.) to 300C (hold 10 min.) @ 9C/min. Inj.: direct, Uniliner liner (cat.# 20335), 200C Detector: ECD, 300C with anode purge Dead time: 1.9 min. Head pressure: 8.7psi (constant) Flow rate: 1.3mL/min. @ 120C, helium

On-column concentration:

Organochlorine Pesticides US EPA Method 8081 Rtx-CLPesticides & Rtx-CLPesticides2 (0.53mm ID)
19

Rtx-CLPesticides 30m, 0.53mm ID, 0.50m (cat.# 11140)

19

Rtx-CLPesticides2 30m, 0.53mm ID, 0.42m (cat.# 11340)


22

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

2,4,5,6-tetrachloro-m-xylene -BHC (-HCH) -BHC (lindane) -BHC (-HCH) -BHC (-HCH) heptachlor aldrin heptachlor epoxide -chlordane -chlordane 4,4'-DDE endosulfan I dieldrin endrin 4,4'-DDD endosulfan II 4,4'-DDT endrin aldehyde methoxychlor endosulfan sulfate endrin ketone decachlorobiphenyl

22 11 1 2 3 6 4 5 7 8 10 9 12 13 17 15 18 14 16 20

1 11 2 13 3 5 6 7 9 8 10 4 15 14 16 17 20 18 21

21

12

min. 10

12

14

16

18

20

22

min. 10 GC_EV00547

12

14

16

18

20

22

24

On-column concentration: Oven temp.: Inj. port: Detector: Dead time: Head pressure: Flow rate:

16160pg organochlorine pesticide Mix AB#2 (cat.# 32292) 120C (hold 1 min.) to 300C (hold 10 min.) @ 9C/min. direct, Uniliner liner (cat.# 20335), 200C ECD, 300C with anode purge 1.9 min. 3psi (constant) 2.83mL/min. @ 120C, helium

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Pesticides
Organochlorine Pesticides US EPA Method 8081 Rtx-CLPesticides

571

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

2,4,5,6-tetrachloro-m-xylene -BHC -BHC -BHC -BHC heptachlor aldrin heptachlor epoxide -chlordane -chlordane 4,4'-DDE

12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

endosulfan I dieldrin endrin 4,4'-DDD endosulfan II 4,4'-DDT endrin aldehyde methoxychlor endosulfan sulfate endrin ketone decachlorobiphenyl

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Rtx-CLPesticides w/Drilled Uniliner inlet liner

GC_EV00635

Rtx-CLPesticides2 w/Drilled Uniliner inlet liner

GC_EV00636

Rtx-CLPesticides 30m, 0.32mm ID, 0.50m (cat.# 11139) Rtx-CLPesticides2 30m, 0.32mm ID, 0.25m (cat.# 11324) Sample: 20400g/mL Organochlorine Pesticide Mix AB #2 (cat.# 32292) in hexane:toluene (1:1) 200g/mL Pesticide Surrogate Mix (cat.#32000 ) in acetone Inj.: 1.0L direct, open-top Drilled Uniliner inlet liner (cat.# 21054) Inj. temp.: 225C Carrier gas: helium, constant pressure Linear velocity: 53cm/sec. @ 110C Oven temp.: 110C (hold 1 min.) to 245C @ 20C/min. to 310C (hold 1 min.) Det.: ECD @ 330C

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572

Pesticides
Organochlorine Pesticides US EPA Method 8081 Stx-CLPesticides & Stx-CLPesticides2
19

for more info


Stx-CLPesticides and Stx-CLPesticides2 Columns Provide Improved System Inertness for Chlorinated Pesticides Analysis (lit. cat.# 59351B) An inert pathway assures maximum recovery of active chlorinated pesticides Concern about losses of endrin and other active chlorinated pesticides generally is focused on the injection port, but a properly deactivated injection system and an inert analytical column, in combination, are needed to minimize breakdown. Inert Siltek-treated inlet liners, guard columns and Stx-CLPesticides and StxCLPesticides2 analytical columns meet this requirement. This 2-page note also describes deactivated connectors and chromatographic conditions for operating the primary and confirmation column in parallel.

Stx-CLPesticides 30m, 0.32mm ID, 0.5m (cat.# 11544)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

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A Siltek-deactivated inlet liner improves endrin response, relative to conventionally deactivated liners.
5 6 7 1

11 13 14 16 15 17 20 18 10 9 12 8 22 4 2 3 21

10

11

12

13

min.

Stx-CLPesticides2 30m, 0.32mm ID, 0.25m (cat.# 11444)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

2,4,5,6 tetrachloro-m-xylene (SS) -BHC -BHC -BHC -BHC heptachlor aldrin heptachlor epoxide -chlordane -chlordane 4,4'-DDE endosulfan I dieldrin endrin 4,4'-DDD endosulfan II 4,4'-DDT endrin aldehyde methoxychlor endosulfan sulfate endrin ketone decachlorobiphenyl (SS)

GC_EV00512

Inj.: Oven temp.: Inj. & det. temp.: Carrier gas: Dead time: Inlet liner: Make-up gas:

1L direct injection of 20/40/200ng/mL std. concentration in hexane 110C (hold 1 min.) to 245C @ 20C/min. to 300C @ 6C/min. 210C / 310C helium 0.8min. @ 120C Siltek-deactivated Drilled Uniliner inlet liner (cat.# 21055-214.5) nitrogen

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Pesticides
Organochlorine Pesticides US EPA Method 8081A Rtx-CLPesticides & Rtx-CLPesticides2
3

573

free literature
Rtx-CLPesticides
26

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

29

1. dibromochloropropane 2. hexachlorocyclopentadiene 3. 2,4,5,6-tetrachloro-m-xylene 4. hexachlorobenzene 5. cis-diallate 6. -BHC 7. trans-diallate 8. -BHC 9. -BHC 10. -BHC 11. heptachlor 1 12. aldrin 13. isodrin 14. heptachlor epoxide 15. -chlordane 16. -chlordane 17. 4,4'-DDE 18. endosulfan I 19. dieldrin 20. chlorobenzilate 21. endrin 22. 4,4'-DDD 23. endosulfan II 24. 4,4'-DDT 25. endrin aldehyde 26. methoxychlor 27. endosulfan sulfate 28. endrin ketone 29. decachlorobiphenyl

17 19 6,7 4 2 10 8 11 12 16 15 14 13 21 25 18 20,22 23 24 28 27

9 5

GC Analysis of US EPA Method 504.1 Organochlorine Pesticides, Using the Rtx-CLPesticides and Rtx-CLPesticides2 Columns (lit. cat.# 59539)

A versatile column pair for analyzing organochlorine pesticides, herbicides, or PCBs


Analysts following Method 504.1 in monitoring 1,2-dibromoethane (EDB), 1,2-dibromo-3chloropropane (DBCP), and 1,2,3-trichloropropane (TCP) in drinking water will value RtxCLPesticides and Rtx-CLPesticides2 columns because this same primary column/confirmation column pair can be used to perform numerous related analyses: organochlorine pesticides (e.g., by EPA Method 608 or 8081), herbicides, or polychlorinated biphenyls (PCBs). Details in this 2-page note show EDB, DBCP , and TCP are fully resolved from common interference compounds, per requirements of Method 504.1.

min.

10

15

20

25

Rtx-CLPesticides2
29

17 19 23

30m, 0.32mm ID, 0.50m Rtx -CLPesticides (cat.# 11139) 30m, 0.32mm ID, 0.25m Rtx-CLPesticides2 (cat.# 11324) On-column conc.: 16160pg Oven temp.: 80C (hold 1 min.) to 300C @ 10C/min. (hold 15 min.) Inj.: direct, Uniliner inlet liner (cat.# 20335) Det.: ECD, 300C, with anode purge Dead time: 1.9 min. Head pressure: 8.7psi (constant) Flow rate: helium @ 1.3mL/min. @ 120C

26 28 6 8 4 10 12 14 11 9 13 16 15 22 21

Rtx-CLPesticides and Rtx-CLPesticides2 columns also are ideal for:

24 27 25

Triazine herbicides (lit. cat.# 59101) PCBs (lit. cat.# 59120) Haloacetic acids (lit. cat.# 59175) Polynuclear aromatic hydrocarbons (lit. cat.# 59196A)

2 1

18

57 20

min.

10

15 GC_EV00077

20

25

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574

Pesticides
Organochlorine Pesticides US EPA Method 8081 Rtx-XLB
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 2,4,5,6-tetrachloro-m-xylene (ss) -BHC -BHC -BHC -BHC heptachlor aldrin heptachlor epoxide -chlordane -chlordane endosulfan I 4,4'-DDE dieldrin endrin 4,4'-DDD endosulfan II endrin aldehyde 4,4'-DDT endosulfan sulfate methoxychlor endrin ketone decachlorobiphenyl (ss)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00720

Rtx-XLB 30m, 0.32 ID, 0.5m (cat.# 12839) Sample: Organochlorine Pesticide Mix AB (cat.# 32292) 80/160ppb in hexane 2,4,5,6-tetrachloro-m-xylene (cat.# 32027) surrogate, 80ppb decachlorobiphenyl (cat.# 32029) surrogate, 160ppb Inj.: 1.0L splitless (0.75 min. hold), 4mm Drilled Uniliner inlet liner (cat.# 21055) Inj. temp.: 220C Carrier gas: hydrogen, constant pressure Linear velocity: 60cm/sec. @ 120C Oven temp.: 120C (hold 0.5 min.) to 260C @ 29C/min. (hold 2.5 min.), to 330C @ 28C/min. (hold 3 min.) Det.: ECD @ 320C

Searching for a chromatogram?

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Pesticides
Organochlorine Pesticides US EPA Method 8081A Rtx-XLB
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 1,2-dibromo-3-chloropropane hexachlorocyclopentadiene 2,4,5,6-tetrachloro-m-xylene (ss) cis-diallate trans-diallate -BHC hexachlorobenzene -BHC -BHC -BHC heptachlor aldrin isodrin heptachlor epoxide 2,4'-DDE -chlordane -chlordane endosulfan I 4,4'-DDE 2,4'-DDD dieldrin chlorobenzilate endrin 2,4'-DDT 4,4'-DDD endosulfan II Kepone endrin aldehyde 4,4'-DDT endosulfan sulfate methoxychlor endrin ketone Mirex decachlorobiphenyl (ss)

575

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00721

Rtx-XLB 30m, 0.32mm ID, 0.5m (cat.# 12839) Sample: 8081A pesticides, 80-160ppb in hexane Inj.: 1.0L splitless (hold 0.75 min.), 4mm Drilled Uniliner inlet liner (cat.# 21055) Inj. temp.: 220C Carrier gas: hydrogen, constant pressure Linear velocity: 60cm/sec. @ 120C Oven temp.: 120C (hold 0.5 min.) to 260C @ 29C/min. (hold 2.5 min.), to 330C @ 28C/min. (hold 3 min.) Det.: ECD @ 320C 8081A Pesticides/Surrogates 8080 Organochlorine Pesticide Mix AB #2 (20 components) 8081a Organochlorine Pesticide Mix C #2 (7 components) 2,4'-DDT 2,4'-DDD 2,4'-DDE Kepone Mirex 2,4,5,6-tetrachloro-m-xylene (ss, 20ppb) decachlorobiphenyl (ss, 40ppb) cat.# 32292 cat.# 32295 cat.# 32200 cat.# 32098 cat.# 32099 custom custom cat.# 32027 cat.# 32029

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576

Pesticides
Organochlorine Pesticides US EPA Method 8081 Rtx-35
1 11 22

16 13 20

19

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

2 7 3 5 6 12 8

21 9 10 15 14 18 17

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

2,4,5,6-tetrachloro-m-xylene (surrogate) -BHC -BHC (lindane) -BHC -BHC heptachlor aldrin heptachlor epoxide -chlordane -chlordane 4,4'-DDE endosulfan I dieldrin endrin 4,4'-DDD endosulfan II 4,4'-DDT endrin aldehyde methoxychlor endosulfan sulfate endrin ketone decachlorobiphenyl (surrogate)

min.

12

15

18 GC_EV00079

21

24

30m, 0.32mm ID, 0.50m Rtx-35 (cat.# 10439) Oven temp.: 120C (hold 1 min.) to 285C @ 8.5C/min. (hold 6 min.). Inj.: direct, Uniliner inlet liner (cat.# 20335), 200C. Det.: ECD, 300C with anode purge Flow rate: helium @ 2.1mL/min. set @ 120C

Organochlorine Pesticides US EPA Method 8081 Rtx-CLPesticides


Fast Analysis!

22

11 1 12 2 3 5 6 7 8 14 4 9 10 15 13 16 17 18 19 21 20

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.
5.0 6.0

2,4,5,6-tetrachloro-m-xylene (surrogate) -BHC -BHC -BHC -BHC heptachlor aldrin heptachlor epoxide -chlordane -chlordane 4,4'-DDE endosulfan I dieldrin endrin 4,4'-DDD endosulfan II 4,4'-DDT endrin aldehyde methoxychlor endosulfan sulfate endrin ketone decachlorobiphenyl (surrogate)

min.

1.0

2.0

3.0 GC_EV00080

4.0

15m, 0.25mm ID, 0.25m Rtx-CLPesticides (cat.# 11120). 2L splitless injection. Conc.: 40 to 80ppb. Oven temp.: 125C to 290C @ 29C/min. (hold 3 min.) Inj./det. temp.: 175C/300C Carrier gas: hydrogen @ 20psi constant pressure. Courtesy of Bill DesJardins, ITSEnvironmental, Colchester, Vermont

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Pesticides
Organochlorine Pesticides US EPA Method 8081 Rtx-5
20 22

577

Organochlorine Pesticides US EPA Method 8081 Rtx-1701


20

22

1 2 3 7 6 4 5

12 21 13 14 16 17 19 15 18 9 8 10 11

min.

10 GC_EV00408

20

30

30m, 0.53mm ID, 0.50m Rtx-5 (cat.# 10240) 1.0L direct injection Conc.: 80800ppb (ng/mL). Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: ECD sensitivity: 150C (hold 5 min.) to 275C @ 4C/min. (hold 5 min.). 200C / 275C helium 40cm/sec. set @ 150C 5.12 x 10-10 AFS

2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

1. 2,4,5,6-tetrachloro-m-xylene (surrogate) -BHC -BHC heptachlor aldrin -BHC -BHC heptachlor epoxide endosulfan I -chlordane -chlordane 4,4'-DDE dieldrin endrin 4,4'-DDD endosulfan II 4,4'-DDT endrin aldehyde endosulfan sulfate methoxychlor endrin ketone decachlorobiphenyl (surrogate)

12 13

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

1 2 34 5 6

15 16 17

19 21

11 7 8 10 9

14 18

min.

10 GC_EV00409

20

30

30m, 0.53mm ID, 0.25m Rtx-1701 (cat.# 12025) 1.0L direct injection Conc.: 80800ppb (ng/mL). Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: ECD sensitivity: 150C (hold 5 min.) to 275C @ 4C/min. (hold 5 min.). 200C/275C helium 40cm/sec. set at 150C. 5.12 x 10-10 AFS

EPA Method 8081 Chlorinated Pesticides Rtx-50


20

22

12 13

21 14 16 17 15 19

3 5

18 6 7 8 10 9 11

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

2,4,5,6-tetrachloro-m-xylene (SS) -BHC -BHC -BHC heptachlor -BHC aldrin heptachlor epoxide -chlordane -chlordane endosulfan I 4,4'-DDE dieldrin endrin 4,4'-DDD endosulfan II 4,4'-DDT endrin aldehyde endosulfan sulfate methoxychlor endrin ketone decachlorobiphenyl

min.

10 GC_EV00410

15

20

25

30m, 0.53mm ID, 0.83m Rtx-50 (cat.# 10569) 1.0L direct injection Conc.: 80800ppb (ng/mL). Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: ECD sensitivity: 150C (hold 5 min.) to 275C @ 8C/min. (hold 5 min.) 200C / 275C helium 40cm/sec. set @ 150C 5.12 x 10-10 AFS

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578

Pesticides
Organophosphorus Pesticides US EPA Method 8141A Rtx-OPPesticides2
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. dichlorvos hexamethylphosphoramide mevinphos trichlorfon TEPP demeton-O thionazin tributyl phosphate (IS) ethoprop naled sulfotepp phorate dicrotophos demeton-S monocrotophos terbufos dimethoate dioxathion 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. fonophos diazinon disulfoton phosphamidon isomer dichlorofenthion chlorpyrifos methyl phosphamidon parathion-methyl ronnel fenitrothion aspon malathion chlorpyrifos trichloronate parathion-ethyl fenthion merphos chlorfenvinphos 37. 38. 39. 40. 41. 42. 43 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. crotoxyphos stirofos tokuthion merphos oxone (breakdown product) ethion fensulfothion bolstar carbophenothion famphur triphenyl phosphate (SS) EPN phosmet leptophos tri-o-cresyl phosphate azinphos-methyl azinphos-ethyl coumaphos

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00602

Column: Sample:

Inj.:

Rtx-OPPesticides2, 30m, 0.25mm ID, 0.25m (cat.# 11243) US EPA Method 8141A Custom Standard Mix 1L 100ppm (100ng on column) Triphenylphosphate Standard (cat.# 32281) Tributylphosphate Standard (cat.# 32280) 8140/8141 OP Pesticides Calibration Mix A (cat.# 32277) 8141 OP Pesticides Calibration Mix B (cat.# 32278) Custom Standard Mixes: Call Restek for More Information 1.0L splitless (hold 0.4 min.), 4mm double gooseneck inlet liner (cat.# 20785)

Inj. temp.: Carrier gas: Flow rate: Oven temp.: Det: Transfer line temp.: Scan range: Ionization:

250C helium, constant flow 1.0mL/min. 80C (hold 0.5 min.) to 140C @ 20C/min. to 210C @ 4C/min. (hold 1 min.) to 280C @ 30C (hold 5 min.) MS 280C 35-400amu EI

for more info


GC Columns for Pesticide Analyses Choose from 9 capillary GC phases for pesticide analyses and more than 50 combinations of column ID and phase film thickness. For descriptions of special purpose columns, see pages 22-23. To locate a column type in this catalog, see page 13.

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Pesticide Standards

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Pesticides
Organophosphorus Pesticides US EPA Method 8141A Rtx-OPPesticides & Rtx-OPPesticides2
dual-column injector GC: splitless, purge on 1.0 min. constant pressure Oven temp.: 80C (hold 0.5 min.) to 280C @ 12C/min. (hold 10 min.) Injector: 200C Inlet liner: 4mm single gooseneck Siltek inlet liner Detector: FPD @ 250C Dead time: 1.03 min. @ 80C Injection: 1L US EPA Method 8141A Custom Standard Mixes (100ng/mL) Triphenylphosphate Standard (cat.# 32281) Tributylphosphate Standard 1 (cat.# 32280) 8140/8141 OP Pesticides Calibration Mix A (cat.# 32277) 8141 OP Pesticides Calibration Mix B (cat.# 32278) 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. dichlorvos hexamethylphosphoramide mevinphos trichlorfon TEPP demeton-O tributyl phosphate (SS) thionazin ethoprop naled sulfotepp phorate dicrotophos monocrotophos demeton-S terbufos dimethoate diazinon dioxathion fonophos disulfoton phosphamidon isomer (breakdown product) dichlorofenthion phosphamidon chlorpyrifos methyl parathion-methyl ronnel aspon fenitrothion malathion chlorpyrifos trichloronate parathion-ethyl fenthion merphos chlorfenvinphos crotoxyphos stirofos tokuthion merphos oxone (breakdown product) ethion fensulfothion bolstar carbophenothion famphur triphenyl phosphate (SS) EPN phosmet leptophos tri-o-cresyl phosphate azinphos-methyl azinphos-ethyl coumaphos
3 10,11 5,20 44,41 28 8 9 27,35 12 13,14 17 23 16 19,21 25 18 31 24 39 38 43 37 49 2 4 15 46 42 51 34 47,48 36,33 40 29 26,30

579

Rtx-OPPesticides 30m, 0.32mm ID, 0.50m (cat.# 11239)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

32

45

50 52 6 53 22

min.

10
11 8

12

14
28 32,33

16

18

20

22

Rtx-OPPesticides2 30m, 0.32mm ID, 0.32m (cat.# 11241)

3 7 9 12

18 17 19,20 21 16 25 23 27 29 30 41 26 34 31

1 5 24 2 4 15 36 14 37 47 10 6 35 13 22 40 49 48 38 39 42 43 44 45 46

50

51

52 53

min. 6

10

12

14
GC_EV00394

16

18

20

Phone: 800-356-1688 or 814-353-1300 www.restek.com

580

Pesticides
Organophosphorus Pesticides US EPA Method 8140/8141/8141A Rtx-1701
7,8 (SS) 2 49

12

26

23,24

41,42

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

30m, 0.32mm ID, 0.25m Rtx-1701 (cat.# 12024) 1L US EPA Method 8141A Custom Standard Mixes (200ng/mL) Triphenylphosphate Standard (cat.# 32281) Tributylphosphate Standard (cat.# 32280) 8140/8141 OP Pesticides Calibration Mix A (cat.# 32277) 8141 OP Pesticides Calibration Mix B (cat.# 32278) Splitless hold time: 1.0 min. Oven temp.: 100C to 180C @ 10C/min. (hold 2 min.), to 300C @ 18C/min. (hold 3 min.) Inj. / det. temp.: 250C / 280C FPD
1

25 21 20 6 3 10,11 13,14,15 16,17 18, 19 9 22 5

29,30

35 33 32 27, 34 28 36 37 40 31 38 39

43(SS) 47 45 46 48 44 50 51 52

53

min. 1. 2. 3. 4 5. 6. 7. 8. 9. 10. 11. dichlorvos hexamethylphosphoramide mevinphos trichlorfon demeton-O thionazin ethoprop tributyl phosphate (SS) TEPP naled phorate 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. sulfotepp terbufos demeton-S diazinon fonophos dicrotophos dioxathion disulfoton dichlorofenthion monocrotophos chlorpyrifos methyl

2 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33.

8 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44.

10
GC_EV00411

12

14 45. 46. 47. 48. 49. 50. 51. 52. 53.

16

18

dimethoate phosphamidon isomer ronnel merphos aspon chlorpyrifos trichloronate parathion-methyl phosphamidon fenthion malathion

fenitrothion parathion-ethyl chlorfenvinphos tokuthion merphos oxone crotoxyphos stirofos ethion bolstar carbophenothion fensulfothion

triphenyl phosphate (SS) famphur leptophos EPN tri-o-cresyl phosphate phosmet azinphos-methyl azinphos-ethyl coumaphos

Organophosphorus Pesticides US EPA Method 8140/8141/8141A Rtx-35


Column: Sample: Rtx-35 30m, 0.32mm ID, 0.25m (cat.# 10424) 0.1g/mL US EPA Method 8141A Custom Standard Mixes (100ng/mL) Triphenylphosphate Standard (cat.# 32281) Tributylphosphate Standard (cat.# 32280) 8140/8141 OP Pesticides Calibration Mix A (cat.# 32277) 8141 OP Pesticides Calibration Mix B (cat.# 32278) Inj.: 0.5L splitless (hold 5 min.), Siltek Drilled Uniliner inlet liner (cat.# 21054-214.1) Inj. temp.: 220C Carrier gas: helium, constant pressure Linear velocity: 42cm/sec. @ 60C Oven temp.: 100C to 180C @10C/min. (hold 2 min.) to 300C @ 18C/min. (hold 10 min.) Det.: FPD @ 280C 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. dichlorvos hexamethylphosphoramide mevinphos trichlorfon tributyl phosphate (SS) demeton-O TEPP thionazin ethoprop sulfotepp naled phorate dicrotophos demeton-S terbufos monocrotophos diazinon fonophos disulfoton 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. dioxathion dimethoate phosphamidon isomer dichlorofenthion chlorpyrifos methyl phosphamidon ronnel parathion-methyl aspon trichloronate chlorpyrifos fenitrothion merphos malathion parathion-ethyl fenthion chlorfenvinphos crotoxyphos merphos oxone 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. tokuthion stirofos ethion bolstar fensulfothion carbofenothion famphur triphenyl phosphate (SS) EPN phosmet leptophos tri-o-cresyl phosphate azinphos-methyl azinphos-ethyl coumaphos

GC_EV00696

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Pesticides
Organophosphorus Pesticides US EPA Method 8140/8141/8141A Rtx-CLPesticides
30m, 0.32mm ID, 0.50m Rtx-CLPesticides (cat.# 11139) 1L US EPA Method 8141A Custom Standard Mixes (200ng/mL) Triphenylphosphate Standard (cat.# 32281) Tributylphosphate Standard (cat.# 32280) 8140/8141 OP Pesticides Calibration Mix A (cat.# 32277) 8141 OP Pesticides Calibration Mix B (cat.# 32278) splitless hold time: 1 min. Oven temp.: 100C to 180C @ 10C/min. (hold 2 min.), to 300C @ 18C/min. (hold 3 min.) Inj. / det. temp.: 250C / 280C FPD
2 10 (SS), 11, 12 50

581

13,14,15 6 29,30

39,40 42 44,45(SS)

1 4

28 7 8

35 37 33 34 43 41

49 47 48

24 27 31 19,20,21 22 32 23 16,17, 18

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

51 46

52 53

36 38

5 9 3 26 25

min. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. dichlorvos hexamethylphosphoramide trichlorfon mevinphos demeton-O thionazin ethoprop phorate naled tributyl phosphate (SS) TEPP 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. sulfotepp demeton-S terbufos fonophos dicrotophos diazinon disulfoton dioxathion monocrotophos dimethoate dichlorofenthion

2 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33.

8 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44.

10
GC_EV00413

12

14 45. 46. 47. 48. 49. 50. 51. 52. 53.

16

18

chlorpyrifos methyl ronnel phosphamidon isomer merphos chlorpyrifos fenthion aspon parathion-methyl trichloronate malathion fenitrothion

phosphamidon parathion-ethyl chlorfenvinphos tokuthion merphos oxone crotoxyphos stirofos bolstar famphur carbophenothion fensulfothion

triphenyl phosphate (SS) leptophos ethion phosmet EPN tri-o-cresyl phosphate azinphos-methyl azinphos-ethyl coumaphos

Organophosphorus Pesticides US EPA Method 8140/8141/8141A Rtx-CLPesticides2


30m, 0.32mm ID, 0.25m Rtx -CLPesticides2 (cat.# 11324) 1L US EPA Method 8141A Custom Standard Mixes (200ng/mL) Triphenylphosphate Standard (cat.# 32281) Tributylphosphate Standard (cat.# 32280) 8140/8141 OP Pesticides Calibration Mix A (cat.# 32277) 8141 OP Pesticides Calibration Mix B (cat.# 32278) splitless hold time: 1 min. Oven temp.: 100C to 180C @ 10C/min. (hold 2 min.), to 300C @ 18C/min. (hold 3 min.) Inj. / det. temp.: 250C / 280C FPD

50

32,33,34 41 45(SS),46 12 8,9 29,30 28 31 20,21 35 1 7(SS) 22 25 24 11 3 18 16 19 13,14, 15 4 5 6 10


17

48,49

39,40 26 42 37 38 36 27 43 44 53 51 52 47

23

2 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. dichlorvos hexamethylphosphoramide mevinphos trichlorfon demeton-O thionazin tributyl phosphate (SS) ethoprop TEPP naled phorate 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. sulfotepp demeton-S dicrotophos dioxathion terbufos monocrotophos fonophos diazinon disulfoton dimethoate dichlorofenthion

4 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33.

6 phosphamidon isomer chlorpyrifos methyl ronnel parathion-methyl phosphamidon aspon chlorpyrifos trichloronate merphos fenitrothion fenthion

8 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44.

10
GC_EV00414

12

14 45. 46. 47. 48. 49. 50. 51. 52. 53.

16

18

min.

malathion parathion-ethyl chlorfenvinphos crotoxyphos tokuthion merphos oxone stirofos famphur bolstar carbophenothion fensulfothion

triphenyl phosphate (SS) ethion EPN phosmet leptophos tri-o-cresyl phosphate azinphos-methyl azinphos-ethyl coumaphos

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582

Pesticides
Organophosphorus Pesticides US EPA Method 8140/8141/8141A Rtx-1

31,32,33

51

13 43,44 24,25 42

18,19 6(IS) 9,10 48 8 3 5 1 11, 12 15 26 14 27 29 34 38 22 35 21 4 16,17 7 23 52 53 39 40 28 36,37 30 41 47 46(IS) 45 50 49

20

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53.

dichlorvos hexamethylphosphoramide mevinphos trichlorfon TEPP thionazin demeton-O ethoprop tributyl phosphate (SS) dicrotophos monocrotophos naled sulfotepp phorate dimethoate demeton-S dioxathion terbufos fonophos phosphamidon isomer diazinon disulfoton phosphamidon dichlorofenthion parathion-methyl chlorpyrifos methyl ronnel fenitrothion malathion fenthion aspon parathion-ethyl chlorpyrifos trichloronate chlorfenvinphos merphos crotoxyphos stirofos tokuthion merphos oxidation product fensulfothion famphur ethion bolstar carbophenothion triphenyl phosphate (SS) phosmet EPN azinphos-methyl leptophos tri-o-cresyl phosphate azinphos-ethyl coumaphos

G C A P P L I C AT I O N S | E N V I R O N M E N TA L
min.

10
GC_EV00415

12

14

16

30m, 0.32mm ID, 0.50m Rtx-1 (cat.# 10139) Total OPP custom standard mix (0.2g/mL), 1L US EPA Method 8141A Custom Standard Mixes (200ng/mL) Triphenylphosphate Standard (cat.# 32281) Tributylphosphate Standard (cat.# 32280) 8140/8141 OP Pesticides Calibration Mix A (cat.# 32277) 8141 OP Pesticides Calibration Mix B (cat.# 32278) splitless hold time: 1 min. Oven temp.: 100C to 180C @ 10C/min. (hold 2 min.), to 300C @ 18C/min. (hold 3 min.) Inj. / det. temp.: 250C / 280C FPD Solvent: hexane Dead time: 0.78min. @ 100C, constant pressure

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Pesticides
Organophosphorus Pesticides (European) Rtx-CLPesticides

583

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18.

Concentration on-column (ng) methamidophos 1.25 dichlorvos 1.25 acephate 0.50 demeton-S-methyl 0.50 tributylphosphate (IS) 1.25 omethoate 2.50 dimethoate 0.50 tolclofos-methyl 0.25 pirimiphos methyl 0.25 chlorpyriphos 0.25 malathion 0.50 tokuthion 0.50 methidathion 0.50 profenfos 0.50 ethion 0.50 triphenylphosphate (surrog.) 1.25 azinphos-methyl 1.00 pyrazophos 1.25

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00676

Rtx-CLPesticides 30m, 0.32mm ID, 0.50m (cat.# 11139) Sample: European OPP Mix (cat.# 32418) 1001000g/mL in acetone Inj.: 0.5L direct, open-top Siltek Drilled Uniliner inlet liner (cat.# 21055-214.5) Inj. temp.: 250C Carrier gas: helium, constant pressure Linear velocity: 35cm/sec. @ 80C Oven temp.: 80C (hold 1 min.) to 150C @ 7C/min. to 280C @ 15C/min. (hold 10 min.) Det.: FPD @ 280C

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584

Pesticides
Organophosphorus Pesticides (European) Rtx-CLPesticides

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00648

Rtx-CLPesticides, 30m, 0.25mm ID, 0.25m (cat.# 11123) Sample: Custom European Mix (call for details) 1-bromo-2-nitrobenzene cat.# 32279 4-chloro-3-nitrobenzotrifluoride cat.# 32282 tributylphosphate cat.# 32280 triphenylphosphate cat.# 32281 Inj.: 1.0L splitless (hold 0.4 min.) 4mm double gooseneck inlet liner (cat.# 20785) Inj. temp.: 250C Carrier gas: helium, constant flow, 6 psi head pressure Flow rate: 0.75mL/min. Linear velocity: 28cm/sec.* Dead time: 1.82 min. @ 80C Oven temp.: 80C (hold 1.0 min.) to 150C @ 7C/min. (no hold) to 280C @ 15C/min. (hold 7 min.) Det.: Agilent 5971A GC/MS Transfer line temp.: 280C Scan range: 35400 amu Solvent Delay 5 min. Tune PFTBA Ionization: EI

*This mix was prepared for FPD analyses. Peaks will be equivalent height with FPD detection if linear velocity is set at 28cm/sec. (0.32mm ID column).

Compound 1. 4-chloro-3-nitro-trifluoride 2. methamidophos 3. dichlorvos 4. 1-bromo-2-nitrobenzene 5. acephate 6. demeton-S-methyl 7. TBP (int. std.) 8. omethoate 9. dimethoate 10. tolclofos-methyl 11. pirimiphos methyl 12. chlorpyrifos 13. malathion 14. quinalphos 15. tokuthion (prothiofos) 16. methidathion 17. profenfos 18. ethion 19. TPP (surrog.) 20. azinphos-methyl 21. pyrazophos

Conc. on-column (ng) 100 50 50 100 20 20 100 100 20 10 10 10 20 10 20 20 20 20 100 40 50

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Pesticides/Herbicides
Nitrogen/Phosphorus Pesticides & Herbicides US EPA Method 619 Rtx-CLPesticides & Rtx-CLPesticides2
1

585

Rtx-CLPesticides

Dual-column analysis
8

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

prometon simazine atraton propazine atrazine terbuthylazine secbumeton simetryne ametryne prometryne terbutryne

CAS No. 1610-18-0 122-34-9 1610-17-9 139-40-2 1912-24-9 5915-41-3 26259-45-0 1014-70-6 834-12-8 7287-19-6 886-50-0

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

5 6 4 3 7 2 9 10 11

min.
3

18

19

20

21

22

23

Rtx-CLPesticides2
4

6 5

2 1

9 7 10 11

min. 18

19

20

21
GC_EV00056

22

23

30m, 0.32mm ID, 0.50m Rtx-CLPesticides (cat.# 11139) and 30m, 0.32mm ID, 0.25m Rtx-CLPesticides2 (cat.# 11324) with a 5m, 0.32mm ID guard column (cat.# 10044) and a Y Press-Tight connector (cat.# 20403). Direct injection using a Uniliner liner (cat.#21303) and adaptor for an HP 5890 (cat.# 20964). On-column concentration 50pg each compound. Oven temp.: Inj./det. temp.: Carrier gas: GC: 100C (hold 0 min.) to 250C @ 4C/min. (hold 5 min.); 250C/275C hydrogen, 9.65psi constant pressure HP 6890 with purged packed injection port.

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586

Pesticides/Herbicides
Nitrogen/Phosphorus Pesticides & Herbicides Rtx-5
30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 0.1L splitless injection, concentration 1.529.9ppm Splitless hold: Oven temp.:
7

Inj. & det. temp.: Carrier gas: Linear velocity: NPD sensitivity:

0.75 min. 100C (hold 5 min.) to 200C @ 15C/min. (hold 8 min.), to 290C @ 15C/min. (hold 5 min.) 290C helium 30cm/sec. set @ 100C 8 x 10-11 AFS

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

3 2 4

1. 2. 3. 4. 5. 6. 7. 8.

2-nitro-m-xylene molinate dimethoate atrazine Diazinon prometryne malathion DEF

min.

10

15
GC_EV00089

20

25

30

Permission to publish this chromatogram granted by Canonie Environmental Services.

Nitrogen/Phosphorus Pesticides & Herbicides Rtx-5


30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 0.1L splitless injection, concentration 1.529.9ppm. Splitless hold: Oven temp.:
3 2 4 5 1 7 6 8

Inj. & det. temp.: Carrier gas: Linear velocity: NPD sensitivity:

0.75 min. 100C (hold 5 min.) to 200C @ 15C/min. (hold 8 min.), to 290C @ 15C/min. (hold 5 min.) 290C helium 30cm/sec. set @ 100C 8 x 10-11 AFS

1. 2. 3. 4. 5. 6. 7. 8.

phorate demeton simazine disulfoton methyl parathion bromacil ethyl parathion ethion

min.

10

15
GC_EV00090

20

25

30

Permission to publish this chromatogram granted by Canonie Environmental Services.

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Herbicides
Chlorophenoxyacid Herbicides US EPA Method 615 Rtx-35

587

for more info


on Pro ezGC software, see page449.

Analysis optimized using Pro ezGC software! See page 449.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

dalapon DCAA (S) dicamba MCPP MCPA DBOB (IS) dichlorprop 2,4-D 2,4,5-TP 2,4,5-T dinoseb 2,4-DB

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

11

8 7 2 3 4 5 9 10 12

30m, 0.53mm ID, 0.50m Rtx-35 (cat.# 10440) 0.5L direct injection of chlorophenoxy herbicides, on-column concentration 1010,000g/mL Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Det.: 60C to 150C @ 8C/min. (hold 5 min.), to 210C @ 4C/min. 250C / 275C helium 35cm/sec. set @ 60C ECD w/anode purge

min.

10

15
GC_EV00094

20

25

30

Chlorophenoxyacid Herbicides US EPA Method 615 Rtx-5

11

Analysis optimized using Pro ezGC software! See page 449.


12

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

dalapon DCAA (S) dicamba MCPP MCPA DBOB (IS) dichlorprop 2,4-D 2,4,5-TP 2,4,5-T dinoseb 2,4-DB

10

3 5 4

30m, 0.53mm ID, 0.50m Rtx-5 (cat.# 10240) 0.5L direct injection of chlorophenoxy herbicides, on-column concentration 1010,000g/mL Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Det.: 20 25 30 60C to 150C @ 8C/min. (hold 5 min.), to 210C @ 4C/min. 250C / 275C helium 35cm/sec. set @ 60C ECD w/anode purge

min.

10

15
GC_EV00095

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588

Herbicides
Triazine Herbicides US EPA Method 619 Rtx-50, Rtx-200
6

3,7

3 4

Rtx-50 30m, 0.53mm ID, 0.50m (cat.# 10540)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

atraton prometon terbutylazine atrazine simazine propazine secbumeton terbutryne ametryne simetryne prometryne

Rtx-200 30m, 0.53mm ID, 0.50m (cat.# 15040)

5 4 6

1 2 9 8 7

11 2 9,11 10 8

10

0.5L direct injection of EPA Method 619 - triazine herbicides. On-column concentration: 50ng Oven temp.: Inj. / det. temp.: Detector: Carrier gas: Linear velocity: 150C to 250C @ 4C/min. (hold 5 min.) 250C /275C TSD helium 40cm/sec. set @ 150C

min.

10

12

14
GC_EV00058

16

min. 4

10

GC_EV00059

a plus 1 story
Thank you for being a top notch GC Analytical Supply Company that always continues to offer newer products & services. John T. Brunette, Chemist, Bausch & Lomb

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Herbicides
Chlorophenoxyacid Herbicides US EPA Method 8151 Rtx-CLPesticides & Rtx-CLPesticides2
9

589

Rtx-CLPesticides

10

17

12 11 4 14,15 16

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18.

dalapon 3,5-dichlorobenzoic acid 4-nitroanisole dicamba MCPP MCPA dichlorprop 2,4-D pentachloroanisole 2,4,5-TP chloramben 2,4,5-T 2,4-DB picloram Rtx-CLPesticides2 bentazon dinoseb DCPA acifluorfen
18

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

10 12 4 11 16

17 14 18

1 DCAA 2 DCAA 3 7 8 13 1 2 6 8 7 5 13 15

6 5

min. 4

10

12

14

16

18

20

22
GC_EV00091

min.

10

15

20

30m, 0.32mm ID, 0.50m, Rtx-CLPesticides (cat.# 11139) and 30m, 0.32mm ID, 0.25m Rtx-CLPesticides2 (cat.# 11324). 1.0L direct injection of derivatized chlorophenoxy herbicides, Uniliner inlet liner (cat.# 20335), on-column conc.: 20020,000pg/mL

Oven temp.: Inj. / det. temp.: Carrier gas: Inlet pressure: Det.:

80C (hold 1 min.) to 300C @ 10C/min. (hold 10 min.) 200C/300C helium 12.5psi set @ 80C ECD w/anode purge

Chlorophenoxyacid Herbicides US EPA Method 515.1 Rtx-50


7 3 2 4 5 8 9

11

6 1

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

dalapon 2,4-dichlorophenylacetic acid dicamba dibromooctafluorobiphenyl 2,4-D pentachlorophenol Silvex (2,4,5-TP) 2,4,5-T dinoseb 2,4-DB picloram

10

min. 4

12

16

20

24
GC_EV00093

28

32

36

40

44

48

30m, 0.25mm ID, 0.50m Rtx-50 (cat.# 10538) 2.0L splitless injection of derivatized chlorophenoxy herbicides. Conc. 10187pg/L Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: Splitless hold time: 50C (hold 0.75 min.) to 84C @ 4C/min., to 165C @ 10C/min., to 270C @ 4C/min., to 300C @ 20C/min. (hold 6 min.) 220C / 320C helium, constant pressure 30cm/sec. set @ 50C 0.75 min.

