Metler Toledo Ttitrator

METTLER TOLEDO Titrators
Dedicated to Mr. Kees Mooibroek
Characteristic Values
Applications brochure 10
Contents
M084 M228 M229 M230 M231 M076 M086 M232 M087 M233 M090 M091 M234 M095 M235 M236 M096 M051 M211 M206 M237 M624 M238 M239 M517 M518 M519 Determination of Acid Values in Organic Solvents, Oils, Fats, Polymers ...................... 1 Acid Number of Castor Oil.................................................................................... 4 Acid NUmber of Cosmetic Creams......................................................................... 7 Neutralizing Value of Baking Powder................................................................... 10 Acid Number of Polyester................................................................................... 13 Free Fatty Acid of Oil and Fat .............................................................................. 16 Epoxide Values ................................................................................................. 19 Epoxide Value of 2,3-Epoxypropylene-Phenyl Ether .............................................. 22 Bromine Number of Petroleum Distillates and Aliphatic Olefins ............................... 25 Low Bromine Index Determination of a Standard Solution ...................................... 28 Determination of Saponification Value ................................................................. 31 Determination of Hydroxyl Value ......................................................................... 34 Hydroxyl Value of Polyols .................................................................................. 37 Determination of Isocyanate Content ................................................................... 40 NCO-Content of Isocyanates by Back-Titration ...................................................... 43 Determination of Free HCl and Isocyanates .......................................................... 46 Iodine Value in Resins and Oils According to Wijs ................................................. 49 Iodine Value of Edible OIls and Fats According to Wijs (AOAC Method 28.023) ........ 52 Iodine Value of Cosmetic Fats According to Wijs ................................................... 55 Determination of Carboxyl Groups in PET ............................................................ 58 Peroxide Value of Lecithin .................................................................................. 61 Peroxide Value of Edible Oils and Fats ................................................................. 64 Determination of Permanganate Index in Waste Water .......................................... 67 Chemical Oxygen Demand (COD) of Waste Water ................................................ 70 Blank Determination According to ASTM D664-89 ................................................ 73 Blank Determination According to ASTM D4739-92.............................................. 76 Acid Number (AN) According to ASTM D664-89 .................................................. 79
M520 M057 M058 M059 M099 M100 M061 M240 M241/1 M241/2 M241/3 M242 M243 M244 M258 M259
Base Number (BN) According to ASTM D4739-92 ............................................... 82 TBN According to ASTM D2896-85 .................................................................... 85 TBN According to ASTM D4739-87 .................................................................... 88 TAN According to ASTM D664-89 ....................................................................... 91 Conductometric Base Number Titration of Motor Oil............................................... 94 Standardization of HCl in Isopropanol by Conductometric Titration .......................... 97 pH, Acidity, Lactone and Formol Value of Honey................................................. 100 Formol Number, Acidity and True Brix Value of Orange Juice ............................... 103 Carbon Black Surface Area (ASTM D3765-99): Standardization .......................... 106 Carbon Black Surface Area (ASTM D3765-99): Linear Regression........................ 109 Carbon Black Surface Area (ASTM D3765-99): Sample Titration .......................... 112 Determination of Amine Number ....................................................................... 115 Free Available Chlorine Residual in Water According to ASTM D1253-86 .............. 118 Total Residual Chlorine in Water According to ASTM D1253-86 ........................... 121 Total Base Number According to DIN ISO 3771 .................................................. 124 CTAB Surface Area on Amorphous Silica ............................................................ 127
METTLER TOLEDO
M084
Determination of Acid Values in Organic Solvents, Oils, Fats, Polymers

The acid number is the amount of potassium hydroxide used to neutralized acidic components in different samples (mg KOH/g). Here the determination of the acid value according to DIN 53402 (1973) is presented. Sample
Organic solvents, resins, oils, fats fatty acids, softeners, polymers
Preparation and Procedures

Solvent mixture according to DIN 53402 (1973): Toluene:ethanol 2:1 Hints: 1) Ensure good stirring. Speed and stirring time can be adapted iaccording to the viscosity or the bad solubility of the sample. 2) If the dissolution of the sample is not straightforward, heating my be applied to improve it. Ultrasonics can also be applied. 3) The titration can also indicated photometrically by a phototrode and a color indicator. It can be affected by the limitations of the indicators, by the formation of precipitates, or by change in turbidity. 4) Use the same amount of solvent mixture for the blank as well as for the sample determination. 5) Substances which undergo side reactions with the alkaline titrant can not be titrated.
Substance Chemicals
Acidic components
40 mL solvent mixture: Toluene:ethanol 2:1
Titrant
KOH in Ethanol: c(KOH) = 0.1 mol/L, c(KOH) = 0.01 mol/L Potassium hydrogen phthalate DL50Graphix, DL53/55/58 DL70ES, DL77
Standard Instruments
Accessories
1 additional burette DV1005, 1 additional burette DV1020 100 mL titration beaker ME-101974 AT261 balance, Printer DG113-SC
Remarks
This application describes the determination of the acid value of resins, oils, fats, fatty acids, solvents, softeners, polymers and other technical organic products. Due to better solubility properties, this kind of titration is often carried out in a binary solvent mixture. The titrant is dissolved in a solvent wich is miscible with the solvent mixture, i.e. in ethanol or methanol. If needed, an auxiliary solvent like acetone can be added to improve solubility. The whole acidic components are neutralized, including half of the acid anhydride. Since the content of free anhydride is small, this error can be generally neglected. On the other hand, if significant amounts of anhydride are present, an additional titration with aqueous potassium hydroxide solution must be performed to determine the second missing half anhydride.
Indication Chemistry
OH- + H+ = H2O
Calculation
Blank determination (Meth. 084B): R1 = Q R1 is stored as aux. value H8 Acid value determination (Meth: 084A): R1 = (Q1 - H8)*C1/m ; C1 = 56.1
Results
Waste disposal
Organic solvent waste (chlorinated and not chlorinated)
Literature: DIN 53402, 51588 ISO 3682
Author
Kees Mooibroek
Results
Method 084A Acid Values, Solvent Blank 13-Apr-1994 User K.M. Measured 13-Apr-1994 11:09 RESULTS No ID1 ID2 Sample amount and results 1/1 Solv.Bl. Blank 40.0 g Weight m R1 = 0.006 mmol Blank Acid No 1/2 Solv.Bl. Blank 40.0 g Weight m R1 = 0.005 mmol Blank Acid No 1/3 Solv.Bl. Blank 40.0 g Weight m R1 = 0.005 mmol Blank Acid No 1/4 Solv.Bl. Blank 40.0 g Weight m R1 = 0.001 mmol Blank Acid No STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation Outlier test : sample No. Number results R1 Mean value Standard deviation Rel. standard deviation AUXILIARY VALUE New value Method User Measured n x s srel n x s srel H8 = = = = = = = = 4 0.004 0.002337 59.191 1/4 3 0.004 0.000592 11.626 10:38
mmol mmol % mmol mmol %
Blank Acid No Blank Acid No
Blank Acid No Blank Acid No
= 0.005091
Blank Acid No 15-Apr-1994 14:35
084B Acid Values (non aqueous) K.M. 15-Apr-1994 16:18
RESULTS No ID1 ID2 Sample amount and results 1/1 Acid val Terpentine 43.003 g Weight m R1 = 0.290 mg KOH/g Acid value 1/2 Acid val Terpentine 42.662 g Weight m R1 = 0.304 mg KOH/g Acid value ................................................................ 1/7 Acid val Terpentine 42.896 g Weight m R1 = 0.300 mg KOH/g Acid value STATISTICS Number results R1 n = 7 Mean value x = 0.298 mg KOH/g Acid value Standard deviation s = 0.004793 mg KOH/g Acid value Rel. standard deviation srel = 1.606 % Outlier test: no outliers!
Table of measured values
Titration curve
Method
Method 084B Version Acid values (non aqueous) 15-Apr-1994 14:35 Method 084A Version Acid Values, Solvent Blank 13-Apr-1994 10:38 Title Method ID . . . . . . . . . . . . . 084B Title . . . . . . . . . . . . . . . Acid values (non aqueous) Date/time . . . . . . . . . . . . . 15-Apr-1994 14:35 Sample Number samples . . . . . . . . . . . 7 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.0 Upper limit [g] . . . . . . . . . 50.0 ID1 . . . . . . . . . . . . . . . . Acid val Molar mass M . . . . . . . . . . . . 0.0 Equivalent number z . . . . . . . . 1 Temperatur sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 60 Time [s] . . . . . . . . . . . . . . 60 Titration Titrant . . . . . . . . . . . . . . KOH (Isoprop.) Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 1.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 500 EQP range . . . . . . . . . . . . Yes Limit A [mV, pH,...] . . . . . +500 Limit B [mV, pH,...] . . . . . -500 Maximum volume [mL] . . . . . . . 20.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure. . . . . . . Standard Calculation Result name . . . . . . . . . . . . Acid Value Formula . . . . . . . . . . . . . . R1=(Q1-H8)*C1/m Constant . . . . . . . . . . . . . . C1=56.1 Result unit . . . . . . . . . . . . mg KOH/g Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Printer Results last sample . . . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Outlier test . . . . . . . . . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes Title Method ID . . . . . . . . . . . . . 084A Title . . . . . . . . . . . . . . . Acid Values, Solvent Blank Date/time . . . . . . . . . . . . . 13-Apr-1994 10:38 Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.0 Upper limit [g] . . . . . . . . . 50.0 ID1 . . . . . . . . . . . . . . . . SolvBl. Molar mass M . . . . . . . . . . . . 0.0 Equivalent number z . . . . . . . . 1 Temperatur sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 60 Time [s] . . . . . . . . . . . . . . 60 Titration Titrant . . . . . . . . . . . . . . KOH (Isoprop.) Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 500 EQP range . . . . . . . . . . . . Yes Limit A [mV, pH,...] . . . . . +500 Limit B [mV, pH,...] . . . . . -500 Maximum volume [mL] . . . . . . . 20.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure. . . . . . . Standard Calculation Result name . . . . . . . . . . . . Blank Acid No Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Printer Results last sample . . . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Outlier test . . . . . . . . . . . . Yes Auxiliary value ID text . . . . . . . . . . . . . . Blank Acid No. Formula . . . . . . . . . . . . . . H8=x Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes
METTLER TOLEDO
M228
Acid Number of Castor Oil

Determination of the acid number of castor oil according to DAB (Deutsches Arzneimittelbuch).
Sample
Castor oil, 9-11 g

1 mL hydrochloric acid 0.1 mol/L is added to both solvent and sample solutions (Spiking)
Substance Chemicals
Acidic components
50 mL toluene 1 mL hydrochloric acid
Titrant
KOH in Ethanol: c(KOH) = 0.1 mol/L,
Potassium hydrogen phthalate DL50Graphix, DL53/55/58 DL70ES, DL77
Accessories
100 mL titration beaker ME-101974 Printer Balance
Remarks Indication Chemistry

DG113-SC
1) One mL hydrochloric acid has been added to both 50 mL solvent and samle solution to test the system (spiking). 2) The first equivalent point is due to the neutralization of 1 mL hydrochloric acid. The method has been programmed to detect only the second equivalent point.
Calculation
Blank determination (Meth. SZ-bw): R1 = Q R1 is stored as auxiliary value H4 Acid value det. (Meth: SZtit): R1 = (Q1 - H4)*C1/m C1 = 56.1
Results
Waste disposal
Organic solvent waste
Literature: DAB
Author
Dieter Rehwald
Results
METTLER TOLEDO DL58 Method Measured User ALL RESULTS No 1 2 3 4 5 ID Sample amount and results 12.4 R1 = 5.308 R2 = 0.601 9.4 R1 = 4.989 R2 = 0.603 10.6 R1 = 5.131 R2 = 0.610 11.6 R1 = 5.225 R2 = 0.602 9.6 R1 = 5.034 R2 = 0.616 g ml mg g ml mg g ml mg g ml mg g ml mg VBR. TM Surezahl VBR. TM Surezahl VBR. TM Surezahl VBR. TM Surezahl VBR. TM Surezahl Titrator V2.1 RatzFatz *1999* Team Ost:ms/rd 030-35503603 Help-Hotline: 0172-2727849 22-Feb-1999 19:42
SZtit Surezahl Rizinull/DAB 22-Feb-1999 20:48 DR
KOH/g KOH/g KOH/g KOH/g KOH/g
STATISTICS Number results R2 Mean value Standard deviation Rel. standard deviation Sample No. 5 deleted
n x s srel
= = = =
4 0.604 0.00377 0.625
mg KOH/g Surezahl mg KOH/g Surezahl %
Titration curve
Method
Method SZtit Version Surezahl Rizinusl/DAB 22-Feb-1999 19:42 Method SZ-bw Version Blank value with EQP tit. 23-Feb-1999 17:09 Title Method ID . . . . . . . . . . . . . SZtit Title . . . . . . . . . . . . . . . Surezahl Rizinusl/DAB Date/time . . . . . . . . . . . . . 22-Feb-1999 19:42 Sample Sample ID . . . . . . . . . . . . . Entry type . . . . . . . . . . . . . Weight Lower limit [g] . . . . . . . . . 9.0 Upper limit [g] . . . . . . . . . 11.0 Molar mass M . . . . . . . . . . . . 56.1 Equivalent number z . . . . . . . . 1 Titration stand . . . . . . . . . . Stand 1 Temperatur sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 20 EQP Titration Titrant . . . . . . . . . . . . . . KOH/EtOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113 Unit of meas. . . . . . . . . . . . mV Predispensing . . . . . . . . . . . No Titrant addition . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . 8.0 dV(min) [mL] . . . . . . . . . . 0.02 dV(max) [mL] . . . . . . . . . . 0.3 Measure mode . . . . . . . . . . . . Equilibrium controlled dE [mV] . . . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . 30.0 Recognition Threshold . . . . . . . . . . . . 100 Steepest jump only . . . . . . . Yes Range . . . . . . . . . . . . . . Yes Limit A [mV, pH,...] . . . . . -100 Limit B [mV, pH,...] . . . . . -500 Tendency . . . . . . . . . . . . Negative Termination Maximum volume [mL] . . . . . . . 10.0 at potential . . . . . . . . . . Yes Potential [mV, pH,...] . . . . -450 at slope . . . . . . . . . . . . No after number EQPs . . . . . . . . No comb. termination conditions . . No Evaluation Procedure . . . . . . . . . . . . Standard Potential 1 . . . . . . . . . . . No Potential 2 . . . . . . . . . . . No Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0 Calculation Formula . . . . . . . . . . . . . . R1=VEQ Constant . . . . . . . . . . . . . . Decimal places . . . . . . . . . . . 3 Result unit . . . . . . . . . . . . ml Result name . . . . . . . . . . . . VBR. TM Statistics . . . . . . . . . . . . . No Calculation Formula . . . . . . . . . . . . . . R2=(Q-H4)*C2/m Constant . . . . . . . . . . . . . . C2=M/z Decimal places . . . . . . . . . . . 3 Result unit . . . . . . . . . . . . mg KOH/g Result name . . . . . . . . . . . . Surezahl Statistics . . . . . . . . . . . . . Yes Calculation Formula . . . . . . . . . . . . . . Constant . . . . . . . . . . . . . . Decimal places . . . . . . . . . . . 0 Result unit . . . . . . . . . . . . Result name . . . . . . . . . . . . Statistics . . . . . . . . . . . . . Report Output unit . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . No All results . . . . . . . . . . . . Yes Raw results . . . . . . . . . . . . No Table of values . . . . . . . . . . Yes Sample data . . . . . . . . . . . . No E - V curve . . . . . . . . . . . . Yes dE/dV - V curve . . . . . . . . . . Yes d2E/dV2 - V curve . . . . . . . . . No log dE/dV - V curve . . . . . . . . No E - t curve . . . . . . . . . . . . No V - t curve . . . . . . . . . . . . No dV/dt - t curve . . . . . . . . . . No Title Method ID . . . . . . . . . . . . . SZ-bw Title . . . . . . . . . . . . . . . Blank value with EQP tit. Date/time . . . . . . . . . . . . . 23-Feb-1999 17:09 Sample Sample ID . . . . . . . . . . . . . Entry type . . . . . . . . . . . . . Volume Volume [mL] . . . . . . . . . . . 50.0 Molar mass M . . . . . . . . . . . . 56.1 Equivalent number z . . . . . . . . 1 Titration stand . . . . . . . . . . Stand 1 Temperatur sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 20 EQP Titration Titrant . . . . . . . . . . . . . . KOH/EtOH Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113 Unit of meas. . . . . . . . . . . . mV Predispensing . . . . . . . . . . . No Titrant addition . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . 8.0 dV(min) [mL] . . . . . . . . . . 0.02 dV(max) [mL] . . . . . . . . . . 0.3 Measure mode . . . . . . . . . . . . Equilibrium controlled dE [mV] . . . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . 30.0 Recognition Threshold . . . . . . . . . . . . 200 Steepest jump only . . . . . . . Yes Range . . . . . . . . . . . . . . Yes Limit A [mV, pH,...] . . . . . -100 Limit B [mV, pH,...] . . . . . -500 Tendency . . . . . . . . . . . . Negative Termination Maximum volume [mL] . . . . . . . 10.0 at potential . . . . . . . . . . Yes Potential [mV, pH,...] . . . . -450 at slope . . . . . . . . . . . . No after number EQPs . . . . . . . . No comb. termination conditions . . No Evaluation Procedure . . . . . . . . . . . . Standard Potential 1 . . . . . . . . . . . No Potential 2 . . . . . . . . . . . No Stop for reevaluation . . . . . . No Calculation Formula . . . . . . . . . . . . . . R1=Q Constant . . . . . . . . . . . . . . Decimal places . . . . . . . . . . . 3 Result unit . . . . . . . . . . . . mmol Result name . . . . . . . . . . . . Statistics . . . . . . . . . . . . . Yes Calculation Formula . . . . . . . . . . . . . . Constant . . . . . . . . . . . . . . Decimal places . . . . . . . . . . . 0 Result unit . . . . . . . . . . . . Result name . . . . . . . . . . . . Statistics . . . . . . . . . . . . . Auxiliary value ID text . . . . . . . . . . . . . . Blindwert Formula . . . . . . . . . . . . . . H4=x Report Output unit . . . . . . . . . . . . Printer Results . . . . . . . . . . . . . . No All results . . . . . . . . . . . . Yes Raw results . . . . . . . . . . . . No Table of values . . . . . . . . . . Yes Sample data . . . . . . . . . . . . No E - V curve . . . . . . . . . . . . Yes dE/dV - V curve . . . . . . . . . . Yes d2E/dV2 - V curve . . . . . . . . . No log dE/dV - V curve . . . . . . . . No E - t curve . . . . . . . . . . . . No V - t curve . . . . . . . . . . . . No dV/dt - t curve . . . . . . . . . . No
METTLER TOLEDO
M229
Acid Number of Cosmetic Creams

Determination of the acid number of cosmetic creams
Sample
Cosmetic creams, 1-2 g

1) A ethanol:toluene 1.1 mixture is used to dissolve the cosmetic creams.
Substance Chemicals
Acidic components
2) To ensure complete dissolution, the sample solution is dissolved under stirring at 40C.
25 mL ethanol 25 mL toluene
Titrant
KOH in Ethanol: c(KOH) = 0.1 mol/L
Accessories

DG113-SC
1) The customer always titrates manually to the phenolphtalein colour change. Therefore an endpoint titration was performed to an absolute Ep value of -310 mV, although this point has no real meaning. 2) In addition, an EQP titration was performed. Two equivalence points have been found. 3) The arrows in the titration curve indicate two equivalence points due to the presence of at least two acids of different strength.
Calculation
Blank determination (Meth. blv): R1 = Q R1 is stored as auxiliary value H5 Acid value det. (Meth: 40012): R1 = (Q1 - H5)*C1/m C1 = 56.1
Results
Waste disposal
Literature: Application DL40RC No. 117.
Author
U. Bchi/P. Schauwecker
Results
Results from endpoint titration to EPA = -310 mV (phenolphtalien colour change): DL40RC: *** 17-NOV-81 *** 1321 81596 2 5.8836
PROV. 11321 IDENT. SAMPLE NO. *R * TAN STATISTICS: N MEAN STAND.DEV.%
2 5.9188 .84
Titration curve
Method
Method 40012 Version Acid No. Cosm. Cream 11-Dec-2001 10:00 . . . . . . . 40012 . . . . . . . Acid No. Cosm. Cream . . . . . . . 11-Dec-2001 10:00 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Weight 1.0 2.0 56.1 1 Stand 1 Manual Method blv Version Blank value 11-Dec-2001 10:05 Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Lower limit [g] . . Upper limit [g] . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Titrant addition . . . dE(set) [mV] . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Volume [mL] . . . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Titrant addition . . . dE(set) [mV] . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . .
. . . . . . . blv . . . . . . . Blank value . . . . . . . 11-Dec-2001 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Volume 50.0 56.1 1 Stand 1 Manual
10:05
. . . . . . . 50 . . . . . . . 90 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . KOH/EtOH 0.1 DG113 mV No Dynamic 8.0 0.02 0.3 Equilibrium controlled 0.5 1.0 3.0 30.0 100 No No Negative 10.0 No No No No Standard No No Yes neq=0 R1=VEQ 3 ml Consumption No R2=(Q-H5)*C2/m C2=M/z 3 mg KOH/g Acid No. Yes
. . . . . . . 50 . . . . . . . 90 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . KOH/EtOH 0.1 DG113 mV No Dynamic 8.0 0.02 0.3 Equilibrium controlled 0.5 1.0 3.0 30.0 100 No No Negative 10.0 No No No No Standard No No Yes neq=0 R1=Q 3 mmol Yes
dE [mV] . . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . . Tendency . . . . . . . . . . Termination Maximum volume [mL] . . . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs . . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . . Potential 1 . . . . . . . . . Potential 2 . . . . . . . . . Stop for reevaluation . . . . Condition . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Report Output unit . . . . . . . . . . Results . . . . . . . . . . . . All results . . . . . . . . . . Raw results . . . . . . . . . . Table of values . . . . . . . . Sample data . . . . . . . . . . E - V curve . . . . . . . . . . dE/dV - V curve . . . . . . . . d2E/dV2 - V curve . . . . . . . log dE/dV - V curve . . . . . . E - t curve . . . . . . . . . . V - t curve . . . . . . . . . . dV/dt - t curve . . . . . . . .
. . . 0 . . . . . . . . . . . . . . . . Printer No Yes No Yes No Yes Yes No No No No No
dE [mV] . . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . . Tendency . . . . . . . . . . Termination Maximum volume [mL] . . . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs . . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . . Potential 1 . . . . . . . . . Potential 2 . . . . . . . . . Stop for reevaluation . . . . Condition . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Auxiliary value ID text . . . . . . . . . . . . Formula . . . . . . . . . . . . Report Output unit . . . . . . . . . . Results . . . . . . . . . . . . All results . . . . . . . . . . Raw results . . . . . . . . . . Table of values . . . . . . . . Sample data . . . . . . . . . . E - V curve . . . . . . . . . . dE/dV - V curve . . . . . . . . d2E/dV2 - V curve . . . . . . . log dE/dV - V curve . . . . . . E - t curve . . . . . . . . . . V - t curve . . . . . . . . . . dV/dt - t curve . . . . . . . .
. . . 0 . . .
. . Blindwert . . H5=x . . . . . . . . . . . . . . . . . . . . . . . . . . Printer No Yes No Yes No Yes Yes No No No No No
METTLER TOLEDO
M230
Neutralizing Value of Baking Powder

