Академический Документы
Профессиональный Документы
Культура Документы
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
Pharmaceutical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .509-527
Analgesics, Antiarrhythmics, Antiasthmatics, Antibiotics, Antidepressants, Anti-Diabetics, Anti-Inflammatories, Anti-Ulceratives, Bronchodilators, Corticosteroids, Steroid Hormones, Mixed Drugs, Sedatives, Xanthenes
Forensics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .654-660
Blood Alcohol, Drugs of Abuse, Anesthetics, Solvents, Inhalants, Arson Accelerants
Pharmaceutical . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .690-704
Antidepressants, Antihistamines, Antiepileptics, Barbiturates, Basic Drugs, Chiral Analyses, Pharmaceutical Solvents, Steroids, Sympathomimetic Amines
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
A P P L I C AT I O N S
463
A P P L I C AT I O N S
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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Compound Index
starting on page 738
Larry Peters
HPLC Manufacturing Technician
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
20L 20mM ammonium acetate, pH 5.8 Ultra IBD 9175565 150 x 4.6mm 5m 100
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
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:
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
10
LC_0128
12
14
16
18
min.
4
LC_0133
6 min.
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
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.
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.
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
10
15
LC_0136
20
25 min.
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
0
LC_0307
4
LC_0146
10
min.
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
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
0
LC_0168
4
LC_0142
7 min.
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
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.:
4 min.
LC_0140
LC_0228
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.:
H P LC A P P L I C AT I O N S
LC_0306
LC_0229
free literature
HPLC Columns and Accessories General-purpose and unique special-purpose columns, guard columns, column kits, and bulk materials, of course, but also instrument parts, innovative tools, accessories, and many example chromatograms. Our four silica bases have characteristics tailored to meet specific analytical requirements. Request lit. cat.# 59241B (100+ pages).
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Genuine Restek Replacement Parts for HPLC Systems (lit. cat.# 59012*) Over time, detector lamps, check valves, pump piston seals, and other components wear out or become contaminated. Working with defective parts means poor chromatography and, possibly, shortened column lifetimes. This 4-page publication lists a wide selection of Restek parts for Agilent, Beckman, Hitachi, PerkinElmer, Shimadzu, and Waters instruments, to keep these systems running smoothly and chromatography sharp. Genuine Restek Replacement Parts equal or exceed the performance of original equipment components.
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
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.
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
3 45
7 8 9 10 11 12 13
8
LC_0052
10
12
14
16 min.
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
LC_0298
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
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
10 11 12 13 14 15
LC_0294
10
12
14
min.
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
LC_0319
LC_0320
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.:
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.
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LC_0161
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
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
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.
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
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.
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.
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
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
LC_0313
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.
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
LC_0190
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
LC_0309
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
LC_0305
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
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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.
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
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
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
LC_0225
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
%B 20 40 40 70 20
LC_0310
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
LC_0312
482
Environmental
Phenols on Pinnacle DB C18
1
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.:
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.:
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
min.
diquat 308nm
100g/mL
Column: Cat. #: Dimensions: Particle size: Conditions: Mobile phase: Flow: Temp.: Det.: Sample: Inj.: Conc.:
40g/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.
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
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
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
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.
484
Environmental
Polynuclear Aromatic Hydrocarbons on Pinnacle II PAH
Sample: Inj.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
10
H P LC A P P L I C AT I O N S
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
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
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
LC_0317
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
LC_0318
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
%B 50 60 100 100 50
LC_0315
%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
LC_0316
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
LC_0295
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
LC_0270
LC_0269
488
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
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
6 1 4 5 3
4
LC_0057
8 min.
10
15
LC_0056
20
25 min.
489
Peak List: Ret. time (min.) 1. caffeine 2.733 2. acetylsalicylic acid 4.588 3. benzoic acid 7.738
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
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.:
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.
490
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
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
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
491
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
free literature
For more information about Pinnacle DB columns, request applications note #59742.
LC_0249
492
H P LC A P P L I C AT I O N S
LC_0233
LC_0234
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
493
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H P LC A P P L I C AT I O N S
LC_0162
LC_0278
LC_0286
494
5L methanol
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
LC_0284
LC_0283
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
www.restek.com
1
4
LC_0058
8 min.
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.:
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.
0
LC_0163
3
LC_0200
6 min.
496
4 2
H P LC A P P L I C AT I O N S
min.