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590

Herbicides
Nitrogen-Containing Herbicides Rtx-5
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. Eptam Sutan Vernam Tillam Ordram propachlor Ro-Neet Treflan Balan simazine atrazine 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. propazine Tolban terbacil Sencor bromacil Dual Paarlan Prowl oxadiazon GOAL hexazinone 30m, 0.53mm ID, 0.50m Rtx-5 (cat.# 10240) 0.2L direct injection, Uniliner inlet liner, concentration approximately 10ng per component. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 60C (hold 1 min.) to 290C @ 15C/min. (hold 5 min.) 290C helium 40cm/sec. (flow rate: 5.2cc/min.) 16 x 10-11 AFS

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

6 7 2 4 3 5 9 8 12 11 10 14 13 15 16 22 17 19 18 20 21

min.

10
GC_EV00087

12

14

16

18

Nitrogen-Containing Herbicides Rtx-35

30m, 0.53mm ID, 0.50m Rtx-35 (cat.# 10440) 0.2L direct injection, Uniliner liner, concentration approximately 10ng per component. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity:
18,19

60C (hold 1 min.) to 290C @ 15C/min. (hold 5 min.) 290C helium 40cm/sec. (flow rate: 5.2cc/min.) 16 x 10-11 AFS

9 8 1 2 34 5 67 12 10 11 13 14

16 17 20 21 15 22

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

Eptam Sutan Vernam Tillam Ordram Treflan Balan Ro-Neet propachlor Tolban propazine

12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

atrazine simazine terbacil Sencor Dual Paarlan Prowl bromacil oxadiazon GOAL hexazinone

min.

10

12
GC_EV00088

14

16

18

20

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Herbicides
Triazine Herbicides (French) & Degradation Products Rtx-OPPesticides2
Peak List: 1. trifluraline 2. desisopropylatrazine 3. desethyl-atrazine 4. desethyl-terbuthylazine 5. simazine 6. atrazine 7. terbumeton 8. terbuthylazine 9. secbumeton 10. cyanazine CAS# 1582-09-8 1007-28-9 6190-65-4 122-34-9 1912-24-9 33693-04-8 5915-41-3 26259-45-0 21725-46-2

591

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Rtx-OPPesticides2 30m, 0.25mm ID, 0.25m (cat.# 11243) Sample: custom standard, 100ng/L each component Inj.: 1.0L splitless (hold 0.5 min.), 4mm single gooseneck inlet liner (cat.# 20904) Inj. temp.: 300C Carrier gas: helium, constant pressure Flow rate: 1.0mL/min @ 80C (27.22cm/sec) Oven temp.: 80C (hold 1 min.) to 140C @ 25C/min. (hold 5 min.) to 165C @ 1C/min. to 300C @ 15C (hold 1 min.) Det: Agilent 5971A GC/MS Transfer line temp.: 280C Scan range: 35-360amu Ionization: EI

GC_EV00626

three simple words...


Plus One service exceeding your expectations in everything we do Innovative products and processes Execution in our commitment to deliver a product, technical support, or other needs

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592

PCB Mixtures (Aroclor)


PCBs: Aroclor 1242 Rtx-5 using GC Racer PCBs: Aroclor 1248 Rtx-5 using GC Racer

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00581

GC_EV00582

PCBs: Aroclor 1254 Rtx-5 using GC Racer

PCBs: Aroclor 1260 Rtx-5 using GC Racer

GC_EV00583

GC_EV00584

Rtx-5 15m, 0.32mm ID, 0.50m (cat.# 10236) Inj.: 1L splitless (hold 0.5 min.), Siltek Drilled Uniliner inlet liner (cat.# 21054-214.1) Conc.: 400 ppb Inj. temp.: 250C Carrier gas: hydrogen Linear velocity: head pressure at 5 psi Oven temp.: 110C (hold 1 min.), 60C/min. to 300C, (hold 5 min.) Det. temp.: 310C

for more info


GG Racer Temperature Programmer is described on page 149.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

PCB Mixtures (Aroclor)


PCBs: Aroclor Quick Screening Rtx-5

593

Aroclor 1221 Mix (cat.# 32007)

Aroclor 1232 Mix (cat.# 32008)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

min.

4 6 GC_EV00096

min.

6 GC_EV00097

10

Aroclor 1242 Mix (cat.# 32009)

Aroclor 1248 Mix (cat.# 32010)

min.

6 GC_EV00098

min.

6 8 GC_EV00099

10

Aroclor 1254 Mix (cat.# 32011)

Aroclor 1260 Mix (cat.# 32012)

min.

6 8 GC_EV00100

10

min.

6 GC_EV00101

10

15m, 0.53mm ID, 0.50m Rtx-5 (cat.# 10237) 1.0L direct injection Conc.: 50ppm Oven temp.: 150C to 300C @ 12C/min. (hold 5 min.) Inj. / det. temp.: 250C / 310C Carrier gas: helium Linear velocity: 30cm/sec. set @ 150C ECD sensitivity: 16kHz full scale

Phone: 800-356-1688 or 814-353-1300 www.restek.com

594

PCB Mixtures (Aroclor)


PCBs: Aroclor 1016 Rtx-CLPesticides & Rtx-CLPesticides2
DCB 6 8 10 12 14 16 18 20 22 8 10 12 GC_EV00440 14 16 18 20 22 DCB min. 2 4 6 6 8 10 12 14 16 18 20 6 8 10 12 14 GC_EV00448 16 18 20 22 DCB min. 2 4 DCB

Rtx-CLPesticides

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

min.

Rtx-CLPesticides2

30m, 0.32mm ID, 0.50m Rtx-CLPesticides (cat.# 11139). 30m, 0.32mm ID, 0.25m Rtx-CLPesticides2 (cat.# 11324). 0.5L direct injection, 160pg on-column concentration. Oven temp.: 120C (hold 1 min.) to 300C @ 9C/min. (hold 10 min.) Inj. temp.: 210C Det.: ECD with anode purge, 310C Carrier gas: helium

PCBs: Aroclor 1221 Rtx-CLPesticides & RtxCLPesticides2

Rtx-CLPesticides

min.

Rtx-CLPesticides2

Phone: 800-356-1688 or 814-353-1300 www.restek.com

PCB Mixtures (Aroclor)


PCBs: Aroclor 1232 Rtx-CLPesticides & Rtx-CLPesticides2
Rtx-CLPesticides
DCB

595

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

min.

10

12

14

16

18

20

22

Rtx-CLPesticides2

min.

10

12 GC_EV00450

14

16

18

20

22

30m, 0.32mm ID, 0.50m Rtx-CLPesticides (cat.# 11139). 0.32mm ID, 0.25m Rtx-CLPesticides2 (cat.# 11324). 0.5L direct injection, 160pg on-column concentration. Oven temp.: 120C (hold 1 min.) to 300C @ 9C/min. (hold 10 min.) Inj. temp.: 210C Det.: ECD with anode purge, 310C Carrier gas: helium

PCBs: Aroclor 1242 Rtx-CLPesticides & Rtx-CLPesticides2

Rtx-CLPesticides
DCB min. 2 4 6 8 10 12 14 16 18 20 22

Rtx-CLPesticides2
DCB min. 2 4 6 8 10 12 GC_EV00451 14 16 18 20 22

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DCB

596

PCB Mixtures (Aroclor)


PCBs: Aroclor 1248 Rtx-CLPesticides & Rtx-CLPesticides2
Rtx-CLPesticides
DCB 6 8 10 12 14 16 18 20 22 6 8 10 12 GC_EV00453 14 16 18 20 22 6 8 10 12 14 16 18 20 22 8 10 12 GC_EV00454 14 16 18 20 22 DCB DCB DCB min. 2 4

min.

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Rtx-CLPesticides2

30m, 0.32mm ID, 0.50m Rtx-CLPesticides (cat.# 11139). 0.32mm ID, 0.25m Rtx-CLPesticides2 (cat.# 11324). 0.5L direct injection of commercial Aroclor mixtures, 160pg on-column concentration. Oven temp.: 120C (hold 1 min.) to 300C @ 9C/min. (hold 10 min.) Inj. temp.: 210C Det.: ECD with anode purge, 310C Carrier gas: helium

PCBs: Aroclor 1254 Rtx-CLPesticides & Rtx-CLPesticides2


Rtx-CLPesticides

min.

Rtx-CLPesticides2

min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

PCB Mixtures (Aroclor)


PCBs: Aroclor 1260 Rtx-CLPesticides & Rtx-CLPesticides2

597

Rtx-CLPesticides2 Rtx-CLPesticides

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

DCB

min.

10

12

14

16

18

20

22

min. GC_EV00456

10

12

14

16

18

20

22

30m, 0.32mm ID, 0.50m Rtx-CLPesticides (cat.# 11139). 0.32mm ID, 0.25m Rtx-CLPesticides2 (cat.# 11324). 0.5L direct injection, 160pg on-column concentration. Oven temp.: 120C (hold 1 min.) to 300C @ 9C/min. (hold 10 min.) Inj. temp.: 210C Det.: ECD with anode purge, 310C Carrier gas: helium

dependable execution
Tom consistently goes above and beyond to satisfy customers and complete his job duties. On a Friday morning last October, Tom arrived at 4:30am, to make sure a number of GC columns went out in the mail and to ensure that he had time for a training session, which was planned for the same day. Tom Barone, Applied Technology Manufacturing Technician

Phone: 800-356-1688 or 814-353-1300 www.restek.com

DCB

598

PCB Mixtures
PCB Congeners Rtx-XLB

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00730

Column: Sample: Inj.: Inj. temp.: Carrier gas: Linear velocity: Oven temp.: Det.:

Rtx-XLB 30m, 0.32mm ID, 0.50m (cat.# 12839) 200ppb each PCB congener in hexane (cat.# 32416), 200ppb 2,4,5,6-tetrachloro-m-xylene (SS) (cat.# 32027), 100ppb decachlorobiphenyl (IS) (cat.# 32289) 1.0L splitless (hold 0.75 min.), 4mm Drilled Uniliner inlet liner (cat.# 21055) 220C hydrogen, constant pressure 66cm/sec. @ 120C 120C (hold 0.5 min.) to 260C @ 29C/min. (hold 2.5 min.), to 330C @ 28C/min. (hold 5 min.) ECD @ 320C

Compound 1. 2-chlorobiphenyl 2. 2,4,5,6 tetrachloro-m-xylene (SS) 3. 2,3-dichlorobiphenyl 4. 2,2',5-trichlorobiphenyl 5. 2,4',5-trichlorobiphenyl 6. 2,2',5,5'-tetrachlorobiphenyl 7. 2,2',3,5'-tetrachlorobiphenyl 8. 2,3',4,4'-tetrachlorobiphenyl 9. 2,2',4,5,5'-pentachlorobiphenyl 10. 2,2',3,4,5'-pentachlorobiphenyl 11. 2,3,3',4',6-pentachlorobiphenyl 12. 2,2',3,5,5',6-hexachlorobiphenyl 13. 2,2',4,4',5,5'-hexachlorobiphenyl 14. 2,2',3,4,5,5'-hexachlorobiphenyl 15. 2,2',3,4,4',5'-hexachlorobiphenyl 16. 2,2',3,4',5,5',6-heptachlorobiphenyl 17. 2,2',3,4,4',5',6-heptachlorobiphenyl 18. 2,2',3,4,4',5,5'-heptachlorobiphenyl 19. 2,2',3,3',4,4',5-heptachlorobiphenyl 20. 2,2',3,3',4,4',5,5',6-nonachlorobiphenyl 21. decachlorobiphenyl (SS)

RT (min.) 3.86 4.53 4.83 5.17 5.63 5.89 6.09 6.64 6.84 7.24 7.39 7.51 8.15 8.35 8.61 8.76 8.84 9.50 9.86 10.87 11.17

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Chlorinated Disinfection Byproducts


Chlorinated Disinfection Byproducts US EPA Method 551.1 Rtx-5
3 4

599

16 19

6 11 2 9 7 1 5

14 21 15 18 12 13 17 10 20

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

chloroform 1,1,1-trichloroethane carbon tetrachloride trichloroacetonitrile trichloroethylene bromodichloromethane chloral hydrate dichloroacetonitrile 1,1-dichloro-2-propanone 1,1,2-trichloroethane chloropicrin dibromochloromethane 1,2-dibromoethane (EDB) tetrachloroethylene bromochloroacetonitrile 1,1,1-trichloro-2-propanone bromoform dibromoacetonitrile 1,2,3-trichloropropane 4-bromofluorobenzene (IS) 1,2-dibromo-3-chloropropane (DBCP)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

min.

10
GC_EV00023

20

30

30m, 0.25mm ID, 1.0m Rtx-5 (cat.# 10253) 1.0L split injection. 1ng on-column concentration. Oven temp.: 35C (hold 22 min.) to 200C @ 10C/min. Inj./det. temp.: 200C/290C Carrier gas: helium Linear velocity: 30cm/sec. @ 50C ECD sensitivity: 20kHz full scale Split ratio: 10:1

Chlorinated Disinfection Byproducts US EPA Method 551.1 Rtx-200


3 4 14/8

5/6 16 19/18 21 2 12 13/11 1 7 9 15 17 10 20

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

chloroform 1,1,1-trichloroethane carbon tetrachloride trichloroacetonitrile trichloroethylene bromodichloromethane chloral hydrate dichloroacetonitrile 1,1-dichloro-2-propanone 1,1,2-trichloroethane chloropicrin dibromochloromethane 1,2-dibromoethane (EDB) tetrachloroethylene bromochloroacetonitrile 1,1,1-trichloro-2-propanone bromoform dibromoacetonitrile 1,2,3-trichloropropane 4-bromofluorobenzene (IS) 1,2-dibromo-3-chloropropane (DBCP)

min.

10

20
GC_EV00024

30

30m, 0.25mm ID, 1.0m Rtx-200 (cat.# 15053) 1.0L split injection. 1ng on-column concentration. Oven temp.: 35C (hold 22 min.) to 200C @ 10C/min. Inj./det. temp.: 200C/290C Carrier gas: helium Linear velocity: 30cm/sec. @ 50C ECD sensitivity: 20kHz full scale Split ratio: 10:1

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600

Dioxins
TCDD Isomers Rtx-2330
60m, 0.25mm ID, 0.20m Rtx-2330 (cat.# 10726) 2.0L splitless injection of TCDD isomers, approximately 0.5ng each isomer. Splitless hold: Oven temp.:
3

4, 5

Inj. & det. temp.: Carrier gas: Linear velocity: ECD sensitivity:

0.45 min. 200C (hold 1 min.) to 250C @ 8C/min. (hold 15 min.), to 275C @ 15C/min. (hold 5 min.) 275C hydrogen 40cm/sec. 21 kHz full scale

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

1. 2. 3. 4. 5. 6. 7.
2 1 6 7

1,4,7,8-TCDD 2,3,7,8-TCDD 1,2,3,4-TCDD 1,2,3,7 1,2,3,8-TCDD 1,2,7,8-TCDD 1,2,6,7-TCDD

also available
For Rtx-Dioxin2 columns designed specifically for dioxin/furan analysis, see page 66.

min.

10
GC_EV00108

12

14

16

18

20

TCDD Isomers Rtx-2330


60m, 0.32mm ID, 0.20m Rtx-2330 (cat.# 10727) 1.5L cold on-column injection of TCDD isomers, approximately 0.5ng each isomer.
4, 5

Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: ECD sensitivity:

200C (hold 1 min.) to 240C @ 3C/min. (hold 6 min.), to 275C @ 15C/min. (hold 30 min.) 275C hydrogen 40cm/sec. (flow rate: 3.2cc/min.) 5 kHz full scale

1. 2. 3. 4. 5. 6. 7.
6 7

1,4,7,8-TCDD 2,3,7,8-TCDD 1,2,3,4-TCDD 1,2,3,7 1,2,3,8-TCDD 1,2,7,8-TCDD 1,2,6,7-TCDD

2 1

min.

10

12
GC_EV00109

14

16

18

20

22

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Endocrine Disruptors
Endocrine Disruptors: Alkyl Phenols Rtx-5MS
1. 2. 3. 4. 5. 6. 7. 8.
3 5 6

601

Endocrine Disruptors: Phthalate Esters 4 Rtx-5MS 3


5 6 1 2 8 9 10

tert-butyl phenol n-pentyl phenol n-hexyl phenol n-heptyl phenol tert-octyl phenol n-octyl phenol n-nonyl phenol bisphenol A

11

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

7 2 4 7

8 1

min.

12

14

16

18
GC_EV00046

20

22

24 min.18 1. 2. 3. 4. 5. 6. 20 22 24
GC_EV00049

26 7. 8. 9. 10. 11.

28

30

32

30m, 0.25mm ID, 0.25m Rtx-5MS (cat.# 12623). Conc.: 510ng on-column Inj.: splitless, purge on @ 1 min. Oven temp.: 35C (hold 1 min.) to 300C @ 10C/min. (hold 15 min.) Inj./det. temp.: 275C/310C Carrier gas: helium

dimethyl phthalate diethyl phthalate isobutyl phthalate dibutyl phthalate dipentyl phthalate dihexyl phthalate

benzylethyl phthalate diheptyl phthalate 2-ethylhexyl phthalate cyclohexyl phthalate dioctyl phthalate

30m, 0.25mm ID, 0.50m Rtx-5MS (cat #12638). 100pg on-column injection MS-SIM. Oven temp.: 35C (hold 1 min.) to 285C @ 10C/min. Pressure: 7.5psi constant pressure

Endocrine Disruptors: Butyl Tins (hexyl derivatives) Rtx-5


1. 2. 3. 4. 5. 6.
3 2 4 6

Endocrine Disruptors: Butyl Tins (hexyl derivatives) Rtx-35


tetrapropyltin tetrabutyltin tributyltin dibutyltin tripentyltin monobutyltin
4 1 5 2 3 6 5

1. 2. 3. 4. 5. 6.

tetrapropyltin tetrabutyltin tributyltin dibutyltin tripentyltin monobutyltin

min. 6 min. 6 8 10
GC_EV00047

10
GC_EV00048

12

14

12

14

also available
Butyl tins reference materials available from Restek, see page 419.

30m, 0.32mm ID, 0.50m Rtx-5 (cat.# 10239) 500pg on-column direct injection Oven temp.: 100C (hold 1 min.) to 285C @ 10C/min. Inj./det. temp.: 250C Carrier gas: helium Linear velocity: 45cm/sec. Detector: FPD with 610nm filter

30m, 0.32mm ID, 0.50m Rtx-35 (cat.# 10439) 500pg on-column direct injection Oven temp.: 100C (hold 1 min.) to 285C @ 10C/min. Inj./det. temp.: 250C Carrier gas: helium Linear velocity: 45cm/sec. Detector: FPD with 610nm filter

Phone: 800-356-1688 or 814-353-1300 www.restek.com

602

Explosives
Explosives Rtx-200
15

5 6

11,12 22 18,19

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

8 4

13 9 17 10 14 16

2 3 1

20 21

7 23

min.

10

15

20

25

30

35
GC_EV00060

40

45

50

55

30m, 0.25mm ID, 0.25m Rtx-200 (cat.# 15023) 1.0L splitless injection of an explosives sample. Concentration 20ng/L. Oven temp.: Injector temp.: Det.: Carrier gas: Linear velocity: Splitless hold time: 80C (hold 2 min.) to 260C @ 3C/min. (hold 2 min.) 280C MS, 300C helium 20cm/sec. set @ 80C 0.6 min.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

2-nitrotoluene 3-nitrotoluene 4-nitrotoluene 2,3-diaminotoluene 2,6-diaminotoluene 2,4-diaminotoluene 1,4-dinitrobenzene 2,6-dinitrotoluene 2-amino-6-nitrotoluene 1,3-dinitrobenzene 2,4-dinitrotoluene 2-amino-4-nitrotoluene

13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23.

2,3-dinitrotoluene 3,4-dinitrotoluene 3-nitrobiphenyl 2,4,6-trinitrotoluene 2,4,5-trinitrotoluene 4-amino-2,6-dinitrotoluene 2,3,4-trinitrotoluene 1,3-dinitronaphthalene 2,6-diamino-4-nitrotoluene 2-amino-4,6-dinitrotoluene 2,2'-dinitrobiphenyl

Searching for a chromatogram?

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Explosives
Explosives US EPA Method 8095 Rtx-TNT & Rtx-TNT2
Rtx-TNT

603

restek innovation!
Improved resolution of nitroaromatic compounds such as those listed in US EPA Method 8095
9 7 15

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

11 8 10 6 13 1 5 2 34 12 14

16

17

18

min.

6
GC_EV00406

10

12

6m, 0.53mm ID, 1.50m Rtx-TNT (cat.# 12998) Direct injection using a 1mm Siltek Uniliner inlet liner (cat.# 21052-214.1). On-column conc.: 200-1000pg/compound. 8095 Calibration Mix A (cat.# 31607), 8095 Calibration Mix B (cat.# 31608), and 3,4-dinitrotoluene (cat.# 31452). Oven temp.: 80C (hold 1 min.) to 180C @ 10C/min. to 300C @ 30C/min. (hold 3 min.) Inj. temp.: 250C Det.: ECD @ 330C with anode purge Dead time: 4.4 sec. Head pressure: helium @ 3psi (20.7 KPa) Flow rate: helium @ 17mL/min. @ 80C.

Rtx-TNT2

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18.

nitrobenzene 2-nitrotoluene 3-nitrotoluene 4-nitrotoluene nitroglycerine 1,3-dinitrobenzene 2,6-dinitrotoluene 2,4-dinitrotoluene 3,4-dinitrotoluene (IS) 1,3,5-trinitrobenzene trinitrotoluene PETN RDX 4-amino-2,6-dinitrotoluene 3,5-dinitroaniline 2-amino-4,6-dinitrotoluene tetryl HMX

15,13

9 16 11 8 6 10 17 18 12,14

5 1 2 3 4

min.

6
GC_EV00407

10

12

6m, 0.53mm ID, 1.50m Rtx-TNT2 (cat.# 12999) Direct injection using a 1mm Siltek Uniliner inlet liner (cat.# 21052-214.1). On-column conc.: 200-1000pg/compound. 8095 Calibration Mix A (cat.# 31607), 8095 Calibration Mix B (cat.# 31608), and 3,4-dinitrotoluene (cat.# 31452) Oven temp.: 80C (hold 1 min.) to 180C @ 10C/min. to 300C @ 30C/min. (hold 3 min.) Inj. temp.: 250C Det.: ECD @ 330C with anode purge Dead time: 4.4 sec. Head pressure: helium @ 3psi (20.7 KPa) Flow rate: helium @ 17mL/min. @ 80C

Phone: 800-356-1688 or 814-353-1300 www.restek.com

604

Gasoline Range Organics (GRO)


Alaska Method AK101AA Rtx-5Sil MS

restek innovation!
Rtx-5Sil MS column resolves alkyl benzenes and branched aromatic compounds listed in Alaska GRO Method AK101AA, for more accurate identification and quantitation.
2

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

1. 2. 3. 4. 5. 6. 7. 8. 9.

hexane benzene ,,-trifluorotoluene (SS) toluene ethylbenzene m-xylene p-xylene o-xylene isopropylbenzene

10. 11. 12. 13. 14. 15. 16. 17. 18.

4-bromofluorobenzene (SS) n-propylbenzene 1-ethyl-3-methylbenzene 1-ethyl-4-methylbenzene 1,3,5-trimethylbenzene 1-ethyl-2-methylbenzene 1,2,4-trimethylbenzene decane 1,2,3-trimethylbenzene

18

16 14 2 6,7

16,17 18

15 4 10 5 8 9 12 3 13 11 3 1 4 5

6,7

15 14

13 8 9 11 12 10

PID

FID

min.

10

12

14

16 GC_EV00402

min.

10

12

14

16

40m, 0.45mm ID, 1.50m Rtx-5Sil MS (cat.# 12798). Injection of 4-bromofluorobenzene (cat.# 30026); ,,-trifluorotoluene (cat.# 30048), decane, hexane, and Alaska aliphatic/aromatic GRO mix (cat.# 30461). Conc.: 10ppb in 5mL RO water GC: Finnigan 9001 Column flow: 9mL/min. Concentrator: Tekmar LSC-3000 Purge & Trap, BTEX trap Interface: direct with Siltek transfer line Oven temp.: 40C (hold 2 min.) to 85C @ 4C/min. (hold 1 min.) to 225C @ 40C/min. (hold 2 min.) Det.: FID (280C)/PID (200C) Make-up flow rate: 15mL/min.

free literature
State of Alaska UST Monitoring (lit. cat.# 59503)

Reference materials for the state underground storage tank program


To help laboratories comply with and use applicable analytical procedures, Restek has carefully reviewed and followed state guidelines in formulating analytical reference materials for AK101, AK102, and AK103 UST monitoring. Calibration mixes described in this 6-page note are appropriate for Alaska methodology. Also described are retention time, surrogate, internal standard, fractionation check, matrix spike, and pattern recognition mixtures.

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Gasoline Range Organics (GRO)


Volatile Petroleum Hydrocarbons (VPH) Massachusetts Department of Environmental Protection Rtx-502.2
For VPH analysis on an Rtx-502.2 column, use PID for aromatic compounds and FID for aliphatic compounds.
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. methanol methyl tert-butyl ether (60ng) benzene (20ng) toluene ethylbenzene (20ng) p+m-xylene (40ng ea.) o-xylene (40ng) 1,2,4-trimethylbenzene (40ng) naphthalene (40ng) 2,5-dibromotoluene (SS)
4 7 10 9 1 3 2 5

605

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

6 8

PID
min. 4 8

12

16

20

24

28

32

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.

methanol n-pentane (40ng) 2-methylpentane (60ng) methyl tert-butyl ether (60ng) 2,2,4-trimethylpentane (60ng) benzene (20ng) toluene (60ng) n-nonane (40ng) ethylbenzene (20ng) p+m-xylene (40ng ea.) o-xylene (40ng) 1,2,4-trimethylbenzene (40ng) naphthalene (40ng) 2,5-dibromotoluene (SS)
10 12 7 3 1 2 5 6 4 8 9 13 14 11

FID
min. 4 8

12

16 GC_EV00063

20

24

28

32

Column: Concentration: Oven temp: Carrier gas: Trap: Purge: Dry purge: Desorb preheat: Desorb: Bake:

105m, 0.53mm ID, 3.0m Rtx-502.2 (cat.# 10910). on-column at levels listed 45C to 90C @ 3C/min., to 140 @ 5C/min., to 230C @ 45C/min. (hold 8 min.) helium @ 15mL/min. Tekmar Model LSC 2000 BTEX helium @ 40mL/min. for 11 min. 2 min. 245C 2 min. @ 250C 6 min. @ 260C

free literature
Optimizing Massachusetts Volatile Petroleum Hydrocarbon GC Analysis (lit. cat.# 59150) Select a trap and analytical column that avoid retention and quantification problems
Massachusetts VPH affords more reliable quantification of volatile petroleum hydrocarbons, relative to older "analytical window" methods, and has been adopted by other states and in Canada. This 2-page note offers valuable tips for selecting a trap and a capillary GC column compatible with the methodology. Reference mixes specifically designed for MA VPH are described.

Chromatograms courtesy of Severn Trent Laboratories, Burlington, VT.

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606

Gasoline Range Organics (GRO)


Texas UST: Alternate Boiling Point/Carbon Number Distribution Marker Rtx-5
1. 2. 3. 4. 5. 6. 7. 8. 9. hexane (C6) octane (C8) decane (C10) dodecane (C12) hexadecane (C16) heneicosane (C21) octacosane (C28) pentatriacontane (C35) hexatriacontane (C36)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Rtx-5 15m, 0.25 ID, 0.25m (cat.# 10220) Sample: 200g/mL Alternate BP/CN Distribution Marker Stock Solution (cat.# 31639) in pentane Inj.: 0.5L splitless (hold 0.2 min.), 4mm drilled Uniliner inlet liner (hole at bottom) (cat.# 20756) Inj. temp.: 285C Carrier gas: helium, constant pressure Linear velocity: 27cm/sec. @ 30C Oven temp.: 30C (hold 1 min.) to 330C @ 60C/min. (hold 6 min.) with GC Racer for Agilent 5890 Series II GC (cat.# 23024) Det.: FID @ 330C

GC_EV00690

Texas UST: diesel/gas composites Rtx-5


1. 1-chlorooctane (surrogate) 2. 2-fluorobiphenyl (surrogate) Rtx-5 15m, 0.25mm ID, 0.25m (cat.# 10220) Sample: 1000g/mL unleaded gas and diesel fuel #2 composites standard (cat.# 31483) in pentane 250g/mL 2-fluorobiphenyl standard (cat.# 31096) in dichloromethane 250g/mL 1-chlorooctane (cat.# 30084) in P&T methanol Inj.: 0.5L splitless (hold 0.2 min.), 4mm drilled Uniliner inlet liner (hole at bottom) (cat.# 20756) Inj. temp.: 285C Carrier gas: helium, constant pressure Linear velocity: 27cm/sec. @ 30C Oven temp.: 30C (hold 1 min.) to 330C @ 60C/min. (hold 6 min.) with GC Racer for Agilent 5890 Series II GC (cat.# 23024) Det.: FID @ 330C

GC_EV00692

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Gasoline Range Organics (GRO)


Texas UST: Alternate BP/CN Distribution Marker Rtx-5
1. 2. 3. 4. 5. 6. 7. 8. 9.

607

n-hexane(C6) n-octane(C8) n-decane(C10) n-dodecane(C12) n-hexadecane(C16) n-heneicosane(C21) n-octacosane(C28) n-pentatriacontane n-hexatriacontane(C36)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00691

Rtx-5 30m, 0.25mm ID, 0.50m (cat.# 10238) Sample: 1L Alternate Boiling Point/Carbon Number Distribution Marker Stock Solution (cat.# 31639), 200g/mL each component in pentane Carrier gas: hydrogen @ 40cm/sec. Oven temp.: 40C (hold 2 min.) to 330C @ 10C/min. (hold 5 min.) Inj. temp.: 250C Det. temp.: 330C Detector: FID

Wisconsin GRO Mix, plus C12 4 Rtx-502.2


3

6 7 8 10

105m, 0.53mm ID, 3.0m Rtx-502.2 (cat.# 10910) GRO + C12 standard. Conc.: 200ppb each in 5mL of H2O. Oven temp.: Inj. / det. temp.: Carrier gas: Flow rate: Trap: Purge: Desorb preheat: Desorb temp.: Desorb time: Desorb flow: FID sensitivity:
9

40C (hold 1 min.) to 100C @ 5C/min. to 240C @ 8C/min. (hold 8 min.) 200C / 250C helium 10mL/min. Tenax, silica gel, charcoal 12 min. @ 40mL/min. 175C 180C 2 min. 10mL/min. 16 x 10-11 AFS

1 2

4 3 6 7 8

10

FID
min. 10 20 30 5

Standard used is GRO Mix (WISC) + C12 (cat.# 30069): 1. 3-methylpentane 2. 2,2,4-trimethylpentane (isooctane) 3. benzene 4. toluene 5. ethylbenzene 6. m-xylene 7. o-xylene 8. 1,2,4-trimethylbenzene 9. dodecane 10. naphthalene
GC_EV00071

PID
min. 10 20 30

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608

Gasoline Range Organics (GRO)


Oxygenates Rtx-VGC
25 22 23 24

15, 16 20

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

9 12 13 14 4 5 3 6 10 11 19 17 18 21

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25.

2-methylpentane 3-methylpentane methyl-tert-butyl ether tert-butanol diisopropyl ether ethyl-tert-butyl ether isooctane n-heptane benzene tert-amyl-methyl ether ,,-trifluorotoluene toluene 1-chloro-3-fluorobenzene ethylbenzene m-xylene p-xylene o-xylene isopropylbenzene ethylmethylbenzene 1,3,5-trimethylbenzene 1,2,4-trimethylbenzene 4-bromochlorobenzene naphthalene 2-methylnaphthalene 1-methylnaphthalene

see conditions below

12

8 7

min.

10 GC_EV00465

15

20

BTEX Rtx-VGC
1. 2. 3. 4. 5. 6. 7. 8. 9. benzene ,,-trifluorotoluene toluene ethylbenzene chlorobenzene m-xylene p-xylene o-xylene 4-bromo-1-chlorobenzene
1 3 4 5 8 6/7

Unleaded Gasoline Rtx-VGC


1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. benzene toluene ethylbenzene m-xylene p-xylene o-xylene isopropylbenzene ethylmethylbenzene 1,2,3-trimethylbenzene 1,2,4-trimethylbenzene naphthalene 2-methylnaphthalene 1-methylnaphthalene

min. 0

10 GC_EV00468

15

20

Conditions for all chromatograms on this page: 30m, 0.45mm, 2.55m Rtx-VGC (cat.# 19408) each component 100ppb in 5mL of RO water, except tert-butanol 5000ppb; 2/1-methynapthalene 150ppb; ethylmethylbenzene 50ppb. Concentrator: Tekmar LSC-3100 Purge and Trap Trap: Vocarb 3000 Purge: 11 min. @ 40mL/min. @ 35C Dry purge: 1 min. (MCS bypassed) GC: Finnigan 9001 Oven temp.: 40C (hold 2 min.) to 130C @ 6C/min. (hold 0 min.) to 230C @ 30C/min. (hold 2 min.). Carrier gas: helium @ ~8mL/min. Detector: Finnigan PID, make up 7mL min., purge 7mL/min., set @ 0.35mV, base temperature 200C.
GC_EV00467

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Gasoline Range Organics (GRO)


BTEX Rtx-502.2
4 6 8

609

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

1 2

3 10

FID
min. 10 20 30

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

3-methylpentane 2,2,4-trimethylpentane (isooctane) benzene toluene ethylbenzene m-xylene o-xylene 1,2,4-trimethylbenzene dodecane naphthalene

10 9

PID
min. 10 GC_EV00073 20 30

105m, 0.53mm ID, 3.0m Rtx-502.2 (cat.# 10910) 2500L/mL injection of Unleaded Gasoline Composite Standard (cat.# 30081), 10L spiked into 5mL H2O. Oven temp.: Inj. / det. temp.: Carrier gas: Flow rate: Trap: Purge: Desorb preheat: Desorb temp.: Desorb time: Desorb flow: FID sensitivity: 40C (hold 1 min.) to 100C @ 5C/min., to 240C @ 8C/min. (hold 8 min.) 200C / 250C helium 10mL/min. Tenax, silica gel, charcoal 12 min. @ 40mL/min. 175C 180C 2 min. 10mL/min. 16 x 10-11 AFS

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610

Gasoline Range Organics (GRO)


Oxygenates Rtx-VGC

restek innovation!
Resolve gasoline components and common oxygenated additives!
20,21

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

23 24 25

19 18 17 2 16 22

26

29 27 6,7 9 3 5 11 1 4 12 13 15 14 10 28 30

8 10 14 GC_EV00401

min.

18

22

26

30m, 0.25mm, 1.40m Rtx-VGC (cat.# 19415) 10:1 split at injection port; 1mm ID liner Compounds at 100ppb in 5mL of RO water (unless otherwise noted) Oven program: 35C (hold 14 min.) to 220C @ 24C/min. (hold 6 min.) Carrier gas: helium @ ~1mL/min. constant flow Concentrator: Tekmar LSC-3100 Purge and Trap Trap: Vocarb 3000 Purge: 11 min. @ 40mL/min. @ ambient temperature Dry purge: 1 min. @ 40mL/min. (MCS bypassed using Silcosteel tubing) Desorb preheat: 245C Desorb: 250C for 2 min., Flow 10mL/min. Bake: 260C for 8 min. Interface: transfer line 0.32mm ID Siltek fused silica Detector: Agilent 5973 MS Scan range: 25-300amu

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

methanol (100,000ppb) ethanol (10,000ppb) 2-methylpentane 2-propanol (500ppb) 3-methylpentane hexane methyl tert-butyl ether tert-butanol (500ppb) diisopropyl ether ethyl-tert-butyl ether isooctane benzene n-heptane tert-amyl methyl ether 1-butanol (500ppb)

16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30.

,,-trifluorotoluene toluene 1-chloro-3-fluorobenzene ethylbenzene m-xylene p-xylene o-xylene isopropylbenzene decane 1,3,5-trimethylbenzene 1,2,4-trimethylbenzene 4-bromochlorobenzene naphthalene 2-methylnaphthalene (150ppb) 1-methylnaphthalene (150ppb)

free literature
Resolving Oxygenates from Gasoline Additives, Using an Rtx-VGC GC Column (lit. cat.# 59345) Avoid coelution of compounds that share quantification ions Successful analysis of oxygenates in environmental samples depend on the ability of the analytical column to resolve the oxygenates from early-eluting alkanes, alkenes, and alkynes. Nonpolar columns are used for this application, but they are incompatible with polar compounds, and thus can give broad peaks and reduced sample capacity for the alcohols. The unique polarity of Rtx-VGC columns makes them ideal for oxygenates analysis. Example chromatograms with both PID and MS detection are shown in this 4-page note; purge and trap conditions also are discussed.

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Gasoline Range Organics (GRO)


Unleaded Gasoline Rtx-5
Rtx-5 15m, 0.25mm ID, 0.25m (cat.# 10220) Sample: 500g/mL Unleaded Gasoline Standard (unweathered) (cat.# 30096) in methylene chloride Inj.: 1.0L splitless (hold 0.5 min.), 4mm single gooseneck inlet liner (cat.# 20904) Inj. temp.: 260C Carrier gas: helium, constant pressure Linear velocity: 76cm/sec. @ 50C Oven temp.: 35C (2 min.) to 330C @ 60C/min. using GC Racer Det.: FID @ 330C

611

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00671

Jet Fuel Rtx-5


Rtx-5 15m, 0.25mm ID, 0.25m (cat.# 10220) Sample: 500g/mL Jet Fuel A standard (cat.# 31215) in methylene chloride Inj.: 1.0L splitless (hold 0.5 min.), 4mm single gooseneck inlet liner (cat.# 22405) Inj. temp.: 260C Carrier gas: helium, constant pressure Linear velocity: 76cm/sec. @ 50C Oven temp.: 50C (1 min.) to 330C @ 60C/min. (hold 0.5 min.) using GC Racer Det.: FID @ 330C

for more info


FAST analyses, using a GC Racer temperature programmer described on page 149.

GC_EV00670

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612

Diesel Range Organics (DRO)


Motor Oil Rtx-5

for more info


Rtx-5 15m, 0.25mm ID, 0.25m (cat.# 10220) Sample: 500g/mL motor oil in methylene chloride Inj.: 1.0L splitless (hold 0.5 min.), 4mm single gooseneck inlet liner (cat.# 22405) Inj. temp.: 260C Carrier gas: helium, constant pressure Linear velocity: 76cm/sec. @ 50C Oven temp.: 50C (1 min.) to 330C @ 60C/min. (hold 0.5 min.) using GC Racer Det.: FID @ 330C

FAST analyses, using a GC Racer temperature programmer described on page 149.

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_EV00675

All 3 chromatograms on pages 612-613 were run at equivalent conditionsall runs less than 10 min.

Searching for a chromatogram?

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Diesel Range Organics (DRO)


Diesel Fuel Rtx-5
Rtx-5 15m, 0.25mm ID, 0.25m (cat.# 10220) Sample: 500g/mL Diesel Fuel Composite standard (cat.# 31093) in methylene chloride Inj.: 1.0L splitless (hold 0.5 min.), 4mm single gooseneck inlet liner (cat.# 20904) Inj. temp.: 260C Carrier gas: helium, constant pressure Linear velocity: 76cm/sec. @ 50C Oven temp.: 50C (1 min.) to 330C @ 60C/min. (hold 0.5 min.) using GC Racer Det.: FID @ 330C

613

20C/min. temperature program

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

for more info


FAST analyses, using a GC Racer temperature programmer described on page 149.