Determination of the neutralizing value of baking powder by titration with sodium hydroxide.
Sample
Baking powder, 10 g Use 5 mL aliquots

1) 100 mL sulphuric acid c(1/2 H2SO4) = 0.5 mol/L are added carefully to the weighed sample and stirred during 10 min. 2) The sample solution is subsequently filtered. CO2 is then removed from the filtrate in an ultrasonic bath. (CO2 can also be removed by heating the solution prior titration). 3) For the titration, 5 mL aliquot samples are taken. Procedure: 1) A known amount of sulphuric acid is added to the sample. 2) Baking powder kan be either acidic or alkaline. Therefore, the result in mmol/g can be negative or positive: Negative result: Baking powder is alkaline (Sulphuric acid amount higher than equivalent value of titrant) Positive result: Baking powder is acidic (Sulphuric acid amount lower than equivalent value of titrant) For a final result in %, multiply with M/(10*z), where M/z is the equivalent mass of the acidic or alkaline compound.
Substance Chemicals
Acidic / basic components
100 mL Sulphuric acid, H2SO4 , c(1/2 H2SO4) = 0.5 mol/L
Titrant
Sodium hydroxide, NaOH c(NaOH) = 0.25 mol/L
Accessories

DG111-SC
1) The method can be used for both alkaline and acidic baking powders. 2) The amount of sulphuric acid added before titration, expressed in mmol, is introduced as auxiliary value H6 in the titrator. 3) The exact amount of sulphuric acid is determined by a similar method using only 5 mL of sulphuric acid (see method "back"). In this way, it is not necessary to perform a standardization of the sulphuric acid solution.
Method "back": H2SO4 + 2 NaOH = Na2SO4 + 2 H2O Method 40013: Acidic/alkaline components
Calculation
Method "back": R1=Q*C1 ; C1=1/z ; mmol H2SO4 R1 stored as aux. value H6 Method 40013 (sample deter.): R2=(H6-Q)*C2/m ; C2=1/z Neutral. value mmol/g Aqueous waste (after neutralization)
Results
Waste disposal
Author
K. Mooibroek/P. Schauwecker
10
Results
DL40RC: *** 20-NOV-81 *** 0.527 85.09 2.5067 1521 85.09 8 .13275
INPUT: WEIGHT IDENT. BLANK MEQ METHOD 118 IDENT. SAMPLE NO. *R * /G
STATISTICS: N MEAN STAND.DEV.% 8 0.12 /G 10.0
Titration curve
11
Method
Method 40013 Version Neutr.Value 11-Dec-2001 Method 11:00 back Version Back value 11-Dec-2001 11:05 Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Volume [mL] . . . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Titrant addition . . . dE(set) [mV] . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Volume [mL] . . . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Titrant addition . . . dE(set) [mV] . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . .
. . . . . . . 40013 . . . . . . . Neutr.Value . . . . . . . 11-Dec-2001 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Baking Pwd. Fixed volume 5.0 100.0 2 Stand 1 Manual
11:00
. . . . . . . Back . . . . . . . Back value . . . . . . . 11-Dec-2001 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . H2SO4 Volume 5.0 98.08 2 Stand 1 Manual
11:05
. . . . . . . 50 . . . . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . NaOH 0.1 DG111 mV No Dynamic 8.0 0.02 0.3 Equilibrium controlled 1.0 4.0 3.0 30.0 60 No No Negative 10.0 No No No No Standard No No Yes neq=0 R1=VEQ 3 ml Consumption No R2=(H6-Q)*C2/m C2=1/z 3 mmol/g Neutral. value Yes
. . . . . . . 50 . . . . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . NaOH 0.25 DG111 mV No Dynamic 8.0 0.02 0.3 Equilibrium controlled 1.0 4.0 3.0 30.0 60 No No Negative 10.0 No No No No Standard No No Yes neq=0 R1=Q*C1 C1=1/z 3 mmol mmol H2SO4 Yes
. . . 0 . . .
. . Back value . . H6=x . . . . . . . . . . . . . . . . . . . . . . . . . . Printer No Yes No Yes No Yes Yes No No No No No
12
METTLER TOLEDO
M231
Acid Number of Polyester

Determination of the acid number of polyester
Sample
Polyester, 0.2-0.4 g
Substance Chemicals
Acidic components
50 mL tetrahydrofuran
Titrant
KOH in Ethanol: c(KOH) = 0.1 mol/L
Accessories

DG113-SC
If needed, a blank value determination is performed. The blank value is stored as auxiliary value H7.
Calculation
Blank determination (Meth. blk): R1 = Q R1 is stored as auxiliary value H7 Acid value det. (Meth: 2): R1 = (Q1 - H7)*C1/m C1 = 56.1
Results
Waste disposal
Author
R. Boehlen, MT-CH
13
Results
METTLER TOLEDO DL58 Titrator V2.4 5121086246 05-04-2001 15:33
Method Measured User ALL RESULTS No 1 ID
2 Surezahl 05-04-2001 15:44 RB
Sample amount and results 0.3113 R1 = 26.78 R2 = 2.08 g mg/g mL Surezahl Verbrauch
Titration curve
14
Method
Method 2 Version Saeurezahl 05-04-2001 Method 15:53 blk Version Blindwert 05-04-2001 15:05 Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Lower limit [g] . . Upper limit [g] . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Titrant addition . . . dE(set) [mV] . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Volume [mL] . . . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Titrant addition . . . dE(set) [mV] . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . .
. . . . . . . 2 . . . . . . . Saeurezahl . . . . . . . 05-04-2001 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Polyester Weight 0.2 0.4 56.1 1 Stand 1 Manual
15:33
. . . . . . . blk . . . . . . . Blindwert . . . . . . . 05-04-2001 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . THF Volume 50.0 56.1 1 Stand 1 Manual
15:05
. . . . . . . 70 . . . . . . . 240 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . KOH/EtOH 0.1 DG113 mV No Dynamic 8.0 0.1 0.5 Equilibrium controlled 0.5 1.0 2.0 20.0 500 No No Negative 20.0 No No Yes 1 No Standard No No No R=(Q-H7)*C/m C=M/z 2 mg/g Saeurezahl Yes R2=VEQ 2 mL Verbrauch Yes
. . . . . . . 50 . . . . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . KOH/EtOH 0.1 DG113 mV No Dynamic 8.0 0.02 0.5 Equilibrium controlled 0.5 1.0 2.0 20.0 500 No No Negative 20.0 No No Yes 1 No Standard No No No R1=Q 3 mmol Yes
dE [mV] . . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . . Tendency . . . . . . . . . . Termination Maximum volume [mL] . . . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs . . . . . . n = . . . . . . . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . . Potential 1 . . . . . . . . . Potential 2 . . . . . . . . . Stop for reevaluation . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Report Output unit . . . . . . . . . . Results . . . . . . . . . . . . All results . . . . . . . . . . Raw results . . . . . . . . . . Table of values . . . . . . . . Sample data . . . . . . . . . . E - V curve . . . . . . . . . . dE/dV - V curve . . . . . . . . d2E/dV2 - V curve . . . . . . . log dE/dV - V curve . . . . . . E - t curve . . . . . . . . . . V - t curve . . . . . . . . . . dV/dt - t curve . . . . . . . .
dE [mV] . . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . . Tendency . . . . . . . . . . Termination Maximum volume [mL] . . . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs . . . . . . n = . . . . . . . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . . Potential 1 . . . . . . . . . Potential 2 . . . . . . . . . Stop for reevaluation . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Auxiliary value ID text . . . . . . . . . . . . Formula . . . . . . . . . . . . Report Output unit . . . . . . . . . . Results . . . . . . . . . . . . All results . . . . . . . . . . Raw results . . . . . . . . . . Table of values . . . . . . . . Sample data . . . . . . . . . . E - V curve . . . . . . . . . . dE/dV - V curve . . . . . . . . d2E/dV2 - V curve . . . . . . . log dE/dV - V curve . . . . . . E - t curve . . . . . . . . . . V - t curve . . . . . . . . . . dV/dt - t curve . . . . . . . .
. . . 0 . . .
15
METTLER TOLEDO
M076
Free Fatty Acid of Oil and Fat

Determination of the acid number of free fatty acids of oils, fats, and butter
Sample
Oil, fat, butter, 0.5-10 g

1) For oil, fat and butter a 1:1 mixture of ether and ethanol is generally usedas a solvent. It can be added automatically with a function DISPENSE.
Substance Chemicals
Free fatty acids
40 mL 1:1 ethanol:ether
2) To achieve a complete dissolution of the sample, an additional stirring with higher stirrer speed during 1-2 minutes is used. 3) Calculations: The acid number of an oil or fat is the amount of of potassium hydroxide in mg required to neutralize 1 g of the sample. The result is expressed as mg KOH/g sample or as percentage of free acidity: Acid number AN = 5.61*a*t/m Free Fatty acid FFA = a*t*M/(100*m) mg KOH/g %
Titrant
KOH in ethanol: c(KOH) = 0.05 mol/L
Benzoic acid DL50Graphix, DL53/55/58 DL70ES, DL77
Accessories
1 additional burette drive DV90 1 additional burette DV1020 100 mL beaker ME-101974 Printer, Balance DG113-SC
M = Molecular mass of the fatty acid involved: M = 288 (oleic acid) M = 256 (palmitic acid, in palm oil) M = 200 (lauric acid, in palm kernel and coconut oils) M = 338 (eruca acid, in rape oil, rape fat) a = KOH consumption (mL) t =Titer (KOH)
Remarks
1) The acid number is a measure of the decomposition by lipase enzyme of the glycerides in oil ands fats.The decomposition is accelerated by heat and light. Rancidity idue to decomposition is usually accompanied by free fatty acid formation. 2) Blank determination (method 076b): Acidic impurities in the solvent are taken into account by a blank value H8, or the solvent is neutralized before titration
R-COOH + OH- = R-COO- + H2O
Calculation
Blank determination (Meth. 076b): R1 = Q R1 is stored as auxiliary value H8 Acid value det. (Meth: 076a): R1 = (Q1 - H8)*C1/m C1 = M/z
3) Electrode conditioning: To ensure hydration of the membrane glass, the Dg113 electrode is stoed over night in water. Before titraiton, clean the electrode with solvent. 4) Butter and coconut fats: For a complete dissolution 5 minutes high speed stirring is required. After each sample, the fatty layer on the electrode must be removed by rinsing it with solvent. The titration curve of butter is flat. The threshold hs to lowered to 400 mV. 5) Difficult samples: Samples can show a rather flat curve, and noise can appear.The addition of 1 mL 0.05 mol/L benzoic acid to the sample solves the problem.
Results
Waste disposal
Author
A. Aichert
16
Results
METTLER DL77 Titrator *114* V3.1 Mettler-Toledo AG Market Support Laboratory 28-Sep-1994 12:18
Method User Measured RESULTS No 1/1 1/2 1/3 1/4 1/5 1/6 ID1
076a FFA in Oil and Fat dw 28-Sep-1994 16:16
ID2
Sample amount and results 6.444 R1 = 0.477 6.447 R1 = 0.481 6.448 R1 = 0.482 6.442 R1 = 0.481 6.445 R1 = 0.482 6.444 R1 = 0.477 g mg g mg g mg g mg g mg g mg Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g m Acid m Acid m Acid m Acid m Acid m Acid Value Value Value Value Value Value
Thistle oil Thistle oil Thistle oil Thistle oil Thistle oil Thistle oil
STATISTICS Number results R1 n Mean value x Standard deviation s Rel. standard deviation srel Outlier test: no outliers!
= = = =
6 0.480 0.0022 0.449
mg KOH/g mg KOH/g
Acid Value Acid Value
Titration curve
17
Method
Method 076a Version FFA in Oil and Fat 28-Sep-1994 12:18 . . . . 076a . . . . FFA in Oil and Fat . . . . 28-Sep-1994 12:18 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Stand 1 Weight m 0.5 10.0 Thistle 56.11 1 Manual Method 076b Version FFA in Oil and Fat / Blank 28-Sep-1994 11:33 Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperatur sensor . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mV] . . . . . Titrant addition . . . . dE(set) [mV] . . . . . Limits dV . . . . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . Table of values . . . . . . E - V curve . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Title Method ID . . . . . . . . . . . . . 076b Title . . . . . . . . . . . . . . . FFA in Oil and Fat / Blank Date/time . . . . . . . . . . . . . 28-Sep-1994 11:33 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.5 Upper limit [g] . . . . . . . . . 5.0 ID1 . . . . . . . . . . . . . . . . Blank Molar mass M . . . . . . . . . . . . 56.11 Equivalent number z . . . . . . . . 1 Temperatur sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 0 Time [s] . . . . . . . . . . . . . . 0 Dispense Titrant . . . . . . . . . . . . . . EtOH/Ether Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 40.0 Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 5 Titration Titrant . . . . . . . . . . . . . . KOH/EtOH Concentration [mol/L] . . . . . . . 0.05 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 10.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.005 dV(max) [mL] . . . . . . . 0.04 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 1.0 dt [s] . . . . . . . . . . . 1.5 t(min) [s] . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 800.0 Maximum volume [mL] . . . . . . . 0.3 Evaluation procedure . . . . . . Standard Calculation Result name . . . . . . . . . . . . Blank FFA Formula . . . . . . . . . . . . . . R=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Printer Raw results last sample . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Outlier test . . . . . . . . . . . . Yes Auxiliary value ID text . . . . . . . . . . . . . . FFA Blank Formula . . . . . . . . . . . . . . H8=x Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes
. . . . 0 . . . . 0 . . . . EtOH/Ether . . . . 1.0 . . . . 40.0 . . . . 70 . . . . 60 . . . . 50 . . . . 5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . KOH/EtOH 0.05 DG113-SC mV EQP mL 0.5 DYN 8.0 Absolute 0.01 0.2 EQU 1.0 1.5 2.0 20.0 1000.0 5.0 Yes 1 Standard Acid Value R=(Q-H8)*C/m C=M/z mg KOH/g 3 Printer Yes Yes Yes R1 Yes Yes Yes
. . . . Printer . . . . Yes
18
METTLER TOLEDO
M086
Epoxide Values
Determination of the epoxide values in resins according to ASTM D1652-80 and DIN 53188
Sample
AralditRM powders

1) Epoxide resins are dissolved in a mixture consisting of four parts dichloromethane (water content <0.02%) and one part glacial acetic acid (water content <0.5%).
Substance Chemicals
Epoxide end groups
50 mL Dichloromethane:glacial acetic acid 4:1 ; 2 g Tetra-n-butylammonium iodide Perchloric acid in acetic acid, HClO4 c(HClO4) = 0.1 mol/L Tris(hydroxymethyl)aminomethane DL50Graphix, DL53/55/58 DL70ES, DL77
2) The resin is weighed and dissolved in 50 mL solvent mixture. The sample size is selected according to the epoxide equivalent weight. It is selected in order to get a titrant consumption in the order of 10-20 mL. 3) The solution can be warmed up to 50C to improve dissolution, and cooled to room temperature before starting tiration. Generally, solid resins are completely dissolved after ten minutes stirring time (see method 086). 4) 2 g Tetra-n-butylammonium iodide are added to the sample solution, and the titration method is started.
Titrant
Accessories
1 additional burette drive DV90 1 additional burette DV1020 100 mL glass beaker ME-101974 Printer, Balance DG113-SC
Remarks
1) This method describes the determination of epoxide value based on to DIN 53188 and ASTM D1652-80. Epoxide resins are resins which contains epoxide end goups. 2) Water in the solvent can affect the results. Therefore, only anhydrous reagents should be used. 3) This application can not be used for epoxide resins containing alkaline groups.
Calculation
Blank determination (method 086b): R1 = Q ; mmol R1 is stored as auxiliary value H9. Epoxide value det. (Method 086a): R1 = (Q-H9)/(10*m) ; mg Mol/100g R2 = (m*1000)/(Q1-H9) ; g/Mol R3 = (Q1-H9)*1.6/m ; %
4) Perchloric acid reacts stoichiometrically with epoxide end groups. 5) Calculations: The epoxide equivalent weight (EEW) is the amount of epoxide resin in g which contains 16 g of oxigen bound as epoxide: EEM = m * 1000 / Q g/Mol The epoxide value (EV) indicates the amount-of-substance of epoxide groups in 100 g of an epoxide resin: EV = 100 / EEM Mol/100 g sample The content of oxirane oxigen in % = 1.6*Q/m Literature: ASTM D 1652-80, DIN 53188
Results
Waste disposal
Halogenated, organic solvent waste
Author
K. Mooibroek
19
Results
METTLER DL67 Titrator DL67(1) V3.1 Mettler-Toledo AG Market Support Laboratory 09-Mar-1994 15:28
Method User Measured
086a Epoxy Content K.M. 10-Mar-1994 11:10
RESULTS LAST SAMPLE No 1/2 ID1 Polymer ID2 Sample amount and results 2.0734 R1 = 0.069 R2 = 1439.246 R3 = 1.112 g Weight Mol/100g g/Mol % m Epoxy Content Epoxide Eq.W. Oxirane O 2
No.
Probe
Einwaage (g) (g)
Epoxide equiv. weight (g/mol) 1482.188 1440.431
Epoxide value (mol/100 g) 0.068 0.069
Oxiran oxygen (%) 1.084 1.111
srel (%) 6.632 0.1062
1 2
Araldit 2 Araldit 9
0.4973 - 0.5562 2.0 - 2.5053
6 4
Titration curve
20
Method
Method 086a Version Epoxy Content 09-Mar-1994 15:28 . . . . 086a . . . . Epoxy Content . . . . 09-Mar-1994 15:28 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Stand 1 Weight m 0.0 2.0 Polymer 0 1 Manual Method 086b Version Blank 17-Dec-2001 10:15 . . . . 086a . . . . Blank . . . . 17-Dec-2001 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Stand 1 Weight m 0.0 2.0 Polymer 0 1 Manual Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperatur sensor . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Titrant addition . . . . dE(set) [mV] . . . . . Limits dV . . . . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . EQP range . . . . . . . . Limit A . . . . . . . Limit B . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . Results last sample . . . . Table of values . . . . . . E - V curve . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . Short-form method . . . . . All results . . . . . . . . Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperatur sensor . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Titrant addition . . . . dE(set) [mV] . . . . . Limits dV . . . . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . EQP range . . . . . . . . Limit A . . . . . . . Limit B . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . Table of values . . . . . . E - V curve . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . .
10:15
. . . . 75 . . . . 600 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HClO4 0.1 DG113-SC mV EQP DYN 8.0 Absolute 0.02 0.2 EQU 0.1 5.0 5.0 20.0 75.0 Yes -1000 1000 20.0 Yes 1 Standard Epoxy Content R1=(Q1-H9)/(10*m) Mol/100g 3 Epoxide Eq.W. R1=(m*1000)/(Q1-H9) g/Mol 3 Oxirane O2 R3=(Q1-H9)*1.6/m % 3 Printer Yes Yes Yes Yes R1 Yes Yes Yes
. . . . 50 . . . . 15 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HClO4 0.1 DG113-SC mV EQP DYN 8.0 Absolute 0.005 0.2 EQU 0.1 5.0 5.0 20.0 75.0 Yes -1000 1000 20.0 Yes 1 Standard Blank R=Q mmol 3 Printer Yes Yes Yes R1 Yes Yes Yes
. . . . Epoxide Blank . . . . H9=x . . . . Printer . . . . Yes
. . . . R2 . . . . Yes . . . . Yes . . . . . . . . . . . . . . . . R3 Yes Yes Yes
. . . . Printer . . . . Yes . . . . Yes
21
METTLER TOLEDO
M232
Epoxide Value of 2,3-Epoxypropylene-Phenyl Ether

Determination of the epoxide value by titration with HClO4
Sample
0.1 g 2,3-epoxypropylene-phenyl ether, 99%

1) 0.1 g sample are dissolved in 50 mL 0.4 mol/L TEAB solution 2) TEAB: tetraethylammonium bromide
Substance Chemicals
Epoxide end groups
50 mL 0.4 mol/L TEAB solution (Tetraethylammonium bromide in glacial acetic acid), M(TEAB)= 210.16 Perchloric acid in acetic acid, HClO4 c(HClO4) = 0.1 mol/L Tris(hydroxymethyl)aminomethane DL50Graphix, DL53/55/58 DL70ES, DL77
Titrant
Accessories
100 mL glass beaker ME-101974 Printer, Balance