LC_0184
LC_0187
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
497
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
4
LC_0174
min.
LC_0165
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
LC_0166
LC_0175
498
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
10L methanol
H P LC A P P L I C AT I O N S
10
LC_0198
12
14
16
18 min.
LC_0195
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
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.
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.
500
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.:
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
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
LC_0227
LC_0167
501
H P LC A P P L I C AT I O N S
4
LC_0155
10 min.
4
LC_0181
7 min.
4
LC_0156
10 min.
LC_0160
502
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
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
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
0
LC_0176
3
LC_0177
min.
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
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
3
LC_0142
6 min.
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
504
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
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
0
LC_0297
6
LC_0153
9 min.
505
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
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.
506
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.
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
507
Peak List: 1. fructose 2. glucose Sample: Inj.: Solvent: 10.0L 10% cola in solvent acetonitrile:water (70:30, v/v)
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.
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
10
LC_0148
12
14
16
18 min.
LC_0251
508
H P LC A P P L I C AT I O N S
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
Pharmaceutical
Analgesic Acetaminophen on Pinnacle II C18
1
509
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
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
20mM ammonium acetate, pH 4.5: acetonitrile (85:15, v/v) 1.0mL/min. 30C UV @ 280nm
3 4
min.
LC_0082
LC_0218
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:
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:
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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LC_0209
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
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
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
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:
A: 20mM potassium phosphate monobasic pH=2.5 B: methanol (90A:10B, v/v) 1.5mL/min. 27C UV @ 284nm
LC_0213
LC_0210
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
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
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
H P LC A P P L I C AT I O N S
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
5
LC_0062
9 min.
LC_0250
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)
LC_0091
LC_0071
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
H P LC A P P L I C AT I O N S
LC_0090
LC_0092
Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase: Flow rate: Temp.: Det.:
Column: Cat. #: Dimensions: Particle size: Pore size: Conditions: Mobile phase:
LC_0086
LC_0074
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
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
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.
516
Pharmaceutical
Antiasthmatic Beclomethasone on Ultra C18
1 1
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
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
1.0
2.0 min.
5
LC_0101
9 min.
LC_0124
Pharmaceutical
Antibiotic Cephaloridine on Ultra IBD (Reversed Phase)
1
517
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
min.
10 min.
LC_0102
LC_0094
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
518
Pharmaceutical
Antibiotic Penicillin V on Ultra IBD
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
10
12.5
15
17.5 min.
LC_0096
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
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
0 0 2 4 6 8
LC_0067
5
LC_0053
9 min.
10
12
14 min.
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
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
9 min. 0
8
LC_0079
10
12
14 min.
LC_0112
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
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3
LC_0069
min.
520
Pharmaceutical
Anti-inflammatory Naproxen on Pinnacle DB Cyano
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.
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
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.
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
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.
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
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
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
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1 3
5
LC_0186
9 min.
Pharmaceutical
Hormones -Estradiol, Norethindrone and Ethynyl Estradiol on Ultra C18
3
523
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
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.
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
6 min.
6 min.
LC_0085
LC_0099
524
Pharmaceutical
Hormones Norgestrel and Ethynyl Estradiol on Allure Basix
Sample: Inj.: Conc.: Solvent: Column: Cat. #: Dimensions: Particle size: Pore size:
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
6
LC_0100
min.
2.5
7.5
10
12.5
LC_0116
15
17.5
20
22.5 min.
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.
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
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
0.5
1.5
2
LC_0083
2.5
3.5
min.
5
LC_0084
9 min.
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
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
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.:
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
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: 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
0
LC_0212
min.
LC_0088
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.
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
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
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
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.
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
Rtx-502.2
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
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
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
Rtx-502.2
Rtx-624
270
240
no
Rtx-200
13/17,36/37
320
240
no
Rtx-35
2/3,
270
240
no
Rtx-50
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.
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).
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
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.
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
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
63 40 59
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
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
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
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
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)
534
Volatiles
Volatile Organics US EPA Method 502.2 Rtx-502.2
14
16
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
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
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
Volatiles
Volatile Organics US EPA Method 601/602 Rtx-502.2
Confirmation column to Rtx-VGC.
535
36 35
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
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
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
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
Volatiles
Volatile Organics US EPA Method OLC 03.2 Rtx-VMS
537
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
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
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.:
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
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
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
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)
53-55 60,61
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
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
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
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
55-56 57 59 54
93,94
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
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.