GC_EV00668

Diesel Fuel Rtx-5


Rtx-5 15m, 0.25mm ID, 0.25m (cat.# 10220) Sample: 500g/mL Diesel Fuel Composite standard (cat.# 31093) in methylene chloride Inj.: 1.0L splitless (hold 0.5 min.), 4mm single gooseneck inlet liner (cat.# 20904) Inj. temp.: 260C Carrier gas: helium, constant pressure Linear velocity: 76cm/sec. @ 50C Oven temp.: 50C (1 min.) to 330C @ 20C/min. Det.: FID @ 330C

60C/min. temperature program

GC_EV00669

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614

Diesel Range Organics (DRO)


DRO Mix Rtx-5

3 4 5 6 7

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

9 10

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

C10 C12 C14 C16 C18 C20 C22 C24 C26 C28

30m, 0.53mm ID, 1.0m Rtx-5 (cat.# 10255) Direct injection of DRO Mix (cat.# 31064) Conc.: 50ng/L Oven temp.: Inj. / det. temp.: Carrier gas: FID sensitivity: 40C (hold 2 min.) to 310C @ 12C/min. (hold 10 min.) 280C / 310C helium @ 65cm/sec. 8 x 10-11 AFS

min.

10

15 GC_EV00069

20

25

Diesel Fuel Rtx-5

30m, 0.53mm ID, 1.0m Rtx-5 (cat.# 10255) Direct injection of Diesel Fuel #2 Composite (cat.# 31093) Conc.: 500ng/L Oven temp.: Inj. / det. temp.: Carrier gas: FID sensitivity: 40C (hold 2 min.) to 310C @ 12C/min. (hold 10 min.) 280C / 310C helium @ 65cm/sec. 8 x 10-11 AFS

min.

10

15 GC_EV00070

20

25

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Glycols
Glycols Rtx-Wax

615

1. propylene glycol 2. ethylene glycol

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

30m, 0.53mm ID, 1.0m Rtx-Wax (cat.# 12455) Inj.: direct Inj. / det. temp.: 220C / 270C Oven temp.: 80C (hold 1 min.) to 120C @ 8C/min. (hold 3 min.) 10psi pressure Std. = 100g/mL

min.

1.50

2.50

3.50

4.50

5.50

6.50

7.50

8.50

9.50

10

GC_EV00444

free literature
Techniques to Optimizing GC Analysis of Ethylene Glycol in Water
(lit. cat.# 59187)

Glycols Rtx-200

Avoid the problems that aqueous samples can create


Direct injections of water-based samples, such as samples containing ethylene glycol, can cause problems for chromatographers. This 4-page note alerts analysts to the potential for poor peak shape, sample carryover, and FID flameout, and describes approaches to follow to avoid these problems. With care, detection limits of 1-10ppm ethylene glycol can be attained.

2 1

1. ethylene glycol 2. propylene glycol 30m, 0.53mm ID, 1.0m Rtx-200 (cat.# 15055) Inj.: direct Inj. / det. temp.: 220C / 270C Oven temp.: 80C (hold 1 min.) to 200C @ 8C/min. (hold 3 min.) 10psi pressure Std. = 100g/mL

min.

0.20

0.40

0.60

0.80

1.00

1.20

1.40

1.60

1.80

2.00

2.20

2.40

2.60

2.80

3.00

3.20

3.40

3.60

3.80

4.00

GC_EV00445

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616

Glycols
Glycols Stabilwax
1. 2. 3. 4. 5. 6. 7. 1,2-propylene glycol ethylene glycol 1,3-butylene glycol 1,3-propylene glycol 1,4-butylene glycol diethylene glycol glycerol

Glycols Stabilwax

30m, 0.53mmID, 1.0m Stabilwax (cat.# 10655) 1.0L direct injection of glycol mix, open-top Uniliner liner without wool (cat.# 20843-205) Conc.: 150ppm Solvent: water/methanol (50:50)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Oven temp.: Septa Purge: Carrier Gas: Linear Velocity: Column Flow Rate: Detector: Make up Gas Flow:

80C to 200C @ 8C/min. (hold 10 min.) 5.0cc/min. helium 50cm/sec. 6.9mL/min. FID/270C 45cc/min.

1. propylene glycol 2. ethylene glycol

30m, 0.53mm ID, 1.0m Stabilwax (cat.# 10655) 1.0L of direct injection of glycols in water. Open-top Uniliner, liner without wool (cat.# 20843-205). Conc.: 100ppm Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Detector: Septum Purge: 80C (hold 1 min.) to 200C @ 8C/min. (hold 5 min.) 225C/250C helium 50cm/sec. FID 5.0cc/min.

~ ~
min.8.0
GC_EV00476

9.0

10.0
GC_EV00546

11.0

Glycols Rtx-BAC1 & Rtx-BAC2


Rtx-BAC1 Rtx-BAC2

1. ethylene glycol 2. propylene glycol

30m, 0.32mm ID, 1.8m Rtx-BAC1 (cat.# 18003) 30m, 0.32mm ID, 1.2m Rtx-BAC2 (cat.# 18002) 0.5L split injection Conc.: 1% Solvent: methanol Oven temp.: Inj. temp.: Inj. mode: Liner: Septa purge: Carrier gas: Pressure: Linear velocity: Column flow rate: Detector: Make-up gas flow: 100C to 240C @ 5C/min. (hold 5 min.) 240C 100:1 split Agilent 4mm single gooseneck 5.0cc/min. helium, constant pressure 12psi 37cm/sec. 2.1mL/min. FID/240C 40cc/min.

GC_EV00474

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Haloacetic Acids
Haloacetic Acids US EPA Method 552.2 Rtx-5

617

10 8

6/7 5

11

12

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

monochloroacetic acid (MCAA) monobromoacetic acid (MBAA) dichloroacetic acid (DCAA) dalapon 1,2,3-trichloropropane (I.S.) bromochloroacetic acid (BCAA) trichloroacetic acid (TCAA) dibromoacetic acid (DBAA) bromodichloroacetic acid (BDCAA) 2,3-dibromopropionic acid (Surr.) chlorodibromoacetic acid (CDBAA) tribromoacetic acid (TBAA)

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

(All compounds derivatized)


2 3 4

min.

10

12

14

16

18

20

22

24

26

GC_EV00025

30m, 0.25mm ID, 1.0m Rtx-5 (cat.# 10253) 1.0L split injection. 1ng on-column concentration. Oven temp.: 50C (hold 10 min.) to 225C @ 8C/min. Inj./det. temp.: 200C/290C Carrier gas: helium Linear velocity: 30cm/sec. @ 50C ECD sensitivity: 20kHz full scale Split ratio: 10:1

Haloacetic Acids US EPA Method 552.2 Rtx-200


8 10 9 11 6 7 12 2/3

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

monochloroacetic acid (MCAA) monobromoacetic acid (MBAA) dichloroacetic acid (DCAA) dalapon 1,2,3-trichloropropane (I.S.) bromochloroacetic acid (BCAA) trichloroacetic acid (TCAA) dibromoacetic acid (DBAA) bromodichloroacetic acid (BDCAA) 2,3-dibromopropionic acid (Surr.) chlorodibromoacetic acid (CDBAA) tribromoacetic acid (TBAA)

(All compounds derivatized)

4 5 1

min.

10

12

14

16

18

20

22

24

26

GC_EV00026

30m, 0.25mm ID, 1.0m Rtx -200 (cat.# 15053) 1.0L split injection. 1ng on-column concentration. Oven temp.: 50C (hold 10 min.) to 225C @ 8C/min. Inj./det. temp.: 200C/290C Carrier gas: helium Linear velocity: 30cm/sec. @ 50C ECD sensitivity: 20kHz full scale Split ratio: 10:1

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618

Haloacetic Acids
Haloacetic Acids US EPA Method 552.2 Rtx-CLPesticides & Rtx-CLPesticides2
Rtx-CLPesticides 30m, 0.32mm ID, 0.50m (cat.# 11139)
1. monochloroacetic acid 2. monobromoacetic acid 3. dichloroacetic acid 4. dalapon 5. 1,2,3-trichloropropane 6. trichloroacetic acid 7. bromochloroacetic acid 8. dibromoacetic acid 9. bromodichloroacetic acid 10. chlorodibromoacetic acid 11. 2,3-dibromopropionic acid 12. tribromoacetic acid C = contaminant in solvent Compounds derivatized to esters MCAA MBAA DCAA DL IS TCAA BCAA DBAA BDCAA CDBAA SURR TBAA RT 4.41 5.75 5.92 6.35 6.97 7.20 7.31 8.43 8.52 9.68 9.82 10.73
10 11 12

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

7 9

8 2 3 6

4 C 1 5

min.

6
GC_EV00399

10

11

10 11

12

Rtx-CLPesticides2 30m, 0.32mm ID, 0.25m (cat.# 11324)


1. monochloroacetic acid 2. monobromoacetic acid 3. dichloroacetic acid 4. dalapon 6. trichloroacetic acid 5. 1,2,3-trichloropropane 7. bromochloroacetic acid 9. bromodichloroacetic acid 8. dibromoacetic acid 10. chlorodibromoacetic acid 11. 2,3-dibromopropionic acid 12. tribromoacetic acid C = contaminant in solvent (Compounds derivatized to esters) MCAA MBAA DCAA DL TCAA IS BCAA BDCAA DBAA CDBAA SURR TBAA RT 3.70 5.43 5.50 5.78 6.83 6.98 7.17 8.43 8.49 9.80 9.86 11.04
2 4+C 1

9 7

8 3 6

min.

6
GC_EV00400

10

11

2L splitless injection of custom haloacetic acid methyl derivatives std. [20-200g/mL] mix in MTBE Oven temp.: 40C (hold 4 min.) to 200C @ 14C/min. Inj. temp.: 200C Carrier gas: helium Linear velocity: 46cm/sec. ECD temp.: 300C

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Air Analysis
US EPA TO-14 Compounds Rtx-1
60m, 0.32mm ID, 3.0m Rtx-1 (cat.# 10187) 5mL of 2ppmv TO-14 standard. Oven temp.: Detector: Det. temp.: Carrier gas: Linear velocity: Ionization: Scan range: 30C (hold 4 min.) to 250C @ 7C/min. (hold 15 min.). MS 250C helium 21cm/sec. set @ 30C EI 18 34-280 AMU 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 26 13. 14. 15. 16. 17. 18. 19. 20.
27 14 11 19 28 13 8 3 1 5 9 10 12 15 17 23 29,30 32,33 37 39 41 24

619

Preconcentrator conditions: Nutech 3550 A Preconcentrator Cryotrap temp.: -160C Cryotrap desorb temp.: 150C Cryofocusing unit temp.: -190C Cryofocusing desorb temp.: 150C
7

16

20

dichlorodifluoromethane chloromethane 1,2-dichlorotetrafluoroethane vinyl chloride bromomethane chloroethane trichlorofluoromethane 1,1-dichloroethene methylene chloride 3-chloropropene 1,1,2-trichloro-1,2,2-trifluoroethane 1,1-dichloroethane cis-1,2-dichloroethene chloroform 1,2-dichloroethane 1,1,1-trichloroethane benzene carbon tetrachloride 1,2-dichloropropane trichloroethene

21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41.

cis-1,3-dichloropropene trans-1,3-dichloropropene 1,1,2-trichloroethane toluene 1,2-dibromoethane tetrachloroethene chlorobenzene ethylbenzene m-xylene p-xylene styrene o-xylene 1,1,2,2-tetrachloroethane 4-methyltoluene 1,3,5-trimethylbenzene 1,2,4-trimethylbenzene 1,3-dichlorobenzene 1,4-dichlorobenzene 1,2-dichlorobenzene 1,2,4-trichlorobenzene hexachlorobutadiene

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

34 21 25 38 35 36 40

22 6

31

min.

10

15

20
GC_EV00018

25

30

35

Ozone Precursors Rtx-1


1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. ethylene acetylene ethane propylene propane isobutane 1-butene n-butane trans-2-butene cis-2-butene isopentane 2-methyl-1-butene n-pentane trans-2-pentene cis-2-pentene cyclopentane isohexane 3-methylpentane n-hexane methylcyclopentane benzene isoheptane 2,3-dimethylpentane 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 3-methylhexane 2,2,4-trimethylpentane n-heptane methylcyclohexane 2,2,3-trimethylpentane toluene ethylbenzene m-xylene p-xylene o-xylene n-nonane n-propylbenzene p-ethyltoluene 1,3,5-trimethylbenzene 1,2,4-trimethylbenzene

60m, 0.32mm ID, 3.0m Rtx-1 (cat.# 10187) 0.5L of C2-C9 gas standard cryogenically concentrated; 15nL/component desorbed onto column. Oven temp.: Carrier gas: Linear velocity: FID sensitivity: -60C (hold 5 min.) to 100C @ 8C/min., to 150C @ 6C/min., then to 240C @ 8C/min. helium 30cm/sec. (flow rate: 1.8cc/min.) 64 x 10-12 AFS

23 24 18 19 20 21 13 12 11 9 8 7 10 14 15 16 17 22 25 26 27 28 29

31,32 30 33 34

35

36,37 38

6 4

1 2 3

min.

10

15

20
GC_EV00019

25

30

35

Permission to publish this chromatogram granted by Radian Corporation.

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620

Air Analysis
Air Toxins Rtx-502.2

56 32 46

47 67

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

36,37

48,49

51,52 60 62 5 1 7 6 4 10 8 9 12 14 13 17 16 18 15 20 22,23 24 19 21 30 35 28 31 44 27 45 42 29 34 54 11 25,26 38 40 41 43 55 59 61 68 71 33 39 50 58 53 57 64 65 66 63 69 70

min.

10

15

20
GC_EV00022

25

30

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18.

chlorodifluoromethane dichlorodifluoromethane dichlorotetrafluoroethane chloromethane butane vinyl chloride 1,3-butadiene acetaldehyde bromomethane chloroethane trichlorofluoromethane isopropanol acetone 1,1-dichloroethene acetonitrile dichloromethane acrylonitrile 1-propanol

19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36.

trans-1,2-dichloroethene 1,1-dichloroethane methyl ethyl ketone cis-1,2-dichloroethene methacrylonitrile chloroform bromochloromethane tetrahydrofuran 1,1,1-trichloroethane n-butanol heptane 1,2-dichloroethane benzene 1,4-difluorobenzene trichloroethene ethyl methacrylate 1,2-dichloropropane 1,4-dioxane

37. 38. 39. 40. 41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54.

bromodichloromethane 4-methyl-2-pentanone octane toluene 2-hexanone 1,1,2-trichloroethane tetrachloroethene dibromochloromethane 1,2-dibromoethane chlorobenzene-d5 chlorobenzene m-xylene p-xylene 2-heptanone styrene o-xylene isopropylbenzene bromoform

55. 56. 57. 58. 59. 60. 61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71.

1,1,1,2-tetrachloroethane 4-bromofluoromethane n-propylbenzene 1,3,5-trimethylbenzene -methylstyrene tert-butylbenzene 1,2,4-trimethylbenzene sec-butylbenzene 1,3-dichlorobenzene 1,4-dichlorobenzene butylbenzene 1,2-dichlorobenzene dodecane dibromochloropropane 1,2,4-trichlorobenzene hexachlorobutadiene naphthalene

60m, 0.32mm ID, 1.8m Rtx-502.2 (cat.# 10920) 500mL of 10ppbv standard. Concentrated on an AEROCAN 6000 using a glass bead trap at 165C then desorbed at 200C for 4 min. @ 1mL/min. Cryofocused @ -175C then desorbed @ 150C. Oven temp.: Det. & det. temp.: Carrier gas: Linear velocity: Scan range: Solvent delay: 35C (hold 6 min.) to 120C @ 15C/min., then to 200C @ 5C/min., then to 220C @ 25C/min. (hold 10 min.). Agilent-5971A GC/MS, 280C helium @ 1mL/min. 20cm/sec. 28-260 AMU 4 min.

Permission to publish this chromatogram granted by Tekmar Company.

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Air Analysis
US EPA TO-14/TO-15 Compounds Rtx-1

621

54

BFB

47 50 53 63 55 3 1 9/10 15 31 35/36 34 33 37 32 46 49 48 45 41 42 39 43 44 38 29 25 40 52 51 57 56 62 58 59 60

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

61

22/23

24

27 30 28 26

12 16 13 6 5 2 4 7 8 11 14 17 18 20 19 21

10

11

12

13

14
GC_EV00379

15

16

17

18

19

20

21

22

23 min.

Rtx-1 60m, 0.32mm ID, 1.0m (cat.# 10157). 200mL of 10ppbv TO-15 standard (cat.# 34436), injected into TO-Can canister and humidified to 70% RH. Concentrator: Nutech 3550 Preconcentrator 200mL of sample concentrated at 160C, thermally desorbed at 150C, and cryofocused at 185C. Oven temp.: 30C (hold 4 min.) to 175C @ 9C/min. to 220C @ 40C/min. Carrier gas: helium @ 1.2mL/min. Det.: Agilent 5971 MS Scan range: 35-265amu

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

dichlorofluoromethane chloromethane dichlorotetrafluoroethane vinyl chloride 1,3-butadiene bromomethane chloroethane bromoethene acetone trichlorofluoromethane isopropyl alcohol 1,1-dichloroethene methylene chloride 3-chloropropene carbon disulfide Freon TF trans-1,2-dichloroethene 1,1-dichloroethane methyl tert-butyl ether methyl ethyl ketone cis-1,2-dichloroethene bromochloromethane (IS)

23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44.

n-hexane chloroform tetrahydrofuran 1,2-dichloroethane 1,1,1-trichloroethane benzene carbon tetrachloride cyclohexane 1,4-difluorobenzene (IS) 1,2-dichloropropane bromodichloromethane trichloroethene 1,4-dioxane 2,2,4-trimethylpentane n-heptane cis-1,3-dichloropropene methyl isobutyl ketone trans-1,3-dichloropropene 1,1,2-trichloroethane toluene methyl butyl ketone dibromochloromethane

45. 1,2-dibromoethane 46. tetrachloroethene 47. chlorobenzene-d5 (IS) 48. chlorobenzene 49. ethylbenzene 50a. m-xylene 50b. p-xylene 51. bromoform 52. styrene 53. 1,1,2,2-tetrachloroethane 54. o-xylene 55. 2-chlorotoluene 56. 4-ethyltoluene 57. 1,3,5-trimethylbenzene 58. 1,2,4-trimethylbenzene 59. 1,3-dichlorobenzene 60. 1,4-dichlorobenzene 61. 1,2-dichlorobenzene 62. 1,2,4-trichlorobenzene 63. hexachlorobutadiene

Chromatogram courtesy of Gina Maio, Severn Trent Laboratories, Inc., Burlington, VT.

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622

Air Analysis
US EPA TO-15 Compounds Rtx-1

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

Rtx-1 30m, 0.32mm ID, 1.0m (cat.# 10157) Sample: TO-15 standard (cat.# 34436) humidified to 33% RH in a 6L SilcoCan canister (cat.# 24182) Concentrator: Nutech 3550A cryogenic concentrator; 300mL sample concentrated at -160C, thermally desorbed at 150C, cryofocused at -185C, thermally desorbed to column at 150C Carrier gas: helium, constant flow Flow rate: 1.2mL/min. Oven temp.: 30C (hold 4 min.) to 175C @ 8C/min., to 220C @ 20C/min. (hold 2 min.) Det.: MS Transfer line temp.: 150C Scan range: 35280 amu Ionization: EI Mode: scan

GC_AR00748

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

propylene Freon-12 (dichlorodifluoromethane) chloromethane Freon-114 (dichlorotetrafluoroethane) vinyl chloride 1,3-butadiene bromomethane chloroethane carbon disulfide acetone Freon-11 (trichlorofluoromethane) isopropyl alcohol 1,1-dichloroethene methylene chloride Freon-113 (1,1,2-trichloro-1,2,2-trifluoroethane) trans-1,2-dichloroethene 1,1-dichloroethane methyl tert-butyl ether vinyl acetate methyl ethyl ketone cis-1,2-dichloroethene

22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42.

hexane chloroform ethyl acetate tetrahydrofuran 1,2-dichloroethane 1,1,1-trichloroethane benzene carbon tetrachloride cyclohexane 1,2-dichloropropane trichloroethylene bromodichloromethane 1,4-dioxane heptane cis-1,3-dichloropropene methyl isobutyl ketone trans-1,3-dichloropropene 1,1,2-trichloroethane toluene methyl butyl ketone dibromochloromethane

43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60. 61.

1,2-dibromoethane tetrachloroethylene chlorobenzene ethylbenzene p-xylene m-xylene bromoform styrene o-xylene 1,1,2,2-tetrachloroethane 4-ethyltoluene 1,3,5-trimethylbenzene 1,2,4-trimethylbenzene 1,3-dichlorobenzene benzyl chloride 1,4-dichlorobenzene 1,2-dichlorobenzene 1,2,4-trichlorobenzene hexachloro-1,3-butadiene

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Air Analysis
Massachusetts APH Mix Rtx-1

623

G C A P P L I C AT I O N S | E N V I R O N M E N TA L

GC_AR00697

Rtx-1 60m, 0.32mm ID, 1.0m (cat.# 10157) Sample: Massachusetts APH Mix, (cat.# 34446) Concentrator: Nutech 3550A Air Preconcentrator, 100mL of a 40ppbv standard concentrated at -160C, thermally desorbed at 150C and cryofocused at -185C. Carrier gas: helium Flow rate: 1mL/min. Oven temp.: Det: Transfer line temp.: Scan range: Ionization: Mode: 35C (hold 1 min.) to 220C @ 8C/min. MS, HP5971 250C 35-280amu EI scan

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

1,3-butadiene isopentane methyl tert-butyl ether hexane benzene cyclohexane 2,3-dimethylpentane heptane toluene-D8 toluene octane ethylbenzene 2,3-dimethylheptane

14a. m-xylene 14b. p-xylene 15. o-xylene 16. nonane 17. isopropylbenzene 18. 1-methyl-3-ethylbenzene 19. 1,3,5-trimethylbenzene 20. decane 21. 1,2,3-trimethylbenzene 22. p-isopropyltoluene 23. butylcyclohexane 24. undecane 25. dodecane

a plus 1 story
Restek is a first class company with excellent customer service. Courtesy is always extended to both my company and myself when communicating with Restek employees Rich Whitney, Mass Spec Manager, ProChem Analytical

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624

Antioxidants, Preservatives
BHA and BHT Rtx-50

1. BHA 2. BHT

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GC_FF00630

Rtx-50, 30m, 0.53mm ID, 0.50m (cat.# 10540) Sample: 50ppm each in methanol Inj.: 1.0L direct, gooseneck splitless inlet liner, 4mm (cat.# 20798) Inj. temp.: 280C Carrier gas: helium, constant pressure Linear velocity: 60cm/sec. @ 50C Oven temp.: 50C to 240C @15C/min. (hold 3 min.) Det.: FID @280C

Tocopherols and Tocotrienols Rtx-20


Rtx-20, 30m, 0.53mm ID, 0.5m (cat.# 10340) Sample: 1mg/mL each component in isooctane Inj.: 1.0L split (split ratio 20:1), 4mm inlet liner (cat.# 20814) Inj. temp.: 320C Carrier gas: hydrogen, constant flow Flow rate: 5.2mL/min. Oven temp.: 270C to 290C @ 2C/min. 290C to 320C @ 10C/min. (1 min. hold) Det.: FID @ 320C

1. 2. 3. 4. 5. 6. 7. 8. 9.

-tocopherol -tocopherol -tocopherol dl--tocotrienol -tocopherol dl--tocotrienol dl--tocotrienol hexadecyl hexadecanoate dl--tocotrienol

GC_FF00634

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Chiral Separations
Lemon Oil Rt-DEXsm
1. (-/+)-pinene 2. (+/-)-pinene 3. (-/+)limonene
2 3 3

625

30m, 0.32mm ID, 0.25m Rt-DEXsm (cat.# 13104) Oven temp.: 40C (hold 1 min.) to 200C @ 2C/min. (hold 3 min.) Carrier gas: hydrogen Linear velocity: 80cm/sec. Det.: FID set @ 220C

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

min.

10

15

20

25 GC_FF00146

30

35

40

45

Rosemary Oil Rt-DEXsm


1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. (-/+)-pinene (+/-)camphene (+/-)-pinene (-/+)limonene eucalyptol (1,8-cineole) (-/+)linalool (+/-)camphor (-/+)terpinen-4-ol (+/-)isoborneol (+/-)borneol (+/-)-terpineol

5 4 7

10 2

30m, 0.32mm ID, 0.25m Rt-DEXsm (cat.# 13104) Oven temp.: 40C (hold 1 min.) to 200C @ 2C/min. (hold 3 min.) Carrier gas: hydrogen Linear velocity: 80cm/sec. Det.: FID set @ 220C

4 6 3 9 9

11 11 10

min.

10

20 GC_FF00147

30

40

Geranium Oil (Commercial) Rt-DEXsa


1a. 1b. 2a. 2b. 3. 4. 5a. 5b. 6a. 6b. 7. 8. (+)-(2R,4S)-cis-rose oxide (-)-(2S,4R)-cis-rose oxide (-)-(2R,4R)-trans-rose oxide (+)-(2S,4S)-trans-rose oxide isomenthone menthone (-)-(R)-linalool (+)-(S)-linalool (-)-(S)--citronellol (+)-(R)--citronellol geraniol citronellyl formate

6a 6b

8 3 7

30m, 0.25mm ID, 0.25m Rt-DEXsa (cat.# 13109) Oven temp.: 60C to 110C @ 1C/min. (hold 30 min.) Carrier gas: hydrogen Linear velocity: 40cm/sec. set @ 60C Det.: FID set @ 220C
min. 20

5a 5b 1b 1a 2a 2b 4

30

40 GC_FF00148

50

60

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626

Chiral Separations
Menthol - Rt-DEXsp
2 1

Irone Isomers - Rt-DEXcst


4

1. (-)menthol 2. (+)menthol

8 5

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

(-)-(2R,6R)-trans--irone (+)-(2S,6S)-trans--irone (+)-(2R,6R)-trans--irone (-)-(2S,6S)-trans--irone (+)-(2R,6S)-cis--irone (+)-(2R,6S)-cis--irone (-)-(2S,6R)-cis--irone (-)-(2S,6R)-cis--irone (+)-(2R)--irone (-)-(2R)--irone

7 12

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

min.

30 GC_FF00149

30m, 0.32mm ID, 0.25m Rt-DEXsp (cat.# 13110) Oven temp.: 60C (hold 1 min.) to 200C @ 2C/min. Carrier gas: hydrogen Linear velocity: 80cm/sec. set @ 40C Det.: FID set @ 220C

30m, 0.32mm ID, 0.25m Rt-DEXcst (cat.# 13108) Oven temp.: 40C (hold 1 min.) to 9 230C @ 2C/min. (hold 3 min.) 10 Carrier gas: hydrogen Linear velocity: 80cm/sec. set @ 40C Det.: FID set @ 220C

min.

40 GC_FF00150

1-octen-3-ol and carvone - Rt-DEXsa


1. (+/-)1-octen-3-ol 2. (-)carvone 3. (+)carvone
1 2 3

-lactones - Rt-DEXcst
4 3 2 1

1. 2. 3. 4. 5.

(+/-)-heptalactone (+/-)-octalactone (+/-)-nonalactone (+/-)-decalactone (+/-)-dodecalactone

30m, 0.32mm ID, 0.25m Rt-DEXcst (cat.# 13102) Oven temp.: 60C (hold 1 min.) to 200C @ 1C/min. Carrier gas: hydrogen Linear velocity: 40cm/sec. set @ 60C Det.: FID set @ 220C
min. 20 GC_FF00151 30 40

30m, 0.32mm ID, 0.25m Rt-DEXsa (cat.# 13108) Oven temp.: 40C (hold 1 min.) to 230C @ 2C/min. (hold 3 min.) Carrier gas: hydrogen Linear velocity: 80cm/sec. set @ 40C Det.: FID set @ 220C

min.

100

120 GC_FF00152

140

-citronellol - Rt-DEXsa
1 2

-lactones - Rt-DEXcst
1 2 3 4 5 6 7

1.(-)-(S)--citronellol 2.(+)-(R)--citronellol

30m, 0.32mm ID, 0.25m Rt-DEXsa (cat.# 13108) Oven temp.: 40C (hold 1 min.) to 230C @ 2C/min. (hold 3 min.) Carrier gas: hydrogen Linear velocity: 80cm/sec. set @ 40C Det.: FID set @ 220C

1. 2. 3. 4. 5. 6. 7.

(+/-)-pentalactone (+/-)-hexalactone (+/-)-heptalactone (+/-)-octalactone (+/-)-nonalactone (+/-)-decalactone (+/-)-dodecalactone

30m, 0.32mm ID, 0.25m Rt-DEXcst (cat.# 13102) Oven temp.: 60C (hold 1 min.) to 200C @ 1C/min. Carrier gas: hydrogen Linear velocity: 40cm/sec. set @ 60C Det.: FID set @ 220C

min.

51

52 GC_FF00153

53

min.

100

120 GC_FF00154

140

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Chiral Separations
Apple Juice with Added Standards Rt-DEXsm
3

627

Apple Juice Rt-DEXsm

1. 2. 3. 4.
2

(R)-ethyl 2-methylbutyrate (S)-ethyl 2-methylbutyrate (R)-2-methylbutyrate (S)-2-methylbutyrate

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

1 4

min.

6 GC_FF00155

10

min.

6 GC_FF00156

10

30m, 0.32mm ID, 0.25m Rt-DEXsm (cat.# 13104) 1.0L split injection On-column conc. (standards): ~50ng each labeled enantiomer Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: 40C (hold 1 min.) to 220C @ 2C/min. 220C hydrogen 80cm/sec.

Apple Juice with Added Standards Rt-DEXse

Apple Juice Rt-DEXse

1. 2. 3. 4.

(R)-ethyl 2-methylbutyrate (S)-ethyl 2-methylbutyrate (R)-2-methylbutyrate (S)-2-methylbutyrate


3

2 1 4

min.

10 GC_FF00157

12

14

min.

10 GC_FF00158

12

14

30m, 0.32mm ID, 0.25m Rt-DEXse (cat.# 13106) 1.0L split injection On-column conc. (standards): ~50ng each labeled enantiomer Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: 40C (hold 1 min.) to 220C @ 2C/min. 220C hydrogen 80cm/sec.

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628

Chiral Separations
Grape Juice Extract Rt-DEXsa
4

1. 2. 3. 4.
1 2

methyl (S)-(+)-3-hydroxybutyrate methyl (R)-(+)-3-hydroxybutyrate ethyl (S)-(+)-3-hydroxybutyrate ethyl (R)-(+)-3-hydroxybutyrate

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

min. 20

22

24 GC_FF00159

26

28

30m, 0.32mm ID, 0.25m Rt-DEXsa (cat.# 13112) 1.0L split injection On-column conc.: ~150ng/enantiomer Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Split ratio: 40C (hold 1 min.) to 200C @ 2C/min. 220C/230C hydrogen 80cm/sec. set @ 40C 25:1

free literature
foods, flavors, & fragrances (lit. cat.# 59260A) A brief summary of many applications and chromatography products
This guide is a good overview of the foods - flavors - fragrances applications for which Restek GC and HPLC columns have been used. Application areas include amino acids, carbohydrates, chiral separations, essential oils, fats and oils, flavors and fragrances, organic acids, preservatives, and vitamins. Includes a handy index of retention times for many flavor and fragrance compounds on a dimethylpolysiloxane or a PEG-type capillary GC column.

A Guide to the Analysis of Chiral Compounds by GC (lit. cat.# 59889) Resolve critical enantiomer pairs quickly and reliably
In some analyses, particularly with pharmaceutical or flavor and fragrance compounds, enantiomer pairs must be resolved for separate quantification. Five cyclodextrin-based Restek chiral capillary GC columns offer a unique range of selectivities, to enable you to accomplish these often-difficult separations. Many example chromatograms in this 24-page guide will help you find the best column - or columns - for your particular need.

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Chiral Separations
Raspberry Flavor - Rt-DEXsa

629

1. (R)--ionone 2. (S)--ionone 30m, 0.32mm ID, 0.25m Rt-DEXsa (cat.# 13108) Oven temp.: 60C (hold 2 min.) to 200C @ 3C/min. Carrier gas: helium; 60cm/sec. set @ 60C Det.: MS set @ 220C.

1 2

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

min.

10

20 GC_FF00161

30

40

Peach/Vanilla Flavor - Rt-DEXsa


1. 2. 3. 4. 5. (R)--octalactone (S)--octalactone (R)--decalactone (R)--undecalactone (S)--undecalactone

45

30m, 0.32mm ID, 0.25m Rt-DEXsa (cat.# 13108) Oven temp.: 60C (hold 2 min.) to 100C @ 15C/min. to 220C @ 3C/min. Carrier gas: helium, 60cm/sec. set @ 60C Det.: MS set @ 220C
3 1 2

min. 0

19 GC_FF00162

38

Bergamot Flavor - Rt-DEXse


2 5 6

1. 2. 3. 4. 5. 6.

(S)-limonene (R)-limonene (R)-linalool (S)-linalool (R)-linalyl acetate (S)-linalyl acetate

30m, 0.32mm ID, 0.25m Rt-DEXse (cat.# 13106) Oven temp.: 40C (hold 1 min.) to 200C @ 4C/min. Carrier gas: helium, 60cm/sec. set @ 40C Det.: MS set @ 220C

min.

8 GC_FF00163

13

18

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630

Fatty Acids
Fatty Acids (Free) Rt-QPLOT Fatty Acids (Free) Rtx-200
5 6 78

1. 2. 3. 4. 5. 6.

acetic acid propionic acid isobutyric acid n-butyric acid isovaleric acid n-valeric acid

2 3

4 5

6
3

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

1. acetic acid 2. propionic acid 3. isobutyric acid 4. n-butyric acid 5. isovaleric acid 6. n-valeric acid 7. isocaproic acid 8. caproic acid 9. heptanoic acid

10

12
GC_FF00496

14

16

18

30m, 0.32mm ID, 10m Rt-QPLOT (cat.# 19718) Sample: fatty acids mix Conc.: 5% of each compound in water Sample size: 0.5L Inlet liner: 3mm split w/glass wool (cat.# 20936-202.1) Oven temp.: Injector: Carrier gas: Head pressure: Column flow rate: Split ratio: Detector: Make-up gas flow: 75C to 240C @ 10C/min. (hold 15 min.) split @ 240C hydrogen (constant pressure mode) 12.0psi 1.1cc/min. @ 100C 100:1 FID @ 240C 40cc/min.

min.

2
GC_CH00282

30m, 0.25mm ID, 0.25m Rtx-200 (cat.# 15023) Sample: 0.8L split injection of a free fatty acid standard. Conc.: approximately 10 to 20ng/L. Oven temp.: 90C Inj. & det. temp.: 250C Carrier gas: hydrogen Linear velocity: 40cm/sec. (flow rate: 1.4cc/min.) FID sensitivity: 4 x 10-11 AFS Split vent: 40cc/min.

Fatty Acids (Free) Stabilwax-DA


1. 2. 3. 4. 5. 6. 7. 8. 9.
7 4 6 8 9

Fatty Acids (Free) Rtx-1


acetic acid propionic acid isobutyric acid n-butyric acid isovaleric acid n-valeric acid isocaproic acid caproic acid heptanoic acid
7 8 9

5 3

1. 2. 3. 4. 5. 6. 7. 8. 9.

acetic acid propionic acid isobutyric acid n-butyric acid isovaleric acid n-valeric acid isocaproic acid caproic acid heptanoic acid

6 5

34

2 2 1

min.

8
GC_CH00280

12

min. 4 30m, 0.25mm ID, 0.25m Stabilwax-DA (cat.# 11023) 1.0L split injection of a free acid standard. Concentration approximately 10 to 20ng/L. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 145C 250C hydrogen 40cm/sec. 2 x 10-11 AFS 50:1
GC_CH00281

30m, 0.53mm ID, 5.0m Rtx-1 (cat.# 10179) 0.2L injection of a 1020ng/L free fatty acid standard in water. Direct injection using a Uniliner inlet liner. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 60C to 180C @ 15C/min. 250C hydrogen 50cm/sec. (flow rate: 6cc/min.) 4 x 10-11 AFS

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Fatty Acids
Fatty Acids (Free) Stabilwax-DA

631

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

C4:0 - butyric acid C6:0 - caproic acid C8:0 - caprylic acid C10:0 - capric acid C12:0 - lauric acid C14:0 - myristic acid C16:0 - palmitic acid C18:0 - stearic acid C18:1 - oleic acid C18:2 - linoleic acid C18:3 - linolenic acid C20:0 - arachidic acid C22:0 - behenic acid

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

GC_FF00653

Stabilwax-DA 30m, 0.32mm ID, 0.25m (cat.# 11024) Sample: 1.0L FFA Mix Solvent: water Conc.: 5mg/mL in methanol Inj.: splitless/250C Splitless hold time: 0.25min. Carrier gas: hydrogen (constant flow mode) Flow rate: 6.0mL/min. Split flow: 75mL/min. Det.: FID/250C Inlet liner: laminar cup splitter Oven temp.: 40C to 250C @ 10C/min. (hold 15 min.)

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632

FAMEs
FAMEs (AOAC 996.06 Standard) Rt-2560

Food Industry FAME Mix cat. # 35077

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

GC_FF00649

Compound 1. C4:0 methyl butyrate 2. C6:0 methyl hexanoate 3. C8:0 methyl octanoate 4. C10:0 methyl decanoate 5. C11:0 methyl undecanoate 6. C12:0 methyl laurate 7. C13:0 methyl tridecanoate 8. C14:0 methyl myristate 9. C14:1 methyl myristoleate (cis-9) 10. C15:0 methyl pentadecanoate 11. C15:1 methyl pentadecenoate (cis-10) 12. C16:0 methyl palmitate 13. C16:1 methyl palmitoleate (cis-9) 14. C17:0 methyl heptadecanoate 15. C17:1 methyl heptadecenoate (cis-10) 16. C18:0 methyl stearate 17. C18:1 methyl elaidate (trans-9) 18. C18:1 methyl oleate (cis-9) 19. C18:2 methyl linoleaidate (trans-9,12) 20. C18:2 methyl linoleate (cis-9,12) 21. C20:0 methyl arachidate 22. C18:3 methyl -linolenate (cis-6,9,12) 23. C20:1 methyl eicosenoate (cis-11) 24. C18:3 methyl linolenate (cis-9,12,15) 25. C21:0 methyl heneicosanoate 26. C20:2 methyl eicosadienoate (cis-11,14) 27. C22:0 methyl behenate 28. C20:3 methyl eicosatrienoate (cis-8,11,14) 29. C22:1 methyl erucate (cis-13) 30. C20:3 methyl eicosatrienoate (cis-11,14,17) 31. C20:4 methyl arachidonate (cis-5,8,11,14) 32. C23:0 methyl tricosanoate 33. C22:2 methyl docosadienoate (cis-13,16) 34. C24:0 methyl lignocerate 35. C20:5 methyl eicosapentaenoate (cis-5,8,11,14,17) 36. C24:1 methyl nervonate (cis-15) 37. C22:6 methyl docosahexaenoate (cis-4,7,10,13,16,19)

% in Mix 4.0 4.0 4.0 4.0 2.0 4.0 2.0 4.0 2.0 2.0 2.0 6.0 2.0 2.0 2.0 4.0 2.0 4.0 2.0 2.0 4.0 2.0 2.0 2.0 2.0 2.0 4.0 2.0 2.0 2.0 2.0 2.0 2.0 4.0 2.0 2.0 2.0

Rt-2560, 100m, 0.25mm ID, 0.2m (cat.# 13199) Sample: Food Industry FAME Mix (cat.# 35077), 30mg/mL total FAMEs in methylene chloride Inj.: 2.0L split (split ratio 200:1), 4mm inlet liner (cat.# 20814) Inj. temp.: 225C Carrier gas: hydrogen, constant flow Flow rate: 1.2mL/min. Oven temp.: 100C (4 min. hold) to 240C @ 3C/min. (10 min. hold) Det.: FID @ 250C

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FAMEs
FAMEs (NLEA Mix) Rt-2560

633

did you know?