DG113-SC
1) Water in the solvent can affect the results. Therefore, only anhydrous reagents should be used. 2) Perchloric acid reacts stoichiometrically with epoxide end groups. 3) After each meausrement the electrode was placed in water for approximately 5 minutes.
Calculation
Blank determination (method vsb): R1 = Q ; mmol R1 is stored as auxiliary value H10. Epoxide value det. (Method vsa): R1 = (Q-H10)*C/m ; C=1/z ; mol/kg R2 = VEQ ; mL R3 = 1000/R1 ; Epoxide value
Results
Waste disposal
Halogenated, organic solvent waste
Author
Viola Mueller-Schindler
22
Results
METTLER TOLEDO DL58 Method Measured User ALL RESULTS No 1 ID Sample amount and results 0.116 R1 = 6.6592 R2 = 7.7246 R3 = 150.2 0.0955 R1 = 6.6948 R2 = 6.3935 R3 = 149.4 0.1035 R1 = 6.6692 R2 = 6.9026 R3 = 149.9 0.0964 R1 = 6.6767 R2 = 6.4363 R3 = 149.8 n x s srel n x s srel = = = = = = = = g mol/kg mL g mol/kg mL g mol/kg mL g mol/kg mL Gehalt Epoxyd Wert Gehalt Epoxyd Wert Gehalt Epoxyd Wert Gehalt Epoxyd Wert Titrator V2.0 Titrations-Kurs 20.-29. Mai 1997 27-Mai-1997 14:58
vsa Epoxid Bestimmung 27-Mai-1997 15:59 VS
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation STATISTICS Number results R2 Mean value Standard deviation Rel. standard deviation
4 6.6750 0.01504 0.225 4 6.8643 0.61818 9.006
mol/kg mol/kg % mL mL %
Gehalt Gehalt
Titration curve
23
Method
Method vsa Version Epoxid Bestimmung 27-Mai-1997 14:58 . . . . . . . . . . . . . . Epoxid Bestimmung . . . . . . . 27-Mai-1997 14:58 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Weight 0.02 5.0 1 1 Stand 1 Manual Method vsb Version Blank 27-Mai-1997 14:30 Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Lower limit [g] . . Upper limit [g] . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Volume [mL] . . . . Wait time [s] . . . Titrant addition . . . dV [mL] . . . . . . Measure mode . . . . . Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Volume [mL] . . . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Titrant addition . . . dV [mL] . . . . . . Measure mode . . . . .
. . . . . . . vsb . . . . . . . Blank . . . . . . . 27-Mai-1997 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Volume 50.0 1 1 Stand 1 Manual
14:30
. . . . . . . 50 . . . . . . . 120 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HClO4 0.1 DG113 mV Yes 1.0 0 Incremental 0.1 Equilibrium controlled 0.5 3.0 2.0 30.0 170 Yes No Positive 20.0 No No Yes 1 No Standard No No No R=(Q-H10)*C/m C=1/z 4 mol/kg Gehalt Yes R2=VEQ 4 mL Yes R3=1000/R1 1 Epoxid Wert No Printer Yes Yes Yes Yes No Yes Yes No No No No No
. . . . . . . 50 . . . . . . . 20 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HClO4 0.1 DG113 mV No Incremental 0.02 Equilibrium controlled 0.5 3.0 2.0 30.0 170 Yes No Positive 20.0 No No Yes 1 No Standard No No No No R1=Q 3 mmol Yes
dE [mV] . . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . . Tendency . . . . . . . . . . Termination Maximum volume [mL] . . . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs . . . . . . n = . . . . . . . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . . Potential 1 . . . . . . . . . Potential 2 . . . . . . . . . Stop for reevaluation . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Report Output unit . . . . . . . . . . Results . . . . . . . . . . . . All results . . . . . . . . . . Raw results . . . . . . . . . . Table of values . . . . . . . . Sample data . . . . . . . . . . E - V curve . . . . . . . . . . dE/dV - V curve . . . . . . . . d2E/dV2 - V curve . . . . . . . log dE/dV - V curve . . . . . . E - t curve . . . . . . . . . . V - t curve . . . . . . . . . . dV/dt - t curve . . . . . . . .
dE [mV] . . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . . Tendency . . . . . . . . . . Termination Maximum volume [mL] . . . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs . . . . . . n = . . . . . . . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . . Potential 1 . . . . . . . . . Potential 2 . . . . . . . . . Stop for reevaluation . . . . Stop for reevaluation . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Auxiliary value ID text . . . . . . . . . . . . Formula . . . . . . . . . . . . Report Output unit . . . . . . . . . . Results . . . . . . . . . . . . All results . . . . . . . . . . Raw results . . . . . . . . . . Table of values . . . . . . . . Sample data . . . . . . . . . . E - V curve . . . . . . . . . . dE/dV - V curve . . . . . . . . d2E/dV2 - V curve . . . . . . . log dE/dV - V curve . . . . . . E - t curve . . . . . . . . . . V - t curve . . . . . . . . . . dV/dt - t curve . . . . . . . .
. . . 0 . . .
24
METTLER TOLEDO
M087
Bromine Number of Petroleum Distillates and Aliphatic Olefins

Bromine number determinations of petroleum distilates according to ASTM D1159-89 and IP130/85
Sample
Petroleum distillates and aliphatic olefins

1) Solvent mixture according to ASTM D1159-89: 714 mL glacial acetic acid, 134 mL 1,1,1-trichloroethane 134 mL methanol, and 18 mL 1+5 H2SO4 (16%) Preparation of 1+5 H2SO4 solution: Add 1 volume concentrated H2SO4 (specific gravity 1.84) to 5 volumes deionized water. 2) Cool the solvent to 0-5C before starting titration by setting the temperature of the thermostate.
Substance Chemicals
Carbon-Carbon double bounds
50 mL solvent mixture
Titrant
Bromide-Bromate, Br-/BrO3c(Br2) = 0.05 mol/L
3) The DK102A polrization current is set to 0.5 A, and it is connected to sensor input 1. Voltametric end point indication allows a fast and accurate deterimantion. At the appearance of unreacted bromine a significant potential change is monitored. 4)The commercially available Bromide-Bromate solution is used as a titrant. It is stable and does not need a standardization. If necessary (e.g. by home-made titrant) reagents and titrant are checked by titrating standards as given in ASTM D1159-89. 5) A blank is determined for every new batch of solvent mixture (Method 087B)
DL70ES, DL77
Accessories
1 additional burette drive DV90 Thermostatable vessel ME-23517 DT120 Temperature sensor (Pt100) AT261 balance, Printer DM143-SC with DK102A, cables Ban. -SC 51108061, LEMO-SC 89601 Bromine generation: BrO3- + 5Br- + 6H+ = 3Br2 + 3H2O Bromine addition to C=C double bond: R-CH=CH-R2 + Br2 = R-CHBr-CHBr-R2
Remarks
1) The bromine number is the number of grams of bromine which react completely with 100 g of the sample under the conditions indicated by the standard ASTM 1159-89. It gives the quantity of bromine reactive components, and it also characterizes the degree of unsaturation of the sample, based only the addition reaction. 2) By choosing the appropriate reaction conditions -i.e. the composition of the solvent and a reaction temperature between 0-5C- only the additoon reaction takes place, while substitution and oxidation reactions are suppressed. 3) Method 087A is especially designed for fast voltametric end point titration with continuous titrant addtion according to ASTM D1159-89 (delay time 30 s, increment 0.1 mL)
Calculation
Blank determination (Meth. 087B): R1 = Q R1 is stored as aux. value H11 Bromine No. det. (Meth: 087A): R1 = (Q-H11)*15.98/m
Results
Waste disposal
Chlorinated organic solvents
Literature: ASTM D1159-89, IP130/85
Author
Kees Mooibroek
25
Results
No. Sample Weight (g) 1 2 3 4 5 Gasoline A Gasoline B 1-Decene Cyclopentene Cyclohexene 0.2165 0.2 - 0.5 0.03296 0.03033 0.0518 6 8 6 6 6 n Bromine Number (g/100g) 55.4 25.9 106 232 198 srel (%) 3.03 1.56 1.82 1.43 2.57 time (min) 3 4 8 2 3
Titration curve
26
Method
Method 087A Version Bromine number 25-Oct-1993 4:07 pm . . . 087A . . . Bromine number . . . 25-Oct-1993 4:07 pm . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Stand 1 Weight m 0.0 2.0 Bromine 159.8 1 TEMP A Method 087B Version Bromine Number:Blank 21-Oct-1993 6:31 pm . . . 087B . . . Bromine Number:Blank . . . 21-Oct-1993 6:31 pm . . . . . . . . . . . . . . . . . . . . . . . . 4 Stand 1 Fixed volume U 50.0 Blank 159.8 1 TEMP A Title Method ID . . . . . . . . . . Title . . . . . . . . . . . . Date/time . . . . . . . . . . Sample Number samples . . . . . . . . Titration stand . . . . . . . Entry type . . . . . . . . . . Lower limit [g] . . . . . . Upper limit [g] . . . . . . ID1 . . . . . . . . . . . . . Molar mass M . . . . . . . . . Equivalent number z . . . . . Temperatur sensor . . . . . . Stir Speed [%] . . . . . . . . . . Time [s] . . . . . . . . . . . Temperature Sensor . . . . . . . . . . . . Unit of meas. . . . . . . . . dT [C,F,K] . . . . . . . . . dt [s] . . . . . . . . . . . . t(min) mode . . . . . . . . . Set value [C,F,K] . . . . t(max) [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . . Concentration [mol/L] . . . . Sensor . . . . . . . . . . . . Unit of meas. . . . . . . . . Titration mode . . . . . . . . Titrant addition . . . . . Control band [mV,pH,...] Delay [s] . . . . . . . dV(min) [mL] . . . . . . End point mode . . . . . . Potential [mV,pH,...] . Tendency . . . . . . . . . Maximum volume [mL] . . . . Calculation Result name . . . . . . . . . Formula . . . . . . . . . . . Constant . . . . . . . . . . . Result unit . . . . . . . . . Decimal places . . . . . . . . Record Output unit . . . . . . . . . Results last sample . . . . . Table of values . . . . . . . E - V curve . . . . . . . . . Statistics Ri (i=index) . . . . . . . . . Standard deviation s . . . . . Rel. standard deviation srel . Outlier test . . . . . . . . . Record Output unit . . . . . . . . . All results . . . . . . . . . Title Method ID . . . . . . . . . . Title . . . . . . . . . . . . Date/time . . . . . . . . . . Sample Number samples . . . . . . . . Titration stand . . . . . . . Entry type . . . . . . . . . . Volume [mL] . . . . . . . . ID1 . . . . . . . . . . . . . Molar mass M . . . . . . . . . Equivalent number z . . . . . Temperatur sensor . . . . . . Stir Speed [%] . . . . . . . . . . Time [s] . . . . . . . . . . . Temperature Sensor . . . . . . . . . . . . Unit of meas. . . . . . . . . dT [C,F,K] . . . . . . . . . dt [s] . . . . . . . . . . . . t(min) mode . . . . . . . . . Set value [C,F,K] . . . . t(max) [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . . Concentration [mol/L] . . . . Sensor . . . . . . . . . . . . Unit of meas. . . . . . . . . Titration mode . . . . . . . . Titrant addition . . . . . Control band [mV,pH,...] Delay [s] . . . . . . . dV(min) [mL] . . . . . . End point mode . . . . . . Potential [mV,pH,...] . Tendency . . . . . . . . . Maximum volume [mL] . . . . Calculation Result name . . . . . . . . . Formula . . . . . . . . . . . Constant . . . . . . . . . . . Result unit . . . . . . . . . Decimal places . . . . . . . . Record Output unit . . . . . . . . . Results last sample . . . . . Statistics Ri (i=index) . . . . . . . . . Standard deviation s . . . . . Rel. standard deviation srel . Outlier test . . . . . . . . . Auxiliary value ID text . . . . . . . . . . . Formula . . . . . . . . . . . Record Output unit . . . . . . . . . All results . . . . . . . . .
. . . 60 . . . 120 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . TEMP A C 1.0 2.0 T < set value 5.0 600.0 Bromide-Bromate 0.05 DK102A/DM143 mV EP Continuous 3000 30 0.02 EPA -150.0 Positive 20.0 Bromine Number R=(Q-H11)*C/m C=M/(10*z) g Br2/100g 2 Printer Yes Yes Yes R1 Yes Yes Yes
. . . 60 . . . 120 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . TEMP A C 1.0 2.0 T < set value 5.0 600.0 Bromide-Bromate 0.05 DK102A/DM143 mV EP Continuous 3500 30 0.001 EPA -150.0 Positive 5.0 Blank R1=H11 mmol/50 mL 3
. . . Printer . . . Yes . . . . . . . . . . . . R1 Yes Yes Yes
. . . Blank value Bromine . . . H11=x . . . Printer . . . Yes
. . . Printer . . . Yes
27
METTLER TOLEDO
M233
Low Bromine Index Determination of a Standard Solution

Bromine index determinations of a standard solution according to ASTM D2710-99 and IP299/92
Sample
Cyclohexene in glacial acetic acid, 5-10 ppm

1) Solvent mixture according to ASTM D2710-89: 714 mL glacial acetic acid, 134 mL 1,1,1-trichloroethane 134 mL methanol, and 18 mL 1+5 H2SO4 (16%) Preparation of 1+5 H2SO4 solution: Add 1 volume concentrated H2SO4 (specific gravity 1.84) to 5 volumes deionized water. 2) Cool the solvent to 0-5C before starting titration by setting the temperature of the thermostate.
Substance Chemicals
Carbon-Carbon double bounds (Cyclohexene) 50 mL solvent mixture
Titrant
Bromide-Bromate, Br-/BrO3c(Br2) = 0.05 mol/L
3) Voltametric end point indication allows a fast and accurate deterimantion. At the appearance of unreacted bromine a significant potential change is monitored. 4) The commercially available Bromide-Bromate solution is used as a titrant. It is stable and does not need a standardization. If necessary (e.g. by home-made titrant) reagents and titrant are checked by titrating standards as given in ASTM D2710-99. 5) A blank is determined for every new batch of solvent mixture (Method 111)
DL38 DL50Graphix, DL53/55/58 with KF Option and DV705 KF titration stand Thermostatable vessel ME-51 107 497 AT261 balance, Printer
Accessories

DM143-SC, or Pt885-NS-S7/105 (ME-59 904 435) Bromine generation: BrO3- + 5Br- + 6H+ = 3Br2 + 3H2O Bromine addition to C=C double bond: R-CH=CH-R + Br2 = R-CHBr-CHBr-R
1) The bromine index is the number of milligrams of bromine which react completely with 100 g of the sample under the conditions indicated by the standard ASTM 2710-99. It gives the quantity of bromine reactive components, and it also characterizes the degree of unsaturation of the sample, based only the addition reaction. 2) By choosing the appropriate reaction conditions -i.e. the composition of the solvent and a reaction temperature between 0-5C- only the addition reaction takes place, while substitution and oxidation reactions are suppressed. 3) For very low bromine index values the platinum double ring electrode Pt885-NS-S7/105 (ME-59 904 435) was found to be very suitable. In this case, it is recommended to replace the DM143 electrode with the Pt885 electrode.
Calculation
Blank determination (Meth. 111): R1 = VEQ , stored as blank Bromine Index. det. (Meth. 112): R1 = (Consumption-Blank)*Conc*15980/m
Results
Waste disposal
Chlorinated organic solvents
Literature: ASTM D2710-99, IP299/92
Author
Cosimo De Caro
28
Results
METTLER TOLEDO DL38 V1.2 ------------------------------------------------------------------------------Method: 112 Br. Index 20-11-2000 15:37 User: Cosimo Measured: 22-11-2000 9:35 File: C:\COSIMO\RECKB112.008 Printed: 20-12-2001 10:41 ------------------------------------------------------------------------------Calculation factor f1 = 1.0000 Calculation factor f2 = 1.0000 Calculation factor f3 = 0.0500 RESULTS Br No. determination No. 1 Sample-ID Sample size and results
10mL4.724E-5g/mL 10.5 g Bromine index = 9.09 R2 = 0.292 mL R3 = 0.0146 mmol 5mL4.724E-5g/mL 5.25 g Bromine index = 9.89 R2 = 0.237 mL R3 = 0.0119 mmol 3mL4.724E-5g/mL 3.15 g Bromine index = 7.86 R2 = 0.203 mL R3 = 0.0102 mmol 1mL4.724E-5g/mL 1.04 g Bromine index = 9.60 R2 = 0.185 mL R3 = 0.0092 mmol
STATISTICS Bromine index n = 4 Mean value = 9.11 Std. devn = 0.896352 srel = 9.836 % STATISTICS No. results R3 n = 4 Mean value = 0.0115 mmol Std. devn = 0.002350 mmol srel = 20.523 %
Titration curve
29
Method
Method . . . . . . . . . . . . . . . . . . . . . 112 Title . . . . . . . . . . . . . . . . . . . . Br. Index Version . . . . . . . . . . . . . . . . . . . 20-11-2000 15:37 Author . . . . . . . . . . . . . . . . . . . CDC Sample parameters ID . . . . . . . . . . . . . . . . . . . . . Request Type . . . . . . . . . . . . . . . . . . . . Mass Minimum [g] . . . . . . . . . . . . . . . . . 8.0000 Maximum [g] . . . . . . . . . . . . . . . . . 30.0000 Entry . . . . . . . . . . . . . . . . . . . . Before Speed [%] . . . . . . . . . . . . . . . . . . . 40 Mix time [s] . . . . . . . . . . . . . . . . . . 300 Titrant . . . . . . . . . . . . . . . . . . . . Br-/BrO3Predisp.[mL] . . . . . . . . . . . . . . . . . . 0.0000 Wait time [s] . . . . . . . . . . . . . . . . . 0 Control parameters Current [uA] . . . . . . . . . . . . . . . . 1 End point [mV] . . . . . . . . . . . . . . . 150 dVmin [uL] . . . . . . . . . . . . . . . . . 1.0 dVmax [uL] . . . . . . . . . . . . . . . . . 20.0 dVmax factor [%] . . . . . . . . . . . . . . 100 Start . . . . . . . . . . . . . . . . . . . . Cautious Termination param. Max. time [s] . . . . . . . . . . . . . . . . 6000 Delay [s] . . . . . . . . . . . . . . . . . . 30 Vmax [mL] . . . . . . . . . . . . . . . . . . 20.000 Blank [mmol] . . . . . . . . . . . . . . . . . . Request Calculation 1 R1 = . . . . . . . . . . . . . . . . . . . . x [Br index]*f1 f1 = . . . . . . . . . . . . . . . . . . . . 1.0000 Unit Decimal places . . . . . . . . . . . . . . . 2 Statistics . . . . . . . . . . . . . . . . . Yes Max. srel [%] . . . . . . . . . . . . . . . . 0.00 Calculation 2 R2 = . . . . . . . . . . . . . . . . . . . . x [mL]*f2 f2 = . . . . . . . . . . . . . . . . . . . . 1.0000 Unit . . . . . . . . . . . . . . . . . . . . mL Decimal places . . . . . . . . . . . . . . . 3 Statistics . . . . . . . . . . . . . . . . . No Max. srel [%] . . . . . . . . . . . . . . . . 0.00 Calculation 3 R3 = . . . . . . . . . . . . . . . . . . . . x [mL]*f3 f3 = . . . . . . . . . . . . . . . . . . . . 0.0500 Unit . . . . . . . . . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . . . . . 4 Statistics . . . . . . . . . . . . . . . . . Yes Max. srel [%] . . . . . . . . . . . . . . . . 0.00 Report Output . . . . . . . . . . . . . . . . . . . Computer Method . . . . . . . . . . . . . . . . . . . . . 111 Title . . . . . . . . . . . . . . . . . . . . Blank Br.Ind Version . . . . . . . . . . . . . . . . . . . 20-11-2000 15:32 Author . . . . . . . . . . . . . . . . . . . CDC Sample parameters ID . . . . . . . . . . . . . . . . . . . . . Request Type . . . . . . . . . . . . . . . . . . . . Fixed volume Density [g/mL] . . . . . . . . . . . . . . . 1.000 Volume [mL] . . . . . . . . . . . . . . . . . 55 Speed [%] . . . . . . . . . . . . . . . . . . . 40 Mix time [s] . . . . . . . . . . . . . . . . . . 300 Titrant . . . . . . . . . . . . . . . . . . . . Br-/BrO3Predisp.[mL] . . . . . . . . . . . . . . . . . . 0.0000 Wait time [s] . . . . . . . . . . . . . . . . . 0 Control parameters Current [uA] . . . . . . . . . . . . . . . . 1 End point [mV] . . . . . . . . . . . . . . . 150 dVmin [uL] . . . . . . . . . . . . . . . . . 1.0 dVmax [uL] . . . . . . . . . . . . . . . . . 5.0 dVmax factor [%] . . . . . . . . . . . . . . 100 Start . . . . . . . . . . . . . . . . . . . . Cautious Termination param. Max. time [s] . . . . . . . . . . . . . . . . 6000 Delay [s] . . . . . . . . . . . . . . . . . . 30 Vmax [mL] . . . . . . . . . . . . . . . . . . 5.000 Blank [mmol] . . . . . . . . . . . . . . . . . . 0 Calculation 1 R1 = . . . . . . . . . . . . . . . . . . . . x [mL]*f1 f1 = . . . . . . . . . . . . . . . . . . . . 0.0500 Unit . . . . . . . . . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . . . . . 4 Statistics . . . . . . . . . . . . . . . . . Yes Max. srel [%] . . . . . . . . . . . . . . . . 0.00 Calculation 2 R2 = . . . . . . . . . . . . . . . . . . . . x [mL]*f2 f2 = . . . . . . . . . . . . . . . . . . . . 1.0000 Unit . . . . . . . . . . . . . . . . . . . . mL Decimal places . . . . . . . . . . . . . . . 3 Statistics . . . . . . . . . . . . . . . . . Yes Max. srel [%] . . . . . . . . . . . . . . . . 0.00 Calculation 3 Report Output . . . . . . . . . . . . . . . . . . . Computer
30
METTLER TOLEDO
M090
Determination of Saponification Value

Determination of saponification value in resins according to DIN 53401
Sample
Resin, 3 g