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
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.
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).
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
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
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
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
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
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
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
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
Semivolatiles
Phthalate Esters US EPA Method 606 Rtx-5
2 2
547
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
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
1. 2. 3. 4.
1
1. 2. 3. 4.
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
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
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
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
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
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
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
2 3 4 1 5 6
7 8 9 10 12 11
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
www.restek.com
Phone: 800-356-1688 or 814-353-1300 www.restek.com
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.
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
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
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
3 1
1. 2. 3. 4. 5. 6. 7. 8. 9.
10
aniline benzyl alcohol 2-methylphenol 4-methylphenol benzoic acid 4-chloroaniline 2-methylnaphthalene 2,4,5-trichlorophenol 2-nitroaniline dibenzofuran 3-nitroaniline 4-nitroaniline
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
40C to 280C @ 8C/min. (hold 15 min.) 200C / 300C helium 20cm/sec. (flow rate: 2.5cc/min.)
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
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
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.:
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
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
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
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
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
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
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
Semivolatiles
Semivolatile Organics US EPA Method 8270 Rtx-5Sil MS
559
please note
highlighted regions from c-grams on page 558.
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
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
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
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
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
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
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
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)
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
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.
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
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.)
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
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
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
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
19
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
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
GC_EV00635
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
572
Pesticides
Organochlorine Pesticides US EPA Method 8081 Stx-CLPesticides & Stx-CLPesticides2
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
11 13 14 16 15 17 20 18 10 9 12 8 22 4 2 3 21
10
11
12
13
min.
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
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)
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
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
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
www.restek.com
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
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
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
Pesticides
Organochlorine Pesticides US EPA Method 8081 Rtx-5
20 22
577
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
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
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
Pesticide Standards
For more information on the ChemService product line, please see page 377 or visit www.restek.com/csi.
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
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
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
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
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
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
GC_EV00696
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
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
50
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
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
582
Pesticides
Organophosphorus Pesticides US EPA Method 8140/8141/8141A Rtx-1
31,32,33
51
13 43,44 24,25 42
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
Pesticides
Organophosphorus Pesticides (European) Rtx-CLPesticides
583
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
www.restek.com
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
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.
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.
min.
10
15
GC_EV00089
20
25
30
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
Herbicides
Chlorophenoxyacid Herbicides US EPA Method 615 Rtx-35
587
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
11
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
588
Herbicides
Triazine Herbicides US EPA Method 619 Rtx-50, Rtx-200
6
3,7
3 4
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
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
Herbicides
Chlorophenoxyacid Herbicides US EPA Method 8151 Rtx-CLPesticides & Rtx-CLPesticides2
9
589
Rtx-CLPesticides
10
17
12 11 4 14,15 16
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
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.
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
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
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
592
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
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
593
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
min.
6 GC_EV00098
min.
6 8 GC_EV00099
10
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
594
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
Rtx-CLPesticides
min.
Rtx-CLPesticides2
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
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
DCB
596
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
min.
Rtx-CLPesticides2
min.
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
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
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
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
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
also available
For Rtx-Dioxin2 columns designed specifically for dioxin/furan analysis, see page 66.
min.
10
GC_EV00108
12
14
16
18
20
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
2 1
min.
10
12
GC_EV00109
14
16
18
20
22
Endocrine Disruptors
Endocrine Disruptors: Alkyl Phenols Rtx-5MS
1. 2. 3. 4. 5. 6. 7. 8.
3 5 6
601
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
1. 2. 3. 4. 5. 6.
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
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.
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
www.restek.com
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
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
604
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
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)
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
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.
606
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
GC_EV00692
607
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
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
608
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
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
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
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
610
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
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.
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
GC_EV00670
612
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.
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613
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_EV00668
GC_EV00669
614
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
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
Glycols
Glycols Rtx-Wax
615
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
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
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.
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
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
Haloacetic Acids
Haloacetic Acids US EPA Method 552.2 Rtx-5
617
10 8
6/7 5
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
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
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)
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
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
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
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
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
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
min.
10
15
20
GC_EV00022
25
30
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.
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.
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
1,3-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
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
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
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
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
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
626
Chiral Separations
Menthol - Rt-DEXsp
2 1
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
-lactones - Rt-DEXcst
4 3 2 1
1. 2. 3. 4. 5.