The Rt-2560 column provides the resolution of cis & trans FAMEs needed for AOAC Method 996.06

NLEA FAME Mix cat.# 35078

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

GC_FF00651

Column: Sample: Inj.: Inj. temp.: Carrier gas: Flow rate: Oven temp.: Det.:

Rt-2560 100m, 0.25mm ID, 0.20m (cat.# 13199) NLEA FAME Mix (cat.# 35078), 30mg/mL total FAMEs in methylene chloride 1.0L split (split ratio 100:1), 4mm inlet liner (cat.# 20814) 225C hydrogen, constant flow 1.2 mL/min. 100C (4 min. hold) to 240C @ 3C/min. (10 min. hold) FID @ 250C

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

C4:0 methyl butyrate C6:0 methyl hexanoate C8:0 methyl octanoate C10:0 methyl decanoate C11:0 methyl undecanoate C12:0 methyl laurate C13:0 methyl tridecanoate C14:0 methyl myristate C14:1 methyl myristoleate (cis-9) C15:0 methyl pentadecanoate

11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

C16:0 C16:1 C17:0 C18:0 C18:1 C18:1 C18:2 C18:2 C20:0 C20:1

methyl palmitate methyl palmitoleate (cis-9) methyl heptadecanoate methyl stearate methyl elaidate (trans-9) methyl oleate (cis-9) methyl linoelaidate (trans-9,12) methyl linoleate (cis-9,12) methyl arachidate methyl eicosenoate (cis-11)

21. 22. 23. 24. 25. 26. 27. 28.

C18:3 C22:0 C22:1 C23:0 C24:0 C20:5 C24:1 C22:6

methyl linolenate (cis-9,12,15) methyl behenate methyl erucate (cis-13) methyl tricosanoate methyl lignocerate methyl eicosapentaenoate (cis-5,8,11,14,17) methyl nervonate (cis-15) methyl docosahexaenoate (cis-4,7,10,13,16,19)

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634

FAMEs
FAMEs (cis/trans isomers) Rtx-Wax
8

1. 2. 3. 4. 5. 6. 7. 8.

C14:0 C14:1n5 cis C14:1n5 trans C16:0 C16:1n7 cis C16:1n7 trans C18:0 C18:1 cis isomers (n12, n9, n7)

10. 11. 12. 13. 14.

9. C18:1 trans isomers (n12, n9, n7) C18:2n6 cis C18:2n6 trans C20:0 C20:1n9 cis C20:1n9 trans

9 2 3 4 5,6 12 7

14 13

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

10 11

min.

15

20
GC_FF00121

25

30

35

60m, 0.25mm ID, 0.25m Rtx-Wax (cat.#12426) On-column conc.: 4075ng. Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Split ratio: 165C to 250C @ 2C/min. 220C/250C helium 20cm/sec. set @ 165C 50:1

FAMEs (cis/trans isomers) Rt-2560

excellent resolution of cis & trans isomers

cis/trans FAME Mix cat. # 35079

GC_FF00652

Rt-2560, 100m, 0.25mm ID, 0.2m (cat.# 13199) Sample: cis/trans FAME Mix (cat.# 35079), 10mg/mL total FAMEs in methylene chloride Inj.: 1.0L split (split ratio 20:1), 4mm inlet liner (cat.# 20814) Inj. temp.: 225C Carrier gas: hydrogen, constant flow Flow rate: 1.2mL/min. Oven temp.: 100C (4 min. hold) to 240C @ 3C/min. (10 min. hold) Det.: FID @ 250C

Compound 1. C18:0 methyl stearate 2. C18:1 methyl petroselaidate (trans-6) 3. C18:1 methyl elaidate (trans-9) 4. C18:1 methyl transvaccenate (trans-11) 5. C18:1 methyl petroselinate (cis-6) 6. C18:1 methyl oleate (cis-9) 7. C18:1 methyl vaccenate (cis-11) 8. C18:2 methyl linoleate (cis-9,12)

% in Mix 20.0 8.0 10.0 12.0 8.0 10.0 12.0 20.0

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FAMEs
FAMEs (Commercial Margarine) Rtx-2330
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. C16:0 C18:0 C18:1 trans C18:1 trans C18:1 trans C18:1 trans C18:1 cis C18:1 cis C18:1 cis C18:1 cis C18:2 C20:0

635

11

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

105m, 0.25mm ID, 0.20m Rtx-2330 (cat.# 10729) 1.0L split injection of a commercial margarine mixture. Conc.: approximately 5g.
2

5 6 7 4 3 9 10 12

Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio:

165C 275C hydrogen 40cm/sec. 4 x 10-11 AFS 50:1

min.

12

16

20

24
GC_FF00123

28

32

36

40

44

48

FAMEs (Cocoa Butter) Stabilwax


2 5 6

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

C14:0 C16:0 C16:1n7 C17:0 C18:0 C18:1n9 C18:2n6 C18:3n3 C20:0 C20:1n9 C22:0

FAMEs (Saw Palmetto) Rtx-Wax Peak List


1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

Conc. (mg/mL) methyl caproate (C6:0) 0.4 methyl caprylate (C8:0) 0.4 methyl nonanoate (C9:0) 2.0 methyl caprate (C10:0) 0.4 methyl laurate (C12:0) 5.0 methyl myristate (C14:0) 2.0 methyl palmitate (C16:0) 2.0 methyl palmitoleate (C16:1) 0.4 methyl stearate (C18:0) 0.4 methyl oleate (C18:1) 5.0 methyl linoleate (C18:2) 1.0 methyl linolenate (C18:3) 0.4

3 1

10

11

min.

4
GC_FF00120

8
GC_FF00538

30m, 0.25mm ID, 0.25m Stabilwax (cat.# 10623) 1.0L split injection of a FAME reference standard for cocoa butter. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 200C to 250C @ 8C/min. (hold 3 min.) 250C hydrogen 31.4cm/sec. set @ 200C 8 x 10-11 AFS 45:1

30m, 0.25mm, 0.25m Rtx-Wax (cat.# 12423) 1L split injection of saw palmetto standard Conc.: see peak list Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Split ratio: 120C (hold 3 min.) to 220C at 20C/min. (hold 12 min.) 250C/300C helium 1mL/min. (34 cm/sec.) 100:1

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636

FAMEs
FAMEs (Marine Oil Standard) FAMEWAX
FAMEWAX 30m, 0.32mm ID, 0.25m (cat.# 12498) Sample: 12mg/mL total FAMEs Inj.: 0.5L, split (150:1), 3mm ID split liner for Trace Series GCs, packed with glass wool (cat.# 20936-202.1) Inj. temp.: 250C Carrier gas: hydrogen, constant flow Linear velocity: 62cm/sec. Oven temp.: 195C to 240C @ 5C/min. (hold 1 min.) Det.: FID, 250C

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

FAST analysis of marine oil FAMEs

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.

C14:0 C15:0 C16:0 C16:1 C16:2 C17:0 C17:1 C16:4 C18:0 C18:1 (oleate) C18:1 (vaccenate) C18:2n6cis C18:3n3 C18:4n6

15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

C18:4n3 C20:0 C20:1n7 C20:1n9 C20:4n6 C20:4n3 C20:5n3 C22:1n7 C21:5n3 C23:0 (IS) C22:5n6 C22:5n3 C22:6n3 C24:1

GC_FF00568

FAMEs (Marine Oil Standard) FAMEWAX


30m, 0.32mm ID, 0.25m FAMEWAX (cat. # 12498) Inj.: 1L Conc.: 10,000g/mL in isooctane (total FAMES; see breakdown in peak list) Oven temp.: Inj. / det. temp.: Carrier gas: Flow rate: Split ratio: 195240C at 5C/min., 1 min. hold 250C / 275C hydrogen 3 mL/min. (constant flow) 100:1

GC_FF00499

Peak List 1. C14:0 2. C14:1 3. C16:0 4. C16:1 5. C18:0 6. C18:1 (oleate) 7. C18:1 (vaccenate) 8. C18:2 9. C18:3 10. C20:0 11. C20:1 12. C20:2 13. C20:4 14. C20:3 15. C20:5 16. C22:0 17. C22:1 18. C24:0 19. C22:6 20. C24:1

Conc. (g/mL) g 600 100 1600 500 800 1300 400 200 200 100 900 100 300 100 1000 100 300 100 1200 100

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FAMEs
FAMEs (PUFA, marine source) 1. C14:0 Rtx-2330 2. C16:0
3. 4. 5. 6. 7. 8. 9.
6 5 9 18 12 8 7 11 10 13 14 17 16 12 6 13 15 9

637

C16:1n7 C18:1n9 C18:1n7 C18:2n6 C18:3n3 C20:1n11 C20:1n9

10. 11. 12. 13. 14. 15. 16. 17. 18.

C20:1n7 C18:4n3 C22:1n11 C22:1n9 C20:4n3 C20:5n3 C21:5n3 C22:5n3 C22:6n3

FAMEs (PUFA, animal source) Rtx-2330


2 4 5 7 11

15

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

C14:0 C16:0 C16:1n7 C18:0 C18:1n9 C18:1n7 C18:2n6 C18:3n6 C18:3n3 C20:3n6 C20:4n6 C20:5n3 C22:4n6 C22:5n3 C22:6n3

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

min. 5

10
GC_FF00118

15

20
8 1 3 10 14

30m, 0.25mm ID, 0.20m Rtx -2330 (cat.# 10723) 0.5L split injection of a PUFA mix. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 160C to 225C @ 2C/min. 225C/250C hydrogen 45cm/sec. set @ 160C 8 x 10-11 AFS 35:1

min.

12

16
GC_FF00119

20

24

28

30m, 0.32mm ID, 0.20m Rtx-2330 (cat.# 10724) 0.1L split injection of PUFA 2 mix. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 160C to 250C @ 2C/min. (hold 10 min.) 260C hydrogen 40cm/sec. 8 x 10-11 AFS 20:1

FAMEs (PUFA, animal source) MXT-WAX


30m, 0.28mm ID, 0.25m MXT-WAX (cat.# 70624) 0.1L split injection of PUFA 2 mix.
2 4 5

Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio:
13 7

160C to 250C @ 2C/min. (hold 10 min.) 260C hydrogen 40cm/sec. 8 x 10-11 AFS 20:1 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. C14:0 C16:0 C16:1n7 C18:0 C18:1n9 C18:1n7 C18:2n6 C18:3n3 C18:4n3 C20:1n9 C20:2n6 C20:3n6 C20:4n6 C20:5n3 C22:4n6 C22:5n3 C22:6n3 C24:1n9

17 8

6 15

18 16 9 1 3 10 11 12 14

min.

12

16

20

24

28

32

GC_FF00117

Phone: 800-356-1688 or 814-353-1300 www.restek.com

638

FAMEs
FAMEs (Evening Primrose Oil) FAMEWAX 4 FAMEs (Flax Seed Oil) FAMEWAX

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

1. 2. 3. 4. 5.

C16:0 C18:0 C18:1n9 C18:2n6 C18:3n6

1. 2. 3. 4. 5. 6.

C16:0 C18:0 C18:1n9 C18:2n6 C18:3n6 C18:3n3

1 1

3 5 2

min. min. 20
GC_FF00363

20
GC_FF00364

40

40

FAMEs (Black Currant Seed Oil) FAMEWAX


4

FAMEs (Borage Seed Oil) FAMEWAX

1. 2. 3. 4. 5. 6.

C16:0 C18:0 C18:1n9 C18:2n6 C18:3n6 C18:3n3

1. 2. 3. 4. 5.
5 3 6

C16:0 C18:0 C18:1n9 C18:2n6 C18:3n6

3 5

2 2

min.

20
GC_FF00365

40 min. Column and conditions for all four oils analyses: 30m, 0.25mm ID, 0.25m FAMEWAX (cat.# 12497). Oven temp.: 165C (hold 30 min.) to 220C @ 1.5C/min. (hold 15 min.) Inj. temp.: 225C Det. temp.: 230C Carrier gas: helium @ 40cm/sec. 20
GC_FF00366

40

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Essential Oils
Lemon Oil Rtx-5
7,8 15 2 356 14 38 29 32 33

639

36 17 26 13 12 35

10 11 18 19 16

20

21 22 24 23

25

27,28 30

31 34

37

1 min. 2 4 6 8 10 12 14 GC_FF00138 16 18 20 22 24 26 28

30m, 0.32mm ID, 0.25m Rtx-5 (cat.# 10224) Wet needle split injection of a neat lemon oil Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 75C (hold 8 min.) to 250C @ 4C/min. 250C hydrogen 40cm/sec. (flow rate: 3.2cc/min.) 2 x 10-11 AFS 100:1

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

heptanol -thujene -pinene camphene sabinene -pinene 6-methyl-5-hepten-2-one myrcene octanal -phellandrene 3-carene -terpinene p-cymene limonene -terpinene octanol terpinolene linalool nonanal citronellal terpinene-4-ol -terpineol decanol octyl acetate nerol neral carvone geraniol geranial nonyl acetate citronellyl acetate neryl acetate geranyl acetate dodecanal -caryophyllene trans--bergamotene -humulene -bisabolene

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

Spearmint Oil (Native ) Stabilwax

4 6 7

13

15

19

25

16

18 28 29 24 9 5 8 10 11 12 14 30 20 22 23 26 27

17

21

min.

10

12

14

16

18

20

22

24

26

28

30

32

GC_FF00140

60m, 0.25mm ID, 0.25m Stabilwax (cat.# 10626) 0.2L split injection of a neat spearmint oil Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 75C (hold 4 min.) to 200C @ 4C/min. (hold 10 min.) 250C hydrogen 40cm/sec. set @ 160C 4 x 10-11 AFS 100:1

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

-pinene -pinene sabinene myrcene -terpinene l-limonene 1,8-cineole cis-ocimene -terpinene p-cymene

11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

terpinolene 3-octyl acetate 3-octanol l-menthone trans-sabinenehydrate -bourbonene linalool terpinene-4-ol -caryophyllene dihydrocarvone

21. 22. 23. 24. 25. 26. 27. 28. 29. 30.

trans-dihydrocarvyl acetate trans--farnesene -terpineol germacrene- carvone cis-carvyl acetate trans-carveol cis-carveol cis-jasmone viridiflorol

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640

Essential Oils
Peppermint Oil MXT-WAX
7 14,15 17 20 22 24

16 2 21 27

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

-pinene -pinene sabinene myrcene -terpinene l-limonene 1,8-cineole cis-ocimene -terpinene p-cymene terpinolene 3-octanol 1-octen-3-ol l-menthone trans-sabinenehydrate

16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29.

menthofuran d-isomenthone -bourbonene linalool menthyl acetate neo-menthol -caryophyllene terpinene-4-ol l-menthol pulegone -terpineol germacrene- piperitone viridiflorol

23

3 5

9 28 8 4 11 10 12 13 18 19 25 26

Inert stainless steel equivalent to Stabilwax fused silica columns!


29

min.

12

16

20 GC_FF00141

24

28

32

36

30m, 0.28mm ID, 0.50m MXT-WAX (cat.# 70639) 1.0L split injection of peppermint oil Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 75C (hold 4 min.) to 240C @ 4C/min. 250C hydrogen 40cm/sec. set @ 75C 16 x 10-11 AFS 50:1

free literature
foods, flavors, & fragrances (lit. cat.# 59260A) A brief summary of many applications and chromatography products
This guide is a good overview of the foods - flavors - fragrances applications for which Restek GC and HPLC columns have been used. Application areas include amino acids, carbohydrates, chiral separations, essential oils, fats and oils, flavors and fragrances, organic acids, preservatives, and vitamins. Includes a handy index of retention times for many flavor and fragrance compounds on a dimethylpolysiloxane or a PEG-type capillary GC column.

A Guide to the Analysis of Chiral Compounds by GC (lit. cat.# 59889) Resolve critical enantiomer pairs quickly and reliably
In some analyses, particularly with pharmaceutical or flavor and fragrance compounds, enantiomer pairs must be resolved for separate quantification. Five cyclodextrin-based Restek chiral capillary GC columns offer a unique range of selectivities, to enable you to accomplish these often-difficult separations. Many example chromatograms in this 24-page guide will help you find the best column - or columns - for your particular need.

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Essential Oils
Synthetic Mushroom Aroma Rtx-20
1 12 17 14

641

3 2 10 9

11

13 15 16 18 19

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

acetone ethyl acetate 1-butanol 3-methyl-1-butanol 1-pentanol hexanal furfural amyl acetate 1-octen-3-ol 3-octanol 3-octanone benzaldehyde octyl alcohol benzyl alcohol phenylacetaldehyde nonanal -terpineol 2,4-nonadienal 2,4-decadienal
min. 4

7 4 5

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

12

16

20 GC_FF00142

24

28

32

36

30m, 0.32mm ID, 1.0m Rtx-20 (cat.# 10354) 1.0L split injection of a synthetic mushroom aroma. Conc.: 10ng per component. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 45C (hold 8 min.) to 250C @ 4C/min. 260C hydrogen 40cm/sec. 4 x 10-11 AFS 100:1

Synthetic Mushroom Aroma Stabilwax

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

acetone ethyl acetate methylene chloride (solvent) hexanal amyl acetate 1-butanol 3-methyl-1-butanol 1-pentanol 3-octanone 3-octanol nonanal 1-octen-3-ol furfural benzaldehyde octyl alcohol phenylacetaldehyde -terpineol 2,4-nonadienal 2,4-decadienal benzyl alcohol

3 14 10 9 7 6 1 11 2 4 5 16 8 13 15 12 17

20

18 19

min.

10

12

14

16 GC_FF00143

18

20

22

24

26

28

30

30m, 0.32mm ID, 1.0m Stabilwax (cat.# 10654) 1.0L split injection of a synthetic mushroom aroma Conc.: 10ng per component Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 40C to 220C @ 6C/min. 260C hydrogen 40cm/sec. 4 x 10-11 AFS 100:1

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642

Essential Oils
Citronella Java Oil Rtx-1
1 2 4 10 14 7 11

16

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

12 9 15 3 13

6 8

min.

10

12

14

16

18 GC_FF00144

20

22

24

26

28

60m, 0.25mm ID, 0.25m Rtx-1 (cat.# 10126) 1.0L split injection of citronella Java oil Oven temp.: Inj. / det. temp.: Det. type: Carrier gas: Linear velocity: FID sensitivity: Split vent: 100C to 260C @ 4C/min. (hold 1 min.) 250C / 280C MSD helium 30cm/sec. set @ 50C 2 x 10-11 AFS 100cc/min. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. limonene citronellal linalool borneol -elemene -caryophyllene neryl acetate -terpineol germancrene- -citronellol geranyl acetate -cadenene nerol geraniol eugenol -bergamotene

Citronella Java Oil Stabilwax

10,11

14

16

5 4

9 12

3 15 13 6 8

min.

10

15 GC_FF00145

20

25

60m, 0.25mm ID, 0.25m Stabilwax (cat.# 10626) 1.0L split injection of citronella Java oil Oven temp.: Inj. / det. temp.: Det. type: Carrier gas: Linear velocity: FID sensitivity: Split vent: 100C to 260C @ 4C/min. (hold 1 min.) 250C / 280C MSD helium 30cm/sec. set @ 50C 2 x 10-11 AFS 100cc/min.

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Essential Oils
Flavor Volatiles 3 4,5 11 Rtx-1 12 1,2 7,810 13
9 23 28,29 33 22 30 16 21 32 31 34 36 38 35 40 41 42 48 45 46 50 39 44 14 15 17 18 19,20 24 25 26 27 37 43 49

643

47

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

min. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. methanol acetaldehyde ethanol acetone isopropyl alcohol methylene chloride hexane ethyl acetate ethyl propionate n-hexanal

12 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

16

20

24

28

32 21. 22. 23. 24. 25. 26. 27. 28. 29. 30.

36

40

44

48

52 31. 32. 33. 34. 35. 36. 37. 38. 39. 40.

56

60

64

68

72

76 41. 42. 43. 44. 45. 46. 47. 48. 49. 50.

80

GC_FF00536

ethylbutyrate furfural trans-2-hexenal -thujene -pinene camphene sabinene -pinene octanal myrcene

-phellandrene -terpinene p-cymene -limonene -terpinene octanol terpinolene nonanal linalool cis-limonene monoxide

trans-limonene monoxide citronellal terpinene-4-ol -terpineol decanal d & l carveol neral carvone geranial neryl acetate

geranyl acetate -ionone -caryophyllene trans--bergamotene BHA -ionone valencene -elemene -bisabolene nootketone

60m, 0.53mm ID, 0.50m Rtx-1 (cat.# 10143) 0.8L split injection of a flavor volatiles test mix Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 70 (hold 15 min.) to 190C @ 2C/min. (hold 5 min.) 220C/260C helium 20cm/sec. set @ 70C 64 x 10-11 AFS 20:1

Flavor Volatiles Stabilwax

4,5 1 2 7,8 10 13 14 15 16 17 1112

19 21 20

30 32

37 39

36 18 3 9 6 23 24 22 26 25 29 28 27 31 33 35 34

38

40

41 42

43 44

min. 1. 2. 3. 4. 5. 6. 7. 8. 9. hexane acetaldehyde acetone methanol ethyl acetate isopropyl alcohol ethanol methylene chloride ethyl propionate

4 10. 11. 12. 13. 14. 15. 16. 17. 18.

12

16

20

24

28 19. 20. 21. 22. 23. 24. 25. 26. 27.

32

36

40

44

48 28. 29. 30. 31. 32. 33. 34. 35. 36.

52

56

60

64

68 37. 38. 39. 40. 41. 42. 43. 44.

72 valencene geranial carvone geranyl acetate d/l carveol -ionone d/l carveol -ionone

GC_FF00537

-pinene ethylbutyrate n-hexanal -pinene sabinene myrcene -limonene 1,8-cineole trans-2-hexenal

-terpinene p-cymene terpinolene octanal nonanal cis-limonene monoxide trans-limonene furfural citronellal

decanal linalool octanol trans--bergamotene -caryophyllene terpinene-4-ol neral -terpineol neryl acetate

60m, 053mm ID, 0.50m Stabilwax (cat.# 10643) 0.8L split injection of a flavor volatiles test mix Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 70C (hold 15 min.) to 190C @ 2C/min. (hold 5 min.) 220C/260C helium 20cm/sec. set @ 70C 64 x 10-11 AFS 20:1

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644

Flavors & Fragrances


Malt Whiskey Stabilwax-DA
Stabilwax-DA 30m, 0.18mm ID, 0.18m (cat.# 550752) Inj.: Std. conc.: Gerstel CIS Injector: Helium vent flow: Carrier gas: Linear velocity: Oven temp.: 10L large volume injection (splitless), at 10L/min. neat 35C (hold 2 min.), to 300C @ 10C/sec. (hold 5 min.) 600mL/min. with 1.8 min. vent end time helium 45cm/sec. 60C (hold 2 min.) to 100C @ 20C/min., to 240C @ 5C/min. (hold 10 min.) MSD 240C 150C 230C 30400amu 70eV EI

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

Det.: Transfer line temp.: Quadrupole temp.: MS source temp.: Scan range: Ionization: Mode:

Chromatogram courtesy of Kevin MacNamara, Ph.D., Irish Distilleries, Ltd.

GC_FF00603

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

ethyl octanoate acetic acid siloxane 1-hydroxy-2,3-butadione 1-hydroxy-2-propanone acetate furfural formic acid propionic acid isobutyric acid dimethyl sulfoxide 5-methyl furfural methyl decanoate + unknown butyric acid siloxane ethyl decanoate furfuryl alcohol isoamyl octanoate isovaleric acid 2-methylbutyric acid diethyl succinate 3-methyl-2(5H)-furanone (possible) valeric acid

23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41.

ethyl undecanoate isobutyl decanoate 2(5H)-furanone unknown di(ethyleneglycol) butyl ether siloxane methyl dodecanoate 2-phenylethyl acetate methylcyclopentenolone hexanoic acid ethyl dodecanoate isoamyl decanoate guaiacol dodecyl acetate (possible) whiskey lactone (1) 2-phenylethanol heptanoic acid siloxane dimethoxybenzene or 4-methylguaiacol 42. whiskey lactone (2) 43. dodecanol

44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59 60. 61. 62. 63. 64. 65.

unknown phenol methyl tetradecanoate nerolidol diethyl malate ethyl tetradecanoate octanoic acid unknown p-cresol siloxane diethyl octanedioate monomethyl succinate (possible) 3,5-dimethyl-2,4(5H)furandione nonanoic acid diethyl 2-hydroxyglutarate unknown tetradecanol 4-vinylguaiacol diethyl nonanedioate methyl hexadecanoate ethyl -lactone 2-hydroxyglutarate ethyl hexadecanoate

66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77. 78. 79. 80. 81. 82. 83. 84. 85.

decanoic acid ethyl 9-hexadecanoate triacosan unknown phthalide diethyl phthalate hexadecanol 4-hydroxycinnamic acid (decomp.) methyl stearate benzoic acid methyl 8-octadecenoate ethyl stearate dodecanoic acid hydroxymethylfurfural ethyl linoleate 4-allyl-2,6-dimethoxyphenol diisobutyl phthalate vanillin sinapic acid (decomp.) 2-phenylethyl decanoate +2 unknowns 86. 4-propenyl-2,6-dimethoxyphenol

87. 88. 89. 90. 91. 92. 93. 94.

ethyl vanillate acetovanillone vanillin methyl ketone tetradecanoic acid ethyl homovanillate propiovanillone fatty acid ester (similar to 4-allyl-2,6dimethoxyphenol) 95. unknown 96. hexadecanoic acid 97. syringealdehyde

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Flavors & Fragrances


Rum Rtx-1301
1. 2. 3. 4. 5. 6. 7. 8.
7

645

acetaldehyde methanol ethanol acetone ethyl formate isopropanol n-propanol ethyl acetate
10

9. 10. 11. 12. 13.

sec-butanol isobutanol isoamyl alcohol active amyl alcohol n-amyl alcohol

Rum CarboBlack B
5% Carbowax 20M 80/120 CarboBlack B (cat.# 80105) 2m, 1/8" OD x 2mm ID SilcoSmooth tubing 0.5L on-column injection, on-column conc.: neat Oven temp.: 65C (hold 5 min.) to 150C @ 4C/min. 200C / 250C FID nitrogen 20mL/min. 1.28 x 10-10 AFS 1. acetaldehyde 2. methanol 3. acetone 4. ethyl formate 5. ethanol 6. ethyl acetate 7. n-propanol 8. sec-butanol 9. isobutanol 10. active amyl alcohol 11. isoamyl alcohol 12. n-amyl alcohol

11 5

13

Inj./det. temp.: Det.: Carrier gas: Column flow rate: FID sensitivity:

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

9 2

12 4 1 5 6 7 2

8 9 11

min. 5

10

15
GC_FF00110

20

25
1 3 6 4 8 10 12

60m, 0.25mm ID, 1.4m Rtx-1301 (cat.# 16016) 1.0L split injection using a Cyclosplitter liner (cat.# 20706). Conc.: neat Oven temp.: Inj./det. temp.: Carrier gas: Split ratio: 35C (hold 5 min.) to 100C @ 1C/min. 150C / 200C hydrogen @ 40cm/sec. 100:1 min.

10
GC_FF00111

20

Scotch Rtx-1301

1. 2. 3. 4. 5. 6.

acetaldehyde methanol ethanol acetone isopropanol n-propanol

7. 8. 9. 10. 11.

ethyl acetate isobutanol acetic acid isoamyl alcohol active amyl alcohol

Scotch CarboBlack B
3

10 11

1. 2. 3. 4. 5. 6. 7. 8. 9.

acetaldehyde methanol ethanol ethyl acetate n-propanol isobutanol acetic acid active amyl alcohol isoamyl alcohol

6 5 acetic acid 9 1 4 5 1 8 2 4 7

min. min. 5 10 15
GC_FF00112

10
GC_FF00113

15

20

25

60m, 0.25mm ID, 1.4m Rtx-1301 (cat.# 16016) 1.0L split injection using a Cyclosplitter sleeve (cat.# 20706). Conc.: neat Oven temp.: Inj./det. temp.: Carrier gas: Split ratio: 35C (hold 5 min.) to 100C @ 1C/min. 150C / 200C hydrogen @ 40cm/sec. 100:1

5% Carbowax 20M 80/120 CarboBlack B (cat.# 80105) 2m, 1/8" OD x 2mm ID Silcosmooth tubing 0.5L on-column injection, on-column conc.: neat Oven temp.: Inj./det. temp.: Det.: Carrier gas: Column flow rate: FID sensitivity: 70C to 150C @ 4C/min. 200C / 250C FID nitrogen 20mL/min. 1.28 x 10-10 AFS

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646

Flavors & Fragrances


Alcoholic Beverage Standard: Acids and Esters Stabilwax-DA
Peak List 1. ethyl octanoate 2. acetic acid 3. propionic acid 4. isobutyric acid 5. 3-decanol 6. ethyl decanoate 7. ethyl laurate 8. cis-lactone 9. 2-phenylethanol 10. trans-lactone 11. methyl myristate 12. ethyl myristate 13. octanoic acid 14. ethyl palmitate 15. decanoic acid 16. dodecanoic acid 17. vanillin Conc. (ppm) 100 100 100 100 50 50 50 100 50 100 50 50 100 50 100 100 100

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

GC_FF00500

Stabilwax-DA 30m, 0.18mm ID, 0.18m (cat.# 550752) Inj.: 1L splitless (hold 0.5 min.) at conc. shown in peak list, in ethyl acetate, 4mm ID splitless liner w/wool (cat.# 20814-202.1) Inj. temp.: 240C Carrier gas: hydrogen Make-up gas: nitrogen Linear velocity: 28psi @ 240C Oven temp.: 70C to 240C at 12C/min. (hold 3 min.) Det.: FID

free literature
Analyzing Alcoholic Beverages by Gas Chromatography (lit. cat.# 59462) Selectivity, sensitivity, and minimal sample preparation make GC a powerful tool for monitoring alcoholic beverage composition
Volatile component profiles of alcoholic beverages reveal a wide range of compounds: acids, alcohols, aldehydes, and others. This 16-page guide describes packed column GC and capillary GC approaches to monitoring these complex mixtures of analytes. A separate section is devoted to detailed information about quantifying trace sulfur compounds in beer.

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Flavors & Fragrances


5% Fragrance Materials Association Mix Rtx-1
FMA Reference Mix cat. # 31807

647

Rtx-1, 60m, 0.25mm ID, 0.25m (cat.# 10126) Sample: 5% FMA mix in acetone (cat.# 31807) Inj.: 1.0L split (split ratio 40:1), 4mm inlet liner (cat.# 20814) Inj. temp.: 285C Carrier gas: helium, constant flow Flow rate: 0.6mL/min. Oven temp.: 50C to 270C @ 3C/min. Det.: FID @ 300C

Compound 1. ethyl butyrate 2. limonene 3. eucalyptol 4. benzoic acid 5. cinnamic aldehyde 6. geraniol 7. hydroxycitronellal 8. thymol 9. cinnamyl alcohol 10. vanillin 11. cinnamyl acetate 12. benzyl salicylate

% in the FMA mix 35.7 20.0 0.5 1.0 0.5 0.6 5.0 0.3 0.3 0.1 0.3 35.7

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

GC_FF00657

5% Fragrance Materials Association Mix Rtx-1701

Rtx-1701, 60m, 0.25mm ID, 0.25m (cat.# 12026) Sample: 5% FMA mix in acetone Inj.: 1.0L split (split ratio 40:1), 4mm inlet liner (cat.# 20814) Inj. temp.: 285C Carrier gas: helium, constant flow Flow rate: 0.6mL/min. Oven temp.: 50C to 270C @ 3C/min. Det.: FID @ 300C

Compound 1. ethyl butyrate 2. limonene 3. eucalyptol 4. geraniol 5. benzoic acid 6. cinnamic aldehyde 7. hydroxycitronellal 8. thymol 9. cinnamyl alcohol 10. cinnamyl acetate 11. vanillin 12. benzyl salicylate

% in FMA Mix 35.7 20.0 0.5 0.6 1.0 0.5 5.0 0.3 0.3 0.3 0.1 35.7

GC_FF00658

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648

Flavors & Fragrances


Flavor & Fragrance Compounds Rt-CW20M F&F
Carbowax column
1 2 3 67 9 10 11 15

Rt-CW20M F&F column


1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. methyl heptanoate hexanol methyl octanoate nonanal menthone citronellal methyl nonanoate 2,3-butanediol linalool linalyl acetate methyl decanoate menthol -terpineol -terpineol methyl undecanoate
1 2 3 67 9 10 11

15

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

13

better response for 2,3-butanediol


13

5 12 8 14

8 5 12 14

min.

10

15

20

GC_FF00433

min.

10

15

20

50m, 0.32mm ID, 0.33m, traditional Carbowax 20M or Rt-CW20M F&F (cat.# 12539) On-column injection of 5ng to 150ng each compound in methylene chloride, split 10:1 Carrier gas: Inj. & det. temp.: Oven temp.: hydrogen, 40cm/sec. 220C 110C isothermal

a plus one story


Thank you for being a top notch GC Analytical Supply Company that always continues to offer newer products & services. John T. Brunette, Chemist, Bausch & Lomb

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Food Contaminants
Acrylamide Stabilwax Acrylamide (Potato Chip Extract) Stabilwax

649

1. acrylamide

1. acrylamide

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

blank

GC_FF00642

GC_FF00643

Stabilwax 15m, 0.53 ID, 0.50m (cat.# 10637) Sample: 25g/mL acrylamide standard in water Inj.: 1.0L, 0.5min hold Liner: 2mm splitless with wool (cat.# 20830) Inj. temp.: 260C Carrier gas: helium, constant pressure Linear velocity: 62cm/sec. @ 100C Oven temp.: 100C (hold 0.5 min.) to 200C @ 15C/min. Det.: FID @ 260C

Stabilwax 15m, 0.53mm ID, 0.50m (cat.# 10637) Sample: 1g of potato chips spiked with 100g acrylamide Inj.: 1.0L, 0.5min hold Liner: 2mm splitless with wool (cat.# 20830) Inj. temp.: 260C Carrier gas: helium, constant pressure Linear velocity: 62cm/sec. @ 100C Oven temp.: 100C (hold 0.5 min.) to 200C @ 15C/min. Det.: FID @ 260C

Sulfur Compounds in Beverage Grade CO2 Rt-XLSulfur

Sulfur Compounds in Beer Headspace Rt-XLSulfur

1. 2. 3. 4.

hydrogen sulfide carbonyl sulfide methyl mercaptan ethyl mercaptan and/or dimethyl sulfide 5. dimethyl disulfide

1. hydrogen sulfide 2. methyl mercaptan 3. dimethyl sulfide and/or ethyl mercaptan 4. unknown

GC_FF00491

1m, 0.75mm ID Sulfinert tubing Rt-XLSulfur 100/120 mesh (cat.# 19806) Conc.: sulfur standard @ 20ppb each in CO2 Inj.: 1cc sample loop, 6-port Valco valve Carrier gas: helium Flow rate: 10mL/ min. @ ambient temp. Oven temp.: 60C to 260C @ 15C/min. (hold 5 min.) Det. sensitivity: SCD, attn. x 1 Det. temp.: 800C

GC_FF00494

1m, 0.75mm ID Sulfinert tubing Rt-XLSulfur 100/120 mesh (cat.# 19806) Conc.: headspace of a domestic (US) beer sample Inj.: 1cc sample loop, 6-port Valco valve Carrier gas: helium Flow rate: 10mL/min. @ ambient temp. Oven temp.: 60C to 260C @ 15C/min. (hold 5 min.) Det. sensitivity: SCD, attn. x 1 Det. temp.: 800C

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650

Food Contaminants
Food Packaging Volatiles (Volatiles Standard) Rtx-5MS
Volatiles Standard 1. isopropanol 2. methylene chloride 3. 2-methyl-1-propanol 4. tetrahydrofuran 5. benzene 6. toluene 7. hexanal 8. furfural 9. 4-heptanone (IS) 10. butyl ether 11. styrene 12. dodecane 30m, 0.25 mm ID, 1m Rtx-5MS (cat.# 12653)
1

12

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

11

5 4 3 6 7 8 10

Concentrator: Trap: Purge: Dry purge: Desorb preheat: Desorb: Bake: Interface: Transfer line: Oven temp.: Inj. temp.: Carrier gas: Linear velocity: Split ratio: Det.: Det. temp.: Scan range: Ionization:

Tekmar LSC-3100 purge & trap Vocarb 3000, type K 10 min. @ 40mL/min. @ 60C 3 min. @ 40mL/min. 220C 245C, 2 min., 40mL/min. 230C, 6 min. 1:20 split at injection port with 1mm ID liner 0.53mm ID Silcosteel MXT tubing, cat.# 20591 50C to 92C @ 3C/min., to 220C @ 20C/min., hold 1 min. 250C helium 36cm/sec (1mL/min.) 20:1 MSD 280C 35260 AMU EI @ 70 eV

10 11 12 13 14 15 16 17 18 19 20 21

GC_FF00457

Food Packaging Volatiles Rtx-5MS

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

tetrahydrofuran 1-butanol toluene hexanal ethylbenzene 4-heptanone butyl ether styrene 1-methylethylbenzene propylbenzene benzaldehyde benzeneacetaldehyde acetophenone benzoic acid, methyl ester decanal

Rtx-5MS 30m, 0.25 mm ID, 1m (cat.# 12653) Concentrator: Tekmar LSC-3100 purge & trap Trap: Vocarb 3000, type K Purge: 10 min. @ 40 mL/min., @ 60C Dry purge: 3 min. @ 40mL/min. Desorb preheat: 220C Desorb: 245C, 2 min., 40mL/min. Bake: 230C, 6 min. Interface: 1:20 split at injection with 1mm ID liner Transfer line: 0.53mm ID Silcosteel MXT tubing (cat.# 20591) Inj. temp.: 250C Carrier gas: helium Linear velocity: 36cm/sec. (1mL/min.) Split ratio: 20:1 Oven temp.: 50C to 92C @ 3C/min., to 220C @ 20C/min, hold for 1 min. Detector : MSD (Agilent 5973) Det. temp.: 280C Scan range: 35-260amu Ionization: EI @ 70 eV

GC_FF00459

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Sterols
Sterols (Olive Oil) XTI-5
1. 2. 3. 4. 5. 6. 7. 8. cholesterol brassicasterol campesterol stigmasterol -sitosterol avenasterol-d5 erythrodiol uvacol

651

Phytosterols (Saw Palmetto) Rtx-5

1. 2. 3. 4. 5.

cholesterol brassicasterol campesterol stigmasterol -sitosterol


3

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

7 6 3 1 2 4 8 4 1 2

min.

10
GC_FF00131

15

20

30m, 0.25mm ID, 0.25m XTI-5 (cat.# 12223) 0.5L splitless injection of a sterol fraction from olive pomace oil Conc.: 102500ng Oven temp.: 227C to 305C @ 8C/min. (hold 10 min.) Inj. & det. temp.: 300C Carrier gas: helium Linear velocity: 35cm/sec. set @ 227C (1.3mL/min.) FID sensitivity: 8 x 10-11 AFS Splitless hold time: 1.00 min.

min.

5
GC_FF00368

10

60m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10226). 1L splitless injection*. Oven temp.: 200C (hold 1 min.) to 340C @ 15C/min. (hold 10 min.) Inj./FID temp.: 345C/355C. *Split injection may be used, but results can have greater variability. A split flow of 112mL/min. is suggested.

Chromatogram provided by the Institute for Nutraceutical Advancement (INA)

Sterols (Cholesterol) XTI-5


1

Sterols XTI-5

3 2

1. 5--cholestane 2. coprosterol 3. cholesterol

1. 2. 3. 4. 5. 6. 7. 8. 9.

5--cholestane coprosterol cholesterol brassicasterol ergosterol campesterol stigmasterol -sitosterol lanosterol

5 6 9 4 7

min. min. 2 4 6
GC_FF00132

6
GC_FF00133

10

10

30m, 0.25mm ID, 0.50m XTI-5 (cat.# 12238) 1.0L split injection, 250ng on-column Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 330C 300C helium 30cm/sec. set @ 40C 8 x 10-11 AFS 100:1

30m, 0.25mm ID, 0.50m XTI-5 (cat.# 12238) 1.0L split injection. On-column conc.: 250ng Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 330C 300C helium 30cm/sec. set @ 40C 8 x 10-11 AFS 100:1

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652

Triglycerides; Sugars
Butter Triglycerides Rtx-65TG

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

T26 T28 T32 T34

T36 T38 T40 T42 T44 T46 T48 T50 T52 T54

min.