Sample preparation 1) The sample is dissolved in 50 mL toluene in a 100 mL Erlenmeyer beaker. Note: The Erlenmeyer beaker must be fit the reflux condenser. 2) 20 mL 0.5 ml/L KOH are added to the sample solution. 3) Boil under reflux condition for 30 minutes. 4) Cool down the sample solution to room temperature before starting titration. Boiling under reflux condiction: 1) The boiling time is crucial 2) Use organic solvents (or solvent mixtures) which do not undergo saponification and other side reactions: methanol, ethanol, toluene, isopropanol, ethylene glycol. The saponification temperature is determined by the solvent used. 3) If necessary: The reaction of the sample with carbon dioxide is preventeed by flushing the titration vessel and reflux condenser with nitrogen gas. Titration: The saponification value is determined by back-titration with HCl after saponification reaction. This is achieved by addition of a known amount of KOH and subsequent reflux boiling. Unreacted KOH is then determined by titration with HCl.
Substance Chemicals
Saponifiable esterified acids
Toluene, 50 mL Ethanolic KOH, 20 mL c(KOH)=0.5 M
Titrant
Hydrochloric acid in isopropanol c(HCl) = 0.5 mol/L
KHP for KOH, THAM for HCl DL67/70ES/77, DL50 Graphix, DL53/55/58
Accessories
Reflux condenser, water bath thermostat, 100 mL Erlenmeyer beaker, AT261 Balance, printer, DL55/58, DL70ES/77: addi. burettes DG113-SC
Remarks
The saponification value is a reference value for the amount of saponified acidic components present in the sample. It corresponds to the amount of KOH (in mg) used for the saponification. The described procedure is used for the determination of the content of esterified acids in products such as solvents, oils, fats, resins, fatty acids as well as softeners used in the polymer industry. Free acidic as well as anhydrous compounds are also included. Two titration methods are used in this analysis: a blank and a sample titration. The blank value is stored as auxiliary value H12 in the titrator. Literature: 1. DIN 53401, 51559, 53404 2. Schweizerisches Lebensmittelbuch, 5 th edition, Eidgenssische Druck- und Materialzentrale, Bern, 1993 3. Application M618, Mettler-Toledo Application brochure 24, ME-51725054
R1-CO-O-R2 + OH- = R1-COO- + HO-R2
Calculation
Blank (Method 090B): R1=Q ; mmol Stored as auxiliary value H12 Saponification value (Method 090A): R1=(H12-Q)*(C1/m) C1=56.1 ; mg KOH/g
Results
Waste disposal
Organic solvents (halogenated or not)
Author
Kees Mooibroek
31
Results
METTLER DL67 Titrator DL67 (1) V3.1 Mettler-Toledo AG Market Support Laboratory 06-Apr-1994 11:42
Method User Measured RESULTS No 1/1 1/2 1/3 1/4 1/5 1/6 ID1
090A Saponification Value K.M. 06-Apr-1994 13:31
ID2
Sample amount and results 2.902 R1 = 157.266 2.9075 R1 = 159.202 2.8983 R1 = 158.912 2.9696 R1 = 155.148 2.9056 R1 = 158.750 2.902 R1 = 159.590 g mg g mg g mg g mg g mg g mg Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g m Saponif.value m Saponif.value m Saponif.value m Saponif.value m Saponif.value m Saponif.value
Saponif. Resin 1 Saponif. Resin 2 Saponif. Resin 3 Saponif. Resin 4 Saponif. Resin 5 Saponif. Resin 6
= = = =
6 158.144 1.668318 1.055
mg KOH/g mg KOH/g %
Saponif.value Saponif.value
Titration curve
32
Method
Method 090A Version Saponification Value 06-Apr-1994 11:42 . . . . 090A . . . . Saponification Value . . . . 06-Apr-1994 11:42 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Stand 1 Weight m 0.0 20.0 Saponif. 0 1 Manual Method 090B Version Saponification, Blank 30-Mar-1994 13:46 . . . . 090B . . . . Saponification, Blank . . . . 30-Mar-1994 13:46 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Stand 1 Fixed volume U 20.0 Saponif. 0 1 Manual Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperatur sensor . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . . . . Titrant addition . . . . dE(set) [mV] . . . . . Limits dV . . . . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . EQP range . . . . . . . . Limit A . . . . . . . Limit B . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Results last sample . . . . Table of values . . . . . . E - V curve . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Volume [mL] . . . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperatur sensor . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . . . . Titrant addition . . . . dE(set) [mV] . . . . . Limits dV . . . . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . EQP range . . . . . . . . Limit A . . . . . . . Limit B . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Results last sample . . . . Table of values . . . . . . E - V curve . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . .
. . . . 60 . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HCl 0.5 DG111-SC mV EQP mL 0.0 DYN 8.0 Absolute 0.02 0.2 EQU 0.5 1.0 3.0 30.0 250.0 Yes -500 +500 40.0 Yes 1 Standard Saponif.value R1=(H12-Q1)*(C1/m) C1=56.1 mg KOH/g 3 Printer Yes Yes Yes R1 Yes Yes Yes
. . . . 50 . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HCl 0.5 DG111-SC mV EQP mL 12.0 DYN 8.0 Absolute 0.02 0.2 EQU 0.5 1.0 3.0 30.0 500.0 Yes -500 +500 40.0 Yes 1 Standard Blank R1=Q mmol 3 Printer Yes Yes Yes R1 Yes Yes Yes
. . . . Printer . . . . Yes
. . . . Saponification . . . . H12=x . . . . Printer . . . . Yes
33
METTLER TOLEDO
M091
Determination of Hydroxyl Value

Determination of hydroxyl value according to DIN 53240
Sample
Trimethylolpropane (3-ethyl-2-(Hydroxymethyl)-1,3-propan ediol) Hydroxyl groups

The sample is dissolved in a mixture of 25 mL catalyst solution and 3 mL acetylation mixture. The acetylation mixture can be added either by pipette/dosing unit, or using a burette. Catalyst solution: 12 g 4-Dimethylaminopyridine in 1 L DMF (DMF = N,N-Dimethylformamide), Acetylation mixture: 250 mL acetic acid anhydride with 770 mL DMF 1) The acetylation reaction is catalysed by 4-dimethyl amine pyridine. This reaction takes place during the first stirring function. The stirring time must be adapted to the speed of acetylation reaction. The dosing precision of the acetylation mixture also determines the overall accuracy of the analysis. Note: Water affects acetylation reaction. 2) After completion of acetylation water is addded to the sample mixture to hydrolize excess of acetic acid anhydride which is not used for the acetylation. The reaction time is defined in the second stirring function. 3) As a result, acetic acid is formed which is then back-titrated with methanolic KOH solution.
Substance Chemicals
Catalyst solution: see preparation and procedures Acetylation mixture: see preparation and procedures Potassium hydroxide in methanol, c(KOH) = 0.5 mol/L (A second burette is used for water) KHP DL70ES/77, DL55+, DL58
Titrant
Accessories
AT261 Balance, printer DL55/58, DL70ES/77: two additional burettes, ev. 1 DU200

DG113-SC
The hydroxyl value is a reference number used to characterize polyoles. It is expressed as the amount of KOH in mg to neutralize the consumed equivalent amount of acetic acid used for the acetylation of 1 g of sample. Two titration methods are used in this analysis: a blank and a sample titration. The blank value is stored as auxiliary value H13 in the titrator.
Acetylation:
Calculation
Blank (Method 091B): R1 = Q1 ; mmol Stored as auxiliary value H13 Hydroxyl value (Method 091A): R1 = (H13-Q)*(C1/m) C1 = 56.1 ; mg KOH/g
Literature: 1. DIN 53240, ASTM 2849 (without refluxing at elevated temperature of sample/mixture solution).
Results
Waste disposal
Aromatic organic solvents
Author
Kees Mooibroek
34
Results
METTLER DL67 Titrator DL67 (1) V3.1 Mettler-Toledo AG Market Support Laboratory 20-Jul-1994 11:32
Method User Measured RESULTS No 1/1 1/2 1/3 1/4 1/5 1/6 ID1 Sample Sample Sample Sample Sample Sample
091A Hydroxyl Number, Sample K.M. 20-Jul-1994 17:41
ID2 3779 3779 3779 3779 3779 3779
Sample amount and results 0.5006 R1 = 536.64 0.5006 R1 = 665.83 0.5006 R1 = 665.96 0.5006 R1 = 654.04 0.5006 R1 = 655.31 0.5006 R1 = 608.25 g mg g mg g mg g mg g mg g mg Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g m Hydroxyl m Hydroxyl m Hydroxyl m Hydroxyl m Hydroxyl m Hydroxyl No. No. No. No. No. No.
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation Outlier test : sample No. Number results R1 Mean value Standard deviation Rel. standard deviation
n x s srel n x s srel
= = = = = = = =
6 631.01 50.94823 8.074 1/1, 1/6 4 660.29 6.502444 0.985
mg KOH/gHydroxyl No. mg KOH/gHydroxyl No. %
mg KOH/gHydroxyl No. mg KOH/gHydroxyl No. %
Titration curve
35
Method
Method 091A Version Hydroxyl Number, Sample 20-Jul-1994 11:32 Method 091B Version Hydroxyl number, Blank 23-Jun-1994 8:35 Title Method ID . . . . . . . . . . . . . 091A Title . . . . . . . . . . . . . . . Hydroxyl Number, Sample Date/time . . . . . . . . . . . . . 20-Jul-1994 11:32 Sample Number samples . . . . . . . . . . . 6 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.0 Upper limit [g] . . . . . . . . . 20.0 ID1 . . . . . . . . . . . . . . . . Sample Molar mass M . . . . . . . . . . . . 0.0 Equivalent number z . . . . . . . . 1 Temperatur sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 900 Dispense Titrant . . . . . . . . . . . . . . Deionised water Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 10.0 Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 300 Titration Titrant . . . . . . . . . . . . . . KOH (MeOH) Concentration [mol/L] . . . . . . . 0.5 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 15.0 Threshold . . . . . . . . . . . . 250.0 EQP range . . . . . . . . . . . . Yes Limit A . . . . . . . . . . . 0 Limit B . . . . . . . . . . . -600 Maximum volume [mL] . . . . . . . 50.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Calculation Result name . . . . . . . . . . . . Hydroxyl No. Formula . . . . . . . . . . . . . . R1=(H13-Q1)*(C1/m) Constant . . . . . . . . . . . . . . C1=56.1 Result unit . . . . . . . . . . . . mg KOH/g Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Printer Results last sample . . . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Outlier test . . . . . . . . . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes Title Method ID . . . . . . . . . . . . . 091B Title . . . . . . . . . . . . . . . Hydroxyl number, Blank Date/time . . . . . . . . . . . . . 23-Jun-1994 8:35 Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 3.0 ID1 . . . . . . . . . . . . . . . . Blank Molar mass M . . . . . . . . . . . . 0.0 Equivalent number z . . . . . . . . 1 Temperatur sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 900 Dispense Titrant . . . . . . . . . . . . . . Deionised water Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 10.0 Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 300 Titration Titrant . . . . . . . . . . . . . . KOH (MeOH) Concentration [mol/L] . . . . . . . 0.5 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 20.0 Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 15.0 Threshold . . . . . . . . . . . . 500.0 EQP range . . . . . . . . . . . . Yes Limit A . . . . . . . . . . . 0 Limit B . . . . . . . . . . . -600 Maximum volume [mL] . . . . . . . 50.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Calculation Result name . . . . . . . . . . . . Blank Formula . . . . . . . . . . . . . . R1=Q1 Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 2 Record Output unit . . . . . . . . . . . . Printer Results last sample . . . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Outlier test . . . . . . . . . . . . Yes Auxiliary value ID text . . . . . . . . . . . . . . Blank (acetylation) Formula . . . . . . . . . . . . . . H13=x Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes
36
METTLER TOLEDO
M234
Hydroxyl Value of Polyols

Determination of the hydroxyl value of polyols in polyurethane foams ccording to ASTM D2474
Sample
Polyurethane foams, 1-2 g

The sample is dissolved in 50 mL ethanol:toluene 1:1 mixture. Note: A titration in isopropanol gives a more noisy titration curve.
Substance Chemicals
Hydroxyl groups
Ethanol:Toluene 1:1
Titrant
KOH, c(KOH) = 0.05 mol/L
Accessories

DG113-SC
Two titration methods are used: 1) Method BlOH allows the determination of the solvent blank value which is automatically stored as auxiliary value H14. 2) Method OH allows the determination of the hydroxide value in polyols.
Calculation
Blank determination (Method BlOH): R1 = Q R1 is stored as auxiliary value H14 Acid value det. (Method OH): R1 = (Q1 - H14)*C1/m C1 = 56.1
Results
Waste disposal
Aromatic organic solvents
Literature: ASTM D2474 (see www.astm.org)
Author
Ch. Walter, K. Racman
37
Results
METTLER DL77 Titrator *114* OH V3.1 Mettler-Toledo AG Market Support Laboratory 31-Jul-1994 13:16
Method User Measured RESULTS No 1/1 1/2 1/3 ID1
Hydr. Value Polyol Ester 15:48
31-Jul-1994
ID2
Sample amount and results 1.5022 R1 = 1.132 1.8042 R1 = 1.143 1.7529 R1 = 1.155 g Weight mg KOH/g g Weight mg KOH/g g Weight mg KOH/g m Hydr. Value m Hydr. Value m Hydr. Value
= = = =
3 1.143 0.011567 1.1012
mg KOH/gHydr. Value mg KOH/gHydr. Value %
Titration curve
38
Method
Method OH Version Hydr. Value Polyol Ester 31-Jul-1994 13:16 Method BlOH Version Blank Hydr. Value Polyol 31-Jul-1994 12:27 Title Method ID . . . . . . . . . . . . . OH Title . . . . . . . . . . . . . . . Hydr. Value Polyol Ester Date/time . . . . . . . . . . . . . 31-Jul-1994 13:16 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.0 Upper limit [g] . . . . . . . . . 6.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 0.0 Equivalent number z . . . . . . . . 1 Temperatur sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 100 Time [s] . . . . . . . . . . . . . . 200 Titration Titrant . . . . . . . . . . . . . . KOH Concentration [mol/L] . . . . . . . 0.05 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 0.2 Titrant addition . . . . . . . . INC V [mL] . . . . . . . . . . . 0.025 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 700 Maximum volume [mL] . . . . . . . 2.0 Evaluation procedure . . . . . . Standard Calculation Result name . . . . . . . . . . . . Hydr. Value Formula . . . . . . . . . . . . . . R1=(Q-H14)*C1/m Constant . . . . . . . . . . . . . . C1=56.1 Result unit . . . . . . . . . . . . mg KOH/g Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Printer Results last sample . . . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Outlier test . . . . . . . . . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes Title Method ID . . . . . . . . . . . . . BlOH Title . . . . . . . . . . . . . . . Blank Hydr. Value Polyol Date/time . . . . . . . . . . . . . 31-Jul-1994 12:27 Sample Number samples . . . . . . . . . . . 2 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 50.0 ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0 Equivalent number z . . . . . . . . 1 Temperatur sensor . . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10 Titration Titrant . . . . . . . . . . . . . . KOH Concentration [mol/L] . . . . . . . 0.05 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . INC V [mL] . . . . . . . . . . . 0.01 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 100 Maximum volume [mL] . . . . . . . 3.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Calculation Result name . . . . . . . . . . . . Blank Formula . . . . . . . . . . . . . . R=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Auxiliary value ID text . . . . . . . . . . . . . . Blank Formula . . . . . . . . . . . . . . H14=x Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes
39
METTLER TOLEDO
M095
Determination of Isocyanate Content

Determination of the isocyanate content in resins according to DIN 53185 and 16945
Sample
Resin (Desmodur), 4-5 g

1) Dissolve the sample in 25 mL monochlorobenzene and 20 mL methylethylketone.
Substance Chemicals
Isocyanate groups, -NCO
2) Add manually 10 mL 2 mol/L diisobutylamine in chlorobenzene or by means of an additional burette or a DU200 Dispensing unit. 3) Start back titration of excess diisobutylamine with hydrochloric acid. Note: Isocyanates are toxic compounds. Appropriate working condictions are needed (fumehood, gloves, googles). The stirring time must be long enough to ensure complete dissolution and reaction of the sample before the back titration starts. In most cases, chlorobenzene is able to dissolve the sample. If this is not the case, the mixture can be heated using a thermostatable beaker with a reflux condenser. The sample solution should not be overheated since diisobutylamine might decompose. If the sample solution becomes turbid, a more diluted solution in a larger titraiton vessel must be used. Auxiliary solvents (depending on the sample): methylethylketone,methanol, ethanol, acetone
25 mL monochlorobenzene 10 mL diisobutylamine in Cl-benzene 20 mL methylethlyketone Hydrochloric acid, HCl, in methanol c(HCl) = 1 mol/L
Titrant
THAM DL50Graphix, DL53/55/58 DL70ES, DL77
Accessories
Glass titration beaker ME-101446 Printer, balance Complete automation: additional burette DV1010, or use a DU200 Dosing unit. DG113-SC
Remarks
The isocyanate content is an indication for the number of isocyanate groups -NCO in the sample. The determination is achieved by a back titration. An excess diisobutylamine is added to the non-aqueous sample solution. Diisobutylamine reacts with isocyanate groups during the stirring time of 300 s. Unreacted diisobutylamine is subsequently titrated with hydrochloric acid. Two titration methods are used: 1) Method 095B allows the determination of the solvent blank value which is automatically stored as auxiliary value H15. 2) Method 095A allows the determination of the isocyanate content. Hints: 1) Rinse accurately the electrode, the stirrer and the burette tip with e.g. acetone at the end of the titration series. 2) The DG113 electrode should be conditioned in pH buffer 7 over night to hydrate the pH glass membrane. Literature: DIN 53185, 16945 (see www.din.de) See also ASTM D1638 (www.astm.org)
R-NCO + NH(iBu)2 = (iBu)2N-CO-NHR NH(iBu)2 + HCl = (H2N(iBu)2)+ Cl-
Calculation
Blank determination (Method 095B): R1 = Q R1 is stored as auxiliary value H15 Acid value det. (Method 095A): R1 = (H15-Q1)*C1/m C1 = M/(10*z)
Results
Waste disposal
Isocyanates solution: special waste Aromatic organic solvents
Author
Kees Mooibroek
40
Results
METTLER DL67 Titrator DL67(1) V3.1 Mettler-Toledo AG Market Support Laboratory 17-Aug-1994 16:03
Method User Measured RESULTS No 1/1 1/2 1/3 1/4 1/5 1/6 1/7 ID1 NCO NCO NCO NCO NCO NCO NCO
095A Isocyanate:Sample Titr. 18-Aug-1994 13:53
ID2 4594 4594 4594 4594 4594 4594 4594
Sample amount and results 4.0 R1 = 9.881 4.0 R1 = 12.874 4.0 R1 = 12.902 4.0 R1 = 12.892 4.0 R1 = 12.880 4.0 R1 = 12.892 4.0 R1 = 12.898 g % g % g % g % g % g % g % Weight NCO Weight NCO Weight NCO Weight NCO Weight NCO Weight NCO Weight NCO m Isocyanate m Isocyanate m Isocyanate m Isocyanate m Isocyanate m Isocyanate m Isocyanate
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation Outlier test : sample No. Number results R1 Mean value Standard deviation Rel. standard deviation
= = = = = = = =
7 12.460 1.137420 9.129 1/1 6 12.890 0.010834 0.084
% NCO % NCO %
Isocyanate Isocyanate
% NCO % NCO %
Isocyanate Isocyanate
Titration curve
41
Method
Method 095A Version Isocyanate:Sample Titr. 17-Aug-1994 16:03 . . . . 095A . . . . Isocyanate:Sample Titr. . . . . 17-Aug-1994 16:03 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 Stand 1 Weight m 0.0 10.0 NCO 42.0171 1 Manual Method 095B Version Isocyanate:Blank Determin. 17-Aug-1994 16:03 Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperature sensor . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . . . . Titrant addition . . . . E(set) [mV] . . . . . Limits V . . . . . . V(min) [mL] . . . V(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . EQP range . . . . . . . . Limit A . . . . . . . Limit B . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Results last sample . . . . Table of values . . . . . . E - V curve . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Title Method ID . . . . . . . . . . . . . 095B Title . . . . . . . . . . . . . . . Isocyanate:Blank Determin. Date/time . . . . . . . . . . . . . 17-Aug-1994 16:03 Sample Number samples . . . . . . . . . . . 4 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U Volume [mL] . . . . . . . . . . . 10.0 ID1 . . . . . . . . . . . . . . . . Reagent Molar mass M . . . . . . . . . . . . 129.25 Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual Dispense Titrant . . . . . . . . . . . . . . Dibutylamine Concentration [mol/L] . . . . . . . 2.0 Volume [mL] . . . . . . . . . . . . 10.0 Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 300 Titration Titrant . . . . . . . . . . . . . . HCl (MeOH) Concentration [mol/L] . . . . . . . 1.0 Sensor . . . . . . . . . . . . . . . DG113-SC Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 17.5 Titrant addition . . . . . . . . DYN E(set) [mV] . . . . . . . . . 8.0 Limits V . . . . . . . . . . Absolute V(min) [mL] . . . . . . . 0.02 V(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 100 EQP range . . . . . . . . . . . . Yes Limit A . . . . . . . . . . . -500 Limit B . . . . . . . . . . . +500 Maximum volume [mL] . . . . . . . 30.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Calculation Result name . . . . . . . . . . . . Isocyan.Blank Formula . . . . . . . . . . . . . . R=Q Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol Decimal places . . . . . . . . . . . 3 Record Output unit . . . . . . . . . . . . Printer Results last sample . . . . . . . . Yes Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Outlier test . . . . . . . . . . . . Yes Auxiliary value ID text . . . . . . . . . . . . . . Blank Isocyanate val Formula . . . . . . . . . . . . . . H15=x Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes
. . . . Dibutylamine . . . . 2.0 . . . . 10.0 . . . . 50 . . . . 300 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HCl (MeOH) 1.0 DG113-SC mV EQP mL 1.0 DYN 8.0 Absolute 0.02 0.2 EQU 0.5 1.0 3.0 20.0 100 Yes -500 +500 30.0 Yes 1 Standard Isocyanate R1=(H15-Q)*C1/m C1=M/(10*z) % NCO 3 Printer Yes Yes Yes R1 Yes Yes Yes
. . . . Printer . . . . Yes
42
METTLER TOLEDO
M235
NCO-Content of Isocyanates by Backtitration

Determination of the isocyanate content in diphenylmethane-4,4-diisocyanate, 0.5 g
Sample
diphenylmethane-4,4-diisocyanate, 0.5 g