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.
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
Chiral Separations
Apple Juice with Added Standards Rt-DEXsm
3
627
1. 2. 3. 4.
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
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.
1. 2. 3. 4.
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.
628
Chiral Separations
Grape Juice Extract Rt-DEXsa
4
1. 2. 3. 4.
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. 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.
www.restek.com
Phone: 800-356-1688 or 814-353-1300 www.restek.com
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
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
1. 2. 3. 4. 5. 6.
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
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.
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
Fatty Acids
Fatty Acids (Free) Stabilwax-DA
631
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.)
632
FAMEs
FAMEs (AOAC 996.06 Standard) Rt-2560
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
FAMEs
FAMEs (NLEA Mix) Rt-2560
633
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)
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)
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)
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
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)
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:
min.
12
16
20
24
GC_FF00123
28
32
36
40
44
48
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
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
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
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
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
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
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
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
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.
1. 2. 3. 4. 5. 6.
1 1
3 5 2
min. min. 20
GC_FF00363
20
GC_FF00364
40
40
1. 2. 3. 4. 5. 6.
1. 2. 3. 4. 5.
5 3 6
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
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
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
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
-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
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.
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
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
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
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.
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
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
12
16
20
24
32
36
40
44
52
56
60
64
72 valencene geranial carvone geranyl acetate d/l carveol -ionone d/l carveol -ionone
GC_FF00537
-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
644
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:
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
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
645
acetaldehyde methanol ethanol acetone ethyl formate isopropanol n-propanol ethyl acetate
10
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.
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
646
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.
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
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
648
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
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
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
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
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
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
Sterols
Sterols (Olive Oil) XTI-5
1. 2. 3. 4. 5. 6. 7. 8. cholesterol brassicasterol campesterol stigmasterol -sitosterol avenasterol-d5 erythrodiol uvacol
651
1. 2. 3. 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
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.
Sterols XTI-5
3 2
1. 2. 3. 4. 5. 6. 7. 8. 9.
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
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
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.)
2 3 4
5 6
78
9 10 11
12
13
14
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
653
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
3 1
1. 2. 3. 4. 5. 6.
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
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
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
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:
4 3
1. 2. 3. 4. 5. 6.
4 3 1 1
min.
min.
GC_PH00239
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
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
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
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
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
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.
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
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.
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
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.
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
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.
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
min.
10
20
30
40
GC_MS00275
50
60
70
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
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
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
662
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
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
Permanent Gases
Permanent Gases ShinCarbon ST
(micropacked)
663
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
1 3 4
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
664
Permanent Gases
Permanent Gases Molecular Sieve 5A and Molecular Sieve 13X
1
1. 2. 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
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)
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
Permanent Gases
Permanent Gases Rt-QPLOT
1 2 1
665
1. 2. 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
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
Detector
[
1 B
1. 2. 3. 4. 5. 6. 7.
Terrific separation!
2 4
ARt-QPLOT
2, 3, 4, 7
BRt-Msieve 5A
3
30C 20L, split injection (10:1), 5% each compound hydrogen, 8psi HP TCD 200C
7
1 2
6 5
min.
10
12
14
Rt-QPLOT
Rt-Msieve 5A
GC_PC00171
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
8,9
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
5,6
8 9 7
14 13 11 12 15
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
1. 2. 3. 4. 5. 6. 7.
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.
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
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
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)
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.
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
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
Hydrocarbon Gases
Hydrocarbon Gases Porous Polymer PLOTs
2,4
669
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.
5 6
min.
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
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
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
2 5 3 7 1 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
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.
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 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
1. 2. 3. 4.
1. 2. 3. 4. 5.
1. 2. 3. 4. 5.
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
672
Hydrocarbon Gases
Propane Fuel Rtx-1
3 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.
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
2 3
6 8
1 9 10 11 13 15 12 14
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
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.
674
Hydrocarbons
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.
1. 2. 3. 4. 5.
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.
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.
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
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
676
Hydrocarbons
Aromatics (Benzene/Toluene/Xylene) MXT-WAX
1
1. 2. 3. 4. 5. 6.
4,5
1. 2. 3. 4. 5. 6.
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
1. 2. 3. 4. 5. 6.
1. 2. 3. 4. 5. 6.