10

20
GC_FF00137

30

40

30m, 0.25mm ID, 0.10m Rtx-65TG (cat.# 17008) 0.2L cold on-column injection of 1% butterfat in isooctane. Oven temp.: 80C (hold 1 min.) to 240C @ 30C/min. to 360C @ 4C/min. (hold 5 min.) Det. temp.: 380C Carrier gas: hydrogen Linear velocity: 70cm/sec. FID sensitivity: 16 x 10-11 AFS SPI injector: high performance capillary insert 60C, 300C/min. to 400C (hold 5 min.)

Sugars (as alditol acetates) Rtx-2330

2 3 4

5 6

78

9 10 11

12

13

14

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.


15

glyceraldehyde deoxyribitol rhamnitol fucitol ribitol arabinitol xylitol deoxyglucitol mannitol galactitol glucitol inositol glucoheptitol n-acetyl galactose amine n-acetyl glucose amine 2-keto-3-deoxyoctanate
16

min.

10

12
GC_FF00127

14

16

18

20

22

15m, 0.32mm ID, 0.20m Rtx-2330 (cat.# 10721) 0.6L split injection Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 175C (hold 2 min.) to 240C @ 8C/min. (hold 1 min.) to 265C @ 8C/min. (hold 12 min.) 275C helium 80cm/sec. (flow rate: 10cc/min.) 2 x 10-11 AFS 20:1

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Sugars, Sugar Alcohols


Sugars (as alditol acetates) Rtx-225

653

1. rhamnitol 2. fucitol 3. ribitol 4. arabinitol 5. mannitol 6. galactitol 7. glucitol 8. inositol

G C A P P L I C AT I O N S | F O O D S , F L AV O R S , & F R AG R A N C E S

78 2 1 3 4 5 6

15m, 0.25mm ID, 0.25m Rtx-225 (cat.# 14020) 0.5L split injection Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 190C (hold 5 min.) to 250C @ 8C/min. (hold 5 min.) 260C hydrogen 42cm/sec. set @ 40C 16 x 10-11 AFS 50:1

min.

2.5

7.5
GC_FF00128

10

12.5

Sugars (TMS Derivatives) 3% Rt-101 on 100/120 Silcoport

Sugar Alcohols (TMS derivatives) 3% Rt-101 on 100/120 Silcoport


1. 2. 3. 4. 5. 6. 7. 8.
7 4

3 1

1. 2. 3. 4. 5. 6.

l-arabinose ribose anomers d-xylose d-fructose d-galactose -d-glucose


1

l-arabinose xylitol d-arabinitol d-mannose l-sorbose d-glucose d-sorbitol inositol

6 2 4 5 6 5 8

min.

10
GC_FF00129

15

20

min.

10
GC_FF00130

15

20

3% Rt-101 on 100/120 Silcoport (cat.# 80400) 2m, 1/8" OD x 2mm ID Oven temp.: Inj./det. temp.: Det.: Carrier gas: Column flow rate: FID sensitivity: 140C to 230C @ 5C/min. (hold 5 min.) 250C / 300C FID helium 35mL/min. 1.28 x 10-10 AFS

3% Rt-101 on 100/120 Silcoport (cat.# 80400) 2m, 1/8" OD x 2mm ID Oven temp.: Inj./det. temp.: Det.: Carrier gas: Column flow rate: FID sensitivity: 140C to 230C @ 5C/min. (hold 5 min.) 250C / 300C FID helium 35mL/min. 1.28 x 10-10 AFS

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654

Blood Alcohol
Blood Alcohol Rtx-BAC1 & Rtx-BAC2 (0.32mm ID Columns)
(headspace analysis)
1. 2. 3. 4. 5. 6.
4 2 6 5 1 5 3 1 3

methanol acetaldehyde ethanol isopropanol acetone n-propanol

Conc. w/v 0.1% 0.2% 0.2% 0.1% 0.01% 0.1%


4

G C A P P L I C AT I O N S | F O R E N S I C S

6 2

min.

1.0

1.2

1.4

1.6

1.8

2.0

2.2

2.4

2.6

2.8

3.0

min.
GC_PH00241

1.0

1.2

1.4

1.6

1.8

2.0

2.2

2.4

2.6

2.8

3.0

30m, 0.32mm ID, 1.8m Rtx-BAC1 (cat.# 18003)

30m, 0.32mm ID, 1.2m Rtx-BAC2 (cat.# 18002)

Dual-column analysis using a two-hole ferrule. 1.0mL headspace sample of a blood alcohol mix Oven temp.: 40C Inj. temp.: 200C Carrier gas: helium Sample equilibration: 70C, 15 min. Vial pressure: 30psi Vial pressurization time: 0.15 min. Vial sampling time: 0.01 min.

Transfer line: tubing Transfer line temp.: Injection port sleeve: Split flow:

0.32mm ID Hydroguard fused silica 200C 2mm ID 20mL/min.

Blood Alcohol Rtx-BAC1 & Rtx-BAC2 (0.53mm ID columns)


(headspace analysis)
2 2

4 3

1. 2. 3. 4. 5. 6.

methanol acetaldehyde ethanol isopropanol acetone n-propanol

4 3 1 1

min.

min.
GC_PH00239

Rtx-BAC1 30m, 0.53mm ID, 3.0m (cat.# 18001)

Rtx-BAC2 30m, 0.53mm ID, 2.0m (cat.# 18000)

1.0mL headspace sample of a blood alcohol mix Sample conc.: 0.1% per compound Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C 200C helium 80cm/sec. set @ 40C 1.28 x 10-10 AFS

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Blood Alcohol
Blood Alcohol 5% Carbowax 20M on 80/120 CarboBlack B
(headspace analysis)
1. 2. 3. 4. 5. 6. acetaldehyde methanol acetone ethanol isopropanol tert-butanol

655

G C A P P L I C AT I O N S | F O R E N S I C S

6 ft x 1/8", 2.0mm ID SilcoSmooth tubing 5% Carbowax 20M on 80/120 CarboBlack B (cat.# 80105) Inj.: 500L, headspace Conc.: 0.05gm/dL Oven temp.: Inj. & det. temp.: Carrier gas: Flow rate: 90C 200C helium 18mL/min.

GC_PH00478

a plus 1 story
Ron developed a program that allows our Applied Science Group to query by several parameters and retrieve information in a timely and useful format, enabling the group to make data-based decisions quickly. Ron Zhao, Programmer/Analyst

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656

Drugs of Abuse
Cannabinoids (TMS Derivatives) Rtx-5 Cocaine & Metabolites (TMS Derivatives) Rtx-5

1. 2. 3. 4. 5. 6. 7.

cannabidiol 8-tetrahydrocannabinol 9-tetrahydrocannabinol cannibinol 11-hydroxy-9-tetrahydrocannabinol 11-nor-9-tetrahydrocannabinol carboxylic acid 11-nor-8-tetrahydrocannabinol carboxylic acid

1 2

4 5 3 1

1. 2. 3. 4. 5.

ecgonine methyl ester (TMS) ecgonine (TMS) cocaine coca ethylene benzoylecgonine (TMS)

G C A P P L I C AT I O N S | F O R E N S I C S

6 7 3

5 4

min.

10

11

12

13

14

15

GC_PH00253

15m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10220) 1.0L splitless injection of cannabinoids Conc.: 100g/mL
min. 2 4 6 8 GC_PH00254 10 12 14 16

Oven temp.: Inj. temp.: Interface temp.: Det.: Ionization: Carrier gas: Scan range: Linear velocity: Splitless hold time:

50C (hold 0.5 min.) to 225C @ 30C/min., to 325C @ 10C/min. 225C 320C MSD EI helium 40-500 AMU 40cm/sec. set @ 50C 0.75 min.

30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 1.0L split injection of cocaine and cocaine metabolites Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 150C to 320C @ 10C/min. 250C / 300C helium 30cm/sec. set @ 50C 2.56 x 10-10 AFS 30:1

Opiates (TMS Derivatives) Rtx-5


1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. meperidine alphaprodine methadone levorphanol (TMS) codeine (TMS) hydrocodone morphine (TMS) hydromorphone (TMS) oxycodone (TMS) oxymorphone (TMS) nalorphine (TMS)

Phencyclidine Rtx-5

1 7,8

1. phencyclidine
5 11

4 1 2 3 6 9 10

min.

8 GC_PH00233

10

11

12

min. 2

10

12

14

16

18

GC_PH00234

30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 2.0L split injection of opiates Conc: 2000ng/L Oven temp.: 200C to 325C @ 7C/min. Inj. / det. temp.: 250C / 300C Det. type: MS Ionization: EI Carrier gas: helium Mode: full scan Linear velocity: 30cm/sec. set @ 200C Split ratio: 50:1

30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 1.0L split injection of phencyclidine Conc.: 1000ng/L Oven temp.: 50C (hold 1 min.) to 250C @ 25C/min., then to 325C @ 10C/min. (hold 2 min.) Inj. / det. temp.: 250C / 325C Carrier gas: helium Linear velocity: 30cm/sec. set @ 50C FID sensitivity: 2.56 x 10-10 AFS Split ratio: 30:1

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Anesthethetics; Solvents
Anesthetics Rtx-BAC1 & Rtx-BAC2
(headspace analysis)
1. 2. 3. 4. isoflurane enflurane halothane methoxyflurane

657

G C A P P L I C AT I O N S | F O R E N S I C S

GC_PH00501

GC_PH00502

30m, 0.53mm ID, 3.0m Rtx-BAC1 (cat.# 18001)

30m, 0.53mm ID, 2.0m Rtx-BAC2 (cat.# 18000)

1.0mL headspace sample Oven temp.: 40C (hold 5 min.) to 240C @ 5C/min. Inj. & det. temp.: 240C Carrier gas: helium Linear velocity: 65cm/sec.

Solvents Rtx-BAC1 & Rtx-BAC2


(headspace analysis)

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17.

ethyl chloride diethyl ether methylene chloride acetonitrile methyl tert-butyl ether chloroform methyl ethyl ketone 1,1,1-trichloroethane benzene trichloroethylene toluene 1,1,2-trichloroethane tetrachloroethene p-xylene m-xylene o-xylene tetrachloroethane

GC_PH00509

GC_PH00510

30m, 0.53mm ID, 3.0m Rtx -BAC1 (cat.# 18001)

30m, 0.53mm ID, 2.0m Rtx-BAC2 (cat.# 18000)

1.0mL headspace sample Oven temp.: 40C (hold 5 min.) to 240C @ 5C/min. Inj. & det. temp.: 240C Carrier gas: helium Linear velocity: 65cm/sec.

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658

Abused Inhalants
Abused Inhalants Rtx-BAC1 & Rtx-BAC2
1 12

Rtx-BAC1
3 8 2 10/11 14 6

G C A P P L I C AT I O N S | F O R E N S I C S

4 7

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

methanol ethanol diethyl ether isopropanol methylene chloride acetone methyl tert-butyl ether hexane chloroform ethyl acetate methyl ethyl ketone benzene trichloroethylene toluene methyl isobutyl ketone

5 13 15

min.

7
14

10

11

15 12 8 6 1 7 9,11 2 4

Rtx-BAC2

10

13

min.

6
GC_PH00446

10

11

30m, 0.32mm ID, 1.80m Rtx-BAC1 (cat.# 18003) 30m, 0.32mm ID, 1.20m Rtx-BAC2 (cat.# 18002) Oven temp.: 40C (hold 4 min.) to 120C @ 10C/min. Carrier gas: helium Linear velocity: 50cm/sec. Detector: FID Sample: 250L headspace Transfer line temp.: 125C Sample loop temp.: 125C Vial temp.: 70C Acknowledgement: Analyses performed using a Tekmar 7000 Headspace Autosampler on loan courtesy of Tekmar-Dohrmann.

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Arson Accelerants
Unleaded Gasoline Rtx-1

659

Unweathered

99% Weathered

G C A P P L I C AT I O N S | F O R E N S I C S

min. 2

10

12 14 16 18

20 22

24 26

28 30 32

34

min.

12

16

20

24

28

32

36

40

44

GC_MS00270

30m, 0.53mm ID, 1.50m Rtx-1 (cat.# 10170) Oven temp.: 40C (hold 3 min.) to 75C @ 15C/min. to 275C @ 20C/min. (hold 5 min.) Inj./det. temp.: 250C/285C Carrier gas: hydrogen Linear velocity: 50cm/sec. set @ 40C FID sensitivity: 4.10 x 10-9 AFS Split ratio: 30:1

Motor Oil Rtx-5

Motor Oil (Used) Rtx-5

min.

10

20

30

40

50

60

min.

10

20

30
GC_MS00273

40

50

60

GC_MS00272

30m, 0.53mm ID, 1.0m Rtx-5 (cat.# 10255) 1.0L split injection of Motor Oil Composite Standard (cat.# 31464)* Conc.: 50,000ppm Oven temp.: 40C (hold 2 min.) to 330C @ 10C/min. (hold 60 min.) Inj./det. temp.: 300/330C Carrier gas: hydrogen Linear velocity: 41cm/sec. Split ratio: 3:1

30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 1.0L split injection of Used Motor Oil Composite Standard (cat.# 31465)* Conc.: 50,000ppm Oven temp.: 40C to 340C @ 10C/min. (hold 15 min.) Inj./det. temp.: 250/340C Carrier gas: hydrogen Linear velocity: 40cm/sec. Split ratio: 15:1

*Prepared from an equal volume blend of 5w30, 10w30, 10w40, and 20w50 motor oil. A precisely weighed amount of the composite is added to a volumetric flask to produce a mixture at 50,000g/mL in methylene chloride, 1mL/ampul.

*Prepared from an equal volume blend from five gasoline powered vehicles. A precisely weighed amount of the composite is added to a volumetric flask to produce a mixture at 50,000g/mL in methylene chloride, 1mL/ampul.

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660

Arson Accelerants
Kerosene Rtx-1
30m, 0.32mm ID, 1.5m Rtx-1 (cat.# 10169) 1.0L split injection of a kerosene standard (cat.# 31094) Conc.: 5000g/mL Oven temp.: 40C (hold 5 min.) to 300C @ 4C/min. (hold 5 min.) Inj. / det. temp.: 275C / 300C Carrier gas: helium Linear velocity: 30cm/sec. set @ 40C Split ratio: 30:1

G C A P P L I C AT I O N S | F O R E N S I C S

min.

10

20

30

40
GC_MS00274

50

60

70

Diesel Fuel Rtx-1


30m, 0.32mm ID, 1.5m Rtx-1 (cat.# 10169) 1.0L split injection of a diesel fuel #2 standard (cat.# 31093) Conc.: 5000g/mL Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: Split ratio: 40C (hold 5 min.) to 300C @ 4C/min. (hold 5 min.) 275C / 300C helium 30cm/sec. set @ 40C 30:1

min.

10

20

30

40
GC_MS00275

50

60

70

Mineral Spirits Rtx-1

30m, 0.32mm ID, 1.5m Rtx-1 (cat.# 10169) 1.0L split injection of a mineral spirits standard (cat.# 31225) Conc.: 5000g/mL Oven temp.: 40C (hold 5 min.) to 300C @ 4C/min. (hold 5 min.) Inj. / det. temp.: 275C / 300C Carrier gas: helium Linear velocity: 30cm/sec. set @ 40C Split ratio: 30:1

min.

10

20

30

40
GC_MS00276

50

60

70

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Cleaning Solvents
Cleaning Solvents Rtx-Wax
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. methanol iso-propanol ethanol n-propanol iso-butanol n-butanol methyl Cellosolve limonene Cellosolve butyl Cellosolve dipropylene glycol monomethyl ether (DPGMME) diethylene glycol ethyl ether (DEGEE) ethylene glycol tripropylene glycol monomethyl ether (TPGMME) phenyl Cellosolve

661

G C A P P L I C AT I O N S | P E R S O N A L C A R E & C L E A N I N G P R O D U C TS

Rtx-Wax, 30m, 0.32mm ID, 0.25m (cat.# 12424) Sample: 1% each solvent in methanol Inj.: 1.0L split (split ratio 100:1), 4mm inlet liner (cat.# 20814) Inj. temp.: 250C Carrier gas: hydrogen, constant flow Flow rate: 3.0 mL/min. Oven temp.: 35C (4 min. hold) to 85C @ 3C/min., to 200C @ 15C/min. (2 min. hold) Det.: FID @ 250C

GC_FF00644

Cleaning Solvents Rtx-VMS

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.

methanol ethanol iso-propanol tert-butanol n-propanol iso-butanol methyl Cellosolve n-butanol Cellosolve ethylene glycol butyl Cellosolve limonene dipropylene glycol monomethyl ether (DPGMME) diethylene glycol ethyl ether (DEGEE) phenyl Cellosolve tripropylene glycol monomethyl ether (TPGMME)

Rtx-VMS, 60m, 0.25mm ID, 1.4m (cat.# 19916) Sample: 1% each solvent in methanol Inj.: 1.0L split (split ratio 100:1), 4mm inlet liner (cat.# 20814) Inj. temp.: 250C Carrier gas: hydrogen, constant flow Flow rate: 1.5 mL/min. Oven temp.: 60C (1 min. hold) to 138C @ 4C/min., to 145C @ 2C/min., to 210C @ 15C/min., to 230C @ 5C/min. Det.: FID @ 250C

GC_FF00645

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662

Cleaning Solvents; Fragrances


Cleaning Solvents (All-Purpose Cleaner) Rtx-VMS Cleaning Solvents (Glass Cleaner) Rtx-VMS
1. iso-propanol 2. butyl Cellosolve

1. butyl Cellosolve 2. limonene

G C A P P L I C AT I O N S | P E R S O N A L C A R E & C L E A N I N G P R O D U C TS

GC_FF00646

GC_FF00647

Rtx-VMS, 60m, 0.25mm ID, 1.4m (cat.# 19916) Sample: approx. 5% cleaner in methanol Inj.: 1.0L split (split ratio 100:1), 4mm inlet liner (cat.# 20814) Inj. temp.: 250C Carrier gas: hydrogen, constant flow Flow rate: 1.5 mL/min. Oven temp.: 60C (1 min. hold) to 138C @ 4C/min. to 145C @ 2C/min. to 210C @ 15C/min. to 230C @ 5C/min. Det.: FID @ 250C

Rtx-VMS, 60m, 0.25mm ID, 1.4m (cat.# 19916) Sample: approx. 5% cleaner in methanol Inj.: 1.0L split (split ratio 100:1), 4mm inlet liner (cat.# 20814) Inj. temp.: 250C Carrier gas: hydrogen, constant flow Flow rate: 1.5 mL/min. Oven temp.: 60C (1 min. hold) to 138C @ 4C/min. to 145C @ 2C/min. to 210C @ 15C/min. to 230C @ 5C/min. Det.: FID @ 250C

Personal Care Product Fragrances Rtx-1


1. eucalyptol 2. camphor 3. menthol

free literature
Analyzing Cleaning and Personal Care Products by Gas and Liquid Chromatography (lit. cat.# 59738)
Soaps, detergents, solvents, and many other components of household cleaners and personal care products are effectively monitored by GC and/or HPLC. Sometimes either approach can be used for the same purpose, but one will offer time, accuracy, or economic advantages over the other. Sometimes the approach is clear, but the choice involves alternative stationary phases. This 16-page guide presents numerous examples of GC and HPLC analyses of these diverse products.
GC_FF00633

Rtx-1, 60m, 0.25mm ID, 0.25m (cat.# 10126) Sample: 130ppm eucalyptus oil, 250ppm camphor, 260ppm menthol in methanol Inj.: 1.0L split (split ratio 20:1), 4mm inlet liner (cat.# 20814) Inj. temp.: 275C Carrier gas: helium, constant flow Flow rate: 0.6 mL/min. Oven temp.: 80C to 180C @ 5C/min. Det.: FID @ 300C

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Permanent Gases
Permanent Gases ShinCarbon ST
(micropacked)

663

Permanent Gases, C1+C2 hydrocarbons ShinCarbon ST


(micropacked)

1. hydrogen 2. oxygen 3. nitrogen 4. carbon monoxide 5. methane 6. carbon dioxide ShinCarbon ST 100/120 mesh 2 meter x 1mm ID micropacked (cat.# 19808) Sample: 5L permanent gases mix, approx. 5 mol. percent each Inj. temp.: Carrier gas: Flow rate: Oven temp.: Det. 100C helium 10mL/min. 40C (hold 3 min.) to 250 @ 8/min. (hold 10 min.) HID @ 200C

1. oxygen 2. nitrogen 3. carbon monoxide 4. methane 5. carbon dioxide 6. acetylene 7. ethylene 8. ethane ShinCarbon ST 100/120 mesh 2 meter x 1mm ID micropacked (cat.# 19808) Sample: Permanent gases-C1+C2 hydrocarbons Sample size: 5L Inj. temp.: 100C Carrier gas: helium Flow rate: 10mL/min. Oven temp.: 40C (hold 3 min.) to 250 @ 8/min. (hold 10 min.) Det. HID @ 200C

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

GC_PC00666

GC_PC00665

Permanent Gases Rt-Msieve 5A PLOT


1. 2. 3. 4. 5. 6. helium argon oxygen nitrogen methane carbon monoxide

1 3 4

Searching for a chromatogram?


2

www.restek.com
5 6

min.

2
GC_PC00165

15m, 0.32mm ID Rt-Msieve 5A PLOT (cat. # 19720) Sample conc.: 2-5 mol% Column temp.: Carrier gas: Linear velocity: Inj. temp.: Det.: Det. temp.: Sensitivity: 70C hydrogen 64cm/sec. 70C HP TCD 200C high

Phone: 800-356-1688 or 814-353-1300 www.restek.com

664

Permanent Gases
Permanent Gases Molecular Sieve 5A and Molecular Sieve 13X
1

1. 2. 3. 4.

oxygen nitrogen methane carbon monoxide

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

Molecular Sieve 5A: excellent resolution of oxygen, nitrogen, methane, and carbon monoxide.

Molecular Sieve 13X: rapid analysis and excellent peak symmetry for carbon monoxide.

10L helium, 510% each component Oven temp.: 50 C Inj./det. temp.: 150 C/200C Carrier gas: hydrogen Flow: 30mL/min., helium Detector: TCD

min.0

4
GC_PC00166

min.0

Molecular Sieve 5A 80/100 mesh 1m x 1/8" x 2mm ID SilcoSmooth tubing (cat.# 80440-800)

Molecular Sieve 13X 80/100 mesh 2m x 1/8" x 2mm (ID) SilcoSmooth tubing (cat.# 80439-800)

Permanent Gases Rt-QPLOT


1. 2. 3. 4. 5.
3 2

Permanent Gases Rt-MSieve 5A PLOT


helium air carbon monoxide methane carbon dioxide
2

1. hydrogen, 29.1 ppm 2. argon, 53.4 ppm 3. oxygen, 31.3 ppm

1 5 4 3

30C
min. 1 min. 1
GC_PC00169

2
GC_PC00170

30m, 0.32mm ID Rt-QPLOT PLOT (cat.# 19718) Sample: 30L split injection (40:1), 2-5 mol% Column temp.: Inj. temp.: Det.: Det. temp.: Carrier gas: Linear velocity: Split flow: 30C 30C HP TCD 200C hydrogen 38cm/sec. 40:1

30m, 0.53mm ID, 50m Rt-Msieve 5A PLOT (cat.# 19723) Sample: 0.5mL (sample loop injection) Column temp.: Carrier gas: Linear velocity: Det.: 27C helium 34cm/sec. Valco HID

Chromatogram courtesy of Larry McElmurry, Mobile Analytical Labs.

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Permanent Gases
Permanent Gases Rt-QPLOT
1 2 1

665

1. 2. 3. 4.

air carbon monoxide methane carbon dioxide


2 3 4

1. nitrogen 2. oxygen 3. argon

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

Subambient Separation: 15C

Subambient Separation: -40C

min.

3
GC_PC00174

min.

30m, 0.32mm ID Rt-QPLOT PLOT column (cat. # 19718) Sample conc.: Inj./det. temp.: Carrier gas: Linear velocity: Split flow: 2-5 mol% 15C hydrogen 34cm/sec. 40:1 Sample conc.: Inj./det. temp.: Carrier gas: Linear velocity: Split flow: 2-5 mol% -40C hydrogen 20cm/sec. 40:1

Permanent Gases Rt-QPLOT and Rt-Msieve 5A (Dual Column Configuration) Injector


Rt-QPLOT Column (30m, 0.53mm ID, cat.# 19716)
50cm from Rt-QPLOT Column

Detector

Universal Y Press-Tight Connector (cat.# 20406)

Universal Y Press-Tight Connector (cat.# 20406)

50cm from Rt-QPLOT Column

[
1 B

1. 2. 3. 4. 5. 6. 7.

helium argon oxygen nitrogen methane carbon dioxide carbon monoxide

Rt-Msieve 5A Column (30m, 0.32mm ID, cat.# 19722)

Fast, complete separation of gases and volatile compounds!


No complicated valve-switching.

Terrific separation!
2 4

ARt-QPLOT
2, 3, 4, 7

BRt-Msieve 5A
3

Oven temp.: Inj.: Carrier gas: Det.: Det. temp.:

30C 20L, split injection (10:1), 5% each compound hydrogen, 8psi HP TCD 200C
7

1 2

6 5

min.

10

12

14

16 0.40 0.60 0.80 2.20

Rt-QPLOT

Rt-Msieve 5A
GC_PC00171

Phone: 800-356-1688 or 814-353-1300 www.restek.com

666

Hydrocarbon Gases
Fluorocarbons ShinCarbon ST
(micropacked)
Peak Ret. Time (min.) 4.95 1. Freon 134a/22 2. Freon 12 7.11 3. Freon 133a 9.19 4. Freon 114 10.85

Hydrocarbon Gases Rt-QPLOT


1. 2. 3. 4. 5. 6. 7. 8. 9. methane ethylene acetylene ethane propylene propane cyclopropane propadiene propyne
14 13 11 15 16 6 1 10 17

8,9

10. 11. 12. 13. 14. 15. 16. 17.

isobutane 1,3-butadiene 1-butene n-butane cis-2-butene trans-2-butene isopentane n-pentane

2,3

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

5 7

12

min. 1

10

11

12

13

14

GC_PC00176

GC_PC00673

ShinCarbon ST 100/120 mesh (cat.# 19809) 1 meter x 1mm ID Silcosteel micropacked column Sample: Inj. temp.: Det.: Carrier gas: Linear velocity: Oven temp.: fluorocarbon blend, 5L ~1-3% each 200C FID/250C helium 10mL/min. 125C to 320C @ 16C/min.

30m, 0.32mm ID Rt-QPLOT PLOT (cat.# 19718) 300L split injection (40:1), 1000ppm Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Split flow: FID sensitivity: 50C (2 min.) to 220C @ 15C/min. 250C helium 42cm/sec. set @ 80C (5.6mL/min.) 40mL/min. 1.28 x 10-10 AFS

Hydrocarbon Gases Rt-UPLOT

5,6

8 9 7

14 13 11 12 15

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17.

methane ethylene ethane acetylene propane propylene cyclopropane propadiene propyne isobutane n-butane 1-butene cis-2-butene trans-2-butene 1,3-butadiene isopentane n-pentane
17

Hydrocarbon Gases Rt-Msieve 13X PLOT


2

1. 2. 3. 4. 5. 6. 7.

argon/oxygen nitrogen C1 carbon monoxide C2 C3 C4

6 3 5 1 7

10

16 4

min.

6 GC_PC00177

10

11

min.

10

12

14

16

18

20

22

24

26

GC_PC00168

30m, 0.32mm ID Rt-UPLOT PLOT (cat.# 19724) 300L split injection (40:1), 1000ppm Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Split flow: FID sensitivity: 50C to 190C @ 10C/min. 250C helium 42cm/sec. set @ 80C (5.6mL/min.) 40mL/min. 1.28 x 10-10 AFS

30m, 0.53mm ID Rt-Msieve 13X PLOT (cat.# 19706) Sample conc.: 2-5 mol% Oven temp.: Carrier gas: Linear velocity: 30C (hold 2 min.) to 300C @ 15C/min. (hold 10 min.) hydrogen 30cm/sec.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Hydrocarbon Gases
Hydrocarbon Gases Rt-QPLOT
30m, 0.32mm ID Rt-QPLOT (cat.# 19718) 30.0L injection of Hydrocarbon Gas Mix Oven temp.: Inj.: Carrier gas: Head pressure: Column flow rate: Linear velocity: Split ratio: Det.: Make-up gas flow: Inlet liner: 40C to 240C @ 8C/min. (hold 10 min.) split/250C helium (constant pressure mode) 18.0psi 1.5cc/min. @ 40C 35cm/sec. @ 40C 20:1 FID/240C 45cc/min. 4mm single gooseneck (cat.# 20798)

667

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.

methane ethene ethane propene propane propadiene isobutane 1,3-butadiene 1-butene isobutene n-butane cis-2-butene trans-2-butene isopentane n-pentane n-hexane

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

GC_PC00521

Hydrocarbon Gases Rt-QPLOT

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

methane ethylene ethane propylene propane isobutane 1,3-butadiene 1-butene isobutene n-butane cis-2-butene trans-2-butene

GC_PC00522

30m, 0.32mm ID Rt-QPLOT (cat.# 19718) 30.0L injection of Hydrocarbon Gas Mix Oven temp.: Injector: Carrier gas: Head pressure: Column flow rate: Linear velocity: Split ratio: Det.: Make-up gas flow: Inlet liner: 35C to 240C @ 10C/min. (hold 10 min.) split/250C helium (constant pressure mode) 18.0psi 1.5cc/min. @ 40C 35cm/sec. @ 40C 20:1 FID/240C 45cc/min. 4mm single gooseneck (cat.# 20798)

Phone: 800-356-1688 or 814-353-1300 www.restek.com

668

Hydrocarbon Gases
Hydrocarbon Gases Rt-QPLOT

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

1. 2. 3. 4. 5. 6. 7. 8.

methane ethane propane isobutane n-butane isopentane n-pentane hexanes

30m, 0.32mm ID Rt-QPLOT (cat.# 19718) 30.0L injection of Hydrocarbon Gas Mix Oven temp.: Injector: Carrier gas: Head pressure: Column flow rate: Linear velocity: Split ratio: Det.: Make-up gas flow: Inlet liner: 40C to 240C @ 10C/min. (hold 10 min.) split/250C helium (constant pressure mode) 18.0psi 1.5cc/min. @ 40C 35cm/sec. @ 40C 20:1 FID/240C 45cc/min. 4mm single gooseneck (cat.# 20798)

GC_PC00523

Natural Gas ShinCarbon ST


(micropacked)

free literature
1. 2. 3. 4. 5. 6. 7. 8. C1 C2 C3 iC4-isobutane C4 iC5-isopentane nC5 hexanes

ShinCarbon ST Micropacked GC Columns: Above-Ambient Analyses of Permanent Gases and Light Hydrocarbons (lit. cat.# 59519A) A ShinCarbon ST micropacked column will separate hydrogen, oxygen, nitrogen, carbon dioxide, carbon monoxide, and methane in 10 minutes, without cryogenic cooling - a separation that has been impossible for a single GC or GSC column without sub-ambient temperature. The 2-page note also shows separations of light hydrocarbon / permanent gas mixtures, natural gas components, sulfur dioxide, and fluorocarbons all obtained using a 1-meter or 2-meter micropacked column and above-ambient initial temperatures.

ShinCarbon ST 100/120 mesh (cat.# 19809) 1 meter x 1mm ID Silcosteel micropacked column Sample: Inj. temp.: Det.: Carrier gas: Linear velocity: Oven temp.: 0.5-8% varied, C1-C6 hydrocarbons 200C FID/250C helium (constant flow) 10mL/min. 125C to 250C @ 16C/min.

GC_PC00672

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Hydrocarbon Gases
Hydrocarbon Gases Porous Polymer PLOTs
2,4

669

Rt-QPLOT column least selective for functional groups.

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

5 6

min.

2 4,3

1. 2. 3. 4. 5. 6.

methane ethylene ethane acetylene propylene propane

Rt-SPLOT column selective for polar, unsaturated compounds.


1

5 6

min.

Rt-UPLOT column most selective for unsaturated compounds.

5,6

min.

5 GC_PC00180

30m, 0.32mm ID (Rt-QPLOT: cat.# 19718; Rt-SPLOT: cat.# 19710; Rt-UPLOT: cat.# 19724) 100L split injection. 1000ppm (v/v) each in helium, Cyclosplitter liner (cat.# 20755). Oven temp.: Inj./det. temp.: Carrier gas: Det.: Split ratio: 50C 200C hydrogen FID 20:1

Phone: 800-356-1688 or 814-353-1300 www.restek.com

670

Hydrocarbon Gases
Refinery Gas Rt-Alumina PLOT
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17.
14 1 9 11 12 13 16 10 17 1 15

4 2 3 5 7 6 8

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

methane ethane ethylene propane cyclopropane propylene isobutane n-butane propadiene acetylene trans-2-butene 1-butene cis-butene isopentane n-pentane 1,3-butadiene propyne

Ethylene Purity Rt-Alumina PLOT


3 2

1. methane 2. ethane 3. ethylene

min. min. 2 4 6 8 GC_PC00183 10 12 14

2 GC_PC00184

50m, 0.53mm ID Rt-Alumina PLOT (cat. # 19701) 100L hydrocarbon mix split injection , 1000ppm (gas-tight syringe) Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: Split flow: FID sensitivity: 40C to 120C @ 5C/min. (hold 5 min.) 200C helium 37.5cm/sec. set @ 80C (5.0mL/min.) 60mL/min. 1.28 x 10-10 AFS

50m, 0.53mm ID Rt-Alumina PLOT (cat. # 19701) 200L gas-tight syringe injection Sample conc.: 99+% ethylene Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: Split flow: FID sensitivity: 40C 200C helium 42cm/sec. set @ 80C (5.6mL/min.) 40mL/min. 1.28 x 10-10 AFS

Propylene Purity Rt-Alumina PLOT

2 5 3 7 1 8 9 10 11 12 13 14 15 16 17

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17.

methane ethane ethylene propane cyclopropane propylene isobutane n-butane propadiene acetylene trans-2-butene 1-butene cis-2-butene isopentane n-pentane 1,3-butadiene propyne

min.

8 GC_PC00185

10

12

14

50m, 0.53mm ID Rt-Alumina (cat.# 19701) 100L hydrocarbon mix (gas-tight syringe) Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: Split flow: FID sensitivity: 40C (hold 3 min.) to 120C @ 10C/min. (hold 5 min.) 200C helium 37.5cm/sec. set @ 80C 60mL/min. 1.28 x 10-10 AFS

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Hydrocarbon Gases
1,3-Butadiene Purity Rt-Alumina PLOT Hydrocarbon Gases HayeSep S
(micropacked)
1

671

1 2

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

methane ethane propane isobutane n-butane trans-2-butene 1-butene isobutylene cis-2-butene isopentane 1,3-butadiene
9

11

5 6 2 3

1. 2. 3. 4. 5. 6. 7.

methane ethylene acetylene ethane propylene propane 1-butene

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

4 5 6 7 min. 2 4 8 10 10 12 min. 4 8 GC_PC00187 12

6 8 GC_PC00186

50m, 0.53mm ID Rt-Alumina PLOT (cat. # 19701) 500L gas-tight syringe injection Sample conc.: 99+% 1,3 butadiene Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: Split flow: FID sensitivity: 80C 200C helium 42cm/sec. set @ 80C (5.6mL/min.) 40mL/min. 1.28 x 10-10 AFS

2m, 0.75mm ID HayeSep S micropacked column (cat.# 19011) 500L split injection of a light hydrocarbon gas mixture Oven temp.: Inj. & det. temp.: Carrier gas: Flow: FID sensitivity: Split ratio: 40C (hold 3 min.) to 150C @ 15C/min. (hold 5 min.) 220C helium 20mL/min. set @ 40C 32 x 10-11 AFS 10:1

Butane Fuel Rtx-1


2 3 4

Butane Fuel Rtx-1


4

Butane Fuel MXT-1


3 4

1. 2. 3. 4.

methane propane isobutane butane

1. 2. 3. 4. 5.

methane ethane propane isobutane butane

1. 2. 3. 4. 5.

methane ethane propane isobutane butane

2 1 min. 2 GC_PC00204 4 min. 1 2 GC_PC00205 4 min.

12

4 GC_PC00206

60m, 0.53mm ID, 5.0m Rtx-1 (cat.# 10183) 1.0L butane fuel from a Microflame torch Direct injection using a Uniliner liner Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C 200C hydrogen 80cm/sec. (flow rate: 10cc/min.) 4 x 10-11 AFS

60m, 0.53mm ID, 5.0m Rtx-1 (cat.# 10183) 1.0L butane fuel from a disposable lighter Direct injection using a Uniliner liner Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C 200C hydrogen 80cm/sec. (flow rate: 10cc/min.) 4 x 10-11 AFS

60m, 0.53mm ID, 5.0m MXT-1 (cat.# 70183) 1.0L direct injection of butane fuel Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C 200C helium 40cm/sec. 4 x 10-11 AFS

Phone: 800-356-1688 or 814-353-1300 www.restek.com

672

Hydrocarbon Gases
Propane Fuel Rtx-1
3 1

Methane Purity Rtx-1

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

1. 2. 3. 4. 5.

methane ethane propane isobutane butane

1. methane 2. trace hydrocarbon contaminants

1 4 2

min.

2 GC_PC00207

min.

4 GC_PC00208

60m, 0.53mm ID, 5.0m Rtx-1 (cat.# 10183) 1.0L propane fuel Direct injection using a Uniliner inlet liner Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C 200C hydrogen 80cm/sec. (flow rate: 10cc/min.) 4 x 10-11 AFS

60m, 0.53mm ID, 5.0m Rtx-1 (cat.# 10183) 1/2cc slow injection (10 sec. duration) of ultra high purity methane Direct injection using a Uniliner inlet liner Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C 200C hydrogen 80cm/sec. (flow rate: 10cc/min.) 4 x 10-11 AFS

Hydrocarbon Test Mix Rt-Alumina PLOT


4 5 7

2 3

6 8

1 9 10 11 13 15 12 14

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17.

methane ethane ethylene propane cyclopropane propylene isobutane n-butane propadiene acetylene trans-2-butene 1-butene cis-2-butene isopentane n-pentane 1,3-butadiene propyne

16

17

min.

8 GC_PC00551

10

12

14

16

50m, 0.53mm ID, 6m Rt-Alumina PLOT (cat. # 19701) 50L gas-tight syringe injection, 1000ppm each analyte Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: Split flow: FID sensitivity: 80C 200C helium 42cm/sec. set @ 80C (5.6mL/min.) 40mL/min. 1.28 x 10-10 AFS

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Hydrocarbons
Gasoline Aromatics Rtx-1
2

673

TIC
4,5

13

6 3

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

1 11 10

12 8

14

17 16 15 20 19 18

21

23 24 22

min.

10

15

20

25

30

35
GC_PC00214

40

45

50

55

60

3 4,5 6

RIC
1

13

9 8 21 11 10

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24.

benzene toluene ethylbenzene m-xylene p-xylene o-xylene isopropylbenzene n-propylbenzene 1-methyl-3-ethylbenzene 1-methyl-4-ethylbenzene 1,3,5-trimethylbenzene 1-methyl-2-ethylbenzene 1,2,4-trimethylbenzene 1,2,3-trimethylbenzene indane 1,4-diethylbenzene butylbenzene 1,2-diethylbenzene 1,2,4,5-tetramethylbenzene 1,2,3,5-tetramethylbenzene pentamethylbenzene naphthalene 2-methylnaphthalene 1-methylnaphthalene

12

14 17 15 16 20 19 23 24 18

22

min.

10

15

20

25

30

35
GC_PC00215

40

45

50

55

60

60m, 0.25mm ID, 1.0m Rtx-1 (cat.# 10156) 1.0L split injection of neat gasoline. Oven temp.: Inj. / det. temp.: Linear velocity: Split ratio: Det.: 50C (hold 1 min.) to 190C @ 2C/min. 250C / 280C 35cm/sec. set @ 50C 200:1 MS, 45-300m/e, 1 scan/sec.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

674

Hydrocarbons
Gasoline Aromatics (ASTM D-5580) 20% TCEP on 80/100 Chromosorb PAW
(micropacked)

Gasoline Aromatics (ASTM D-5580) 20% TCEP on 80/100 Chromosorb PAW


(micropacked)

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

1. 2. 3. 4.

benzene toluene 2-hexanone (ISTD) heavy hydrocarbons

1. 2. 3. 4. 5.