1) Dissolve the sample in 20 mL methylethylketone. 2) Add manually 10 mL 2 mol/L diisobutylamine in isopropanol or by means of an additional burette or a DU200 unit. 3) Add 50 mL isopropanol by means of an additional burette or by using a peristaltic pump. 4) Start back titration of excess diisobutylamine with HCl. Note: Isocyanates are toxic compounds. Appropriate working condictions are needed (fumehood, gloves, googles). The stirring time must be long enough to ensure complete dissolution and reaction of the sample before the back titration starts. Acidic or basic compounds in the sample interfere.
Substance Chemicals
Isocyanate groups, -NCO
20 mL methylethlyketone 10 mL diisobutylamine in isopropanol 50 mL isopropanol Hydrochloric acid, HCl, in isopropanol c(HCl) = 1 mol/L
Titrant
THAM DL50Graphix, DL53/55/58 DL70ES, DL77
Instead of diisobutylamine also di-n-butylamine can be used as a reagent. Toluene can also serve as an alternative solvent for the sample as well as for the titrant. Use dried solvents and reagents.
Accessories
Glass titration beaker ME-101446 Printer, balance Complete automation: two add. burettes DV1010, or use a DU200 Dosing unit. DG113-SC
Remarks
The isocyanate content is an indication for the number of isocyanate groups -NCO in the sample. The determination is achieved by a back titration. An excess diisobutylamine is added to the non-aqueous sample solution. Diisobutylamine reacts with isocyanate groups during the stirring time of 240 s. Unreacted diisobutylamine is subsequently titrated with hydrochloric acid. Two titration methods are used: 1) Method NCOB allows the determination of the solvent blank value which is automatically stored as auxiliary value H16. 2) Method NCO allows the determination of the isocyanate content. Hints: 1) Rinse accurately the electrode, the stirrer and the burette tip with e.g. acetone at the end of the titration series. 2) The DG113 electrode should be conditioned in pH buffer 7 over night to hydrate the pH glass membrane. Literature: ASTM D1638 (www.astm.org) DL40RC Application No. 163
R-NCO + NH(iBu)2 = (iBu)2N-CO-NHR NH(iBu)2 + HCl = (H2N(iBu)2)+ Cl-
Calculation
Blank determination (Method NCOB): R1 = Q R1 is stored as auxiliary value H16 Acid value det. (Method NCO): R1 = (H16-Q1)*C1/m C1 = M/(10*z)
Results
Waste disposal
Isocyanates solution: special waste Aromatic organic solvents
Author
Kees Mooibroek
43
Results
DL40RC: *** 28-JAN-86 *** .5203 12.51 2823 12.51 1 32.718
INPUT: WEIGHT IDENT. METHOD 1631 IDENT. SAMPLE NO. *R * %
STATISTICS: N MEAN STAND.DEV.% 6 32.823 0.29
Titration curve
44
Method
Method NCO Version Isocyanate 31-Jan-1994 Method 14:30 . . . . NCO . . . . Isocyanate . . . . 31-Jan-1994 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 Stand 1 Weight m 0.4 0.5 NCO 42.0171 1 Manual NCOB Version Isocyanate:Blank 31-Jan-1994 14:32 . . . . NCOB . . . . Isocyanate:Blank . . . . 31-Jan-1994 14:32 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 Stand 1 Fixed volume U 10.0 Reagent 129.25 1 Manual Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperature sensor . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . . . . Titrant addition . . . . E(set) [mV] . . . . . Limits V . . . . . . V(min) [mL] . . . V(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . EQP range . . . . . . . . Limit A . . . . . . . Limit B . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Results last sample . . . . Table of values . . . . . . E - V curve . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Volume [mL] . . . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperature sensor . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . . . . Titrant addition . . . . E(set) [mV] . . . . . Limits V . . . . . . V(min) [mL] . . . V(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . EQP range . . . . . . . . Limit A . . . . . . . Limit B . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Results last sample . . . . Table of values . . . . . . E - V curve . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . .
14:30
. . . . Dibutylamine . . . . 2.0 . . . . 10.0 . . . . 50 . . . . 300 . . . . Isopropanol . . . . 1.0 . . . . 50.0 . . . . 50 . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HCl (IPA) 1.0 DG113-SC mV EQP mL 1.0 DYN 8.0 Absolute 0.02 0.2 EQU 1.0 2.0 3.0 20.0 500 Yes -500 +500 25.0 Yes 1 Standard Isocyanate R1=(H16-Q)*C1/m C1=M/(10*z) % NCO 3 Printer Yes Yes Yes R1 Yes Yes Yes
. . . . Dibutylamine . . . . 2.0 . . . . 10.0 . . . . 50 . . . . 300 . . . . Isopropanol . . . . 1.0 . . . . 50.0 . . . . 50 . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HCl (MeOH) 1.0 DG113-SC mV EQP mL 17.5 DYN 8.0 Absolute 0.02 0.2 EQU 1.0 2.0 3.0 20.0 500 Yes -500 +500 30.0 Yes 1 Standard Isocyan.Blank R=Q mmol 3 Printer Yes Yes Yes R1 Yes Yes Yes
. . . . Printer . . . . Yes
. . . . Blank Isocyanate val . . . . H16=x . . . . Printer . . . . Yes
45
METTLER TOLEDO
M236
Determination of Free HCl and Isocyanates

Determination of the content of free hydrochloric acid and isocyanate by titration with sodium hydroxide in a methanolic sample solution. Sample
resins, 0.5-1 g

1) Dissolve the sample in 40 mL methanol. 2) Start titration with sodium hydroxide.
Substance Chemicals
Free HCl and isocyanate groups, -NCO

Note: Isocyanates are toxic compounds. Appropriate working condictions are needed (fumehood, gloves, googles). The titrant must be protected from CO2-intake from the air.
40 mL methanol
Titrant
Sodium hydroxide, NaOH, in methanol c(NaOH) = 0.1 mol/L
KHP DL50Graphix, DL53/55/58 DL70ES, DL77
Accessories
Glass titration beaker ME-101446 Printer, balance

DG113-SC
Hints: 1) The DG113 electrode should be conditioned in pH buffer 7 over night to hydrate the pH glass membrane. 2) Clean the electrode and the stirrer after each sample titration with eg. methanol.
HCl + NaOH = H2O + NaCl R-NCO + NaOH = ??
Calculation
Free HCl content: R1 = Q1*C1/m ; % C1 = 36.5/(10*z) Isocyanate content: R2 = Q2*C2/m ; % C2 = M/(10*z)
Results
Waste disposal
Isocyanates solution: special waste Organic solvents
Author
Roland Boehlen, MT-CH
46
Results
METTLER DL70 Titrator measured Titrator User 26-Oct-1992 BR**** 12:38
7 Free HCl and Isocyanate 26-Oct-1992 12:09 SW Version 2.0 SAMPLE Nr. 1/1 Titration stand Identification R-N:C:O Weight Correction factor TITRATION Titrant Concentration Sensor Consumption Consumption Excess CALCULATION Result CALCULATION Result
Stand 1 m = 0.5654 g f = 1.0 t = 1.0
NaOH 0.1 mol/L Drive 2 20 mL DG113-SC EQP 1 EQP 2 VEQ1 Q1 EPOT1 VEQ2 Q2 EPOT2 VEX QEX = = = = = = = =
0.42703 0.04270 423.4 6.25668 0.62567 -318.8 0.02829 0.00283
mL mmol mV mL mmol mV mL mmol % % Free HCl R-N:C:O
R1 = 0.28 R2 = 28.94
Titration curve
47
Method
Method 7 Version Free HCl and Isocyanate 26-Oct-1992 12:09 . . . . 7 . . . . Free HCl and Isocyanate . . . . 26-Oct-1992 12:09 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 Stand 1 Weight m 0.4 0.6 R-N:C:O 261.5 1 Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Titrant addition . . . . E(set) [mV] . . . . . Limits V . . . . . . V(min) [mL] . . . V(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Results last sample . . . . Table of values . . . . . . E - V curve . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . .
. . . . 50 . . . . 100 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . NaOH 0.1 DG113-SC mV EQP DYN 8.0 Absolute 0.02 0.5 EQU 0.5 1.0 1.0 30.0 500 25.0 Yes 2 Standard Free HCl R1=Q1*C1/m C1=36.5/(10*z) % 2 R-N:C:O R2=Q2*C2/m C2=M/(10*z) % 2 Printer Yes Yes Yes R1 Yes Yes Yes
. . . . Printer . . . . Yes
48
METTLER TOLEDO
M096
Iodine Value in Resins and Oils According to Wijs

Determination of the iodine value in resins and oils according to DIN 53241
Sample
Resins and oils, 0.2-0.7 g

1) The sample is dissolved in 10 mL solvent mixture consisting of glacial acetic acid:cyclohexane 1:4 .
Substance Chemicals
Carbon-carbon double bons, -CH=CH-
10 mL Glacial acetic acid:Cyclohexane 1:4 15 mL, Wijs-sol.: with ICl, c(ICl) = 0.1 M 5 mL , Potassium iodide, KI, c(KI) = 1 mol/L 20 mL, deionized water
2) 15 mL Wijs solution are added automatically by a DV1020 burette. The reaction is stirred during 60 s, and the electrode and stirrer are rinsed with 10 mL ethanol with the diaphragm pump. Use flexible conditioning setup with yellow cllips. 3) The function "Conditioning" is used to allow the sample solution to react completely during 1000 s. If the time is not enough, then the reaction time can be increased by repeatinmg the function "Conditioning" (loop). 4) 5 mL potassium iodide are added by a second burette, and the second diaphragm pump adds 20 mL deionized water. 5) Excess iodine is back-titrated using sodium iodine. The electrode is rinsed with 10 mL ethanol.
Titrant
Sodium thiosulfate, Na2S2O3 c(Na2S2O3)=0.1 mol/L Potassium iodate, KIO3 (see M526) DL70ES, DL77
Accessories
Glass titration beaker ME-101446 Rondo 60 with two diaphragm pumps, Printer, balance two additional burettes DV1020 DM140-SC
Remarks
Iodine value: The iodine value in the amount of ioding in g which reacts with the carbon double bonds in 100 g of sample (unsaturated bonds). It indicates the degree of unsaturation of the sample. Two titration methods are used: 1) Method 096B allows the determination of the solvent blank value which is automatically stored as auxiliary value H17. 2) Method 096A allows the determination of the iodine value by back titration of excess iodine with sodium thiosulphate. Hints: 1) The sample must be completely dissolved before addition of Wijs redution. The stirring time must be selected accordingly. If necessary, a ultrasonic bath can be used to dissolve sample. 2) The composition of the solvent mixture must be adapted to the sample. In this case, the most appropriate solvent is a mixture fo glacial acetic acid and cyclohexane. 3) The appropriate stirring speed for the back titration must be chosen to get an homogeneous phase system. Literature: DIN 53241 (www.din.de) Application M051
I2 + -CH=CH- = -CHI-IHCI2 + 2S2O32- = S4O62- + 2I-
Calculation
Blank determination (Method 096B): R1 = Q R1 is stored as auxiliary value H17 Iodine value det. (Method 096A): R1 = (H17-Q1)*C1/m C1 = M/(10*z)
Results
Waste disposal
Organic solvents
Author
Kees Mooibroek
49
Results
No 1/1 ID1 ID2 Sample amount and results Dammar Resin 25.0 mL Fixed volume U R1 = 1 LOOP .......................................................... 1/5 Dammar Resin 25.0 mL Fixed volume U R1 = 1 LOOP 1/6 Dammar Resin 25.0 mL Fixed volume U R1 = 1 LOOP 1/7 Dammar Resin 25.0 mL Fixed volume U R1 = 1 LOOP 2/1 Dammar Resin 0.275 g Weight m R2 = 79.81 g I2/100g Iodine number 2/2 Dammar Resin 0.275 g Weight m R2 = 74.10 g I2/100g Iodine number 2/3 Dammar Resin 0.275 g Weight m R2 = 73.39 g I2/100g Iodine number 2/4 Dammar Resin 0.275 g Weight m R2 = 72.53 g I2/100g Iodine number 2/5 Dammar Resin 0.275 g Weight m R2 = 72.07 g I2/100g Iodine number 2/6 Dammar Resin 0.275 g Weight m R2 = 71.91 g I2/100g Iodine number 2/7 Dammar Resin 0.275 g Weight m R2 = 71.69 g I2/100g Iodine number STATISTICS Number results R1 n = 7 Mean value x = 1 LOOP STATISTICS Number results R2 n = 7 Mean value x = 73.64 g I2/100g Iodine number Standard deviation s = 2.852742 g I2/100g Iodine number Rel. standard deviation srel = 3.874 % Outlier test : sample No. 2/1 Number results R1 n = 6 Mean value x = 72.62 g I2/100g Iodine number Standard deviation s = 0.942869 g I2/100g Iodine number Rel. standard deviation srel = 1.298 % Weitere Resultate: Sample Kolophonium Dammharz Lrchenl Leinl Blank value H17 Mass (g) 0.41 0.275 0.2326 0.1008 n 7 6 7 4 5 x (g/100g) 60.59 72.62 101.62 176.10 2.9417 mmol srel (%) 0.66 1.30 0.85 0.56 0.04 Time (min) 4 6 4 5 4
Titration curve
50
Method
Method 096A Version Wijs Iodine Number 10-May-1994 9:45 . . . . . . . 096A . . . . . . . Wijs Iodine Value . . . . . . . 10-May-1994 9:45 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 ST20 1 Weight m 0.0 10.0 Polymer 254 2 Manual Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Number samples . . . . Titration stand . . . Entry type . . . . . . Lower limit [g] . . Upper limit [g] . . ID1 . . . . . . . . . Molar mass M . . . . . Equivalent number z . Temperature sensor . . Dispense Titrant . . . . . . . Concentration [mol/L] Volume [mL] . . . . . Stir Speed [%] . . . . . . Time [s] . . . . . . . Calculation Result name . . . . . Formula . . . . . . . Constant . . . . . . . Result unit . . . . . Decimal places . . . . Rinse Auxiliary reagent . . Volume [mL] . . . . . Statistics Ri (i=index) . . . . . Dispense Titrant . . . . . . . Concentration [mol/L] Volume [mL] . . . . . Stir Speed [%] . . . . . . Time [s] . . . . . . . Conditioning Interval . . . . . . . Time [s] . . . . . . . Sample Number samples . . . . Titration stand . . . Entry type . . . . . . Lower limit [g] . . Upper limit [g] . . ID1 . . . . . . . . . Molar mass M . . . . . Equivalent number z . Temperature sensor . . Dispense Titrant . . . . . . . Concentration [mol/L] Volume [mL] . . . . . Pump Auxiliary reagent . . Volume [mL] . . . . . Stir Speed [%] . . . . . . Time [s] . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . . . . Titrant addition . . . . E(set) [mV] . . . . . Limits V . . . . . . V(min) [mL] . . . V(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . EQP range . . . . . . . . Limit A . . . . . . . Limit B . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Condition . . . . . . . . . Condition . . . . . . . . Record Output unit . . . . . . . . Results last sample . . . . Table of values . . . . . . E - V curve . . . . . . . . Condition . . . . . . . . . Condition . . . . . . . . Record Output unit . . . . . . . . Results last sample . . . . Table of values . . . . . . E - V curve . . . . . . . . Condition . . . . . . . . . Condition . . . . . . . . Rinse Auxiliary reagent . . . . . Volume [mL] . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Conditioning Interval . . . . . . . . . . Time [s] . . . . . . . . . . Rinse . . . . . . . . . . . Auxiliary reagent . . . . Volume [mL] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3 0.1 DM140-SC mV EQP mL 1.0 DYN 8.0 Absolute 0.02 0.4 EQU 1.0 1.0 6.0 30.0 300 Yes 1000 -1000 50.0 Yes 1 Standard Iodine Number R1=(H17-Q)*C1/m C1=M/(10*z) % NCO 2 Yes VEQ>0 Printer Yes Yes Yes Yes VEQ>0 Printer Yes Yes Yes Yes VEQ<=0
. . . . . . . Wijs solution . . . . . . . 0.1 . . . . . . . 15.0 . . . . . . . 50 . . . . . . . 60 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . LOOP . R1=1 . . . 0
. . . . . . . Ethanol . . . . . . . 10.0 . . . . . . . R1 . . . . . . . Isopropanol . . . . . . . 1.0 . . . . . . . 50.0 . . . . . . . 0 . . . . . . . 0 . . . . . . . 1 . . . . . . . 1000 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7 ST20 1 Weight m 0.0 10.0 Polymer 254 2 Manual
. . . . Ethanol . . . . 10.0 . . . . . . . . . . . . . . . . R2 Yes Yes Yes
. . . . . . . KI (1) . . . . . . . 1.0 . . . . . . . 5.0 . . . . . . . H2O . . . . . . . 20.0 . . . . . . . 70 . . . . . . . 60
. . . . Printer . . . . Yes . . . . . . . . . . . . . . . . . . . . 1 60 Yes H2O 10.0
Blank Determination: Method 096B is used for the blank determination and is similar to method 096A. The blank value is stored as auxiliary value H17 (function "Auxiliary value")
51
METTLER TOLEDO
M051
Iodine Value of Edible Oils and Fats According to Wijs (AOAC Method
Method for the determination of iodine value (g I2/100g) of edible oils and fats according to Wijs as indicated by AOAC Official Methods of Analysis (1984), Chapter 28.023 Sample
Fats and oils, approx. 25 g / expected Iodine value

1) Dissolve the sample in CCl4, add 25 mL Wijs solution and keep in the dark for approx. 1 hour to complete the reaction. 2) Add deionized water and titrate excess iodine with sodium thiosulphate. Wijs solution: Dissolve 16.2 g iodine monochloride (ICl) in a 1 L volumetric flask with glacial acetic acid. Store the Wijs solution in amber bottle sealed with paraffin until it is used. Wijs solution is sensitive to temperature, moisture and light. Slight variations of the temperature considerably affect titer of the Wijs solution. Therefore it is essential that blanks and samples are titrated at same time. The mean value of the blank determination (method 051b) is automatically stored as auxiliary value H3. Typical results: Blank = 4.94 mmol, srel = 0.04%, n = 5
Substance Chemicals
C-C double bonds, -CH=CH-
15 mL carbon tetrachloride, CCl4 ; 25 mL Wijs solution; 100mL water; 15 mL 10% potassium iodide, KI Sodium thiosulphate, Na2S2O3 c(Na2S2O3)=0.1 mol/L; Potassium iodate, KIO3 DL70, AT250, Matrix printer EPSON FX800 with serial interface
Titrant
Accessories
250 mL Titration beakers ME-23829, Additional burette drive DV90

DM140-SC at Sensor 2
The iodine value is defined as the weight of iodine absorbed by 100 g of an oil or fat. 1) The excess of Wijs solution should be 50-60% of the amount added, ie. 100-150% of amount reacted with the sample.
ICl3 + I2 = 3 ICl ICl + KI = I2 + KCl 2(SO3S)2- + I2 = 2 I- + (S2O6S2)2-
Calculation
Blank determination (Method 096B): R1 = Q R1 is stored as auxiliary value H3 Iodine value det. (Method 096A): R1 = (H3-Q1)*C1/m C1 = M/(10*z)
2) If the result will be assumed (e.g. in routinr quality control) the predispensing can be adjusted accordingly in volume or changed to % nominal content . This also shortens the titration time. 3) The addition of 10 mL 2.5% mercury (II) acetate in glacial acetic acid (after Wijs solution is added) shortens the reaction time to 5 minutes
Results
Literature: AOAC Official Method of Analysis, 1984, Chapter 28.023
Waste disposal
Halogenated organic solvent
Author
Ruth von Rotz
52
Results
METTLER DL70 051a Titrator I2-value of oils and fats 25-June-1991 rvr PT 2 SW 2.0 3:37 pm
Measured User Titrator Version RESULTS No ID1 1/1 1/2 1/3 1/4 1/5
Weight 2.0267 2.0766 2.0892 2.031 2.0863 n x s srel = = = = g g g g g 5 11.85 0.013 0.107
Results 11.85 11.85 11.85 11.84 11.87 g I2/100 gI2-value g I2/100 gI2-value g I2/100 gI2-value g I2/100 gI2-value g I2/100 gI2-value
cocofat cocofat cocofat cocofat cocofat
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation Various Samples Sample Coconut fat Margarine "light" Lard Olive oil Margarine Rape oil Sunflower oil Weight (g) 2.00-2.10 0.40-0.45 0.40-0.45 0.20-0.25 0.50-0.55 0.20-0.25 0.20-0.25
g I2/100 gI2-value g I2/100 gI2-value %
n 5 3 5 5 3 4 3
Iodine value (gI2/100g) 11.8 37.3 57.6 82.5 86.1 113.4 132.7
RSD (%) 0.11 0.26 0.13 0.16 0.21 0.15 0.06
t (min) 5 5 5 6 3 5 4
Titration curve
53
Method
Method 051a Version I2 - value of oils and fats 19-June-1991 16:21 . . . . 051a . . . . I2 - value of oils and . . . . 19-June-1991 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Stand 1 Weight m 0.02 1.5 254 2 16:21 Method 051b Version Blank I2 - value 19-June-1991 16:15 . . . . 051b . . . . Blank I2 - value . . . . 19-June-1991 16:15 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Stand 1 Fixed volume U 25.0 Blank 0.0 1 Title Method ID . . . . . . . . . Title . . . . . . . . . . . fats Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . Predispensing 2 . . . . . slope [mV,pH, .../mL] Titrant addition . . . . dE (set)[mV] . . . . . Limits dV . . . . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t (min) [s] . . . . t (max) [s] . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . E - V curve . . . . . . . . Table of measured values . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Volume [mL] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . Predispensing 2 . . . . . slope [mV,pH, .../mL] Titrant addition . . . . dE (set)[mV] . . . . . Limits dV . . . . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t (min) [s] . . . . t (max) [s] . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . E - V curve . . . . . . . . Table of measured values . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . .
. . . . KI 10% . . . . 10.0 . . . . 15.0 . . . . 50 . . . . 45 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3H2O 0.1 DM140-SC mV EQP mL 20.0 To slope 4.0 DYN 0.02 Absolute 0.02 0.5 EQU 1.0 1.0 6.0 30.0 50.0 50.0 Yes 1 Standard I2 - value R=(H3-Q)*C/m C=M/(10*z) g I2/100g 2 Printer Yes Yes Yes R1 Yes Yes Yes
. . . . KI 10% . . . . 10.0 . . . . 15.0 . . . . 50 . . . . 45 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3H2O 0.1 DM140-SC mV EQP mL 40.0 To slope 4.0 DYN 4.0 Absolute 0.02 0.5 EQU 1.0 1.0 6.0 30.0 50.0 60.0 Yes 1 Standard Blank I2 - value R1=Q[1] mmol 4 Printer Yes Yes Yes R1 Yes Yes Yes I2 - value
. . . . Blank . . . . H3=x . . . . Printer . . . . Yes
. . . . Printer . . . . Yes
54
METTLER TOLEDO
M211
Iodine Value of Cosmetic Fats According to Wijs