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
Hydrocarbons
Aromatics (Xylene Isomers plus Cumene) 5% RT-1200/1.75% Bentone 34 on 100/120 Silcoport
1 2
677
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
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
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
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
3 22 5 7 9 12 11 24 13 14 15 16 18 19 21 23 25
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
Hydrocarbons
Detailed Hydrocarbons Analysis Rtx-1PONA
10
679
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
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.
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.
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
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
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
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
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
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
Hydrocarbons
Carnauba Wax Rtx-1 Petroleum Wax Rtx-1
683
5 2 3 4
1. 2. 3. 4. 5. 6. 7. 8. 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
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
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
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
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.
685
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
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.
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
686
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.)
12
13
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.
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
10
11
6 5
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
688
Sulfur Compounds
Sulfur in Gasoline Rtx-1
6
1. 2. 3. 4. 5. 6. 7. 8.
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
1. sulfur dioxide
5 6 8 9 7 3 2 10 11 14 4 min. 0 4 GC_PC00200 8 12 13
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
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
www.restek.com
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.
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.
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.
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
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
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
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
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
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.
693
10
11
4 3 1 2 5 6 8
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
3,5
28,29
14
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
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
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
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
Basic Drugs
Underivatized Benzodiazepines (Basic Drugs) Rtx-200
695
5,6 1 3 12 7 4 2 8 9 10 11 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
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
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
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
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
698
Chiral Analyses
Fenafluramine (TFAA Derivative) Rt-DEXcst
1
1. 2. 3. 4.
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
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
1. (+/-)-hexobarbital 2. (+/-)-mephobarbital
30m, 0.32mm ID, 0.25m Rt-DEXcst (cat.# 13102) On-column conc.: 25ng/enantiomer
2 1
60C (hold 1 min.) to 220C @ 3C/min. hydrogen 80cm/sec. set @ 60C FID set @ 220C
min.
10
20 GC_PH00245
30
40
50
1. 2. 3. 4.
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
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
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
700
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
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
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
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
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
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.
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.
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.
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
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
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
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
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
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
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
min.
10
15
20
25 GC_CH00341
30
35
40
45
50
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
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
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. 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:
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
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
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
min.
12 GC_CH00346
16
20
24
2 3 4 5 6
1. 2. 3. 4. 5. 6. 7. 8.
acetaldehyde acetone ethyl formate ethyl acetate methanol ethanol n-propanol isobutanol
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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
Solvents
Solvents Rtx-Volatiles
1 3 6 1 2 3
713
1. 2. 3. 4. 5. 6. 7.
1. 2. 3. 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
2 4 5 7
min.
12
16
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
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
714
Solvents
Solvents, Polar Rt-QPLOT
1 3 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.
5 3
1. 2. 3. 4. 5. 6. 7.
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 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
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
Solvents
Solvents, USP Rtx-1
715
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
716
Solvents
Solvents, USP Rtx-200
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
Solvents
Pentane (lot purity analysis) MXT-1
LOT A
1
717
LOT B
1
1. pentane
www.restek.com
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
1. 2. 3. 4. 5. 6. 7. 8.
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.
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
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
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
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
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
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
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
7. 8. 9. 10. 11.
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
10
7 8
11 12 13
3 4 2
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
722
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
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.
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
724
Amines
Ethanolamines Rtx-5 Amine
1 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
2 4
GC_CH00585
1. 2. 3. 4. min. 5
GC_CH00296
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
1. 2. 3. 4. 5. 6. 7.
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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
Amines
Amines & Phenols Rtx-5 Amine
4 9
725
5 3 1 2 13 11
8 6 10
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
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
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.
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
Amines
Amines (low MW) Stabilwax-DB
4
727
1. 2. 3. 4. 5. 6. 7. 8. 9.
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
Amines/Alcohols/Chlorides Stabilwax
2 4 6 7 9 10
16 17
11
1 7 8 9 5 3 8 12
5 6
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
728
Aromatics
Aromatics Rtx-502.2
12 10, 11 13
3 5 6 2 4 1 8
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
Aromatics
Aromatics Stabilwax
6 8 10
729
1. 2. 3. 4. 5. 6.
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
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
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
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.
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
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.
1. 2. 3. 4. 5. 6.
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
732
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.)
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
733
15 3
8 1 11 17
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
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
Glycols; Ketones
Glycols Rtx-200
2 3 1 1 4
735
1. 2. 3. 4.
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
736
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.
1. 2. 3. 4. 5.
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.
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.
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
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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