2-hexanone (ISTD) ethylbenzene p/m-xylene o-xylene C9 + aromatics

4 3 1 2 1

min. min. 10
GC_PC00212

10

20
GC_PC00213

30

}
40 30 20% TCEP on 80/100 Chromosorb PAW 30m, 0.53mm ID, 3.0m Rtx-1 (cat.# 10185) Sample: 0.5L gasoline Oven temp.: Inj. & det. temp.: Flow rate: 60C (hold 6 min.) to 115C @ 2C/min. 250C 2.8mL/min.

20

20% TCEP on 80/100 Chromosorb PAW 0.56m, 0.75mm ID x 0.81mm OD micropacked (cat.# 19040) Sample: 0.5L gasoline Oven temp.: Inj. & det. temp.: Flow rate: 60C (hold 6 min.) to 115C @ 2C/min. 250C 4.4mL/min.

Petroleum Oxygenates (ASTM D4815) TCEP (Micropacked) & Rtx-1


1. 2. 3. 4. 5. 6. 7. 15 8. 9. 10. 11. 12. 13. 14. 15. methanol ethanol isopropanol tert-butanol n-propanol methyl tert-butyl ether sec-butanol diisopropyl ether (DIPE) isbutanol ethyl-tert-butyl ether (ETBE) tert-amyl ether dimethoxyethane (DME) n-butanol benzene tert-amyl methyl ether (TAME) 16. total heavy hydrocarbons

Petroleum Oxygenates Rt-TCEP

6 10

16

1. 2. 3. 4. 5. 6. 7. 8. 9.
1 2 7 8 3 5 6 9

methyl tert-butyl ether n-undecane tert-butanol methanol isopropyl alcohol ethanol n-dodecane n-tridecane n-butanol

12 7 4 3 5 2 1 8 9 13 11 14

min. min. 10
GC_PC00194

10

12

14

16

20
GC_PC00195

0.56m, 0.75mm ID 20% TCEP on Chromosorb P A/W (cat.# 19040) and 30m, 0.53mm ID, 3.0m Rtx-1 (cat.# 10185 connected in series) 0.5L split injection of oxygenates blend 110% wt in surrogate gasoline Oven temp.: Inj. / det. temp.: Carrier gas: Split ratio: 60C 200C / 250C (FID) helium, 5mL/min. set @ 60C 15:1

60m, 0.25mm ID, 0.4m Rt-TCEP (cat.# 10999) 1.0L split injection, components @ 500ppm. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split flow: 60C (hold 5 min.) to 100C @ 5C/min. (hold 10 min.) 200C helium 30cm/sec. set @ 80C 6.4 x 10-11 AFS 46mL/min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Hydrocarbons
Petroleum Oxygenates Stabilwax
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 32 heptane C3 oxide benzene toluene ethylbenzene p-xylene m-xylene cumene o-xylene styrene 2-methylpentanol p-diethylbenzene m-diethylbenzene -methylstyrene o-diethylbenzene phenylacetylene (trace) benzaldehyde monopropylene glycol acetophenone 2-phenyl-2-propanol -methylbenzyl alcohol benzyl alcohol phenylethyl alcohol phenol

675

14,15 1 67 5 4 3 11 2 18 8 24 19 20 13 12 17 21 23

10

22

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

16

min.

10

12

14

16

18

20

22

24

26

28

30

GC_PC00196

30m, 0.53mm ID, 1.0m Stabilwax (cat.# 10655) 0.2L injection of a 15 to 30ng/L synthetic blend Direct injection using a Uniliner liner Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 45C (hold 4 min.) to 220C @ 6C/min. 220C hydrogen 40cm/sec. (flow rate: 5.1cc/min.) 16 x 10-11 AFS

Petroleum Oxygenates (MTBE) Rtx-1

1. 2. 3. 4. 5. 6. 7. 8. 9.

dimethylether methanol C4s tert-butyl alcohol methyl tert-butyl ether sec-butylmethylether diisobutylene 4-vinylcyclohexene-1 (BD1B dimer) triisobutylene

8 1

min.

10

12

14

16

18
GC_PC00197

20

22

24

26

28

30

32

34

60m, 0.53mm ID, 5.0m Rtx-1 (cat.# 10183) 0.1L injection of neat methyl tert-butyl ether. Direct injection using a Uniliner liner. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C (hold 8 min.) to 200C @ 5C/min. 200C hydrogen 40cm/sec. (flow rate: 5cc/min.) 8 x 10-11 AFS

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676

Hydrocarbons
Aromatics (Benzene/Toluene/Xylene) MXT-WAX
1

Aromatics (Benzene/Toluene/Xylene) Rtx-200


1

1. 2. 3. 4. 5. 6.

benzene toluene ethylbenzene p-xylene m-xylene o-xylene

4,5

1. 2. 3. 4. 5. 6.

benzene toluene ethylbenzene m-xylene p-xylene o-xylene

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

3 4

6 3

min.

12

16 min. 4
GC_PC00189

GC_PC00188

30m, 0.28mm ID, 1.0m MXT-WAX (cat.# 70654) 1.0L split injection of BTEX Standard (cat.# 30051) Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 60C 260C hydrogen 38cm/sec. 3.2 x 10-11 AFS 100:1

30m, 0.53mm ID, 0.50m Rtx-200 (cat.# 15040) 0.1L direct injection of BTEX Standard (cat.# 30051) Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 60C 250C hydrogen 40cm/sec. (flow rate: 5.2cc/min.) 4 x 10-11 AFS

Aromatics (Benzene/Toluene/Xylene) Rtx-502.2

Aromatics (Benzene/Toluene/Xylene) Rtx-Wax

1. 2. 3. 4. 5. 6.

methyl tert-butyl ether benzene toluene ethylbenzene m/p-xylene o-xylene


1

1. 2. 3. 4. 5. 6.

benzene toluene ethylbenzene p-xylene m-xylene o-xylene

4 2 3

2 34 5

min.

10 GC_PC00191

15

20

min.

12
GC_PC00190

16

20

105m, 0.53mm ID, 3.0m Rtx -502.2 (cat.# 10910) 0.25L split injection of CA PVOC Mix (cat.# 30071) Conc.: 10005000g/mL

Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split flow:

40C (hold 1 min. ) to 100C @ 5C/min., to 240C @ 8C/min. (hold 8 min.) 200C / 280C helium 67cm/sec. set @ 40C 2.05 x 10-9 AFS 70mL/min.

30m, 0.53mm ID, 1.0m Rtx-Wax (cat.# 12455) 0.1L direct injection of BTEX Standard (cat.# 30051) Oven temp.: 50C Inj. & det. temp.: 250C Carrier gas: hydrogen Linear velocity: 40cm/sec. (flow rate: 5.2cc/min.) FID sensitivity: 16 x 10-11 AFS

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Hydrocarbons
Aromatics (Xylene Isomers plus Cumene) 5% RT-1200/1.75% Bentone 34 on 100/120 Silcoport
1 2

677

Aromatics (Xylene Isomers /BTEX) 5% RT-1200/5% Bentone 34 on 100/120 Silcoport


1. 2. 3. 4. 5. 6.
2

4 3

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.
6 5 7 8

hexane benzene n-octane toluene n-nonane ethylbenzene p-xylene m-xylene o-xylene cumene n-decane

benzene toluene ethylbenzene p-xylene m-xylene o-xylene

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

3 4 5 6

10 11

min. min. 2 4 6 8
GC_PC00192

4
GC_PC00193

10

12

14

5% RT-1200/1.75% Bentone 34 on 100/120 Silcoport (cat.# 80125) 1.8m, 1/8" OD x 2mm ID SilcoSmooth tubing Sample size: 0.1L Conc.: 0.5g/L in hexane Oven temp.: 75C Inj. & det. temp.: 200C Carrier gas: nitrogen Flow rate: 20mL/min. FID sensitivity: 32 x 10-11 AFS

5% RT-1200/5% Bentone 34 100/120 Silcoport (cat.# 80129) 2m, 1/8" OD x 2mm ID SilcoSmooth tubing Sample size: 0.1L Conc.: 0.5g/L in hexane Oven temp.: 100C Inj. & det. temp.: 200C Carrier gas: nitrogen Flow rate: 20mL/min. FID sensitivity: 32 x 10-11 AFS

Aromatics Rt-TCEP
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.
13 1 2 4 6 7 8 3 9 10 11 14 12

n-undecane benzene n-dodecane toluene ethylbenzene p-xylene m-xylene cumene n-propylbenzene o-xylene mesitylene 1-ethyl-2-methylbenzene m-diethylbenzene p-diethylbenzene o-diethylbenzene

60m, 0.25mm ID, 0.40m Rt-TCEP (cat.# 10999) 1.0L split injection, components @ 500ppm (ethylbenzene @ 1000ppm). Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split flow:
15

60C (hold 5 min.) to 100C @ 5C/min. (hold 10 min.). 200C helium 30cm/sec. set @ 80C 6.4 x 10-11 AFS 46mL/min.

min. 0

8
GC_PC00211

10

12

14

16

18

Phone: 800-356-1688 or 814-353-1300 www.restek.com

678

Hydrocarbons
Aromatics, Aliphatics 10% TCEP 100/120 Chromosorb PAW
12 3 4

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

6 7 8

1. 2. 3. 4. 5. 6. 7. 8. 9a. 9b. 10. 11.

n-hexane n-heptane n-octane n-nonane n-decane benzene toluene ethylbenzene m-xylene p-xylene isopropylbenzene o-xylene

10 11

min.

8
GC_PC00217

10

12

14

16

10% TCEP 100/120 Chromosorb PAW (cat.# 80126) 2.5m, 1/8" OD x 2mm ID SilcoSmooth tubing Sample size: 0.1mL neat Oven temp.: 80C Inj./det. temp.: 200C/250C Carrier gas: nitrogen Flow rate: 20mL/min. FID sensitivity: 128 x 10-10 AFS

Hydrocarbons, C7-C42 Rtx-1


1 2 4 6 8 10 17 20

3 22 5 7 9 12 11 24 13 14 15 16 18 19 21 23 25

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 C17 C18 C19 C20 C22

16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27.

C23 C24 C25 C26 C28 C30 C32 C34 C36 C38 C40 C42

26 27

min.

12

16

20

24

28

32

36

40

44

48

52

56

60

GC_PC00216

30m, 0.53mm ID, 0.25m Rtx-1 (cat.# 10125) 0.2L injection of a synthetic hydrocarbon mix, ~ 0.1mg/mL per component Direct injection using a Uniliner liner Oven temp.: 40C to 340C @ 5C/min. Inj. & det. temp.: 340C Carrier gas: hydrogen Linear velocity: 40cm/sec. set @ 40C FID sensitivity: 64 x 10-11 AFS

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Hydrocarbons
Detailed Hydrocarbons Analysis Rtx-1PONA
10

679

Circles indicate critical pairs that must be resolved.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

ethanol C5 tert-butanol 2-methylbutene-2 2,3-dimethylbutane methyl tert-butyl ether (MTBE) C6 1-methylcyclopentene benzene cyclohexane 3-ethylpentane 1-tert-2-dimethylcyclopentane C7 2,2,3-trimethylpentane 2,3,3-trimethylpentane

16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30.

toluene C8 ethylbenzene p-xylene 2,3-dimethylheptane C9 5-methylnonane 1,2-methylethylbenzene C10 C11 (undecane) 1,2,3,5-tetramethylbenzene naphthalene C12 (dodecane) 1-methylnaphthalene C13 (tridecane)
18

Rtx-1PONA, 100m, 0.25mm ID, 0.5m (cat.# 10195) w/ Rtx-5 tuning column, 2.62m, 0.25mm ID, 1.0m, connected via Press-Tight connector (cat.# 20446) Sample: custom detailed hydrocarbons analysis (DHA) mix, neat Inj.: 0.01L, split (split ratio 150:1), 4mm cup inlet liner (cat.# 20709) Inj. temp.: 200C Carrier gas: helium, constant flow Linear velocity: 28cm/sec. (2.3mL/min.) Oven temp.: 5C (hold 15 min.) to 50C @ 5C/min. (hold 50 min.) to 200C @ 8C/min. (hold 10 min.) Det.: FID @ 250C

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

Resolution (1-methylcyclopentane/benzene): 1.28


27

16 1 7 5 11 9 8 13 17 3 12 14 15 19 20 23 22 21 24

28 25 26 29 30

4 2

10

20

30

40

50

60
GC_PC00743

70

80

90 min.

Detailed Hydrocarbons Analysis Rtx-1PONA


1
1. 2. 3. 4. ethanol C5 tert-butanol 2-methylbutene-2 Rtx-1PONA, 100m, 0.25mm ID, 0.5m (cat.# 10195) w/ Rtx-5 tuning column, 2.62m, 0.25mm ID, 1.0m, connected via Press-Tight connector (cat.# 20446) Sample: Inj.: custom detailed hydrocarbons analysis (DHA) mix, neat 0.01L, split (split ratio 150:1), 4mm cup inlet liner (cat.# 20709) Inj. temp.: 200C Carrier gas: helium, constant flow Linear velocity: 28cm/sec. (2.3mL/min.) Oven temp.: 35C Det.: FID @ 250C

C5 efficiency: 613,596 total theoretical plates k' (C5): 0.489 tert-butanol skewness: 1.25 Resolution (tert-butanol/2-methylbutene-2): 5.60

2 3

10
GC_PC00743A

11

12 min.

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680

Hydrocarbons
Reformate Rtx-1
4 5 9 10 17 3 16 11 15 19

18

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

2 6 1 12 7,8 13 14 20 21

min. 2

10

12

14

16
26

18

20

22

24

26

28

30

32

34

36
33

38

40

42

24 25 23

29

34,35 30 31 28 32

22 27

min. 48

50

52

54

56

58

60

62

64

66

68

70

72

74

76

78

80

82

84

86

88

44 37 40 38 36 39 41 42 45 43

46 49 48 47 50 51 52 53

54 55

min. 90

92

94

96

98

100

102

104

106

108

110

112

114

116

118

120

126

128

130

132

134

GC_PC00210

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23.

propane isobutane n-butane isopentane n-pentane 2,2-dimethylbutane cyclopentane 2,3-dimethylbutane 2-methylpentane 3-methylpentane n-hexane 2,2-dimethylpentane methylcyclopentane 2,4-dimethylpentane benzene C7 paraffin C7 paraffin C7 paraffin toluene C8 paraffin C8 paraffin C8 paraffin ethylbenzene

24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40. 41. 42. 43. 44. 45. 46.

m-xylene p-xylene o-xylene isopropylbenzene n-propylbenzene 1-methyl-3-ethylbenzene 1-methyl-5-ethylbenzene 1,3,5-trimethylbenzene 1-methyl-2-ethylbenzene 1,2,4-trimethylbenzene 1,2,3-trimethylbenzene 1-methyl-3-isopropylbenzene 1,3-diethylbenzene 1-methyl-3-n-propylbenzene 1-methyl-4-n-propylbenzene n-butylbenzene 1,2-diethylbenzene 1-methyl-2-n-propylbenzene 1,4-dimethyl-2-ethylbenzene 1,3-dimethyl-4-ethylbenzene 1,2-dimethyl-4-ethylbenzene 1,2,4,5-tetramethylbenzene 1,2,3,5-tetramethylbenzene

47. 48. 49. 50. 51. 52. 53. 54. 55.

C10 indane C12 aromatic naphthalene C12 aromatic C12 aromatic C12 aromatic C12 aromatic 2-methylnaphthalene 1-methylnaphthalene

105m, 0.25mm ID, 0.50m Rtx-1 (cat.# 10144) 1.0L split injection of petroleum standards Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split Ratio: 30C (hold 10 min.) to 200C @ 1C/min. 250C helium 20cm/sec. (flow rate: 0.7cc/min.) 8 x 10-11 AFS 100:1

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Hydrocarbons
Crude Oil, Prudhoe Bay Rtx-1
1. 2. 3. 4. 5a. 5b. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.
23 18 24 25 26 27 28

681

4 5 7 8 9 10 12 11 13 14 15 17 16 6 19 20 21 22

benzene heptane toluene octane m-xylene p-xylene o-xylene nonane decane undecane dodecane tridecane tetradecane pentadecane hexadecane heptadecane pristane

17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

octadecane phytane nonadecane eicosane heneicosane docosane tricosane tetracosane pentacosane hexacosane heptacosane octacosane

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

min.

12

16

20

24

28

32

36

40

44

48

52

56

60

64

68

72

76

80

GC_PC00231

30m, 0.53mm ID, 3.0m Rtx-1 (cat.# 10185) 0.4L split injection of Prudhoe Bay crude oil Oven temp.: 40C to 285C @ 5C/min. (hold 30 min.) Inj. & det. temp.: 285C Carrier gas: hydrogen Linear velocity: 40cm/sec. (flow rate: 5.2cc/min.) FID sensitivity: 256 x 10-11 AFS Split ratio: 50:1

Crude Oil, Arabian Light Rtx-1


1 2

3 4 5 6 7 8 9 10 11 12 13

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

heptane octane nonane decane undecane dodecane tridecane tetradecane pentadecane hexadecane heptadecane

12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22.

octadecane nonadecane eicosane heneicosane docosane tricosane tetracosane pentacosane hexacosane heptacosane octacosane

14 15 16 17 18 19 20 21 22

min.

12

16

20

24

28

32

36
GC_PC00232

40

44

48

52

56

60

64

68

30m, 0.53mm ID, 3.0m Rtx-1 (cat.# 10185) 0.6L split injection of an Arabian light crude oil. Oven temp.: 40C to 285C @ 5C/min. (hold 15 min.) Inj. & det. temp.: 285C Carrier gas: hydrogen Linear velocity: 40cm/sec. (flow rate: 5.2cc/min.) FID sensitivity: 128 x 10-11 AFS Split ratio: 50:1

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682

Hydrocarbons
Crude Oil, Pennsylvania Light MXT-1HT Sim Dist Lubricant (Synthetic) Stabilwax
1 2 3 6 7 9

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

C14 C15 C16 C10 OH C12 ester BHT C12 OH C14 ester C14 OH C16 OH

10 8 4

min.
GC_PC00594

12

16
GC_PC00219

20

24

28

MXT-1HT Sim Dist 5m, 0.53mm ID, 0.10m (cat.# 70100) Oven temp: 50C, 10C/minute, 430C, 6 min. final hold Inj. temp.: oven tracking Det. temp: 430C Carrier gas: helium 1.8 psi, 14mL/min. Inj. volume: 0.2L Std. conc.: approx. 2% in carbon disulfide

30m, 0.53mm ID, 1.0m Stabilwax (cat.# 10655) 1.0L split injection of a synthetic lubricant Oven temp.: 100C to 175C @ 5C/min., to 225C @ 15C/min. (hold 10 min.) Inj. / det. temp.: 250C / 275C Carrier gas: helium Linear velocity: 20cm/sec. (flow rate: 2.6cc/min.) FID sensitivity: 8 x 10-11 AFS Split vent: 40:1

Petroleum Wax MXT-1

1. 2. 3. 4. 5. 6. 7. 8. 9.
6 5 1

hexadecane - C16 eicosane - C20 tetracosane - C24 octacosane - C28 dotricontane - C32 hexatricontane - C36 tetracontane - C40 tetratetracontane - C44 pentacontane - C50

4 8

3 2

min.
GC_PC00218

36

30m, 0.28mm ID, 0.25m MXT-1 (cat.# 70124) 1.0L cool on-column injection of petroleum wax. Conc.: 0.1% w/w in cyclohexane Oven temp.: 50C to 400C @ 10C/min. (hold 10 min.) Det. temp.: 400C Carrier gas: hydrogen Linear velocity: 60cm/sec. set @ 50C FID sensitivity: 64 x 10-11 AFS

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Hydrocarbons
Carnauba Wax Rtx-1 Petroleum Wax Rtx-1

683

5 2 3 4

1. 2. 3. 4. 5. 6. 7. 8. 9.

C24 C28 C32 C36 C40 C44 C48 C52 C56

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

8 1 9

min.

12

16

20
GC_PC00220

24

28

32

36

min.

12

16

20

24

28

32

36

40

GC_PC00221

15m, 0.53mm ID, 0.10m Rtx-1 (cat.# 10107) 0.1L direct injection of carnauba wax Conc.: approximately 80mg/mL Oven temp.: 75C (hold 2 min.) to 340C @ 15C/min. (hold 10 min.) Inj. & det. temp.: 340C Carrier gas: hydrogen Linear velocity: 80cm/sec. FID sensitivity: 32 x 10-11 AFS

30m, 0.53mm ID, 0.25m Rtx-1 (cat.# 10125) 1.5L direct injection, Uniliner liner Oven temp.: 200C to 340C @ 10C/min. Inj. & det. temp.: 340C Carrier gas: hydrogen Linear velocity: 80cm/sec. (flow rate: 10cc/min.) FID sensitivity: 128 x 10-11 AFS

Petroleum Wax (High Temperature) MXT-1

min. 0
GC_PC00223

44 15m, 0.53mm ID, 0.20m MXT-1 (cat.# 70108) 1.0L on-column injection of neat parafin wax in methylene chloride. Oven temp.: 100C to 400C @ 10C/min. (hold 20 min.). Inj. / det. temp.: 103C / 430C Injector type: HP cool on-column pressure programmable Carrier gas: hydrogen Linear velocity: 30cm/sec. FID sensitivity: 2.56 x 10-11 AFS

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684

Hydrocarbons
Hydrocarbons, C44-C100 MXT-1HT Sim Dist

tech tip
Program your Agilent 5890 or 6890 GC to 430C at 60C/min., using a GC Racer! See page 149 for more information.

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

MXT-1HT Sim Dist 5m, 0.53mm ID, 0.10m (cat.# 70100) Sample: Polywax 1000 (cat.# 36227) Solvent: carbon disulfide Sample size: 0.2L Instrument: Agilent 5890 GC w/GC Racer* Injector: on-column (track oven) Carrier gas: hydrogen, constant pressure (1.0psi) Detector: FID/430C Oven temp.: 40C to 430C @ 60C/min. (hold 30 min.) *Manufactured by Zip Scientific, distributed by Restek Corporation.

GC_PC00543

Bleed Profile MXT-1HT Sim Dist

Hydrocarbons, C30-C110 MXT-1HT Sim Dist


C80

60

30

C50

C100

40

430C
C40 C44

C60

50

C70

70

C90

pA

20 10 0 0 10 20 30 40 min.

C30

GC_PC00527

20

30

40

50

C110

min.

GC_PC00530

5m, 0.53mm ID, 0.10m MXT-1HT Sim Dist(cat.# 70100) Oven temp.: 40C to 430C @ 10C/min. (hold 30 min.) Injector: on-column (track oven) Carrier gas: helium (constant pressure) Head pressure: 1.0psi Linear velocity: 60cm/sec. Flow rate: 7.8mL/min. Det.: FID @ 430C Make-up gas flow: 40cc/min.

5m, 0.53mm ID, 0.10m MXT-1HT Sim Dist (cat.# 70100) 0.2L Polywax 1000 standard (cat.# 36227) Solvent: carbon disulfide Oven temp.: 40C to 430C @ 10C/min. (hold 30 min.) Injector: on-column (track oven) Carrier gas: helium (constant pressure) Head pressure: 1.0psi Linear velocity: 60cm/sec. Flow rate: 7.8mL/min. Det.: FID @ 430C Make-up gas flow: 40cc/min.

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Hydrocarbons (Simulated Distillation)


Hydrocarbons, C44-C100 MXT-1HT Sim Dist
(fast GC)

685

Hydrocarbons, C10-C44 MXT-1HT Sim Dist

C11

C10 C9

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

C12 C14 C16 C18

C20

C24

C36

C28

GC_PC00531

C32

C40

C44 25 min.

10

15

20

GC_PC00529

5m, 0.53mm ID, 0.10m MXT-1HT Sim Dist (cat.# 70100) 0.2L injection of Polywax 1000 Solvent: carbon disulfide Oven temp.: 40C to 430C @ 60C/min. (hold 25 min.) Injector: on-column (track oven) Carrier gas: helium (constant pressure) Head pressure: 1.0psi Linear velocity: 60cm/sec. Flow rate: 7.8mL/min. Det.: FID/430C Make up gas flow: 40cc/min.

5m, 0.53mm ID, 0.10m MXT-1HT Sim Dist (cat.# 70100) 0.2L hydrocarbon standard (cat.# 31222) Solvent: carbon disulfide Oven temp.: 40C to 430C @ 10C/min. (hold 30 min.) Injector: on-column (track oven) Carrier gas: helium (constant pressure) Head pressure: 1.0psi Linear velocity: 60cm/sec. Flow rate: 7.8mL/min. Det.: FID @ 430C Make-up gas flow: 40cc/min.

Sim Dist, High-Temperature MXT-1 Sim Dist


(calibration)
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17.
10

Sim Dist, High-Temperature MXT-500 Sim Dist


C6 C7 C8 C9 C10 C11 C12 C14 C16 C18 C20 C24 C28 C32 C36 C40 C44

5 6

7 8

4 3 2

20 24 min.
11 12 13 14 15 16 17

28

32

36

40

44

48

52

56

60

64

68

GC_PC00225

min.

12
GC_PC00224

16

20

24

6m, 0.53mm ID, 0.15m MXT -1 Sim Dist (cat.# 70101) Wet needle on-column injection of ASTM D2887 standard. Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: -12C to 430C @ 20C/min. -17C to 433C/430C hydrogen 40cm/sec. 128 x 10-11 AFS

6m, 0.53mm ID, 0.15m MXT-500 Sim Dist (cat.# 70104) cold on-column injection of Polywax 655 in CS2 Oven temp.: 40C to 430C @ 6C/min. Carrier gas: helium Linear velocity: 40cm/sec. FID sensitivity: 2 x 10-11AFS

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686

Hydrocarbons (Simulated Distillation)


Sim Dist, ASTM D-2887 (C5 to C44 Standard) Rtx-2887 Column
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18.
12 13 14 15 16 17 18

Sim Dist, ASTM D-2887 (Reference Gas Oil #1) Rtx-2887

234 5 6 7 8 9 1

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

10

11

pentane hexane heptane octane nonane decane undecane dodecane tetradecane hexadecane octadecane eicosane tetracosane octacosane dotricontane hexatricontane tetracontane tetratetracontane

min.

10
GC_PC00226

15

20

min.

10
GC_PC00227

15

20

10m, 0.53mm ID, 2.65m Rtx-2887 (cat.# 10199) 1.0L direct injection of a 0.1 to 0.01 wt % hydrocarbon standard in carbon disulfide Oven temp.: 35C to 360C @ 15C/min. (hold 5 min.) Inj. & det. temp.: 360C Carrier gas: nitrogen Linear velocity: 112cm/sec. (15mL/min.)

10m, 0.53mm ID, 2.65m Rtx-2887 (cat.# 70199) 1.0L direct injection of a 0.1 to 0.01 wt % hydrocarbon standard in carbon disulfide. Oven temp.: 35C to 360C @ 15C/min. (hold 5 min.) Inj. & det. temp.: 360C Carrier gas: nitrogen Linear velocity: 112cm/sec. (15mL/min.)

Sim Dist, ASTM D-2887 Rtx-1 SimDist 2887


12 3 4 5 6 7 8 9 10 11

12

13

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18.

pentane hexane heptane octane nonane decane undecane dodecane tetradecane hexadecane octadecane eicosane tetracosane octacosane dotricontane hexatricontane tetracontane tetratetracontane

14

15

16

17

18

min.

10
GC_PC00228

20

30

25" x 1/8" x 2mm ID Rtx-1 SimDist 2887, SilcoSmooth stainless steel (cat.# 80000) 1.0L direct injection, 112% (w/w) each component Oven temp.: 35C to 350C @ 10C/min. (hold 5 min.) Inj. & det. temp.: 350C Carrier gas: helium @ 25mL/min. FID sensitivity: 256 x 10-11 AFS cat.# 31674 (1% each listed analyte in CS2) and cat.# 31675 (5% each, neat) meet requirements of ASTM D2887-01.

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Hydrocarbons (Simulated Distillation)


Sim Dist, ASTM D-3710 Rtx-1 SimDist 2887
(calibration)
4 5 6 7 8 9 10 11 12 13 14 15 16

687

17

18

19

20

21

1 2 3

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21.

n-propane 2-methyl propane n-butane 2-methylbutane n-pentane 2-methylpentane n-hexane 2,4-dimethylpentane n-heptane toluene n-octane p-xylene n-propylbenzene n-decane n-butylbenzene n-dodecane n-tridecane n-tetradecane n-pentadecane n-hexadecane n-heptadecane

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

min.

10
GC_PC00229

15

20

25" x 1/8" OD x 2mm ID Rtx-1 SimDist 2887, SilcoSmooth stainless steel (cat.# 80000) D-3710 Calibration Mix, C3, C4, C16, & C17 added Oven temp: -30C to 250C @ 10C/min. Inj./det. temp.: 250C / 300C Carrier gas: helium @ 25mL/min. FID sensitivity: 256 x 10-11 AFS

Sim Dist, ASTM D-3710 (Gasoline) Rtx-1 SimDist 2887

10

11

6 5

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.


12

n-propane 2-methyl propane n-butane 2-methylbutane n-pentane 2-methylpentane n-hexane 2,4-dimethylpentane n-heptane toluene p-xylene n-propylbenzene n-decane n-butylbenzene

7 2 8 14 9 13

25" x 1/8" OD x 2mm ID Rtx-1 SimDist 2887, SilcoSmooth stainless steel (cat.# 80000) 1.0L direct injection of unleaded gasoline (ASTM D-2887) Oven temp: -30C to 250C @ 10C/min. Inj./det. temp.: 250C/300C Carrier gas: helium @ 25mL/min. FID sensitivity: 256 x 10-11 AFS 15

min. 0

5
GC_PC00230

10

Phone: 800-356-1688 or 814-353-1300 www.restek.com

688

Sulfur Compounds
Sulfur in Gasoline Rtx-1
6

Sulfur in Naphtha by AED Rtx-1


1. 2. 3. 4. 5. hydrogen sulfide thiophene 2-methylthiophene 3-methylthiophene 2-ethylthiophene

1. 2. 3. 4. 5. 6. 7. 8.

thiophene 2-methylthiophene 3-methylthiophene 2-ethylthiophene alkylthiophenes benzothiophene methylbenzothiophenes dimethylbenzothiophenes


7

3 4 5 1 5 8 2

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

3 1 2

min. min. 4 8 12 16
GC_PC00198

10
GC_PC00199

20

20

24

28

30m, 0.32mm ID, 4.0m Rtx-1 (cat.# 10198 ) 1.0L split injection of naphtha containing 500ppm total sulfur 30m, 0.32mm ID, 4.0m Rtx -1 (cat.# 10198) 1.0L split injection of gasoline containing 300ppm total sulfur

Oven temp.: Inj. & det. temp.: Det.: Carrier gas: Linear velocity: Split ratio:

40C (hold 3 min.) to 275C @ 10C/min. (hold 5 min.) 275C SCD helium 70cm/sec. (flow rate: 2.5mL/min.) 10:1

Oven temp.: Inj. & det. temp.: Det.: Carrier gas: Linear velocity: Split ratio:

35C to 275C @ 10C/min. (hold 5 min.). 275C AED (181nm) helium 24cm/sec. (flow rate: 0.8mL/min.) 10:1

Sulfur Dioxide ShinCarbon ST


(micropacked)

Sulfur Compounds Rtx-1

1. sulfur dioxide
5 6 8 9 7 3 2 10 11 14 4 min. 0 4 GC_PC00200 8 12 13

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

hydrogen sulfide sulfur dioxide & carbonyl sulfide methyl mercaptan ethyl mercaptan carbon disulfide dimethyl sulfide 2-propyl mercaptan allyl mercaptan 1-propyl mercaptan ethyl sulfide butyl mercaptan dimethyl disulfide allyl sulfide propyl sulfide butyl sulfide & allyl disulfide

ShinCarbon ST 100/120 mesh (cat.# 19808) 2 meter x 1mm ID Silcosteel Micropacked column Sample: 100ppm sulfur dioxide in helium Inj.: 10L Inj. temp.: 100C Carrier gas: helium Flow rate: 10mL/min. Oven temp.: 150C Det.: HID @ 200C

15

12

free literature
For more information, request lit. cat.# 59519A

60m, 0.53mm ID, 7.0m Rtx-1 (cat.# 10193) 100L direct injection of sulfur compounds Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: Det.: 50C to 200C @ 15C/min. 50C / 230C helium 30cm/sec. set @ 50C FPD

GC_PC00674

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Sulfur Compounds
Sulfur Compounds Rt-XLSulfur
A B 1

689

D E

sulfurs 1. hydrogen sulfide 2. carbonyl sulfide 3. methyl mercaptan 4. ethyl mercaptan 5. dimethyl sulfide 6. dimethyl disulfide hydrocarbons A. methane B. ethane C. propylene D. propane E. isobutane F. butane G. isopentane H. pentane I. hexane
I 6

Searching for a chromatogram?

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4/5 3 2 C G H

G C A P P L I C AT I O N S | P E T R O L E U M & P E T R O C H E M I C A L S

min.

6
GC_PC00436

10

1m, 0.75mm ID Rt-XLSulfur micropacked column (cat.# 19806) Conc.: 50ppb each Oven temp.: 60C to 230C @ 15C/min. Carrier gas: helium Flow rate: 9mL/min. Det.: SCD/FID Sulfur standards courtesy of DCG Partnership 1 Ltd., Pearland, TX.

Sulfur Impurities in Ethylene Rt-Sulfur

Sulfur Impurities in Propylene Rt-Sulfur


1

1. hydrogen sulfide 2. carbonyl sulfide

1. carbonyl sulfide 2. propylene

ethylene

2 2

min.

10 GC_PC00202

15

20 min. 5 10 GC_PC00203 15 20

2m x 1/8" x 2mm Rt-Sulfur (cat.# 80252) 1cc injection of sulfur compounds Oven temp.: Det.: Carrier gas: Flow rate: 40C to 100C @ 5C/min. FPD (sensitivity: range 1) helium 20mL/min.

2m x 1/8" x 2mm Rt-Sulfur (cat.# 80252) 400L injection Oven temp.: Det.: Carrier gas: Flow rate: 60C to 100C @ 5C/min. (hold 15 min.) FPD (sensitivity: range 3) helium 20mL/min.

Phone: 800-356-1688 or 814-353-1300 www.restek.com

690

Antidepressants; Antihistamines
Underivatized Antidepressants (Basic Drugs) Rtx-1701

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

3 5 2 4 7 6 8

1. 2. 3. 4. 5. 6. 7. 8.

amitriptyline trimipramine imipramine nortriptyline doxepin desipramine maprotyline clomipramine

15m, 0.25mm ID, 0.25m Rtx-1701 (cat.# 12020) 1.0L split injection of antidepressants Conc.: 25ng/component Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 225C 250C / 260C helium 30cm/sec. set @ 225C 2.56 x 10-10 AFS 40:1

min.

3 GC_PH00264

Underivatized Antihistamines (Basic Drugs) Rtx-5 Amine

4 6 7 2 3

8 9

11

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

phenylpropanolamine ephedrine pseudoephedrine pheniramine diphenhydramine doxylamine phenyltoloxamine methapyrilene chlorpheniramine brompheniramine triprolidine

10

30m, 0.32mm ID, 1.0m Rtx-5 Amine (cat.# 12354) 1.0L split injection of antihistamines. Conc.: 1000ng/L Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 130C (hold 5 min.) to 305C @ 10C/min. (hold 5 min.) 305C hydrogen 43cm/sec. set @ 130C 6.4 x 10-11 AFS 50:1

min.

10

15
GC_PH00247

20

25

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Antiepileptics
Underivatized Antiepileptics Rtx-20
1 11

691

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

15m, 0.32mm ID, 0.50m Rtx-20 (cat.# 10336) 1.0L split injection of antiepileptic drugs Conc.: 1000ng/L
6 3 4 10 7 5 8 9 12

Oven temp.: Inj. / det. temp.: Det.: Carrier gas: Linear velocity: FID sensitivity: Split ratio:

150C to 280C @ 7C/min. (hold 5 min.) 250C / 270C FID helium 30cm/sec. set @ 150C 1.28 x 10-10 AFS 30:1

min.

10 GC_PH00265

15

20

Underivatized Antiepileptics Rtx-1701

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

valproic acid ethosuximide methsuximide phensuximide desmethyl methsuximide mephenytoin ethotoin PEMA phenobarbital primidone carbamazepine diphenylhydantoin

1 11

15m, 0.32mm ID, 0.50m Rtx-1701 (cat.# 12036) 1.0L split injection of antiepileptic drugs Conc.: 1000ng/L
3 2 4 7 8 9 10 5 12 6

Oven temp.: Inj. / det. temp.: Det.: Carrier gas: Linear velocity: FID sensitivity: Split ratio:

150C to 280C @ 7C/min. (hold 5 min.) 250C / 270C FID helium 30cm/sec. set @ 150C 1.28 x 10-10 AFS 30:1

min.

10 GC_PH00266

15

20

Phone: 800-356-1688 or 814-353-1300 www.restek.com

692

Barbiturates
Underivatized Barbiturates (Acidic/Neutral Drugs) Rtx-35
13 11

8 4 5 6 7 10 12

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

1 2

16

15 14

min.

10 GC_PH00262

15

20

30m, 0.53mm ID, 1.0m Rtx -35 (cat.# 10455) 1.0L splitless injection of acidic/neutral drugs Conc.: 50g/mL Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Splitless hold time: 100C to 280C @ 10C/min. (hold 5 min.) 250C helium 40cm/sec. set @ 100C 5.12 x 10-10 AFS 0.5 min. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.
15 11

Underivatized Barbiturates (Acidic/Neutral Drugs) Rtx-1701


13

ethosuximide barbital methyprylon aprobarbital butalbital amobarbital pentobarbital secobarbital meprobamate carisoprodal glutethimide phenobarbital methaqualone primidone carbamazepine diphenylhydantoin

3 8 5 4 2 9 67 10 14 12 16

min.

10 GC_PH00263

15

20

15m, 0.53mm ID, 0.50m Rtx-1701 (cat.# 12037) 1.0L splitless injection of acidic/neutral drugs 50g/mL concentration Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Splitless hold time: 100C to 280C @ 7C/min. 250C / 275C helium 40cm/sec. set @ 100C 5.12 x 10-10 AFS 0.5 min.

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Barbiturates; Basic Drugs


Underivatized Barbiturates (Acidic/Neutral Drugs) Rtx-35
7

693

Separation optimized using Pro ezGC software! See page 449.

10

11

4 3 1 2 5 6 8

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

barbital aprobarbital butalbital amobarbital talbutal pentobarbital methohexital secobarbital thiopental hexobarbital mephobarbital phenobarbital

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

12

min.

6 GC_PH00267

10

30m, 0.32mm ID, 0.50m Rtx-35 (cat.# 10439) 1.0L split injection of barbiturates Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split vent: 210C (hold 2 min.) to 300C @ 7C/min. (hold 2 min.) 300C helium 35cm/sec. set @ 210C 5.12 x 10-10 AFS 30:1

Underivatized Mixed Basic Drugs Rtx-200

3,5

28,29

14

Analysis on Rtx-5 and Rtx-35 columns: page 694.


8

11 15 13 9 6 2 10 7 4 18 12 16 19 17

22 20,25

31,32 37 21 24 30 35

27 34

33

38

36

1 23 26

min.

10

20

30 GC_PH00237

40

50

60

30m, 0.25mm ID, 0.25m Rtx-200 (cat.# 15023) 1.0L split injection of a basic drug sample (1mg/mL) Conc.: 1000ng/L Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 100C to 325C @ 4C/min. (hold 10 min.) 250C / 320C helium 30cm/sec. set @ 100C 1.28 x 10-10 AFS 50:1

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

nicotine benzocaine cotinine meperidine caffeine benzphetamine ketamine diphenhydramine lidocaine phenyltoloxamine tripelennamine phenothiazine dextromethorphan methadone amitriptyline trimipramine tetracaine pyrilamine medazepam bupivacaine scopolamine codeine morphine diazepam chlorpromazine temazepam flunitrazepam bromazepam prazepam acetopromazine flurazepam papaverine clonazepam haloperidol alprazolam triazolam thioridazine trazodone

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694

Basic Drugs
Underivatized Mixed Basic Drugs Rtx-5
3

14 22 8 13 11 15 30 25 20 21 24 17 16 10 19 28 27 32 31 33 35 34 38 36 29 37

Analysis on Rtx-200 column: page 693

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

4 9 6 2 7 1 5

12

18 26 23

min.