Method for the determination of the iodine value of cosmetic fats according to Wijs.
Sample
Cosmetic fats, 0.1 - 5 g according to the expected iodine value

1) Dissolve the sample in 10 mL carbon tetrachloride. The Wijs solution, mercuric acetate and potassium iodide solution are added automatically by the DL70 titrator. 2) The mercuric acetate in glacial acetic acid, which is only added after the Wijs reagent, is used to speed up the reaction. 3) It is important to determine the blank 3 times before the iodine value determination. The mean value of the three blank determinations is stored as auxiliary value (H3).
Substance Chemicals
C-C double bonds, -CH=CH-
10 mL CCl4 ; 10 mL Wijs solution; 20 mL 2.5 % mercury (II) acetate; 20 mL 20% potassium iodide, KI Sodium thiosulphate, c(Na2S2O3)=0.1 mol/L;
Titrant
Potassium iodate, KIO3 DL70, ST20A Sample changer, AT250 Balance, Matrix printer EPSON FX800 with serial interface Titration beaker ME-101974, 3 Peristaltic pumps ME-65241, 1 Additional burette drive DV90
Note: 1. Wijs solution, c(ICl) = 0.2 mol/L 2. The 2.5% solution is prepared by dissolving mercury (II) acteta in glacial acetic acid.
Accessories

DM140-SC at Sensor 2
The iodine value is defined as the amount of iodine which reacts with 100 g of an oil or fat.
ICl3 + I2 = 3 ICl ICl + KI = I2 + KCl 2(SO3S)2- + I2 = 2 I- + (S2O6S2)2Literature: See Application No. M051, M096 and M617
Calculation
Blank value: R1 = Q1[1] ; in mmol R1 is stored as auxiliary value H3 Iodine value: R2 = (H3-Q1[2])/m ; mmol/g
Results
Waste disposal
Halogenated organic solvents containing mercury ions.
Author
Angelo Bonetti
55
Results
METTLER DL70 Laboratorio controllo M.P. Automatic: Indice di Iodio Measured User Titration Version RESULTS No 1/1 1/2 1/3 2/1 2/2 2/3 ID1 Bianco J Bianco J Bianco J No. Iodio No. Iodio No. Iodio Volume 10.0 10.0 10.0 0.151 0.15 mL mL ml g g Results 1.7659 1.7682 1.7688 87.74 87.84 87.83 mmol mmol mmol gI 2/100g gI 2/100g gI 2/100g Bianco J Bianco J Bianco J Indice Iodio Indice Iodio Indice Iodio 01-Dec-1989 RGF 01-Dec-1989 SW 1.2 11:23 09:46
0.1547 g
STATISTICS Number results Mean value Standard deviation Rel. standard deviation STATISTICS Number results Mean value Standard deviation Rel. standard deviation AUXILIARY VALUE Nouvelle value
= = = = = = = =
3 1.7676 0.00152 0.086 3 87.80 0.056 0.064
mmol mmol %
Bianco J Bianco J
gI 2/100g Indice Iodio gI 2/100g Indice Iodio % Bianco del Wijs
H3 = 1.767644
Titration curve
56
Method
Method 211 Version Automatiz. Indice di Iodio 30-Nov-1989 11.27 . . . . 211 . . . . Automatiz.Indice di . . . . 30-Nov-1989 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11.27 Title Method ID . . . . . . . . . Title . . . . . . . . . . . Iodio Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Volume [mL] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Dispense Titrant . . . . . . . . . . Concentration . . . . . . . Volume [mL] . . . . . . . . Dispense Titrant . . . . . . . . . . Concentration . . . . . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Auxilliary instrument Name . . . . . . . . . . . . Time [s] . . . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predespensing 1 . . . . . Volume [mL] . . . . . Predespensing 2 . . . . . Potential (mV,pH...) . Titrant addition . . . . dV [mL] . . . . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Rinse Solution aux. . . . . . . . Volume [mL] . . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Record All results . . . . . . . . Table of values . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Dispense Titrant . . . . . . . . . . Concentration . . . . . . . Volume [mL] . . . . . . . . Dispense Titrant . . . . . . . . . . Concentration . . . . . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Auxilliary instrument Name . . . . . . . . . . . . Time (s) . . . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predespensing 1 . . . . . Volume [mL] . . . . . Titrant addition . . . . dV (set) [mL] . . . . Limits dV . . . . . . dV (min) [mL] . . . . dV (max) [mL] . . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Rinse Solution aux. . . . . . . . Volume [mL] . . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Record All results . . . . . . . . Table of values . . . . . . . . . . Reatt.di Wijs . . . . 0.2 . . . . 10.0 . . . . (CH3COO)2Hg . . . . 0.0 . . . . 10.0 . . . . 65 . . . . 300 . . . . Pompa KI . . . . 3.0 . . . . 100 . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3 0.1 DM-140-SC mV EQP mL 16.0 DYN 5.0 Absolute 0.03 0.5 EQU 0.5 1.0 2.0 10.0 200.0 25.0 Yes 1 Asymmetric
3 ST20 Fixed volume U 10.0 Bianco J 1.0 1
. . . . Reatt.di Wijs . . . . 0.2 . . . . 10.0 . . . . (CH3COO)2Hg . . . . 0.0 . . . . 10.0 . . . . 60 . . . . 120 . . . . Pompa KI . . . . 3.0 . . . . 100 . . . . 30 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3 0.1 DM-140-SC mV EQP mL 16.0 f (potential) 230.0 INC 0.05 EQU 0.5 1.0 2.0 10.0 350.0 25.0 Yes 1 Asymmetric
. . . . H2O . . . . 10.0 . . . . . . . . . . . . . . . . . . . . Indice Iodio R2=(H3-Q[2])*C2/m C2=M/(10*z) gI2/100g 2
. . . . R2 . . . . Yes . . . . Yes . . . . Yes . . . . Yes
. . . . H2O . . . . 10.0 . . . . . . . . . . . . . . . . . . . . Bianco J R1=Q1[1] mmol 4
. . . . R1 . . . . Yes . . . . Yes . . . . Bianco del Wijs . . . . H3=x . . . . Yes . . . . Yes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 ST20 Poids m 0.05 2.0 No. Iodio 254 2
57
METTLER TOLEDO
M206
Determination of Carboxyl Groups in PET

Carboxyl groups, -COOH, in PET are determined by non-aqueous titration with KOH
Sample
Amorphous PET, 1 g

1) The sample is heated in 50 mL solvent mixture (chloroform:phenol, 3:2) during 1 hour at 130C using a reflux condenser.
Substance Chemicals
Carboxyl goups, -COOH
2) After cooling down at room temperature, the sample istitrated with potassium hydroxide and bromphenol blue as an indicator. 3) A DP550 phototrode is used to monitor the colour chang eof the indicator from yello to blue. 4) A blank value is determined previous tiraiton of the sample. The blank value is stored as auxiliary value H18.
50 mL solvent mixture (Chloroform:phenol 3:2) Indic.: bromphenol blue in ethanol Potassium hydroxide in benzyl alcohol, c(KOH)=0.02 mol/L
Titrant
KHP in benzyl alcohol DL70/DL77 Balance, printer
Accessories
Titration beaker ME-101974 Adapter cable DIN-Lemo ME-89600

DP550 Phototrode, colour indicator: 0.1% Bromphenol blue in ethanol
1) The titer determination is performed using potassium hydrogen phtalate, KHP, as a primary standard: KHP is dissolved in 10 mL deionized water and diluted to 100 mL with benzyl alcohol. 2 mL of this solution was added to 50 mL benzyl alcohol and titrated with KOH. Phenolphtalein in ethanol is used as colour indicator. 2) The DP550 phototrode has to be adjusted to approximately 1000 mV by dipping it in deionized water and turning the knob on the top of the housing.
Calculation
R=Q*C/m C=1000 , in eq/ton
3) The sensor and the stirrer have to be cleaned thoroughly with water and benzyl alcohol afte reach sample deteremination. Literature: See Application No. M051, M096 and M617
Results
Waste disposal
Halogenated organic solvents
Author
Viola Schindler
58
Results
METTLER DL77 Method User Measured RESULTS No 1/1 1/2 1/3 ID1 COOH COOH COOH ID2 Sample amount and results 1.0008 R1 = 21.39511 R2 = 1.3474 1.0008 R1 = 21.51753 R2 = 1.3551 1.0008 R1 = 21.14597 R2 = 1.3317 g Weight eq/ton mL g Weight eq/ton mL g Weight eq/ton mL m COOH content mL consump m COOH content mL consump m COOH content mL consump Titrator 23 V3.1 Mettler - Toledo AG Market Support Laboratory 08-Jan-1997 12:44
206A COOH in PET determination V. Schindler 08-Jan-1997 17:44
STATISTICS Number results n Mean value x Standard deviation s Rel. standard deviation srel Outlier test: no outliers!
= = = =
3 21.35287 0.189344 0.887
eq/ton eq/ton %
COOH content COOH content
Titration curve
59
Method
Method 206A Version COOH in PET determination 08-Jan-1994 12:44 Method 206B Version Blank: COOH in PET 08-Jan-1994 12:47 . . . . 206B . . . . Blank: COOH in PET . . . . 08-Jan-1994 12:47 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Stand 1 Fixed volume U 50.0 COOH 54.02 1 Manual Title Method ID . . . . . . . . . . . . . 206A Title . . . . . . . . . . . . . . . COOH in PET determination Date/time . . . . . . . . . . . . . 08-Jan-1994 12:44 Sample Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Weight m Lower limit [g] . . . . . . . . . 0.0 Upper limit [g] . . . . . . . . . 7.0 ID1 . . . . . . . . . . . . . . . . COOH Molar mass M . . . . . . . . . . . . 54.02 Equivalent number z . . . . . . . . 1 Temeprature sensor . . . . . . . . . Manual Instruction Add bromphenol Blue Stir Speed [%] . . . . . . . . . . . . . 80 Time [s] . . . . . . . . . . . . . . 40 Stir Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 2 Titration Titrant . . . . . . . . . . . . . . KOH Concentration [mol/L] . . . . . . . 0.02 Sensor . . . . . . . . . . . . . . . DP550 Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . INC dV [mL] . . . . . . . . . . 0.1 Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 5.0 t(max) [s] . . . . . . . . . . 40.0 Threshold . . . . . . . . . . . . 250.0 Maximum volume [mL] . . . . . . . 3.0 Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard Calculation Result name . . . . . . . . . . . . COOH content Formula . . . . . . . . . . . . . . R=(Q-H18)*C/m Constant . . . . . . . . . . . . . . C=1000 Result unit . . . . . . . . . . . . eq/ton Decimal places . . . . . . . . . . . 5 Calculation Result name . . . . . . . . . . . . mL consump Formula . . . . . . . . . . . . . . R2=VEQ Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mL Decimal places . . . . . . . . . . . 4 Record Output unit . . . . . . . . . . . . Printer Sample data . . . . . . . . . . . . Yes All results . . . . . . . . . . . . Yes Table of values . . . . . . . . . . Yes dE/dV - V curve . . . . . . . . . . Yes Statistics Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes Outlier test . . . . . . . . . . . . Yes Record Output unit . . . . . . . . . . . . Printer All results . . . . . . . . . . . . Yes Table of values . . . . . . . . . . Yes Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Volume [mL] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temeprature sensor . . . . . Instruction Add bromphenol Blue Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Titrant addition . . . . dV [mL] . . . . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Sample data . . . . . . . . All results . . . . . . . . Table of values . . . . . . dE/dV - V curve . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . .
. . . . 80 . . . . 40 . . . . 50 . . . . 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . KOH 0.02 DP550 mV EQP INC 0.02 EQU 0.5 1.0 5.0 40.0 250.0 3.0 Yes 1 Standard Blank R=Q mmol 5 Printer Yes Yes Yes Yes R1 Yes Yes Yes
. . . . Blank . . . . H18=x . . . . Printer . . . . Yes
60
METTLER TOLEDO
M237
Peroxide Value of Lecithin

Determination of the peroxide value of lecithin
Sample
Lecithin, 5 g

1) Lecithin is dissolved in a solvent mixture consisting of 12 mL chloroform and 18 mL glacial acetic acid.
Substance Chemicals
Peroxide, ROOR
2) After manually adding 0.5 mL saturated potassium iodide solution, the sample is stirred 60 s using the auxiliary function Stir of the titrator. Iodine is generated. 3) 30 mL deionised water are added to the sample together with starch. 4) The sample is titrated using sodium thiosulphate.
12 mL Chloroform, CHCl3 , 18 mL glacial acetic acid, 0.5 mL saturated KI solution, 30 mL deion. water, starch Sodium thiosulfate, Na2S2O3 c(Na2S2O3)= 0.01mol/L; Potassium iodate, KIO3 DL50 Graphix
Titrant
Note: Starch is added in order to select the most appropriate titarnt increment size for the titration depending on the colour obtained: Faint blue: increment size 0.05 mL Dark blue: increment size 0.5 mL
Accessories

DM140-SC
A blank value is determined previous sample titration. This application was perforemd with theDL40RC titrator and the method was adapted tot he DL50 Graphix. The method can be completely automated using a DL58 or a DL7x titrator using the flexible method concept.
2R-OOH + 2KI = 2R-OH + 2KOH + I2 I2 + 2Na2S2O3 = 2NaI + Na2S4O6
Calculation
Peroxide value det. (Method 40014) R = (Q-H2)*C/m C=1000 , meq O2/kg Blank determination (Method 40015) R = Q ; mmol R is stored as auxiliary value H2 Halogenated organic solvents
Results
Waste disposal
Author
R. Gnter, MT-D
61
Results
DL40RC: *** 20-NOV-81 ***
METHOD 2 IDENT. SAMPLE NO. *R *
9147 1.2 1 .10000
STATISTICS: N MEAN STAND.DEV.% 5 3.5 3.1
Titration curve
62
Method
Method 40014 Version Peroxide value 7-Feb-2002 11:00 . . . . . . . 40014 . . . . . . . Peroxide value . . . . . . . 7-Feb-2002 11:00 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Lecithin Weight 4.0 6.0 1.0 1 Stand 1 Manual Method 40015 Version Blank 7-Feb-2002 11:05 Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Lower limit [g] . . Upper limit [g] . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Titrant addition . . . dV[mL] . . . . . . Measure mode . . . . . Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Volume [mL] . . . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Titrant addition . . . dV[mL] . . . . . . Measure mode . . . . .
. . . . . . . 40015 . . . . . . . Blank . . . . . . . 11-Dec-2001 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
11:05
Blank peroxide Volume 60.05 1.0 1 Stand 1 Manual
. . . . . . . 50 . . . . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3 0.01 DM140 mV No Incremental 0.05 Equilibrium controlled 0.2 1.0 5.0 30.0 200 No No Negative 30.0 No No No No Standard No No Yes neq=0 R1=(Q-H1)*C1/m C1=1000 3 meq O2/kg Peroxide value Yes R2=Q 5 mmol Yes
. . . . . . . 50 . . . . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3 0.01 DM140 mV No Incremental 0.02 Equilibrium controlled 0.2 1.0 5.0 30.0 200 No No Negative 5.0 No No No No Standard No No Yes neq=0 R1=Q 5 mmol Yes
. . . 0 . . .
. . Blank peroxide . . H2=x . . . . . . . . . . . . . . . . . . . . . . . . . . Printer No Yes No Yes No Yes Yes No No No No No
63
METTLER TOLEDO
M624
Peroxide Value of Edible oils and Fats

Method for the determination of the peroxide value in oil, fat and margarine.
Sample
Oil, fat, margarine ; 3 g

1) Beakers have to be cleaned very well. Invisible fat residues or metal traces can affect the result strongly.
Substance Chemicals
Peroxide, ROOR
2) About 3 g of sample were dissolved in 20 mL of acetic acid/chloroform (3:2) The acetic acid/chloroform mixture was added by the function DISPENSE. 3) 1 mL of saturated potassium iodide solution is added manually. Thereaction takes place and iodine is formed. 4) 50 mL deionized water are added manually to the sample solution. Iodine is titrated with sodium thiosulphate. Saturated KI solution: 127 g KI were dissolved in 100 mL water to obtain the saturated KI solution. The solution has to be kept in the dark. Optimum stir time Several measurements were made to evaluate the optimal stir time. 300 s were found to be the optimum stir time. A stir time of less than 300 s was found to be insufficient resulting in low results. A stir time of more than 300 s leads to secondary reactions between the liberated iodine and the oil.
20 mL acetic acid/chloroform 1 mL saturated KI solution 50 mL deion. water Sodium thiosulfate, Na2S2O3 c(Na2S2O3)= 0.01mol/L; Potassium iodate, KIO3 DL58; DL70ES/DL77
Titrant
Accessories
Titration beakers ME-101974 Balance, Printer

DM140-SC
Blank value determination Impurities of the solvent are taken into account by a blank value determination. The blank value determination is done under the same conditions as the peroxide value determination itself. The blank value is automatically stored as auxiliary value H1 with the function AUXILIARY VALUE (see method 91015) Definitions Fats and oils undergo changes during storage due to oxidation with air (oxidative rancidity). The compounds formed react as peroxides. Their content is commonly expressed as the "peroxide value" in milliequivalents peroxidic oxygen per kg of sample. Peroxide values higher than 10 to 20 meq O2/kg are commonly interpreted as rancidity. Unrefined oils have higher peroxide values. They are usually in the range between 5 to 20 meq O2/kg. Influence stir time Stir time [s] 60 180 300 600 Result [meq/kg] 3.201 4.947 6.817 6.491
2R-OOH + 2KI = 2R-OH + 2KOH + I2 I2 + 2Na2S2O3 = 2NaI + Na2S4O6
Calculation
Peroxide value det. (Method 91016) R = (Q-H1)*C/m C=1000 , meq O2/kg Blank determination (Method 91015) R=Q Q is stored as auxiliary value H1 The waste contains organic solvents and is disposed accordingly.
Results
Waste disposal
Author
K. Wydler
64
Results
Peroxide value of olive oil ALL RESULTS No. 1 2 3 4 5 ID ROOR ROOR ROOR ROOR ROOR Sample size and results 3.2691 R1 = 16.104 3.1461 R1 = 16.660 3.1838 R1 = 16.783 3.2309 R1 = 16.660 3.0293 R1 = 16.517 g meq/kg g meq/kg g meq/kg g meq/kg g meq/kg Peroxide Val. Peroxide Val. Peroxide Val. Peroxide Val. Peroxide Val.
Etc. STATISTICS Number of results R1 Mean value Standard deviation Rel. standard deviation n x s srel = = = = 5 16.545 meq/kg Peroxide Val. 0.26372 meq/Kg Peroxide Val. 1.594 %
Peroxide value: comparison of different oils and fats
Oil
Sample mass [g] 3.0435 2.3521 1.9836 3.0293 2.3217 3.9440 2.0889 4.2328 4.5656 3.0248 3.2691 3.8720 2.7137 2.6050
Mean value [% water] 18.310 13.880 13.179 16.545 11.680 8.312 5.542
Stand. Deviation [% water] 0.35621 0.75799 0.58047 0.26372 0.62599 0.45597 0.23404
srel [%] 1.945 5.461 4.405 1.594 5.359 5.486 4.224
Thistle oil Sunflower oil Peanut oil Olive oil Palm oil Margarine Coconut fat
5 5 5 5 5 5 5
Titration curve
65
Method
Method 91016 Version Peroxide Value 30-Jul-1999 13:14 . . . 91016 . . . Peroxide Value . . . 30-Jul-1999 13:14 . . . . . . . . . . . . . . . . . . . . . . . . O2 Weight 0.0 5.0 32.0 1 Stand 1 Manual Method 91015 Version Blank Peroxide Value 30-Jul-1999 12:18 . . . 91015 . . . Blank Peroxide Value . . . 30-Jul-1999 13:14 . . . . . . . . . . . . . . . . . . . . . . . . O2 Weight 0.0 5.0 32.0 1 Stand 1 Manual Title Method ID . . . . . . . . Title . . . . . . . . . . Date/time . . . . . . . . Sample Sample ID . . . . . . . . Entry type . . . . . . . . Lower limit [g] . . . . Upper limit [g] . . . . Molar mass M . . . . . . . Equivalent number z . . . Titration stand . . . . . Temperature sensor . . . . Dispense Titrant . . . . . . . . . Concentration [mol/L] . . Volume [mL] . . . . . . . Instruction Text . . . . . . . . . . . Stir Speed [%] . . . . . . . . Time [s] . . . . . . . . . Instruction Text . . . . . . . . . . . EQP titration Titrant/Sensor Titrant . . . . . . . . Concentration [mol/L] . Sensor . . . . . . . . Unit of meas . . . . . Predispensing . . . . . . Titrant addition . . . . . dE(set) [mV] . . . . . dV(min) [mL] . . . . . dV(max) [mL] . . . . . Measure mode . . . . . . dE [mV] . . . . . . . . dt [s] . . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Recognition Threshold . . . . . . . Steepest jump only . . Range . . . . . . . . . Tendency . . . . . . . Termination at maximum volume [mL] at potential . . . . . at slope . . . . . . . afternumber EQPs . . . n = . . . . . . . . comb. term. conditions Evaluation Procedure . . . . . . . Potential 1 . . . . . . Potential 2 . . . . . . Stop for reevaluation . Calculation Formula . . . . . . . . . Constant . . . . . . . . . Decimal places . . . . . . Result unit . . . . . . . Result name . . . . . . . Statistics . . . . . . . . Report Output . . . . . . . . . Results . . . . . . . . . All results . . . . . . . Raw results . . . . . . . Table of measured values . Sample data . . . . . . . E - V curve . . . . . . . dE/dV - V curve . . . . . Title Method ID . . . . . . . . Title . . . . . . . . . . Date/time . . . . . . . . Sample Sample ID . . . . . . . . Entry type . . . . . . . . Lower limit [g] . . . . Upper limit [g] . . . . Molar mass M . . . . . . . Equivalent number z . . . Titration stand . . . . . Temperature sensor . . . . Dispense Titrant . . . . . . . . . Concentration [mol/L] . . Volume [mL] . . . . . . . Instruction Text . . . . . . . . . . . Stir Speed [%] . . . . . . . . Time [s] . . . . . . . . . Instruction Text . . . . . . . . . . . EQP titration Titrant/Sensor Titrant . . . . . . . . Concentration [mol/L] . Sensor . . . . . . . . Unit of meas . . . . . Predispensing . . . . . . Titrant addition . . . . . dE(set) [mV] . . . . . dV(min) [mL] . . . . . dV(max) [mL] . . . . . Measure mode . . . . . . dE [mV] . . . . . . . . dt [s] . . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Recognition Threshold . . . . . . . Steepest jump only . . Range . . . . . . . . . Tendency . . . . . . . Termination at maximum volume [mL] at potential . . . . . at slope . . . . . . . afternumber EQPs . . . n = . . . . . . . . comb. term. conditions Evaluation Procedure . . . . . . . Potential 1 . . . . . . Potential 2 . . . . . . Stop for reevaluation . Calculation Formula . . . . . . . . . Constant . . . . . . . . . Decimal places . . . . . . Result unit . . . . . . . Result name . . . . . . . Statistics . . . . . . . . Auxiliary value ID . . . . . . . . . . . . Formula . . . . . . . . . Report Output . . . . . . . . . Results . . . . . . . . . All results . . . . . . . Raw results . . . . . . . Table of measured values . Sample data . . . . . . . E - V curve . . . . . . . dE/dV - V curve . . . . .
. . . Chloroform/AA . . . 0.1 . . . 20 . . . Add 1 mL KI solution . . . 50 . . . 300 . . . Add 50 mL destilled water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3 0.01 DM140 mV No Dynamic 8.0 0.02 0.2 Equilibrium controlled 0.5 1.0 3.0 30.0 200.0 No No Negative 20.0 No No Yes 1 No Standard No No No R=(Q-H1)*C/m C=1000 3 meq/kg Peroxide Val. Yes Printer No Yes Yes Yes Yes Yes Yes
. . . Chloroform/AA . . . 0.1 . . . 20 . . . Add 1 mL KI solution . . . 50 . . . 300 . . . Add 50 mL destilled water . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3 0.01 DM140 mV No Dynamic 8.0 0.02 0.2 Equilibrium controlled 0.5 1.0 3.0 30.0 200.0 No No Negative 20.0 No No Yes 1 No Standard No No No R=VEQ 3 mL Blank Yes
. . . Blank Peroxide Value . . . H1=x . . . . . . . . . . . . . . . . . . . . . . . . Printer No Yes Yes Yes Yes Yes Yes
66
METTLER TOLEDO
M238
Determination of Permanganate Index in Waste Water