10

20

30 GC_PH00235

40

50

60

30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 1.0L split injection of a basic drug sample. Conc.: 1000ng/L Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 100C to 325C @ 4C/min. (hold 10 min.) 250C / 320C helium 30cm/sec. set @ 100C 1.28 x 10-10 AFS 50:1

Underivatized Mixed Basic Drugs Rtx-35

22

29 8 11 18,20 12 4 6 2 7 10 13 9 16 19 27 31 28 17 21 25 24 32 34 36 38 14 15 30 35 37

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38.

nicotine benzocaine cotinine meperidine caffeine benzphetamine ketamine diphenhydramine lidocaine phenyltoloxamine tripelennamine phenothiazine dextromethorphan methadone amitriptyline trimipramine tetracaine pyrilamine medazepam bupivacaine scopolamine codeine morphine diazepam chlorpromazine temazepam flunitrazepam bromazepam prazepam acetopromazine flurazepam papaverine clonazepam haloperidol alprazolam triazolam thioridazine trazodone

5 1 23 26 33

min.

10

20

30 GC_PH00236

40

50

60

30m, 0.25mm ID, 0.25m Rtx-35 (cat.# 10423) 1.0L split injection of a basic drug sample Conc.: 1000ng/L Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 100C to 325C @ 4C/min. (hold 10 min.) 250C / 320C helium 30cm/sec. set @ 100C 1.28 x 10-10 AFS 50:1

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Basic Drugs
Underivatized Benzodiazepines (Basic Drugs) Rtx-200

695

5,6 1 3 12 7 4 2 8 9 10 11 13

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

medazepam lorazepam diazepam desmethyl diazepam bromazepam prazepam temazepam flurazepam clobazam flunitrazepam clonazepam alprazolam triazolam

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

min.

4 GC_PH00268

10

15m, 0.32mm ID, 0.25m Rtx-200 (cat.# 15021) 1.0L split injection of benzodiazepines Conc.: 15ng/component Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 225C to 325C @ 8C/min. 250C / 320C helium 35cm/sec. set @ 225C 5.12 x 10-10 AFS 60:1

Underivatized Phenothiazines (Basic Drugs) Rtx-5


Separation optimized using Pro ezGC software!
5,6 1 2 3 7 8 9 10

See page 449.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

phenothiazine promethazine trimeprazine promazine chlorprothixene chlorpromazine trifluoperazine acetopromazine prochlorperazine thioridazine

min.

10 GC_PH00269

15

20

25

15m, 0.32mm ID, 0.50m Rtx-5 (cat.# 10236) 1.0L split injection of phenothiazines Conc.: 2000ng/L Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 200C to 325C @ 5C/min. 250C / 315C helium 25cm/sec. set @ 200C 2.56 x 10-10 AFS 30:1

Phone: 800-356-1688 or 814-353-1300 www.restek.com

696

Basic Drugs
Underivatized Cold Medications (Basic Drugs) Rtx-5 Amine
4 6 8 10 5 7 1 3 9

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

phenylpropanolamine phenylephrine guaifenesin pheniramine phenyltoloxamine chlorpheniramine brompheniramine dextromethorphan pyrilamine codeine hydrocodone

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

11

min.

8 GC_PH00469

10

12

14

16

30m, 0.53mm ID, 1.0m Rtx-5 Amine (cat.# 12355) Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Sample size: Split vent flow: Split ratio: 175C to 280C @ 10/min. (hold 5.5 min.) 250C/280C helium 40cm/sec. 1L 88mL/min. 20:1

Underivatized Cold Medications (Basic Drugs) Rtx-35 Amine

Rtx-35 Amine 30m, 0.25mm ID, 0.50m (cat.# 11338) 1.0L split injection of underivatized cold medicines Conc.: 1000ng/L Inj. temp: 250C Carrier gas: helium Linear velocity: 30cm/sec. Oven temp.: 250C to 300C @ 7C/min. (hold 7 min.) Det.: MSD Scan range: 40450amu Ionization: EI Mode: scan

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

guaifenesin pheniramine phenyltoloxamine chlorpheniramine brompheniramine dextromethorphan pyrilamine triprolidine codeine hydrocodone

GC_PH00575

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Chiral Analyses
Underivatized Ibuprofen Rt-DEXsm Underivatized Thalidomide Rt-DEXcst

697

(+/-)ibuprofen

(+/-)thalidomide

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

min.

8
GC_PH00242

min.

20
GC_PH00243

25

30m, 0.32mm ID, 0.25m Rt-DEXsm (cat.# 13104) On-column injection Conc.: 125ng each enantiomer Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Det.: Split ratio: 175C to 200C @ 2C/min. 200C/230C helium 60cm/sec. GC-FID 13:1 using cup splitter liner (cat.# 20709)

30m, 0.32mm ID, 0.25m Rt-DEXcst (cat.# 13102) On-column injection Conc.: approximately 15ng each enantiomer Oven temp.: Inj./det. temp.: Carrier gas: Linear velocity: Detector type: Split ratio: 200C to 230C @ 1C/min. 200C/230C hydrogen 80cm/sec. GC/FID 13:1 using cup splitter liner (cat.# 20709)

a plus 1 story
Ginny and her teammates completed a system upgrade that has improved the efficiency and quality of procedures and processing. Members of the team also dedicated extensive time to preparing and testing before, during, and after the upgrade with some members working nearly two weeks straight, at all hours of the day, including Friday nights, Saturdays, and Sundays.

Ginny Esh, Brian Condo, Karen Urbanik, Steve Kreiser, Christial Morgan, Liz Hamilton, Danielle Hicks, Jim Steyers, Sean Nolan

Phone: 800-356-1688 or 814-353-1300 www.restek.com

698

Chiral Analyses
Fenafluramine (TFAA Derivative) Rt-DEXcst
1

1. 2. 3. 4.

(+)-fenfluramine - TFAA (-)-fenfluramine - TFAA (+)-norfenfluramine - TFAA (-)-norfenfluramine - TFAA

30m, 0.32mm ID, 0.25m Rt-DEXcst (cat.# 13102) On-column injection, 25ng/enantiomer
4

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

Oven temp.: Carrier gas: Linear velocity: Det.:

90C (hold 1 min.) to 200C @ 2C/min. (hold 3 min.) hydrogen 80cm/sec. set @ 60C FID set @ 220C

min.

15

20

25 GC_PH00244

30

35

40

Underivatized Barbiturates Rt-DEXcst

1. (+/-)-hexobarbital 2. (+/-)-mephobarbital

30m, 0.32mm ID, 0.25m Rt-DEXcst (cat.# 13102) On-column conc.: 25ng/enantiomer
2 1

Oven temp.: Carrier gas: Linear velocity: Det.:

60C (hold 1 min.) to 220C @ 3C/min. hydrogen 80cm/sec. set @ 60C FID set @ 220C

min.

10

20 GC_PH00245

30

40

50

Amphetamine and Methamphetamine (TFAA Derivatives) Rt-DEXcst

1. 2. 3. 4.

(+)methamphetamine - TFAA (-)methamphetamine - TFAA (+)amphetamine - TFAA (-)amphetamine - TFAA

30m, 0.25mm ID, 0.25m Rt-DEXcst (cat.# 13103) Oven temp.: 120C (hold 1 min.) to 175C @ 1.5C/min. Carrier gas: helium Linear velocity: 25cm/sec. set @ 120C Det.: MSD set @ 220C.

min.

10

12

14

16

18 GC_PH00246

20

22

24

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Organic Volatile Impurities / Residual Solvents


Organic Volatile Impurities Rtx-5
16,17

699

22

21

11,12

18

15 1 2 3,4 5 6 8 14 7 9 13 23 10 19 20

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23.

methanol ethanol acetone acetonitrile isopropanol ether tert-butanol methylene chloride n-propanol methyl ethyl ketone sec-butanol hexane ethyl acetate chloroform tetrahydrofuran benzene cyclohexane heptane trichloroethylene 1,4-dioxane pyridine toluene dimethylformamide

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

min.

8
GC_PH00256

10

12

14

16

30m, 0.53mm ID, 5.0m Rtx-5 (cat.# 10279) 0.5L split injection of residual solvents Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 35C (hold 7 min.) to 240C @ 15C/min. 180C / 260C helium 25cm/sec. set @ 35C 2.56 x 10-10 AFS 20:1

Organic Volatile Impurities Rtx-1301


17 21

22

18 16 13 1 2 3 4 8 5 6 7 15 9 10 11 12 19 23 14 20

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23.

methanol ethanol ether acetone isopropanol acetonitrile methylene chloride tert-butanol hexane n-propanol methyl ethyl ketone ethyl acetate tetrahydrofuran sec-butanol chloroform cyclohexane benzene heptane trichloroethylene 1,4-dioxane pyridine toluene dimethylformamide

min.

10
GC_PH00257

12

14

16

18

30m, 0.53mm ID, 3.0m Rtx-1301 (cat.# 16085) 0.5L split injection of residual solvents. Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 35C (hold 8 min.) to 240C @ 20C/min. 180C / 260C helium 25cm/sec. set @ 35C 1.28 x 10-10 AFS 30:1

Phone: 800-356-1688 or 814-353-1300 www.restek.com

700

Organic Volatile Impurities / Residual Solvents


Organic Volatile Impurities (USP 467) Rtx-G27 Organic Volatile Impurities (USP 467) Rtx-G43
1. methylene chloride 2. chloroform 3. benzene 4. trichloroethylene 5. 1,4-dioxane

3 1

1 3

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

4 2 5 2

4 5

min.

10
GC_PH00258

12

14

16

18

min.

10

12

14

16

GC_PH00259

30m, 0.53mm ID, 5.0m Rtx-G27 with 5m phenylmethyl Integra-Guard guard column (cat.# 10279-126) Headspace injection of USP 467 Calibration Mix (cat.# 36004) prepared at limit test concentrations Oven temp.: 35C (hold 5 min.) to 175C @ 8C/min., to 260C @ 35C/min. Inj./det. temp.: 180C/260C FID sensitivity: 1 x 10-11 AFS Carrier gas: helium, 35cm/sec. set @ 35C Split ratio: 2:1

30m, 0.53mm ID, 3.0m Rtx-G43 with 5m phenylmethyl Integra-Guard guard column (cat.# 16085-126) Headspace injection of USP 467 Calibration Mix (cat.# 36004) prepared at limit test concentrations Oven temp.: Inj./det. temp.: FID sensitivity: Carrier gas: Split ratio: 40C (hold 20 min.) to 240C @ 35C/min. (hold 10 min.) 180C/260C 1.25 x 10-11 AFS helium, 35cm/sec. set @ 35C 2:1

Organic Volatile Impurities Rtx-G27


18,17,22 25

Organic Volatile Impurities Rtx-G43


25

18 20 12,10 4 8,6,7 21 3 5 19 9 11 13 15 14 16 23 24 12 21 6 9 7 8 12 13 11 14 16 15 17 19 3,4 5 10 20 21 22 23 24

min.

10

12

14

16

18

20

22

min.

10
GC_PH00261

12

14

16

18

GC_PH00260

30m, 0.53mm ID, 5.0m Rtx-G27 with 5m phenylmethyl Integra-Guard guard column (cat.# 10279-126)

30m, 0.53mm ID, 3.0m Rtx-G43 with 5m phenylmethyl Integra-Guard guard column (cat.# 16085-126)

Headspace injection of common solvents for pharmaceutical processing. Prepared to equal about 500ppm in the bulk pharmaceutical. Samples shaken and heated at 90C for 15 minutes, 1mL headspace injection. Oven temp.: Inj./det. temp.: FID sensitivity: Carrier gas: Split ratio: 1. 2. 3. 4. 5. 6. 7. 8. 9. 35C (hold 10 min.) to 100C @ 5C/min., to 240C @ 25C/min. (hold 5 min.) 220C/240C 1.05 x 10-11 AFS helium, 35cm/sec. set @ 35C 2:1 10. 11. 12. 13. 14. 15. 16. 17. 18.

ethylene oxide methanol ethanol diethyl ether 1,1-dichloroethene acetone isopropanol acetonitrile methylene chloride

n-hexane n-propanol methyl ethyl ketone ethyl acetate tetrahydrofuran chloroform 1,1,1-trichloroethane carbon tetrachloride benzene

19. 20. 21. 22. 23. 24. 25.

1,2-dichloroethane heptane trichloroethylene n-butanol 1,4-dioxane pyridine toluene

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Organic Volatile Impurities / Residual Solvents; Steroids


European Pharmacopoeia Class 1 and Class 2 Solvents Rtx-1301
24,25

701

9,10 6 19

22,23 4 1 5 2 3 7 8 16 11 12 13,14 15 17 18 20 21 27 26 28

10

12

14

16

18

20

22

24

26

28

30

32

34

GC_PH00553

30m, 0.53mm ID x 3.0m Rtx-1301 (cat.# 16085) Headspace injection of 28 Class 1 and 2 residual solvents for pharmaceutical processing. Prepared at the regulatory limit concentration, using samples shaken and heated at 80C for 15 minutes, 1mL headspace injection. Oven temp.: Inj./det. temp.: FID sensitivity: Carrier gas: Split ratio: 40C (hold 20 min.) to 240C @ 10C/min. (hold 20 min.) 200C/250C 1.1 x 10-11 AFS hydrogen @ 35cm/sec. 2:1

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. 23. 24. 25. 26. 27. 28.

methanol 1,1-dichloroethene acetonitrile methylene chloride (dichloromethane) hexane (C6) cis-1,2-dichloroethene nitromethane chloroform cyclohexane 1,1,1-trichloroethane carbon tetrachloride benzene 1,2-dimethoxyethane 1,2-dichloroethane trichloroethylene (1,1,2-trichlorethene) methylcyclohexane 1,4-dioxane pyridine toluene 2-hexanone chlorobenzene DMF ethylbenzene m-xylene p-xylene o-xylene N,N-dimethylacetamide 1,2,3,4-tetrahydronaphthalene

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

Underivatized Steroids, Anabolic Rtx-5


1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 5-androstene-3,17-diol 17-methyl-5-androstene-3,17-diol 5-androstan-17-ol-3-one 19-nortestosterone 17-methylandrostan-17-ol-3-one mesterolone testosterone 17-methyltestosterone 1-dehydrotestosterone 1-dehydro-17-methyltestosterone bolasterone oxymethalone 19-nortestosterone-17-propionate testosterone propionate fluoxymesterone 4-chlorotestosterone-17-acetate testosterone-17-cypionate 1-dehydrotestosterone benzoate 1-dehydrotestosterone undecylenate

10,11

3 1 5 8 7 6 9 15 4 12 16 13 14 17 18 19

min.

10 GC_PH00255

12

14

16

18

30m, 0.25mm ID, 0.10m Rtx -5 (cat.# 10208) 0.5L split injection of anabolic steroids Conc.: 1000ng/L Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 180C to 340C @ 10C/min. (hold 3 min.) 280C / 340C helium 35cm/sec. set @ 180C 1.28 x 10-10 AFS 50:1

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702

Sympathomimetic Amines
Underivatized Sympathomimetic Amines (Basic Drugs) Rtx-35 Amine
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. amphetamine methamphetamine N-ethylamphetamine p-methoxyamphetamine (PMA) p-methoxymethamphetamine (PMMA) methylenedioxyamphetamine (MDA) methylenedioxymethamphetamine (MDMA) methylenedioxyethylamphetamine (MDEA) HMMA MBDB

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

GC_PH00574

Rtx-35 Amine 30m, 0.25mm ID, 0.50m (cat.# 11338) 1.0L split injection of underivatized sympathomimetic amines Conc. 1000ng/L Inj. temp: 250C Carrier gas: helium Linear velocity: 30cm/sec. Oven temp.: 150C to 240C @ 7C/min. Det.: MSD Scan range: 40450amu Ionization: EI Mode: scan

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Sympathomimetic Amines
Underivatized Sympathomimetic Amines (Basic Drugs) Rtx-5 Amine
22

703

16 14 2 5 6 10 4 3 13 17 9 1 7 8 11,12 15 18 19 21

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

min.

7.5

10

12.5
GC_PH00438

15

17.5

20

30m, 0.25mm ID, 0.50m Rtx-5 Amine (cat.# 12338) split mode, split vent flow rate 45mL/min. Oven temp.: 100C to 310C @ 10C/min. Varian 3400 GC coupled with Varian Saturn 2000 MS detector Mass spectroscopy data collected using a scan range of 40 amu through 600 amu. Ionization performed in the EI Auto mode. 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20. 21. 22. phenylethylamine amphetamine phentermine methamphetamine fenfluramine mephentermine cathinone phenylpropanolamine methcathinone nicotine ephedrine pseudoephedrine phenmetrazine phendimetrazine methylenedioxyamphetamine diethylpropion methylenedioxymethamphetamine methylenedioxyethylamphetamine 4-methyl-2,5-dimethoxyamphetamine phenylephrine caffeine benzphetamine

Underivatized Sympathomimetic Amines (Basic Drugs) Rtx-200

1,2 15,20

4 11 3 8 12 13 9 19 17

7 10 16 14 5

22 21 18

min.

7.5

10

12.5
GC_PH00439

15

17.5

30m, 0.25mm ID, 0.50m Rtx-200 (cat.# 15038) split mode, split vent flow rate 45mL/min. Oven temp.: 100C to 310C @ 10C/min. Varian 3400 GC coupled with Varian Saturn 2000 MS detector Mass spectroscopy data collected using a scan range of 40 amu through 600 amu. Ionization performed in the EI Auto mode.

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704

Sympathomimetic Amines
Sympathomimetic Amines (TFAA Derivatives) (Basic Drugs) Rtx-5
1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

2,3

7 4 5

amphetamine - TFAA phentermine - TFAA phenylpropanolamine - TFAA ephedrine - TFAA methamphetamine - TFAA fenfluramine - TFAA pseudoephedrine - TFAA methylenedioxyamphetamine - TFAA methylenedioxymethamphetamine - TFAA methylphenidate - TFAA

G C A P P L I C AT I O N S | P H A R MAC E U T I C A L

10 1 6 8 9

min.

10

12
GC_PH00251

14

16

18

30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 1.0L splitless injection of derivatized sympathomimetic amines Conc.: approximately 2.5ng/L Oven temp.: Inj. temp.: Interface temp.: Det.: Ionization: Carrier gas: Linear velocity: Splitless hold time: 40C (hold 1 min.) to 150C @ 30C/min., to 300C @ 5C/min. 225C 275C MSD EI helium 20cm/sec. set @ 100C 1 min.

Sympathomimetic Amines (HFBA Derivatives) (Basic Drugs) Rtx-5


5 7

3 4 2

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

amphetamine - HFBA phentermine - HFBA phenylpropanolamine - HFBA ephedrine - HFBA methamphetamine - HFBA fenfluramine - HFBA pseudoephedrine - HFBA methylenedioxyamphetamine - HFBA methylenedioxymethamphetamine - HFBA methylphenidate - HFBA

1 6 9 8 10

min. 4

10
GC_PH00252

12

14

16

18

30m, 0.25mm ID, 0.25m Rtx-5 (cat.# 10223) 1.0L splitless injection of sympathomimetic amines Conc.: approximately 2.5ng/L. Oven temp.: Inj. temp.: Interface temp.: Det.: Ionization: Carrier gas: Linear velocity: Splitless hold time: 40C (hold 1 min.) to 150C @ 30C/min., to 300C @ 5C/min. 225C 275C MSD EI helium 20cm/sec. set @ 100C 1 min.

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Solvents
Solvent Mixture #1 Rtx-1
60m, 0.53mm ID, 3.0m Rtx-1 (cat.# 10188) 1.0L split injection of solvent mix #1 Oven temp.: Inj. / det. temp.: MSD: Carrier gas: Linear velocity: Split vent: 40C (hold 5 min.) to 285C @ 5C/min. 275C / 285C full scan helium 40cm/sec. 50mL/min.

705

32 33 34

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

17 12 27 15 4 9 5 6,7 8 1 3 16 18 10 11 13 14 20 19 21 23 24 31 26 22 25 30 28 37 36 38 39 35 29

min.

10

15

20

25

30

35 GC_CH00335

40

45

50

55

60

Refer to peak list on page 709.

Solvent Mixture #1 Rtx-200


60m, 0.53mm ID, 3.0m Rtx-200 (cat.# 15088) 1.0L split injection of solvent mix #1.
2

Oven temp.: Inj. / det. temp.: MSD: Carrier gas: Linear velocity: Split vent:

40C (hold 5 min.) to 285C @ 5C/min. 275C / 285C TIC mode helium 40cm/sec. 50mL/min.
17 34

33

39 12 19 15 23 13 26 9 4 1 6 11 10 5 14 28 8 22 18 25 36 37 38 27 29 24 32 31 35

min.

10

15

20

25

30

35 GC_CH00336

40

45

50

55

60

Refer to peak list on page 709. Phone: 800-356-1688 or 814-353-1300 www.restek.com

706

Solvents
Solvent Mixture #1 Stabilwax
60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of solvent mix #1 Oven temp.: Inj. / det. temp.: MS: Carrier gas: Linear velocity: Split vent: 40C (hold 5 min.) to 250C @ 5C/min. 275C / 285C full scan helium 40cm/sec. 50mL/min.

17

33

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

26 24 32 6,13 4 1 23 10 11 7 18 39 12 15 27 5 29 19 8 28 3 36 34 22,14 35 31 37 38 25 9

min.

10

20

30

40 GC_CH00337

50

60

70

Refer to peak list on page 709.

Solvent Mixture #2 Rtx-1


60m, 0.53mm ID, 3.0m Rtx-1 (cat.# 10188) 1.0L split injection of solvent mix #2
2

Oven temp.: Inj. / det. temp.: MS: Carrier gas: Linear velocity: Split vent:

40C (hold 5 min.) to 285C @ 5C/min. 275C / 285C full scan helium 40cm/sec. 51 50mL/min.

68 67 62 61

50 52 49 56 47 42 58 23 63 11 55 53 54 57 59 60 29 40 43 41 4 44 48

65

45,46

34 69 66 35

64

min.

10

15

20

25

30 GC_CH00338

35

40

45

50

55

Refer to peak list on page 709. Phone: 800-356-1688 or 814-353-1300 www.restek.com

Solvents
Solvent Mixture #2 Rtx-200
60m, 0.53mm ID, 3.0m Rtx-200 (cat.# 15088) 1.0L split injection of solvent mix #2 Oven temp.: Inj. / det. temp.: MS: Carrier gas: Linear velocity: Split vent: 40C (hold 5 min.) to 285C @ 5C/min. 275C / 285C full scan helium 40cm/sec. 50mL/min.
61 65

707

67 68 62,34

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

50 47 52 56 49 46 42 44 40 45 11 1 4 41 23 53 54 48 29 58 64 63 66 35 69 57 59

min.

10

15

20

25

30 GC_CH00339

35

40

45

50

55

Refer to peak list on page 709.

Solvent Mixture #2 Stabilwax


60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of solvent mix #2 Oven temp.: Inj. / det. temp.: MS: Carrier gas: Linear velocity: Split vent: 40C (hold 5 min.) to 250C @ 5C/min. 275C / 285C full scan helium 40cm/sec. 50mL/min.
68 62 61

67

56 65 47 52 42 49 46 45 53 29 4 11 35 23 40 54 44 58 57 48 59 34 64 63 66 55 50 41

min.

10

15

20

25

30

35

40

45

50

55

60

GC_CH00340

Refer to peak list on page 709. Phone: 800-356-1688 or 814-353-1300 www.restek.com

708

Solvents
Solvent Mixture #3 Rtx-1
60m, 0.53mm ID, 3.0m Rtx-1 (cat.# 10188) 1.0L split injection of solvent mix #3
2

Oven temp.: Inj. / det. temp.: MS: Carrier gas: Linear velocity: Split vent:

40C (hold 5 min.) to 285C @ 5C/min. 275C / 285C full scan helium 40cm/sec. 50mL/min.

102 99

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

96 90 87 89 85,86 73 84 83 76,77 78 70 1 71 72 74,75 4 35 79 80 81 82 88,11 94 23 91 92 95 98 101 29 34 93 97 100

min.

10

15

20

25 GC_CH00341

30

35

40

45

50

Refer to peak list on page 709.

Solvent Mixture #3 Rtx-200


60m, 0.53mm ID, 3.0m Rtx-200 (cat.# 15088) 1.0L split injection of solvent mix #3 Oven temp.: Inj. / det. temp.: MS: Carrier gas: Linear velocity: Split vent: 40C (hold 5 min.) to 285C @ 5C/min. 275C / 285C full scan helium 40cm/sec. 50mL/min.

99

102

92,87 93 90

100

89 84 80,11 73 83 77 72 1 70 4 76 74 82 78 75 81 79 86

85,91 98 34 95, 11 88 29

35

min.

10

15

20

25 GC_CH00342

30

35

40

45

Refer to peak list on page 709. Phone: 800-356-1688 or 814-353-1300 www.restek.com

Solvents
Solvent Mixture #3 Stabilwax
60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of solvent mix #3 Oven temp.: Inj. / det. temp.: MS: Carrier gas: Linear velocity: Split vent: 40C (hold 5 min.) to 250C @ 5C/min. 275C / 285C full scan helium 99 40cm/sec. 50mL/min.

709

102 100

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

87 86 90 91,34 93 85 98 92 89 80 78,73 11 1 4 72 23 76 81 70 95 75 74 83 79 84 29 82 84 88

min.

10

15

20

25 GC_CH00343

30

35

40

45

50

Components of solvent mixture #1, #2, #3 (see pages 705709 for chromatography)
1. pentane 2. methylene chloride 3. ethylene glycol 4. heptane 5. cyclopentanol 6. 3-hexanol 7. acetamide 8. 2-methyl-1-pentanol 9. furfuryl alcohol 10. butyl ether 11. nonane 12. cumene 13. ethyl amyl ketone 14. heptanol 15. butyl butanoate 16. 17. benzyl alcohol 18. dipropylene glycol 19. diethylbenzene 20. 21. 22. hexachloroethane 23. undecane 24. 1-nonanol 25. p-methoxyphenol 26. triethylene glycol 27. dodecane 28. undecanal 29. tridecane 30. 31. dodecanal 32. dicyclohexylamine 33. bis(2,2-methoxy)ethyl ether 34. pentadecane 35. heptadecane 36. octadecane 37. nonadecane 38. eicosane 39. acetyl tributyl citrate 40. 2-buten-1-ol 41. formamide 42. 3-pentanol 43. 1-nitropropane 44. dimethylformamide 45. 2-methyl-3-pentanol 46. toluene 47. ethyl chloroacetate 48. dimethylacetamide 49. p-xylene 50. sec-tetrachloroethane 51. benzaldehyde 52. o-chlorotoluene 53. 2,6-dimethyl-4-heptanone 54. 2-octanone 55. o-cresol 56. -methylbenzyl alcohol 57. 5-nonanone 58. nonanal 59. decanal 60. 61. 1-decanol 62. 1-undecanol 63. 2-dodecanone 64. 1-dodecanol 65. tetraethylene glycol 66. dibenzyl 67. diethyl phthalate 68. tributyl phosphate 69. diphenyl sulfone 70. allyl alcohol 71. 72. isopropyl acetate 73. benzene 74. 2-nitropropane 75. nitroethane 76. pentanal 77. 2-bromobutane 78. 1-chloropentane 79. cyclopentanone 80. 2-hexanol 81. butyl acetate 82. 2-ethyl-1-butanol 83. 3-ethyl-3-pentanol 84. 1,4-dichlorobutane 85. 2-methyl-2,4-pentanediol 86. butoxyethanol 87. 1,2,3-trichloropropane 88. 1,4-butanediol 89. methyl hexanoate 90. 1,2,4-trimethylbenzene 91. 2-ethyl-1-hexanol 92. dipentene/limonene 93. tetrahydrofurfuryl acetate 94. 95. decahydronaphthalene 96. 97. 98. 2-decanol 99. 1,2-bis(2-methoxyethoxy)ethane 100. 2-phenoxyethanol 101. 102. benzyl ether

applications Table of Contents


see pages 460-463

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710

Solvents
Solvents Rtx-200
12,13 19

18 17

16 9

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

3 4 6 7

14 15

10 8 5 11

2 1

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

methanol trichlorotrifluoroethane methylene chloride chloroform cyclohexane carbon tetrachloride acetone isobutyl alcohol acetonitrile benzene tetrahydrofuran trichloroethylene ethylene dichloride ethyl acetate methyl ethyl ketone toluene pyridine chlorobenzene methylisoamyl ketone

min.

12

16

20

24

28

32

GC_CH00349

85m, 0.53mm ID, 3.0m Rtx-200 (cat.# 50762) 0.1L direct injection of a solvent mixture Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: TCD sensitivity: 40C (hold 5 min.) to 200C @ 5C/min. (hold 10 min.) 250C / 270C helium 31cm/sec. range = 0.50, atten. = 4

Solvents Rtx-1701

Solvents Rtx-1701
2 4 5 7

1. water 2. 2-butanone 3. 2-butanol

1. 2. 3. 4. 5. 6. 7. 8.

acetaldehyde methanol acetone methyl acetate vinyl acetate cyclohexane ethyl acetate crotonaldehyde

3 2 3 6 8

min.

4 GC_CH00350

min.

4 GC_CH00351

30m, 0.53mm ID, 3.0m Rtx -1701 (cat.# 12085) 0.2L split injection

60m, 0.53mm ID, 1.5m Rtx-1701 (cat.# 12073) 0.4L direct injection of a solvent mixture Conc.: 2000 ppm Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C (hold 4 min.) to 100C @ 15C/min. (hold until last compound elutes) 250C hydrogen 40cm/sec. (flow rate: 5cc/min.) 16 x 10-11 AFS

Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: TCD sensitivity: Split ratio:

55C 225C helium 20cm/sec. 8 mV 40:1

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Solvents
Solvents Rtx-1
9,10,11 12 4 1 14,15

711

3 7 6 5 8 18 20

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

methanol methyl formate acetone pentane methylene chloride n-propyl alcohol methyl ethyl ketone sec-butyl alcohol ethyl acetate chloroform hexane tetrahydrofuran 1,1,1-trichloroethane isobutyl alcohol benzene n-butyl alcohol ethoxyethane toluene n-butyl acetate o-xylene

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

19

30m, 0.53mm ID, 5.0m Rtx-1 (cat.# 10179) 0.5mg/mL wet needle injection of a solvent mix Direct injection using a Uniliner liner Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C (hold 4 min.) to 110C @ 4C/min. to 175C @ 15C/min. (hold 5 min.) 250C hydrogen 80cm/sec. (flow rate: 10cc/min.) 64 x 10-11 AFS

13

16,17

min.

10 GC_CH00344

12

14

16

18

Solvents Stabilwax

10

1 11,12

5 8,9 14 19

7 6 13 4 15

16 18 17 20

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

pentane hexane methyl formate acetone tetrahydrofuran 1,1,1-trichloroethane ethyl acetate methyl ethyl ketone methanol methylene chloride chloroform benzene n-propyl alcohol toluene sec-butyl alcohol n-butyl acetate isobutyl alcohol n-butyl alcohol o-xylene ethoxyethane

30m, 0.25mm ID, 0.25m Stabilwax (cat.# 10623) 0.5L split injection of a solvent mixture Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio:
min. 2 4 6 GC_CH00345 8 10

40C (hold 4 min.) to 250C @ 5C/min. 250C hydrogen 40cm/sec. (flow rate: 3.2cc/min.) 16 x 10-11 AFS 40:1

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712

Solvents
Solvents Rtx-5
1 4 14 15

9,10 12

5 3

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18.

acetone acrylonitrile carbon disulfide impurity hexane methyl ethyl ketone ethyl acetate methyl Cellosolve tetrahydrofuran n-butyl alcohol isopropyl acetate heptane n-propyl acetate amyl alcohol toluene n-butyl acetate n-butyl acrylate Cellosolve acetate cyclohexanone

60m, 0.32mm ID, 3.0m Rtx-5 (cat.# 10287) 1.0L split injection of solvents collected on a charcoal tube and extracted in carbon disulfide Oven temp.:
13 7,8 16 17 11 2 18

Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity:

50C (hold 4 min.) to 120C @ 5C/min. (hold 20 min.) 300C hydrogen 40cm/sec. set @ 50C 128 x 10-12 AFS

Permission to publish this chromatogram granted by Kenda McCoy, Rexham Industrial.

min.

12 GC_CH00346

16

20

24

Volatile Solvents Rtx-Wax

2 3 4 5 6

1. 2. 3. 4. 5. 6. 7. 8.

acetaldehyde acetone ethyl formate ethyl acetate methanol ethanol n-propanol isobutanol

Searching for a chromatogram?

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min.

10 GC_CH00347

15

20

30m, 0.53mm ID, 1.0m Rtx-Wax (cat.# 12455) 0.1L split injection of volatile solvents Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 20C (hold 10 min.) to 100C @ 5C/min. 200C helium 40cm/sec. set @ 20C 8 x 10-11 AFS 10:1

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Solvents
Solvents Rtx-Volatiles
1 3 6 1 2 3

713

Solvents, Industrial Stabilwax-DA


4

1. 2. 3. 4. 5. 6. 7.

water methanol ethanol isopropanol ethyl acetate isopropyl acetate 4-methyl-2-pentanone

1. 2. 3. 4.

1,4-dioxane styrene -methylstyrene dipropylene glycol monomethylether 5. acrylic acid

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

2 4 5 7

min.

12

16

GC_CH00352 min. 4 8 12 GC_CH00353 16 20 24

60m, 0.53mm ID, 2.0m Rtx-Volatiles (cat.# 10905) 1.0L split injection of neat solvents Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: TCD sensitivity: TCD current: Split ratio: 40C (hold 2 min.) to 200C @ 5C/min. (hold 10 min.) 250C helium 20cm/sec. (flow rate: 2.6cc/min.) 4 x 10-11 AFS 100mA 40:1

30m, 0.53mm ID, 1.0m Stabilwax-DA (cat.# 11055) 0.1L direct injection of industrial solvents Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 95C (hold 4 min.) to 250C @ 4C/min. 250C helium 40cm/sec. (flow rate: 5cc/min.) 32 x 10-11 AFS

Solvents, Industrial MXT-WAX


2 6,7 10,11 15 19

Solvents, Industrial Stabilwax


2 6,7 10,11 15 19

8,9 16

5 4

14 13 17 18 20

12

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

pentane hexane methyl formate acetone tetrahydrofuran 1,1,1-trichloroethane ethyl acetate methanol methyl ethyl ketone methylene chloride chloroform benzene n-propyl alcohol sec-butyl alcohol toluene n-butyl acetate isobutyl alcohol n-butyl alcohol o-xylene ethoxyethane

1 8,9 16 5 14 13 4 17 18 20

12 3

min.

6 GC_CH00354

10

min.

6 GC_CH00355

10

30m, 0.53mm ID, 1.0m MXT-WAX (cat.# 70655) Wet needle injection of neat solvents Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 50C to 220C @ 10C/min. 250C helium 20cm/sec. 5.12 x 10-10 AFS

30m, 0.53mm ID, 1.0m Stabilwax (cat.# 10655) Wet needle injection of neat solvents Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 50C to 220C @ 10C/min. 250C helium 20cm/sec. 5.12 x 10-10 AFS

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714

Solvents
Solvents, Polar Rt-QPLOT
1 3 4

Solvents, Polar Rt-UPLOT


1 5 4

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

1. 2. 3. 4. 5. 6. 7.

methane methanol ethanol acetone n-pentane ethyl acetate n-hexane

5 3

1. 2. 3. 4. 5. 6. 7.

methane methanol ethanol n-pentane acetone n-hexane ethyl acetate

2 7 6

6 7

min. 1

10

11

12

min. 1

10

11

12

GC_PC00181

GC_PC00182

30m, 0.32mm ID Rt-QPLOT PLOT (cat.# 19718) 20L split injection. 50ppm (w/v) each in helium with a Cyclosplitter liner (cat.# 20755) Oven temp.: Inj./det. temp.: Carrier gas: Det.: Split ratio: 150C 200C hydrogen FID 20/1

30m, 0.32mm ID Rt-UPLOT PLOT (cat.# 19724) 20L split injection. 50ppm (w/v) each in helium with a Cyclosplitter liner (cat.#20755) Oven temp.: Inj./det. temp.: Carrier gas: Detector: Split ratio: 150C 200C hydrogen FID 20/1

Solvents Rt-Q PLOT


7

Solvents HayeSep Q
3 6

1. 2. 3. 4. 5. 6. 7. 8. 9.
1

methane acetaldehyde acetonitrile acetone methylene chloride n-pentane ethyl acetate n-hexane benzene
8 4 9 6 3 2 5

2 4 1

1. 2. 3. 4. 5. 6. 7. 8.
8

methanol ethanol acetonitrile acetone methylene chloride n-pentane chloroform n-hexane

min.

6 GC_CH00348

10

30m, 0.53mm ID Rt-Q PLOT (cat.# 19716) 70L split injection of solvent mixture Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: Split: Column flow: 100C to 220C @ 15C/min. (hold 2 min.) 220C helium 23.6cm/sec. set @ 100C 1.28 x 10-10 AFS 7.7:1 44.5cc/min. 6.6cc/min.

min.

4
GC_CH00328

2m, 1mm ID HayeSep Q (cat.# 19017) 1L direct injection of a neat solvent mixture Oven temp.: Inj. & det. temp.: Carrier gas: Flow: FID sensitivity: 80C to 180C @ 16C/min. (hold 5 min.) 200C helium 20mL/min. set @ 40C 512 x 10-11 AFS

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Solvents
Solvents, USP Rtx-1

715

for more info


Separation on an Rtx-200 column on page 716. Also see pages 699701.

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

GC_EV00463

Rtx-1 60m, 0.53mm, 3.00m (cat.# 10188) Sample: solvents Conc.: ~1.3% each Sample size: wet needle Inj.: split, 250C Septum purge: 5mL/min. Split vent flow: 100mL/min. ~1:13 split Carrier: helium Head pressure: 11.0psi constant pressure Linear velocity: 45.6 cm/sec @ 35C Det: mass selective Scan range: 10amu to 260amu MS interface: open split interface ~1:7 split Oven temp.: 35C (hold 4 min.) to 250C @ 4/min.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

formaldehyde water chloromethane methanol acetaldehyde ethylene oxide chloroethane ethanol acetonitrile acetone 2-propanol 2-chloropropane diethyl ether pentane ethyl formate formic acid methylal 1,1-dichloroethene methyl acetate methylene chloride

21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40.

nitromethane 1-propanol trans-1,2-dichloroethene methyl tert-butyl ether 2-methylpentane (spiked at 9%) 2-butanone (MEK) 2-butanol cis-1,2-dichloroethene acetic acid isopropyl ether ethyl acetate hexane chloroform tetrahydrofuran 2-methoxyethanol 1,2-dichloroethane methyl cyclopentane 1,1,1-trichloroethane 1,2-dimethoxyethane methyl isopropyl ketone

41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60.

2,2-dimethoxypropane isopropyl acetate 1-butanol benzene carbon tetrachloride ethylene glycol formamide 1,4-dioxane trichloroethene isooctane 2-ethoxyethanol n-heptane (C7) isoamyl alcohol hexanone (MIBK) pyridine methyl cyclohexane dimethyl formamide (DMF) 1,1,2-trichloroethane 1-pentanol isobutyl acetate

61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77.

toluene 2-hexanone (MBK) dimethyl sulfoxide butyl acetate 1,1-diethoxypropane N,N-dimethylacetamide chlorobenzene ethylbenzene isoamyl acetate p-xylene m-xylene o-xylene anisole isopropylbenzene (cumene) 1-methyl-2-pyrrolidinone sulfolane 1,2,3,4-tetrahydronaphthalene

*paraldehyde

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716

Solvents
Solvents, USP Rtx-200

for more info


Separation on an Rtx-1 column on page 715. Also see pages 699701.

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

GC_EV00464

Rtx-200 60m, 0.53mm, 3.00m (cat.# 15088) Sample: solvents Conc.: solventless mixture ~1.3% each Sample size: wet needle Inj.: split, 250C Septum purge: 5mL/min. Split vent flow: 100mL/min. ~1:13 split Carrier: helium Head pressure: 11.0psi constant pressure Linear velocity: 45.6 cm/sec @ 35C Det: mass selective Scan range: 10amu to 260amu MS interface: open split interface ~1:7 split Oven temp.: 35C (hold 4 min.) to 250C @ 4/min.

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.

formaldehyde water chloromethane methanol acetaldehyde ethylene oxide chloroethane ethanol acetonitrile acetone 2-propanol 2-chloropropane diethyl ether pentane ethyl formate formic acid methylal 1,1-dichloroethene methyl acetate methylene chloride

21. 22. 23. 24. 25. 26. 27. 28. 29. 30. 31. 32. 33. 34. 35. 36. 37. 38. 39. 40.

nitromethane 1-propanol trans-1,2-dichloroethene methyl tert-butyl ether 2-methylpentane (spiked at 9%) 2-butanone (MEK) 2-butanol cis-1,2-dichloroethene acetic acid isopropyl ether ethyl acetate hexane chloroform tetrahydrofuran 2-methoxyethanol 1,2-dichloroethane methyl cyclopentane 1,1,1-trichloroethane 1,2-dimethoxyethane methyl isopropyl ketone

41. 42. 43. 44. 45. 46. 47. 48. 49. 50. 51. 52. 53. 54. 55. 56. 57. 58. 59. 60.

2,2-dimethoxypropane isopropyl acetate 1-butanol benzene carbon tetrachloride ethylene glycol formamide 1,4-dioxane trichloroethene isooctane 2-ethoxyethanol n-heptane (C7) isoamyl alcohol hexanone (MIBK) pyridine methyl cyclohexane dimethyl formamide (DMF) 1,1,2-trichloroethane 1-pentanol isobutyl acetate

61. 62. 63. 64. 65. 66. 67. 68. 69. 70. 71. 72. 73. 74. 75. 76. 77.

toluene 2-hexanone (MBK) dimethyl sulfoxide butyl acetate 1,1-diethoxypropane N,N-dimethylacetamide chlorobenzene ethylbenzene isoamyl acetate p-xylene m-xylene o-xylene anisole isopropylbenzene (cumene) 1-methyl-2-pyrrolidinone sulfolane 1,2,3,4-tetrahydronaphthalene

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Solvents
Pentane (lot purity analysis) MXT-1
LOT A
1

717

LOT B
1

1. pentane

Searching for a chromatogram?


G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

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min.

8 GC_CH00332

min.

60m, 0.53mm ID, 5.0m MXT-1 (cat.# 70183) 1.0L direct injection of high purity pentane Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C 200C helium 40cm/sec. (flow rate: 10cc/min.) 4 x 10-11 AFS

Solvents, Nitrogen Containing Rtx-1701


1 4

1. 2. 3. 4. 5. 6. 7. 8.

butyronitrile toluene pyrazine pyridine pyrimidine 2-picoline 3-picoline 4-picoline

5 7

min.

10

GC_CH00330

30m, 0.32mm ID, 1.0m Rtx-1701 (cat.# 12054) 1.0L split injection of a neat pyridine standard Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split vent: 80C (hold 4 min.) to 130C @ 5C/min. 200C / 260C helium 26cm/sec. 1.28 x 10-10 AFS 40cc/min.

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718

Solvents
Substituted Pyridine Rtx-1701
1 2 3 4 5 6 7 9 10 11

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

methanol benzene toluene pyridine -picoline 2,6-lutidine -picoline 4-cyanopyridine 3-cyanopyridine 2-cyanopyridine picamide

60m, 0.53mm ID, 3.0m Rtx-1701 (cat.# 12088) 0.1L direct injection of a substituted pyridine standard (0.5-5% per component), Uniliner liner Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 60C to 225C @ 5C/min. 230C hydrogen 40cm/sec. (flow rate: 5.1cc/min.) 32 x 10-11 AFS
8

min.

12

16
GC_CH00333

20

24

28

32

Substituted Pyridine Stabilwax


12 3 4 5 6 7 9 10 11

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

methanol benzene toluene pyridine -picoline 2,6-lutidine -picoline 4-cyanopyridine 3-cyanopyridine 2-cyanopyridine picamide

30m, 0.53mm ID, 1.0m Stabilwax (cat.# 10655) 0.1L direct injection of a substituted pyridine standard (0.5-5% per component), Uniliner liner Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 60C to 225C @ 5C/min. 230C hydrogen 40cm/sec. (flow rate: 5.1cc/min.) 32 x 10-11 AFS

min.

12

16

20
GC_CH00334

24

28

32

36

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Alcohols
Alcohols Rtx-502.2
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. pentane isopropyl alcohol 2-propen-1-ol 2-butanol 2-pentanol 1-pentanol 2-hexanol 2-heptanol 2-octanol undecane 1-octanol 2-nonanol 2-decanol 2-phenoxyethanol tetradecane 1-undecanol
4 3 2 5 16 11

719

15 14 10 13

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

2,2,2-trifluoroethanol pentane 2-methyl-1-propanol 3-buten-2-ol 2-methyl-3-buten-2-ol 2-methoxyethanol 1-penten-3-ol ethylene glycol 2-ethoxyethanol 1-pentanol 2-methyl-1-pentanol

12. 13. 14. 15. 16. 17. 18.

trans-2-hexen-1-ol 2,2-dimethyl-1-pentanol 1,4-butanediol undecane 1-octanol tetradecane 13 1-undecanol


12 10

15

16

17

18

6 9

12

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

7 8,9 2 7 8 1 3 4 5 6

11 14

min.

10

15

20

25

30
GC_CH00286

min.

10

15

20

25

30

105m, 0.53mm ID, 3.0m Rtx-502.2 (cat.# 10910) 1.0L split injection of an alcohol mixture Oven temp.: Inj. / det. temp.: Det. : Carrier gas: Linear velocity: Split ratio: Ionization: 40C (hold 10 min.) to 270C @ 12C/min. (hold 10 min.) 250C / 270C MS helium 56cm/sec. set @ 50C 7:1 EI

Alcohols Rtx-502.2
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. pentane 3-buten-1-ol 3-methyl-1-butanol 3-methyl-3-pentanol 1-pentanol 3-methyl-2-buten-1-ol 3-hexen-1-ol 4-heptanol tetrahydrofurfuryl alcohol 2-(2-ethoxyethoxy)ethanol undecane 1-octanol -methylbenzyl alcohol 2-(2-butoxyethoxy)ethanol tetradecane 2 1-undecanol
1 3 1 3

12

16 15

11 10 7 6 5 4

13 14

8 9

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16.

pentane 2-buten-1-ol 3-methyl -2-butanol 3-pentanol 4-methyl-2-pentanol 1-pentanol 3-hexanol cyclopentanol 2-furanmethanol cyclohexanol hexylene glycol 3-octanol undecane 1-octanol tetradecane 1-undecanol
2 4 5

16 14 15 13

9 10 7 6 8 11 12

min.

10

15
GC_CH00290

20

25

30

min.

10

15
GC_CH00291

20

25

30

105m, 0.53mm ID, 3.0m Rtx-502.2 (cat.# 10910) 1.0L split injection of an alcohol mixture Oven temp.: Inj. / det. temp.: Det. : Carrier gas: Linear velocity: Split ratio: Ionization: 40C (hold 10 min.) to 270C @ 12C/min. (hold 10 min.) 250C / 270C MS helium 56cm/sec. set @ 50C 7:1 EI

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720

Alcohols
Alcohols Stabilwax
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. pentane hexane heptane ethanol decane 1-propanol 1-butanol dodecane 1-pentanol 1-hexanol tetradecane 1-heptanol 1-octanol hexadecane 1-nonanol 1-decanol 1-undecanol 1-dodecanol 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19. 20.
2 3 4 5 7

13 15 10 12 11 9 7 8 14

16 17

18

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

2 3 1

pentane methanol 2-methyl-2-propanol (tert-butylalcohol) 2-methyl-3-buten-2-ol 3-buten-2-ol undecane 2,2-dimethyl-1-propanol (neopentanol) 1-penten-3-ol 2-methoxyethanol 2,2,2-trifluoroethanol 2-ethoxyethanol 15 1-pentanol 2-methyl-1-pentanol 14 16 2,2-dimethyl-1-pentanol 12 tetradecane trans-2-hexen-1-ol 11 1-octanol ethylene glycol 8 13 9 6 1-undecanol 1,4-butanediol 10

19 17

20

18 4 5 6

min.

10

15

20

25
GC_CH00288

min.

10

15

20

25

60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of alcohols Oven temp.: Inj. & det. temp.: Det. : Carrier gas: Linear velocity: Split ratio: Ionization: 45C (hold 10 min.) to 250C @ 12C/min. (hold 20 min.) 250C MS helium 51cm/sec. set @ 50C 8:1 EI

Alcohols Rt-QPLOT

2 4 8 6 3 7 11 10

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

methanol ethanol 2-propanol 1-propanol tert-butanol 2-butanol isobutyl alcohol 1-butanol 2-methyl-2-butanol 3-methyl-1-butanol 4-methyl-2-pentanol

9 5

30m, 0.32mm ID, 10m Rt-QPLOT (cat.# 19718) 1.0L split injection of alcohol mixture Conc.: 1% each in water Oven program: Injector: Carrier gas: Head pressure: Column flow rate: Linear velocity: Split ratio: Detector: min 35 Make-up gas flow: Inlet liner: 100C to 240C @ 5C/min. (hold 10 min.) split @ 250C helium (constant pressure mode) 18.0psi 1.1cc/min. @ 100C 31cm/sec. @ 100C 70:1 FID @ 270C 45cc/min. 4mm single gooseneck (cat.# 20798)

10

15

20

25

30

GC_CH00495

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Alcohols; Alcohols & Aldehydes


Alcohols Rtx-5
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.
4 3 9 5 7 8

721

2 1

methanol ethanol acetone isopropanol 1-propanol ethyl acetate 2-methyl-1-propanol 1-butanol 3-pentanol 3-methyl-1-butanol 2-methyl-1-butanol
10

Alcohols Rtx-Volatiles
1. 2. 3. 4. 5. 6.
2 11 1 5 3 4 6 7

methanol ethanol isopropanol acetone 1-propanol ethyl acetate


8 9

7. 8. 9. 10. 11.

2-methyl-1-propanol 1-butanol 3-pentanol 3-methyl-1-butanol 2-methyl-1-butanol

11 10

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

min.

8
GC_CH00292

10

12

14 min. 2 4 6 8
GC_CH00293

10

12

14

60m, 0.32mm ID, 1.0m Rtx-5 (cat.# 10257) 0.03L split injection of a neat alcohols mix Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 25C (hold 4 min.) to 80C @ 8C/min. (hold 5 min.) 200C hydrogen 40cm/sec. (flow rate: 3.2cc/min.) 128 x 10-11 AFS 40:1

60m, 0.32mm ID, 1.5m Rtx-Volatiles (cat.# 10904) 0.03L split injection of a neat alcohols mix Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 40C (hold 4 min.) to 80C @ 8C/min. (hold 5 min.) 200C hydrogen 40cm/sec. (flow rate: 3.2cc/min.) 64 x 10-11 AFS 40:1

Alcohols & Aldehydes Rtx-502.2


9

10

7 8

11 12 13

3 4 2

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.

heptane 1-penten-3-ol 3-pentanol ethylene glycol furfural 2-furanmethanol cyclohexanol 2-methyl-2,4-pentanediol 1,4-butanediol 3-octanol diethylene glycol benzaldehyde pentadecane nonadecane

14 1

min.

15

20

25
GC_CH00294

30

35

40

105m, 0.53mm ID, 3.0m Rtx-502.2 (cat.# 10910) 1.0L split injection of alcohols and aldehydes Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: Split ratio: Ionization: Mode: 40C (hold 10 min.) to 270C @ 12C/min. (hold 10 min.) 250C / 285C helium 50cm/sec. set @ 50C 7:1 EI scan 10, range 300

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722

Alcohols & Aldehydes; Aldehydes


Alcohols & Aldehydes Stabilwax
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. pentane heptane acetaldehyde dimethoxymethane butyraldehyde 3-pentanol 1-penten-3-ol 3-octanol cyclohexanol furfural pentadecane benzaldehyde ethylene glycol & 2-methyl-2,4-pentanediol furfuryl alcohol nonadecane 1,4-butanediol diethylene glycol
9 14 12,13 7 15 17 8 11

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

6 5 10

16

1 2 3

min.

10

15
GC_CH00295

20

25

60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of alcohols and aldehydes Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: Split ratio: Ionization: Mode: 45C (hold 10 min.) to 250C @ 12C/min. (hold 20 min.) 250C / 285C helium 50cm/sec. set @ 50C 7:1 EI scan 10, range 300

Aldehydes Stabilwax

12

9,10

1. pentane 2. acetaldehyde 3. dimethoxymethane (methylal) 4. propanal 5. 2-methyl propanal 6. methanol 7. pentanal 8. 2-butenal 14 (crotonaldehyde) 9. hexanal 10. undecane 11. heptanal 12. 1-pentanol 13. octanal 14. tetradecane 15. nonanal 16. 2-furancarboxaldehyde 17. decanal 18. benzaldehyde 16 18 19. 1-octanol 15
17 19 13

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3 2 45

8 7

11

min.

10

15
GC_CH00315

20

25

60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of aldehydes Oven temp.: Inj. & det. temp.: Det.: Carrier gas: Linear velocity: Split ratio: Ionization: 45C (hold 10 min.) to 250C @ 12C/min. (hold 20 min.). 250C MSD helium 51cm/sec. set @ 50C 8:1 EI

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Aldehydes; Acrylates
Aldehydes Rtx-Wax
2

723

6 4 5

9 1

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.

ethanal propanal butenal pentanal hexanal heptanal octanal nonanal decanal undecanal

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

10

min.

10
GC_CH00300

15

20

30m, 0.25mm ID, 0.50m Rtx-Wax (cat.# 12438) split injection of C2-C11 aldehydes mixture On-column conc.: 250ng Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 40C (hold 5 min.) to 200C @10C/min. 200C hydrogen 35cm/sec. set @ 40C 82 x 10-11 AFS 100:1

Formaldehyde Rtx-1701

Acrylates Rtx-1701
7 9 11

1. 2. 3. 4. 5.

air water formaldehyde acetaldehyde methanol


5

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

n-butanol methyl methacrylate n-butyl acetate isopropyl methacrylate n-butyl ether isobutyl isobutyrate isobutyl methacrylate n-butyl isobutyrate butyl methacrylate n-butyl n-butyrate n-butyl -hydroxyisobutyrate

2 4 5 1 2 3 8 10

min.

6
GC_CH00313

8 min. 4

12

16

20

24

GC_CH00312

60m, 0.25mm ID, 1.0m Rtx-1701 (cat.# 12056) 0.5L split injection of a formaldehyde sample Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: TCD sensitivity: Split vent: 40C 150C / 175C helium 20cm/sec. (flow rate: 0.8cc/min.) 8 mV 30cc/min.

30m, 0.32mm ID, 1.0m Rtx-1701 (cat.# 12054) 0.5L split injection of acrylates Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 70C (hold 10 min.) to 120C @ 5C/min., to 250C @ 15C/min. 250C hydrogen 40cm/sec. 4 x 10-11 AFS 56:1

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724

Amines
Ethanolamines Rtx-5 Amine
1 3

Ethanolamines Rtx-35 Amine

1. monoethanolamine 2. diethanolamine 3. triethylene glycol monomethylether (IS) 4. triethanolamine

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

2 4

GC_CH00585

1. 2. 3. 4. min. 5
GC_CH00296

monoethanolamine diethanolamine triethyleneglycol monomethylether triethanolamine

10 Rtx-35 Amine 30m, 0.32mm ID, 1.0m (cat.# 11354) Sample: 500g/mL ethanolamine standard in water Inj.: 1.0L split (split ratio 10:1), cup splitter inlet liner (cat.# 20709) Inj. temp.: 300C Carrier gas: helium, constant pressure Linear velocity: 40cm/sec. @ 50C Oven temp.: 50C (hold 0.50min.) to 280C @15C/min. Det.: FID @300C

15m, 0.25mm ID, 0.50m Rtx-5 Amine (cat.# 12335) 1.0L split injection of ethanolamine mix in methanol On-column conc.: 34ng Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 50C (hold 2 min.) to 180C @ 10C/min. (hold 2 min.) 280C / 300C hydrogen 43cm/sec. set @ 50C 6.4 x 10-11 AFS 58:1

Ethyleneamines Rtx-5 Amine


1 2 3 5 7

1. 2. 3. 4. 5. 6. 7.

isopropanol monoethanolamine ethylenediamine piperazine diethylenetriamine aminoethylethanolamine aminoethylpiperazine

remaining impurities consist of ethyleneamine and piperazine derivatives


4 6

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min.

10

15
GC_CH00298

20

25

30m, 0.25mm ID, 0.50m Rtx-5 Amine (cat.# 12338) 3.0L split injection of ethyleneamine industrial sample On-column conc.: ~5-80ng Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 40C (hold 4 min.) to 315C @ 10C/min. (hold 5 min.) 315C hydrogen 43cm/sec. set @ 40C 6.4 x 10-11 AFS 20:1

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Amines
Amines & Phenols Rtx-5 Amine
4 9

725

5 3 1 2 13 11

8 6 10

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

diethylamine pyridine morpholine phenol aniline 2-chlorophenol diethylenetriamine octylamine 1-methyl-2-pyrrolidinone 2-nitrophenol 2,6-dimethylaniline nicotine 2-nitroaniline

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

12

min.

4
GC_CH00301

10

30m, 0.32mm ID, 1.0m Rtx-5 Amine (cat.# 12354) 1.0L split injection of miscellaneous amines and phenols in water On-column conc.: 22ng Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 120C to 220C @ 10C/min. 305C hydrogen 38cm/sec. set @ 120C 6.4 x 10-11 AFS 25:1

Hexamethylenediamine Stabilwax-DB

1 2

10

12

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12.

cyclohexane hexamethyleneimine 1,4-diaminobutane pentamethylenediamine 1,2-diaminocyclohexane 1,5-diamino-2-methylpentane aminomethylcyclopentylamine hexamethylenediamine 6-aminocapronitrile n-valeramide adiponitrile bis-hexamethylenetriamine

10 12

3 2

6 45 7 9 11 4 6 5 7 9 11

min.

12

16

20

24

28

32

min.

12

16

20

24

28

GC_CH00302

GC_CH00303

30m, 0.32mm ID, 0.25m Stabilwax-DB (cat.# 10824) 0.4L direct injection of a neat hexamethylenediamine sample On-column conc.: 10 to 1000ng/component Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 95C (hold 6 min.) to 235C @ 7C/min. (hold 4 min.) 250C hydrogen 40cm/sec. 2 x 10-11 AFS

30m, 0.53mm ID, 0.5m Stabilwax-DB (cat.# 10840) 0.2L direct injection of a neat hexamethylenediamine sample onto a Uniliner liner Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: 95C (hold 6 min.) to 235C @ 7C/min. (hold 2 min.) 255C hydrogen 40cm/sec. (flow rate: 5cc/min.) 64 x 10-11 AFS

Phone: 800-356-1688 or 814-353-1300 www.restek.com

726

Amines
Primary Amines Rtx-35 Amine
2/3

5 4 7

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

6 1

8 9

1. 2. 3. 4. 5. 6. 7. 8. 9.

methylamine dimethylamine trimethylamine ethylamine isopropylamine tert-butylamine n-propylamine diethylamine sec-butylamine

Rtx-35 Amine 30m, 0.53mm ID, 1.0m (cat.# 11355) Sample: primary amines, 50ppm on-column conc. in water Inj.: 1.0L, split (10:1), 4mm base-deactivated single gooseneck (cat.# 20798-210.1) Injector: 250C Carrier gas: helium, constant pressure Linear velocity: 35.7cm/sec Oven temp.: 35C (hold 5.0 min.) Det.: FID @ 300C

GC_CH00578

a plus 1 story
Scott has used his training in computers to improve our QA processes for fused silica columns by building databases for RA testing tracking pass rate. Scott wrote the test methods and recorded all of the temperature profile data for approximately one thousand tests. Scott Sharp, Quality Assurance Analyst

Phone: 800-356-1688 or 814-353-1300 www.restek.com

Amines
Amines (low MW) Stabilwax-DB
4

727

Amines (low MW) Stabilwax-DB

1. 2. 3. 4. 5. 6. 7. 8. 9.

trimethylamine dimethylamine ethylamine methylamine isopropylamine n-propylamine tert-butylamine diethylamine sec-butylamine


1

1. trimethylamine 2. triethylamine 3. methanol


5 3

6 7 8 9 2

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

GC_CH00304

min. 1 2 30m, 0.53mm ID, 1.0m Stabilwax-DB (cat.# 10855) 1.0L direct injection of amines in water Oven temp.: 45C Inj. & det. temp.: 250C Carrier gas: hydrogen Linear velocity: 40cm/sec. (flow rate: 5cc/min.) FID sensitivity: 1 x 10-11 AFS Recommended liner: Uniliner

GC_CH00305 min. 4 30m, 0.53mm ID, 1.0m Stabilwax-DB (cat.# 10855) 0.6L split injection of low molecular weight amines in a methanol Conc.: 500ng/L Oven temp.: 50C Inj. & det. temp.: 200C Carrier gas: hydrogen Linear velocity: 47cm/sec. (flow rate: 3.2cc/min.) FID sensitivity: 4 x 10-11 AFS Split ratio: 40:1

Nitrosamines Stabilwax-DB

1. 2. 3. 4. 5. 6. 7. 8. 9.
4 3

solvent N-nitrosodimethylamine N-nitrosodiethylamine N-nitrosodiisopropylamine N-nitrosodipropylamine N-nitrosodibutylamine N-nitrosopiperidine N-nitrosopyrrolidine N-nitrosomorpholine

Amines/Alcohols/Chlorides Stabilwax
2 4 6 7 9 10

16 17

11

1 7 8 9 5 3 8 12

5 6

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17.

n-octyl,N,N-dimethylamine n-octyl chloride n-decyl,N,N-dimethylamine n-decyl chloride n-octyl alcohol n-dodecyl,N,N-dimethylamine n-dodecyl chloride n-decyl alcohol n-tetradecyl,N,N-dimethylamine n-tetradecyl chloride n-dodecyl alcohol n-hexadecyl,N,N-dimethylamine n-hexadecyl chloride n-tetradecyl alcohol n-octadecyl,N,N-dimethylamine n-hexadecyl alcohol n-octadecyl alcohol

13 14

15

min.

8
GC_CH00306

10

12

14 min. 4 8 12
GC_CH00307

16

20

60m, 0.53mm ID, 1.0m Stabilwax-DB (cat.# 10858) Direct injection of nitrosamines Conc.: 1.0g/mL Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: Detector: 100C (hold 1 min.) to 170C @ 5C/min. 200C helium 100cm/sec. (flow rate: 15cc/min.) TSD

30m, 0.53mm ID, .25m Stabilwax (cat.# 10625) 0.5L split injection Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 100C to 250C @ 8C/min. (hold 5 min.) 250C hydrogen 40cm/sec. (flow rate: 5.2cc/min.) 128 x 10-11 AFS 40:1

Phone: 800-356-1688 or 814-353-1300 www.restek.com

728

Aromatics
Aromatics Rtx-502.2
12 10, 11 13

3 5 6 2 4 1 8

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14.

o-xylene 1,3,5-trimethylbenzene -methylstyrene 1,2,4-trimethylbenzene cymene 1,2,3-trimethylbenzene trans-decahydronaphthalene o-cresol cis-decahydronaphthalene nitrobenzene diisopropylbenzene triethylbenzene pentadecane nonadecane

14

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

9 7

min.

35

40

45

50

55
GC_CH00308

60

65

70

75

105m, 0.53mm ID, 3.0m Rtx-502.2 (cat.# 10910) 1.0L split injection of an aromatics mixture Oven temp.: Inj. / det. temp.: Det.: Carrier gas: Linear velocity: Split ratio: Ionization: 35C (hold 10 min.) to 265C @ 4C/min. (hold 20 min.) 250C / 280C MS helium 50cm/sec. set @ 50C 7:1 EI

Aromatics Stabilwax
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15.

10

14 15

trans-decahydronaphthalene o-xylene cis-decahydronaphthalene 1,3,5-trimethylbenzene p-cymene or p-isopropyltoluene 1,2,4-trimethylbenzene -methyl benzene 1,2,3-trimethylbenzene diisopropylbenzene 2 triethylbenzene pentadecane nitrobenzene nonadecane o-cresol bibenzyl
3 1

5 4 6

7 8 9 12

13

11

min.

15

20

30

35

40
GC_CH00309

45

50

55

60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of an aromatics mixture. Oven temp.: Inj. / det. temp.: Det.: Carrier gas: Linear velocity: Split ratio: Ionization: 40C (hold 10 min.) to 245C @ 4C/min. (hold 20 min.) 250C / 280C MS helium 50cm/sec. set @ 50C 7:1 EI

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Aromatics
Aromatics Stabilwax
6 8 10

729

1. 2. 3. 4. 5. 6.

toluene ethylbenzene p-xylene isopropyl benzene or cumene propylbenzene tert-butylbenzene

7. 8. 9. 10. 11. 12.

styrene butylbenzene pentadecane naphthalene nonadecane p-cresol


4

12 5 7 11

9 2 3

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

min.

12

14

16

18

20
GC_CH00311

22

24

26

28

60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of aromatics Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: Split ratio: Ionization: Mode: 45C (hold 10 min.) to 250C @ 12C/min. (hold 20 min.) 250C / 285C helium 50cm/sec. set @ 50C 7:1 EI scan 10, range 300

Aromatics Rtx-502.2
8 6 4 3 2 1 5 7 9

10 11

12

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

toluene ethylbenzene p-xylene styrene isopropyl benzene or cumene propylbenzene tert-butylbenzene butylbenzene p-cresol naphthalene pentadecane bibenzyl 13 nonadecane

min.

20

25

30
GC_CH00310

35

40

105m, 0.53mm ID, 3.0m Rtx-502.2 (cat.# 10910) 1.0L split injection of aromatics Oven temp.: 40C (hold 10 min.) to 270C @ 12C/min. (hold 20 min.) Inj. / det. temp.: 250C / 285C Carrier gas: helium Linear velocity: 50cm/sec. set @ 50C Split ratio: 7:1 Ionization: EI Mode: scan 10, range 300

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730

Chlorofluorocarbons
Chlorofluorocarbons Rtx-1

2 3

1.Freon 22 2. Freon 12 3. Freon 114 4. Freon 1112a 5. Freon 123 6. Freon 123a 7. Freon 11 8. Freon 113 9. Freon 122

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

7 9 4 6

min.

12

16

20
GC_CH00319

24

28

32

105m, 0.25mm ID, 1.0m Rtx-1 (cat.# 10159) 1.0L split injection of a 99.9% pure Freon 113 standard. Oven temp.: Inj. & det. temp.: Det.: Carrier gas: Linear velocity: Split vent: 35C (hold 20 min.) to 220C @ 20C/min. (hold 30 min.) 250C full scan helium 20cm/sec. set @ 35C 30mL/min.

Chlorofluorocarbons Rtx-1

10

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13.

Freon 115 Freon 22 Freon 12 Freon 124 Freon 114 Freon 1112a Freon 123 Freon 123a Freon 11 Freon 113 Freon 122 Freon 112 Freon 1110

4 3 11 1 2 6 78 9 12

13

min.

10

15

20

25
GC_CH00320

30

35

105m, 0.25mm ID, 1.0m Rtx-1 (cat.# 10159) 1.0L split injection of a 99.9% pure Freon 114 standard. Oven temp.: Inj. & det. temp.: Det.: Carrier gas: Linear velocity: Split vent: 35C (hold 20 min.) to 220C @ 20C/min. (hold 30 min.) 250C full scan helium 20cm/sec. set @ 35C 30mL/min.

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Chlorofluorocarbons
Chlorofluorocarbons Rtx-1
5 6

731

Chlorofluorocarbons Rtx-200
1. Freon 21 2. Freon 123 3. Freon 123a 4. Freon 11 5. dichloromethane 6. Freon 113
1

3 1

1. 2. 3. 4. 5. 6.
2

Freon 21 Freon 11 Freon 123 Freon 123a Freon 113 dichloromethane


4 3 5

2 4

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

min.

20

22

24
GC_CH00321

26

28

30

min.

12

13

14

15
GC_CH00322

16

17

18

105m, 0.53mm ID, 3.0m Rtx-1 (cat.# 10189) 1.0L splitless injection of a 500g/mL mix of Freon compounds Splitless hold: Oven temp.: Inj. temp.: Carrier gas: Linear velocity: MSD: Scan rate: 0.5 min. 35C 220C helium 20cm/sec. set @ 35C TIC mode 1.5 scans/sec.

105m, 0.53mm ID, 3.0m Rtx-200 (cat.# 15091) 1.0L splitless injection of a 500g/mL mix of Freon compounds Splitless hold: Oven temp.: Inj. temp.: Carrier gas: Linear velocity: MSD: Scan rate: 0.5 min. 35C 220C helium 20cm/sec. set @ 35C TIC mode 1.5 scans/sec.

Chlorofluorocarbons 5% Krytox on 60/80 CarboBlack B

1. 2. 3. 4. 5. 6.

Freon 22 Freon 12 Freon 21 Freon 114 Freon 114A isomer Freon 11

min.

8
GC_CH00323

12

16

5% Krytox on 60/80 CarboBlack B (cat.# 80127) 3.05m, 1/8" OD x 2.1mm ID SilcoSmooth stainless steel tubing 1L injected, concentration 20% each component Oven temp.: Inj./det. temp.: Carrier gas: Detector: 50C 200C/250C nitrogen @ 30mL/min. FID

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732

Chlorofluorocarbons; Cresylic Acids


Freon & Ethylene Oxide Rtx-1
1

Freon & Ethylene Oxide Rtx-200


1 2

1. Freon 12 2. ethylene oxide

1. Freon 12 2. ethylene oxide

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

min.

min. 4
GC_CH00325

GC_CH00324

30m, 0.53mm ID, 5.0m Rtx-1 (cat.# 10179) 50L split injection of Freon 12 and ETO Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split vent: 25C 290C hydrogen 40cm/sec. 4 x 10-11 AFS 40:1

30m, 0.53mm ID, 3.0m Rtx-200 (cat.# 15085) 50L direct injection of Freon 12 and ETO Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: 25C 290C hydrogen 40cm/sec. (flow rate: 5.2cc/min.)

Cresylic Acids Stabilwax-DA


16,17 18 19

2 7,8

9 10 14

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18. 19.

2,6-dimethylphenol o-cresol phenol 2,4,6-trimethylphenol 2,3,6-trimethylphenol o-ethylphenol 2,5-dimethylphenol p-cresol 2,4-dimethylphenol m-cresol C3 phenol 2,3-xylenol C3 phenol C3 phenol C3 phenol p-ethylphenol 3,5-xylenol m-ethylphenol 3,4-xylenol

1 11 3,4 6 12
13

15

min.

10

11

12

GC_CH00277

30m, 0.25mm ID, 0.50m Stabilwax-DA (cat.# 11038) Wet needle split injection of cresylic acids Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 180C (hold 2 min.) to 260C @ 2C/min. 250C hydrogen 40cm/sec. (flow rate: 3.2cc/min.) 64 x 10-11 AFS 40:1

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Cresylic Acids; Esters


Cresylic Acids Di-isodecyl Phthalate
2 12 13

733

15 3

8 1 11 17

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. 14. 15. 16. 17. 18.

phenol o-cresol 2,6-xylenol p-cresol m-cresol o-ethylphenol 2,4-xylenol 2,5-xylenol 2,4,6-trimethylphenol 2,3-xylenol p-ethylphenol m-ethylphenol 3,5-xylenol C3 phenol 3,4-xylenol C3 phenol 4-ethyl,2-methylphenol 5-ethyl,2-methylphenol

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

6 10 14 16 18 9

min.

12

16

20
GC_CH00278

24

28

32

36

40

60m, 0.25mm ID, 0.20m DIIDP column (cat.# 50016) Wet needle split injection of cresylic acids Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 130C 130C hydrogen 40cm/sec. 32 x 10-11 AFS 25:1

Esters Stabilwax
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. 13. pentane heptane methyl formate methyl acetate methyl propionate methyl butyrate methyl valerate methyl hexanoate methyl octanoate pentadecane methyl decanoate methyl benzoate nonadecane
10

13

12

11

8 1 7 3 4 5 6

min.

10

12

14
GC_CH00314

16

18

20

22

24

26

60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of esters Oven temp.: Inj. & det. temp.: Det.: Carrier gas: Linear velocity: Split ratio: Ionization: 45C (hold 10 min.) to 250C @ 12C/min. (hold 20 min.) 250C/285C MS helium 50cm/sec. set @ 50C 7:1 EI

Phone: 800-356-1688 or 814-353-1300 www.restek.com

734

Ethers
Ethers Rtx-502.2
105m, 0.53mm ID, 3.0m Rtx-502.2 (cat.# 10910) 1.0L split injection of ethers Oven temp.: 1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 12. methyl ether pentane ethyl ether dimethoxymethane isopropyl ether butenal 1,3-dioxolane 1,2-dimethoxyethane heptane tetrahydro-2-methyl furan allyl ether ethyl acrylate 13. 14. 15. 16. 17. 18. 19. 20. 21. 1,4-dioxane butyl ether bis(2-methoxyethyl)ether 2-ethoxyethyl ether 1,2-bis(2-methoxyethoxy)ethane or triethylene glycol dimethyl ether pentadecane bis(2-(2-methoxyethoxy)ethyl ether or tetraethylene glycol dimethyl ether benzyl ether nonadecane Inj. / det. temp.: Det.: Carrier gas: Linear velocity: Split ratio: Ionization:
19

17

35C (hold 10 min.) to 265C @ 4C/min. (hold 20 min.) 250C/280C MS helium 50cm/sec. set @ 50C 7:1 EI

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

16 15

10 13 11 12

14

18 21 20

3 2 4 5

89 6 7

min.

10

20

30

40
GC_CH00317

50

60

70

Ethers Stabilwax

10

13

1. 2. 3. 4. 5. 6. 7. 8. 9. 10.
1

tetrahydro-2-methyl furan butyraldehyde butyl ether 1,3-dioxolane ethyl acrylate 1,4-dioxane 2-methoxy ethyl ether 2-ethoxy ethyl ether pentadecane 1,2-bis(2-methoxyethoxy)ethane or triethylene glycol dimethylether 11. nonadecane 12. bis(2-(2-methoxyethoxy)ethyl) ether or tetraethylene glycol dimethyl ether 13. benzyl ether

12

11 9

3 2 4 5

min. 5

10

15

20

25

30

35
GC_CH00318

40

45

50

55

60

60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of ethers. Oven temp.: Inj. / det. temp.: Det.: Carrier gas: Linear velocity: Split ratio: Ionization: 40C (hold 10 min.) to 245C @ 4C/min. (hold 20 min.). 250C/280C MS helium 50cm/sec. set @ 50C 7:1 EI

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Glycols; Ketones
Glycols Rtx-200
2 3 1 1 4

735

Glycols & Alcohols XTI-5

1. 2. 3. 4.

ethylene glycol propylene glycol diethylene glycol tetraethylene glycol

1. 2. 3. 4. 5.

n-butyl alcohol ethylene glycol propylene glycol butyl Cellosolve butyl carbitol

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

min.

12

16
GC_CH00326

20

24

28 min. 4 8
GC_CH00327

60m, 0.53mm ID, 3.0m Rtx-200 (cat.# 15088) 1.0L split injection of a glycol sample Conc.: 50ng on-column Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 40C to 250C @ 8C/min. (hold 15 min.) 200C / 250C hydrogen 40cm/sec. (flow rate: 5cc/min.) 6.4 x 10-11 AFS 19:1

30m, 0.53mm ID, 1.0m XTI-5 (cat.# 12255) 1.0L direct injection of glycols and alcohols Conc.: 100ppm Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: 40C to 185C @ 15C/min. (hold 5 min.) 150C / 200C helium 40cm/sec. (flow rate: 5cc/min.) 8 x 10-11 AFS

Ketones Stabilwax
1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11. 2,4-dimethyl-3-pentanone 4-methyl-2-pentanone 4-heptanone 4-methyl-3-penten-2-one 5-methyl-2-hexanone 5-methyl-3-heptanone 4-hexen-3-one 1-pentanol 4-hydroxy-4-methyl-2-pentanone butyrolactone nonadecane

11

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9 4 3 5 6 7 10

1 2

min.

10

15
GC_CH00316

20

25

60m, 0.53mm ID, 1.0m Stabilwax (cat.# 10658) 1.0L split injection of ketones Oven temp.: Inj. & det. temp.: Det.: Carrier gas: Linear velocity: Split ratio: Ionization: 45C (hold 10 min.) to 250C @ 12C/min. (hold 20 min.) 250C MSD helium 51cm/sec. set @ 50C 8:1 EI

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736

Silanes; Styrene Impurities


Silanes Rtx-200
3 4 5 1 2 1

Silanes Rtx-200
3

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

1. 2. 3. 4. 5.

phenyldichlorosilane phenyltrichlorosilane methylphenyl dichlorosilane phenylvinyl dichlorosilane diphenyl dichlorosilane


2 4

1. 2. 3. 4. 5.

dimethylchlorosilane methyldichlorosilane trimethylchlorosilane methyltrichlorosilane dimethyldichlorosilane

min. 4

12
GC_CH00361

16

20

min.

4
GC_CH00362

60m, 0.53mm ID, 3.0m Rtx-200 (cat.# 15088) 0.5L split injection of phenyl silanes Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split vent: 100C to 250C @ 10C/min. (hold 20 min.) 200C / 270C hydrogen 40cm/sec. 1.02 x 10-9 AFS 40cc/min.

60m, 0.53mm ID, 3.0m Rtx-200 (cat.# 15088) 0.5L split injection of methyl silanes Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split vent: 40C to 250C @ 8C/min. (hold 5 min.) 200C / 270C hydrogen 40cm/sec. 1.02 x 10-9 AFS 40cc/min.

Styrene Impurities Stabilwax


2 5 11

Styrene Impurities Rtx-1701


1 6 10

6 7 8

1 10 9 3 4

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

butene 1,3-butadiene diethylhydroxylamine acrylonitrile vinylcyclohexene toluene ethylbenzene m-xylene cumene o-xylene styrene

2 9 11

1. 2. 3. 4. 5. 6. 7. 8. 9. 10. 11.

1,3-butadiene butene acrylonitrile diethylhydroxylamine toluene vinylcyclohexene ethylbenzene m-xylene o-xylene styrene cumene

min.

12

16
GC_CH00356

20

24

28

min.

12

16
GC_CH00357

20

24

28

30m, 0.53mm ID, 0.50m Stabilwax (cat.# 10640) 0.5L split injection of a 95% pure styrene Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split vent: 40C (hold 10 min.) to 150C @ 10C/min. (hold 15 min.) 150C helium 20cm/sec. set @ 40C 16 x 10-11 AFS 40cc/min.

30m, 0.53mm ID, 3.0m Rtx-1701 (cat.# 12085) 0.5mL split injection of a 95% pure styrene Oven temp.: Inj. & det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split vent: 40C (hold 10 min.) to 150C @ 12C/min. (hold 15 min.) 150C helium 20cm/sec. set @ 40C 16 x 10-11 AFS 40cc/min.

Permission to publish this chromatogram granted by Copolymer Rubber and Chemical Corp.

Permission to publish this chromatogram granted by Copolymer Rubber and Chemical Corp.

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Siloxanes
Siloxane (Polysiloxane 20) MXT-5

737

G C A P P L I C AT I O N S | S O LV E N TS & C H E M I C A L S

min.

12

16
GC_CH00359

20

24

28

32

15m, 0.28mm ID, 0.25m MXT-5 (cat.# 70221) 1.0L split injection of diluted polysiloxane 20 in pentane Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split ratio: 75C to 340C @ 15C/min. 250C / 340C hydrogen 40cm/sec. 16 x 10-11 AFS 100:1

Siloxane, Polymethyl Rtx-200

min.

10

12
GC_CH00360

14

16

18

20

22

15m, 0.25mm ID, 0.25m Rtx-200 (cat.# 15020) 1.0L split injection of polymethyl siloxane Oven temp.: Inj. / det. temp.: Carrier gas: Linear velocity: FID sensitivity: Split vent: 40C to 360C @ 15C/min. (hold 30 min.) 250C / 360C hydrogen 40cm/sec. 5.12 x 10-10 AFS 40cc/min.

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