Determination of permanganate index in waste water by titration with potassium permanganate. This application is especially suited for low content of oxidazable substances. Sample
Waste water (low degree), 50 mL

1) The sample is heated for at least 10 minutes at more than 85C.
Substance Chemicals
Oxidazable substances
2) The solution is acidified by adding manually (or with a burette) 5 mL 20 % sulphuric acid. 3) 2 mL 0.1 KMnO4 are dispensed with a burette. After waiting 150 s, an EP titration is started. The time delay is set to 60 s according to the application.
5 mL 20% sulphuric acid, H2SO4
Titrant
Potassium permanganate KMnO4, c(KMnO4) = 0.1 mol/L Sodium oxalate, Na2C2O4 (see M527) DL55+, DL58, DL70ES/DL7 DH100 Heating System, Balance, printer Glass titration beaker ME-101446 2 (1) Additional burette Cable DH100-Titrator (DL5x: 51 07424, DL7x: 51 108404) DM140-SC
Note: 1) The titer determination is performed using sodium oxalate. ca. 25-40 mg are dissolved in 50 mL 5% sulfuric acid and wormed to 80C, since the titration runs slowly at room T. (See application no. M527). 2) Do not dip the tip of the burettes into the sample solution to avoid diffusion into sample solution.
Accessories
Remarks
1) The permanganate index is the amount of oxygen which corresponds to the equivalent of permanganate ions consumend in the reaction. It is an indicative parameter for tjhe amounf ot oxidazable substances, and therefore an indication for hew pollution of waters. 2) Method M238 is a simplified version of the procedure based on on DIN 38409-H5 (ISO 8467). 3) This method is a more easier and straightforward method as th COD determination. Since the oxidative power is lower compared to COD, not all substances are oxidazed.
MnO4- + 5e- + 8H2O = Mn2- + 12H2O
Calculation
R= (QDISP+Q)*C/m C= 1000 , mmol/L DL7x: U ; instead of m
Literature: DIN 38409-H5, ISO 8467
Results
Waste disposal
Aqueous acid solutions containing metal ions.
Author
Ch. Walter, A. Aichert
67
Results
METTLER DL77 Method User Measured RESULTS No 1/1 1/2 1/3 ID1 COOH COOH COOH ID2 Sample amount and results 50.0 R1 = 7.900 50.0 R1 = 2.800 50.0 R1 = 7.700 mL Fixed volume U mmol/L KMnO 4 Number mL Fixed volume U mmol/L KMnO 4 Number mL Fixed volume U mmol/L KMnO 4 Number 238 Titrator IC113 V3.1 Mettler-Toledo AG Market Support Laboratory 12-Jan-1994 11:38
KMnO 4 Number 12:06
12-Jan-1994
STATISTICS Number results n Mean value x Standard deviation s Rel. standard deviation srel Outlier test: no outliers!
= = = =
3 7.800 0.100000 1.282
mmol/L mmol/L
KMnO 4 Number KMnO 4 Number
Titration curve
68
Method
Method 238 Version KMnO4 Number 12-Jan-1994 11:38 . . 238 . . KMnO4 Number . . 12-Jan-1994 11:38 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Stand 1 Fixed volume U 50.0 100.0 1 TEMP A TEMP A C 1.0 2.0 T larger Set 85.0 600.0 Title Method ID . . . . . . . . . . . Title . . . . . . . . . . . . . Date/time . . . . . . . . . . . Sample Number samples . . . . . . . . . Titration stand . . . . . . . . Entry type . . . . . . . . . . . Volume [mL] . . . . . . . . . ID1 . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . Equivalent number z . . . . . . Temperature sensor . . . . . . . Temperature Sensor . . . . . . . . . . . . . Unit of meas. . . . . . . . . . dT [C,F, K] . . . . . . . . . dt [s] . . . . . . . . . . . . . t(min) mode . . . . . . . . . . Set value [C,F, K] . . . . t(max) [s] . . . . . . . . . . . Dispense Titrant . . . . . . . . . . . . Concentration [mol/L] . . . . . Volume [mL] . . . . . . . . . . Measure Sensor . . . . . . . . . . . . . Unit of meas. . . . . . . . . . dE [mV] . . . . . . . . . . . . dt [s] . . . . . . . . . . . . . t(min) mode . . . . . . . . . . Set value [C,F, K] . . . . t(max) [s] . . . . . . . . . . . Titration Titrant . . . . . . . . . . . . Concentration [mol/L] . . . . . Sensor . . . . . . . . . . . . . Unit of meas. . . . . . . . . . Titration mode . . . . . . . . . Predispensing . . . . . . . . Volume [mL] . . . . . . . Titrant addition . . . . . . Control band [mV, pH, ...] Time delay [s] . . . . . . dV [mL] . . . . . . . . . End point mode . . . . . . . Potential [mV, pH, ...] . Tendency . . . . . . . . . . Maximum volume [mL] . . . . . Calculation Result name . . . . . . . . . . Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Result unit . . . . . . . . . . Decimal places . . . . . . . . . Record Output unit . . . . . . . . . . All results . . . . . . . . . . Table of values . . . . . . . . E - V curve . . . . . . . . . . Statistics Ri (i=index) . . . . . . . . . . Standard deviation s . . . . . . Rel. standard deviation srel . . Outlier test . . . . . . . . . . Record Output unit . . . . . . . . . . All results . . . . . . . . . .
. . KMnO4 . . 0.1 . . 2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . DM140-SC mV 0.5 1.0 Fix 150.0 150.0 KMnO4 0.1 DM140-SC mV EP mL 0 Continuous 100.0 60.0 0.05 EPA 1150.0 Positive 10.0 KMnO4 Number R=(QDISP+Q)*C/U C=1000 mmol/L 3 Printer Yes Yes Yes R1 Yes Yes Yes
. . Printer . . Yes
69
METTLER TOLEDO
M239
Chemical Oxygen Demand (COD) of Waste Water

Determination of the COD value in waste water according to DIN 38409 part 4, H4
Sample
Waste water, 20 mL (Or: KHP solution as standard)

1) The sample preparation is performed automatically on the Rondo 60 sample changer using method 4001: 1.1 Add magnetic stirrer into the COD glass tube (boiling add). 1.2 20 mL waste water are added 1.3 Add 10 mL 0.12 molL 1/6 K2Cr2O7 containing Hg2SO4 to mask chloride (conc.: 0.4g/20 mL, commercially available). 1.4 30 mL Ag2SO4/H2SO4 are slowly added by a burette. Be careful: Heat is developed ! 2) The COD glass tubes are brought to the digestor for heating. The sample solutions are boiled at 148 +/- 3C for 2 hours. Afterwards, the COD tubes are let to cool down to at least 60C. 3) The condenser is rinsed with distilled water, and the tubes are filled with distilled water up to 100 mL. The tubes are cooled down to room temperature and placed on the sample changer rack. Excess dichromate solution is titrated with FAS and the results expressed as mg O2/L. The whole COD procedure is tested with 20 mL potassium hydrogen phtalate KHP solution (COD = 200 +/- 8 mg O2/L). Preparation: KHP is dried at 105C for 2 hours. 0.17 g KHP are dissolved in some water in a 1 L volumetric flask. Add 5 mL concentrated H2SO4, and fill up to 1000 mL. The solution remains stable for 1 week when kept cool.
Substance Chemicals
Oxidazable organic substances
10 mL potassium dichromate, K2Cr2O7 c(1/6 K2Cr2O7) = 0.12 mol/L 30 mL 0.1 mol/L Ag2SO4/H2SO4 FAS, (NH4)2Fe(II)(SO4)2 c(FAS)= 0.12 mol/L;
Titrant
K2Cr2O7 (see application M548) DL50Graphix, DL5x, DL70ES/DL77 Rondo 60, Rondo COD Set, magnetic stirrer for Rondo 60. Heater with reflux condenser (third party), 1 additional burette DV1010 (DL7x: two additional burettes), Balance, Printer DM144-SC
Accessories
Remarks
1) Chemical Oxygen Demand (COD) is a summary value that indicates the water quality in the environmental protection field. By means of COD back titration the quantity of oxidazable organic matter -expressed as the equivalent amount of oxygenis determined by oxidation with potassium dichromate. First the amount of dichromate (without sample) is determined using method 4002 and stored as auxiliary value. After oxidation the sample solution is titrated with dichromate using method 4003. 2) The COD value is proportional to the total amount of organic oxidazable matter including non- or hardly biodegradable matter. Therefore all inorganic components that could be oxidized too have to be masked during or removed before oxidation step (masking agent: mercury(II) sulfate). 3) The same special flask of the Rondo 60 COD set is used for the sample preparation (oxidation step) and titration. 4) The titer of FAS must be checked daily. 5) For accurate results, it is recommended to use distilled water instead of deionized water. Literature: DIN 38409 part 4, H4
Cr2O72- + 6Fe2+ + 14H+ = 2Cr3+ + 6Fe3+ + 7H2O 2 Cr3+ = 2 Cr3+ + 6 e1.5 mol O2 = 6 mol 1/6Cr2O72- = 6mol FAS 1 mol O2 = 4 mol 1/6Cr2O72- = 4 mol FAS
Therefore: z = 4
Calculation
COD determination (Method 4003) R = (H18-Q)*C/m C = M*1000/z , mg O2/L Back value determination (4002) R=Q Q is stored as auxiliary value H18 The waste contains organic solvents and is disposed accordingly.
Results
Waste disposal
Author
Peter Burri
70
Results
METTLER TOLEDO DL58 Titrator V2.3 DL Basic Course Titration Basic Course Market Support Analytical 10-May-2000 16:36
Method Measured User ALL RESULTS No. 1 2 3
4003 COD Determination 10-May-2000 16:46 PB
ID 8.0mL FAS 8.0mL FAS 8.0mL FAS
Sample size and results 20.0 R1 = 427.828 R2 = 1.532 20.0 R1 = 427.682 R2 = 1.535 20.0 R1 = 428.336 R2 = 1.523 mL mg O2/L mL mL mg O2/L mL mL mg O2/L mL COD FAS consumed COD FAS consumed COD FAS consumed
STATISTICS Number of results R1 Mean value Standard deviation Rel. standard deviation Number of results R2 Mean value Standard deviation Rel. standard deviation
= = = = = = = =
3 427.948 0.3432 0.080 3 1.530 0.00626 0.409
mg O2/L COD mg O2/L COD % mL
mL %
Titration curve
71
Method
Method 4003 Version COD Determination 10-May-2000 16:36 . . . 4002 . . . COD Determination . . . 10-May-2000 16:36 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Effluent Fixed volume 20.0 32.0 4 ST20A No No Yes H2SO4 5% 20.0 No Manual Method 4003: similar to 4002, an additional auxiliary function is used to store the result in mmol (Q) as auxiliary value H18 Method 4001 Version COD Preparation 08-May-2000 17:12 . . . 4001 . . . COD Preparation . . . 08-May-2000 17:12 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Chemicals Fixed volume 20.0 58.43 1 ST20A No No Yes H2SO4 5% 2.0 No Manual Title Method ID . . . . . . . . Title . . . . . . . . . . Date/time . . . . . . . . Sample Sample ID . . . . . . . . Entry type . . . . . . . . Volume [mL] . . . . . . Molar mass M . . . . . . . Equivalent number z . . . Titration stand . . . . . Pump . . . . . . . . . Pump . . . . . . . . . Rinse . . . . . . . . . Solvent . . . . . . Volume [mL] . . . . Conditioning . . . . . Temperature sensor . . . . Stir Speed [%] . . . . . . . . Time [s] . . . . . . . . . EQP titration Titrant/Sensor Titrant . . . . . . . . Concentration [mol/L] . Sensor . . . . . . . . Unit of meas . . . . . Predispensing . . . . . . Volume [mV] . . . . . . Wait time [s] . . . . . Titrant addition . . . . . dE(set) [mV] . . . . . dV(min) [mL] . . . . . dV(max) [mL] . . . . . Measure mode . . . . . . dE [mV] . . . . . . . . dt [s] . . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Recognition Threshold . . . . . . . Steepest jump only . . Range . . . . . . . . . Tendency . . . . . . . Termination at maximum volume [mL] at potential . . . . . at slope . . . . . . . after number EQPs . . . n = . . . . . . . . comb. term. conditions Evaluation Procedure . . . . . . . Potential 1 . . . . . . Potential 2 . . . . . . Stop for reevaluation . Condition . . . . . Calculation Formula . . . . . . . . . Constant . . . . . . . . . Decimal places . . . . . . Result unit . . . . . . . Result name . . . . . . . Statistics . . . . . . . . Calculation Formula . . . . . . . . . Constant . . . . . . . . . Decimal places . . . . . . Result unit . . . . . . . Result name . . . . . . . Statistics . . . . . . . . Report Output . . . . . . . . . Results . . . . . . . . . All results . . . . . . . Raw results . . . . . . . Table of measured values . Sample data . . . . . . . E - V curve . . . . . . . dE/dV - V curve . . . . . d2E/dV2 - V curve . . . . log dE/dV - v curve . . . E - t curve . . . . . . . V - t curve . . . . . . . dV/dt - t curve . . . . .
. . . 22 . . . 25 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . (NH4)2Fe(II)(SO4)2 0.12 DM144 mV to volume 0.5 10 Dynamic 6.0 0.05 0.5 Equilibrium controlled 0.5 1.0 5.0 30.0 200.0 No No Negative 15.0 No No Yes 1 No Standard No No Yes neq=0 R=(H18-Q)*C/m C=M*1000/z 3 mg O2/L COD Yes R2=VEQ 3 mL FAS consumed Yes Printer No Yes No Yes No Yes Yes No No No No No
Title Method ID . . . . . . . . Title . . . . . . . . . . Date/time . . . . . . . . Sample Sample ID . . . . . . . . Entry type . . . . . . . . Volume [mL] . . . . . . Molar mass M . . . . . . . Equivalent number z . . . Titration stand . . . . . Pump . . . . . . . . . Pump . . . . . . . . . Rinse . . . . . . . . . Solvent . . . . . . Volume [mL] . . . . Conditioning . . . . . Temperature sensor . . . . Dispense Titrant . . . . . . . . . Concentration [mol/L] . . Volume [mL] . . . . . . . Stir Speed [%] . . . . . . . . Time [s] . . . . . . . . . EQP titration Titrant/Sensor Titrant . . . . . . . . Concentration [mol/L] . Sensor . . . . . . . . Unit of meas . . . . . Predispensing . . . . . . Titrant addition . . . . . dV [mL] . . . . . . . . Measure mode . . . . . . dt [s] . . . . . . . . Recognition Threshold . . . . . . . Steepest jump only . . Range . . . . . . . . . Tendency . . . . . . . Termination at maximum volume [mL] at potential . . . . . at slope . . . . . . . after number EQPs . . . Evaluation Procedure . . . . . . . Potential 1 . . . . . . Potential 2 . . . . . . Stop for reevaluation . Calculation Formula . . . . . . . . . Constant . . . . . . . . . Decimal places . . . . . . Result unit . . . . . . . Result name . . . . . . . Statistics . . . . . . . . Report Output . . . . . . . . . Results . . . . . . . . . All results . . . . . . . Raw results . . . . . . . Table of measured values . Sample data . . . . . . . E - V curve . . . . . . . dE/dV - V curve . . . . . d2E/dV2 - V curve . . . . log dE/dV - v curve . . . E - t curve . . . . . . . V - t curve . . . . . . . dV/dt - t curve . . . . .
. . . 1/6 K2Cr2O7 . . . 0.12 . . . 10.0 . . . 25 . . . 20 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . H2SO4/Ag2SO4 0.1 DM144 mV No Incremental 0.5 Timed increment 10.0 400.0 No No None 30.0 No No No Standard No No No R=VEND 3 mL H2SO4 No Printer No Yes No No No No No No No No No No
72
METTLER TOLEDO
M517
Blank determination according to ASTM D664-89

A method for the determination of the blank value for a acid number analysis according to ASTM D664-89.
Sample
60 mL Solvent 664

1) The blank determination of solvent 664 used for AN-Analysis (toluene/2-propanol/water 500:495:5) is done automatically with the sample changer.
Substance Chemicals
Acidic components
Toluene/2-propanol/water 500:495:5
2) 60 mL solvent 664 are added with the pump. After every titration the electrode is conditioned in water for 5 minutes and then rinsed with solvent 664.
Titrant
Potassium hydroxide in 2-propanol c(KOH) = 0.1 mol/L;
Potassium hydrogen phthalate DL50Graphix, DL53/55/58, DL70ES/77 Sample changer, Printer Titration beaker ME-101974 Pump ME-65241
Accessories

DG113
1) The analysis is performed by placing the following succession of beakers on the sample turntable: 1.1 An empty beaker followed by a beaker with 60 mL deion. water for conditioning (indicated with a yellow clip). 1.2 Before starting the method the alkaline buffer potential (buffer B) must be entered as endpoint in the function TITRATION. 1.3 The result of this blank determination is stored as auxiliary value H10. It is used for calculation in the acid number determination (method 90019).
Calculation
R = Q ; mmol R is stored as auxiliary value H10.

Literature: ASTM D664-89 (see www.astm.org) Application brochrue 3, "TAN and TBN", ME-724559
Results
Waste disposal
Aromatic organic waste
Author
A. Aichert, A. Logean
73
Results
METTLER TOLEDO DL53 Method Measured User RESULTS No. 1 2 3 ID Sample size and results 60.0 R1 = 0.0044 60.0 R1 = 0.0041 60.0 R1 = 0.0043 mL mmol mL mmol mL mmol Blank Blank Blank Titrator 010 V1.0 Mettler-Toledo AG Market Support Laboratory 01-Jul-1995 12:00
90017 Blindwert AN 20-Jul-1995 15:04
ASTM D664
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation AUXILIARY VALUE New value
n x s srel
= = = =
3 0.0043 0.00015 3.559 0.00429
mmol mmol %
Blank Blank
H10 =
Blank AN ASTM D
Titration curve
74
Method
Method 90017 Version Blank AN ASTM D664 01-Jul-1995 12:00 . . . . . . 00017 . . . . . . Blank AN ASTM D664 . . . . . . 01-Jul-1995 12:00 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Fixed volume 60.0 100.0 1 ST20A Yes Solvent 664 60.0 Yes Solvent 664 20.0 Yes 300 Yes Solvent 664 20.0 Manual Title Method ID . . . . . . . Title . . . . . . . . . Date/time . . . . . . . Sample Sample ID . . . . . . . Entry type . . . . . . . Volume [mL] . . . . . Molar mass M . . . . . . Equivalent number z . . Titration stand . . . . Pump . . . . . . . . Solvent . . . . . Volume [mL] . . . Rinse . . . . . . . . Solvent . . . . . Volume [mL] . . . Conditioning . . . . Time [s] . . . . . Rinse . . . . . . Solvent . . . . Volume [mL] . . Temperature sensor . . . Stir Speed [%] . . . . . . . Time [s] . . . . . . . . EP titration Titrant/Sensor Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . Unit of meas. . . . . Predispensing . . . . . Titrant addition . . . . dE(set) [mV] . . . . dV(min) [mL] . . . . dV(max) [mL] . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . t(max) [s] . . . . . End point . . . . . . . Potential [mV,pH,..] Tendency Tendency . . . . . . Termination Maximum volume [mL] . Delay [s] . . . . . . Calculation Formula . . . . . . . . Constant . . . . . . . . Decimal places . . . . . Result unit . . . . . . Result name . . . . . . Statistics . . . . . . . Calculation Formula . . . . . . . . Constant . . . . . . . . Decimal places . . . . . Result unit . . . . . . Result name . . . . . . Statistics . . . . . . . Auxiliary value ID . . . . . . . . . . . Formula . . . . . . . . Report Output unit . . . . . . Results . . . . . . . . All results . . . . . . Raw results . . . . . . Table of measured values Sample data . . . . . . E - V curve . . . . . . dE/dV - V curve . . . . d2E/dV2 - V curve . . . log dE/dV - V curve . . E - t curve . . . . . . V - t curve . . . . . . dV/dt - t curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Printer No Yes No Yes No No No No No No No
. . . . . . 50 . . . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . KOH (i-PrOH) 0.1 DG113 mV No Dynamic 4.0 0.02 0.05 0.5 6.0 6.0 30.0 EP absolute -143
. . . . . . Negative . . . . . . 1.0 . . . . . . 0 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . R=Q 4 mmol Blank Yes
. . . 0 . . . No
. . . . . . Blank AN ASTM D664 . . . . . . H10=x
75
METTLER TOLEDO
M518
Blank determination according to ASTM D4739-92

A method for the determination of the blank value for a Base Number analysis according to ASTM D4739-92. Sample
60 mL Solvent 4739

1) The blank determination of solvent 4739 (toluene/2-propanol/chloroform/water 100:100:100:3) is done automatically with the sample changer.
Substance Chemicals
Alkaline components
toluene/2-propanol/chloroform/water 100:100:100:3
2) 60 mL solvent 4739 are added with the pump. After every titration the electrode is conditioned in water for 5 minutes and then rinsed with solvent 4739.
Titrant
Hydrochloric acid in 2-propanol c(HCl) = 0.1 mol/L
KOH 0.1 mol/L DL50Graphix, DL53/55/58, DL70ES/77 Rondo 60 Titration beaker ME-101974, Printer
Accessories

DG113
1) The analysis is performed by placing the following succession of beakers on the sample turntable: 1.1 An empty beaker followed by a beaker with 60 mL deion. water for conditioning (indicated with a yellow clip). 1.2 Before starting the method, the acidic buffer potential (buffer A) must entered as endpoint in the function TITRATION. 2) The result of this blank determination is stored as auxiliary value H11. It is used for calculation in the base number determination (method 90020).
Calculation
R = Q ; mmol R is stored as auxiliary value H11
Results
Waste disposal
The conditioning beakers contain a mixture of water/aromatic organic solvents. For waste disposal, separate water and solvent. A. Aichert, A. Logean
Literature: ASTM D4789-92 (www.astm.org) Application brochure 3, "TAN and TBN", ME-724559
Author
76
Results
METTLER TOLEDO DL53 Method Measured User RESULTS No. 1 2 3 ID Sample size and results 60.0 R1 = 0.0011 60.0 R1 = 0.0010 60.0 R1 = 0.0011 mL mmol mL mmol mL mmol Blank value Blank value Blank value Titrator 010 V1.0 Mettler-Toledo AG Market Support Laboratory 01-Jul-1995 12:00
90018 Blank BN ASTM D4739 18-Jul-1995 15:15
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation AUXILIARY VALUE New value
n x s srel
= = = =
3 0.0011 0.00004 3.467 0.00108
mmol mmol %
Blank value Blank value
H11 =
Blank value BN
Titration curve
77
Method
Method 90018 Version Blank BN ASTM D4739 01-Jul-1995 12:00 . . . . . . 90018 . . . . . . Blank BN ASTM D4739 . . . . . . 01-Jul-1995 12:00 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Fixed volume 60.0 100.0 1 ST20A Yes Solvent 4739 60.0 Yes Solvent 4739 20.0 Yes 300 Yes Solvent 4739 20.0 Manual Title Method ID . . . . . . . Title . . . . . . . . . Date/time . . . . . . . Sample Sample ID . . . . . . . Entry type . . . . . . . Volume [mL] . . . . . Molar mass M . . . . . . Equivalent number z . . Titration stand . . . . Pump . . . . . . . . Solvent . . . . . Volume [mL] . . . Rinse . . . . . . . . Solvent . . . . . Volume [mL] . . . Conditioning . . . . Time [s] . . . . . Rinse . . . . . . Solvent . . . . Volume [mL] . . Temperature sensor . . . Stir Speed [%] . . . . . . . Time [s] . . . . . . . . EP titration Titrant/Sensor Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . Unit of meas. . . . . Predispensing . . . . . Titrant addition . . . . dE(set) [mV] . . . . dV(min) [mL] . . . . dV(max) [mL] . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . t(max) [s] . . . . . End point . . . . . . . Potential [mV,pH,..] Tendency Tendency . . . . . . Termination Maximum volume [mL] . Delay [s] . . . . . . Calculation Formula . . . . . . . . Constant . . . . . . . . Decimal places . . . . . Result unit . . . . . . Result name . . . . . . Statistics . . . . . . . Calculation Formula . . . . . . . . Constant . . . . . . . . Decimal places . . . . . Result unit . . . . . . Result name . . . . . . Statistics . . . . . . . Auxiliary value ID . . . . . . . . . . . Formula . . . . . . . . Report Output unit . . . . . . Results . . . . . . . . All results . . . . . . Raw results . . . . . . Table of measured values Sample data . . . . . . E - V curve . . . . . . dE/dV - V curve . . . . d2E/dV2 - V curve . . . log dE/dV - V curve . . E - t curve . . . . . . V - t curve . . . . . .
. . . . . . 50 . . . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HCl (i-PrOH) 0.1 DG113 mV No Dynamic 4.0 0.02 0.05 0.5 6.0 30.0 90.0 EP absolute 154
. . . . . . Positive . . . . . . 1.0 . . . . . . 0 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . R=Q 4 mmol Blank value Yes
. . . 0 . . . No
. . . . . . Blank value BN D4739 . . . . . . H11=x . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Printer No Yes No Yes No No No No No No No
78
METTLER TOLEDO
M519
AN (acid number) according to ASTM D664-89

Method for the determination of AN (Acid Number) according to ASTM D664-89
Sample
1 - 20 g Oil

1) Weigh in a well homogenised oil sample in the titration beaker and place it on the sample changer.
Substance Chemicals
Acidic components
2) The 60 mL solvent 664 needed to dissolve the sample are added automatically with the pump. The pump also rinses with solvent 664 after titration and conditioning are done.
ASTM 664 solvent Toluene/2-propanol/water 500:495:5
To proceed with this determination, the following steps are needed: 1. Determination of the alkaline buffer value (buffer B). 2. Blank determination of solvent 664 (method 90017). 3. Enter the buffer B value in the function TITRATION of AN determination method 90019 (Parameter: evaluation, as "potential 1" and also as "termination at potential"). General procedure: 1. Titer det. of 0.1 mol/L KOH 0.1 with KHP 2. Determination of the alkaline buffer value (buffer B) 3. Blank determ. of Solvent 664 (M517, Method 90017) 4. Determ. of the base number (AN) (M519, Method 90019)
Titrant
Potassium hydroxide in 2-propanol c(KOH) = 0.1 mol/L;
Potassium hydrogen phthalate, KHP DL50Graphix, DL53/55/58, DL7x Rondo 60,
Accessories
Titration beaker ME-101974 balance, printer

DG113-SC
Acid number according to ASTM D664-89: Consumption of mg KOH/g oil to buffer value B or to the EQP nearest to the buffer value B. Titration parameters: The titration parameters correspond exactly to the standard ASTM D664-89: 1. Titrant addition: max. speed 0.2 mL/min 2. dE< 30 mV/0.1 mL > Increment = 0.1 mL 3. dE> 30 mV/0.1 mL > Increment = 0.05 mL 4. The titration will be terminated if the potential is below buffer value B and the change is smaller than 50 mV/mL KOH. Conditioning After every titration the electrode is conditioned in water for 5 minutes and then rinsed with solvent 664. With this method the conditioning proceeds automatically, if the sample changer holds a conditioning beaker with 60 mL deion. water after every sample. Literature: ASTM D664-89 (see www,astm.org) Application brochure 3, "TAN and TBN", ME-724559
Calculation
R1 = consumption of mg KOH/g oil to the buffer value B R2 = consumption of mg KOH/g oil to EQP nearest to the buffer value B If there is no EQP, the result is negative. (Blank value of the solvent)
Results
Waste disposal
Aromatic organic waste. The conditioning beakers contain a mixture of water and organic solvents.
Author
79
Results
METTLER TOLEDO DL53 Method Measured User RESULTS No. 1 2 3 4 5 ID Oil Oil Oil Oil Oil Sample size and results 7.275 R1 = 1.83 R2 = -0.03 6.768 R1 = 1.81 R2 = -0.04 6.975 R1 = 1.81 R2 = -0.03 6.706 R1 = 1.79 R2 = -0.04 7.227 R1 = 1.73 R2 = -0.03 g mg mg g mg mg g mg mg g mg mg g mg mg KOH/g KOH/g KOH/g KOH/g KOH/g KOH/g KOH/g KOH/g KOH/g KOH/g AN (Buffer B) AN (EQP) AN (Buffer B) AN (EQP) AN (Buffer B) AN (EQP) AN (Buffer B) AN (EQP) AN (Buffer B) AN (EQP) Titrator 010 V1.0 Mettler-Toledo AG Market Support Laboratory 01-Jul-1995 12:00
90019 AN ASTM D664 21-Jul-1995 19:47
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation
n x s srel
= = = =
5 1.79 0.03513 1.960
mg KOH/gAN (Buffer B) mg KOH/gAN (Buffer B) %
Titration curve
80
Method
Method 90019 Version AN ASTM D664 01-Jul-1995 12:00 . . 90019 . . AN ASTM D664 . . 01-Jul-1995 12:00 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Oil Weight 0.1 20.0 56.1 1 ST20A Yes Solvent 664 60.0 Yes Solvent 664 20.0 Yes 300 Yes Solvent 664 20.0 Manual Title Method ID . . . . . . . . . . . Title . . . . . . . . . . . . . Date/time . . . . . . . . . . . Sample Sample ID . . . . . . . . . . . Entry type . . . . . . . . . . . Lower limit [g] . . . . . . . Upper limit [g] . . . . . . . Molar mass M . . . . . . . . . . Equivalent number z . . . . . . Titration stand . . . . . . . . Pump . . . . . . . . . . . . Solvent . . . . . . . . . Volume [mL] . . . . . . . Rinse . . . . . . . . . . . . Solvent . . . . . . . . . Volume [mL] . . . . . . . Conditioning . . . . . . . . Time [s] . . . . . . . . . Rinse . . . . . . . . . . Solvent . . . . . . . . Volume [mL] . . . . . . Temperature sensor . . . . . . . Stir Speed [%] . . . . . . . . . . . Time [s] . . . . . . . . . . . . EQP titration Titrant/Sensor Titrant . . . . . . . . . . . Concentration [mol/L] . . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . . Predispensing . . . . . . . . . Volume [mL] . . . . . . . . . Titrant addition . . . . . . . . dE(set) [mV] . . . . . . . . dV(min) [mL] . . . . . . . . dV(max) [mL] . . . . . . . . Measure mode . . . . . . . . . . dE [mV] . . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . . Limit A [mV,pH,...] . . . Limit B [mV,pH,...] . . . Tendency . . . . . . . . . . Termination at maximum volume [mL] . . . at potential . . . . . . . . Potential [mV,pH,..] . . . at slope . . . . . . . . . . Slope [mV,pH,.../mL] . . . after number EQPs . . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . . Potential 1 . . . . . . . . . Pot. 1 [mV,pH,...] . . . . Potential 2 . . . . . . . . . Stop for reevaluation . . . . Calculation Formula . . . . . . . . Constant . . . . . . . . Decimal places . . . . . Result unit . . . . . . Result name . . . . . . Statistics . . . . . . . Calculation Formula . . . . . . . . Constant . . . . . . . . Decimal places . . . . . Result unit . . . . . . Result name . . . . . . Statistics . . . . . . . Calculation Formula . . . . . . . . Constant . . . . . . . . Decimal places . . . . . Result unit . . . . . . Result name . . . . . . Statistics . . . . . . . Report Output unit . . . . . . Results . . . . . . . . All results . . . . . . Raw results . . . . . . Table of measured values Sample data . . . . . . E - V curve . . . . . . dE/dV - V curve . . . . d2E/dV2 - V curve . . . log dE/dV - V curve . . E - t curve . . . . . . V - t curve . . . . . . dV/dt - t curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . R1=(QP1-H10)*M/m 2 mg KOH/g AN (Buffer B) Yes R2=(Q(EPOT~P1)-H10)*C2 C2=M/m 2 mg KOH/g AN (EQP) Yes
. . . 0 . . . No . . . . . . . . . . . . . Printer No Yes Yes Yes No Yes No No No No No No
. . 60 . . 60 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . KOH (i-PrOH) 0.1 DG113 mV to volume 0.2 Dynamic 30.0 0.05 0.2 Equilibrium controlled 0.5 6.0 30.0 90.0 250.0 No Yes -20 -300 Negative 10.0 Yes -150 Yes 50.0 No Yes Standard Yes -150 No No
81
METTLER TOLEDO
M520
BN (base number) ASTM D4739-92

Method for the determination of BN (Base Number) according to ASTM D4739-92
Sample
1 - 20 g Oil

1) Weigh in a well homogenized oil sample in the titration beaker and place it on the sample changer.
Substance Chemicals
Basic components
2) The 60 mL solvent 4739 needed to dissolve the sample are added automatically with the pump. The pump also rinses with solvent 4739 after titration and conditioning are done. To proceed with this determination, the following steps are needed: 1. Determination of the acid buffer value (buffer A) 2. Blank of solvent 4739 (method 90018) 3. Enter the buffer A value in the function TITRATION of method 90020 (parameter: evaluation, as "potential 1"; also the range for the EQP recognition, "buffer value A +100 mV", and also as termination at potential, "buffer value A + 120 mV"). General procedure: 1. Titer det. of 0.1 mol/L HCl with standardized KOH 0.1 mol/L 2. Determination of the acidic buffer value (buffer A) 3. Blank determ. of Solvent 4739 (M518, Method 90018) 4. Determ. of the base number (BN) (M520, Method 90020)
ASTM 4739 solvent Toluene/2-propanol/chloroform/water 100:100:100:3 Hydrochloric acid in 2-propanol c(HCl) = 0.1 mol/L;
Titrant
DL50Graphix, DL53/55/58, Rondo 60 Sample changer
Accessories
Titration beaker ME-101974 Balance, printer

DG113-SC
Base number according to ASTM D4739-92 Consumption of mg KOH/g oil to buffer value A or to the EQP in the range "buffer value A + 100 mV" Titration parameters The titration parameters correspond exactly to the standard ASTM D4739: 1. Titrant addition 0.1 mL every 90 seconds. 2. The titration will be terminated when the potential is 120 mV above buffer value A.
Calculation
R1 = consumption of mg KOH/g oil to the buffer value A R2 = consumption of mg KOH/g oil to EQP nearest to the buffer value A If there is no EQP, the result is negative. (Blank value of the solvent).
Conditioning After every titration the electrode is conditioned in water for 5 minutes and then rinsed with solvent 4739. With this method the conditioning is automatically proceeded, if on the sample changer after every sample a conditioning beaker with 60 mL deion. water is placed.
Results
Waste disposal
Separate water and halogenated organic solvent before disposing.
Literature: ASTM D4739-92 (www.astm.org) Application brochure 3, "TAN and TBN", ME-724559
Author
82
Results
METTLER TOLEDO DL53 Method Measured User RESULTS No. 1 2 3 4 5 ID Oil Oil Oil Oil Oil Sample size and results 1.7955 R1 = 9.90 R2 = 10.88 2.1974 R1 = 9.79 R2 = 10.92 1.9269 R1 = 9.71 R2 = 10.86 2.1927 R1 = 9.63 R2 = 10.81 1.8911 R1 = 9.67 R2 = 10.83 g mg mg g mg mg g mg mg g mg mg g mg mg KOH/g KOH/g KOH/g KOH/g KOH/g KOH/g KOH/g KOH/g KOH/g KOH/g BN (buffer A) BN (EQP) BN (buffer A) BN (EQP) BN (buffer A) BN (EQP) BN (buffer A) BN (EQP) BN (buffer A) BN (EQP) Titrator 010 V1.0 Mettler-Toledo AG Market Support Laboratory 01-Jul-1995 12:00
90020 BN ASTM D4739 18-Jul-1995 23:44
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation STATISTICS Number results R2 Mean value Standard deviation Rel. standard deviation
= = = = = = = =
5 9.74 0.10709 1.099 5 10.86 0.04364 0.402
mg KOH/gBN (buffer A) mg KOH/gBN (buffer A) %
mg KOH/gBN (EQP) mg KOH/gBN (EQP) %
Titration curve
83
Method
Method 90020 Version BN ASTM D4739 01-Jul-1995 12:00 . . 90020 . . BN ASTM D4739 . . 01-Jul-1995 12:00 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Oil Weight 0.1 20.0 56.1 1 ST20A Yes Solvent 4739 60.0 Yes Solvent 4739 20.0 Yes 300 Yes Solvent 4739 20.0 Manual Title Method ID . . . . . . . . . . . Title . . . . . . . . . . . . . Date/time . . . . . . . . . . . Sample Sample ID . . . . . . . . . . . Entry type . . . . . . . . . . . Lower limit [g] . . . . . . . Upper limit [g] . . . . . . . Molar mass M . . . . . . . . . . Equivalent number z . . . . . . Titration stand . . . . . . . . Pump . . . . . . . . . . . . Solvent . . . . . . . . . Volume [mL] . . . . . . . Rinse . . . . . . . . . . . . Solvent . . . . . . . . . Volume [mL] . . . . . . . Conditioning . . . . . . . . Time [s] . . . . . . . . . Rinse . . . . . . . . . . Solvent . . . . . . . . Volume [mL] . . . . . . Temperature sensor . . . . . . . Stir Speed [%] . . . . . . . . . . . Time [s] . . . . . . . . . . . . EQP titration Titrant/Sensor Titrant . . . . . . . . . . . Concentration [mol/L] . . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . . Predispensing . . . . . . . . . Volume [mL] . . . . . . . . . Titrant addition . . . . . . . . dV [mL] . . . . . . . . . . . Measure mode . . . . . . . . . . dt [s] . . . . . . . . . . . Recognition Threshold . . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . . Limit A [mV,pH,...] . . . Limit B [mV,pH,...] . . . Tendency . . . . . . . . . . Termination at maximum volume [mL] . . . at potential . . . . . . . . Potential [mV,pH,..] . . . at slope . . . . . . . . . . after number EQPs . . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . . Potential 1 . . . . . . . . . Pot. 1 [mV,pH,...] . . . . Potential 2 . . . . . . . . . Stop for reevaluation . . . . Calculation Formula . . . . . . . . Constant . . . . . . . . Decimal places . . . . . Result unit . . . . . . Result name . . . . . . Statistics . . . . . . . Calculation Formula . . . . . . . . Constant . . . . . . . . Decimal places . . . . . Result unit . . . . . . Result name . . . . . . Statistics . . . . . . . Calculation Formula . . . . . . . . Constant . . . . . . . . Decimal places . . . . . Result unit . . . . . . Result name . . . . . . Statistics . . . . . . . Report Output unit . . . . . . Results . . . . . . . . All results . . . . . . Raw results . . . . . . Table of measured values Sample data . . . . . . E - V curve . . . . . . dE/dV - V curve . . . . d2E/dV2 - V curve . . . log dE/dV - V curve . . E - t curve . . . . . . V - t curve . . . . . . dV/dt - t curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . R1=(QP1-H11)*M/m 2 mg KOH/g BN (buffer A) Yes R2=(Q(EPOT~P1)-H11)*C2 C2=M/m 2 mg KOH/g BN (EQP) Yes
. . . 0 . . . No . . . . . . . . . . . . . Printer No Yes Yes Yes No Yes No No No No No No
. . 60 . . 60 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HCl (i-PrOH) 0.1 DG113 mV to volume 0.2 Incremental 0.1 Time incremental 90.0 200.0 No Yes 154 254 Positive 10.0 Yes 300 No No No Standard Yes 154 No No
84
METTLER TOLEDO
M057
TBN According to ASTM D 2896-85

Method for the determination of TBN According to ASTM D 2896-85, in motor oil. This application does not replace the ASTM standard. Sample
Motor oil, 0.1-20 g

1) The sample is weighed in a titration beaker and placed on the sample changer rack. 2) The solvent 2896 is automatically added by the pump (Function PUMP). General procedure for direct titration : 1. Blank determination of solvent 2896 (method 096B). The blank is stored as auxiliary value H10 (mL) 2. Titer determination of perchloric acid using KHP in solvent 2896. The solvent blank H10 in mL has to be taken into account for the titer determination (method 096C). 3. The solvent blank value H10 (mL) is expressed in mmol using the titer. The result is stored as auxiliary value H11. 4. TBN determination (method 096A) Note: If the direct titration cannot find an equivalence point, a back titration has to be performed: a known amount HClO4 is added to the sample, and the excess is titrated with sodium acetate. General procedure (back titration): 1. Titer determination of sodium acetate with standardized perchloric acid. Blank H11 must be taken into account in the calculation for the titer: R=(QDISP-H11)/(VEQ*c) 2. TBN determination by back titration. Blank H11 must be taken into account for the base number: R=(QDISP-H11-Q)*C/m
Substance Chemicals
Basic components
50 mL Solvent mixture (Acetic acid:chlorobenzene, 1:2)
Titrant
0.1 mol/L HClO4 in glacial acetic acid, Sodium acetate in glacial acetic acid c(CH3COONa)= 0.1 mol/L KHP; HClO4 in glacial acetic acid DL70ES, DL77; Rondo 60 Sample changer
Accessories
100 mL beaker ME-101974, 1 additional burette DV1010, 10 mL syringe ME-71482

DG113-SC at Sensor 1
TBN: Consumption of perchloric acid until the inflection point. It is expressed as the equivalent quantity t of mg KOH/g sample. 1) The blank of the solvent has to be determined regularly, at least after preparing a new stock of solvent mixture. 2) After each titration the electrode is conditioned in water. 3) It is recommended to condition a spare electrode in water. This allows an alternating use of the electrodes or a quick replacement. 4) ASTM D2896 specifies saturated sodium perchlorate in acetic acid as electrolyte. The replacement is straighforward. 5) The sample size is calculated according to the standard will give a titrant consumption of about 5 mL.
Calculation
Base no. determination (096A): R = (Q-H11)*C/m C = M/z , where M = 56.1, z = 1 mg KOH/g
Results
Waste disposal
Halogenated organic waste. Separate the aquoeus pahse (upper) from the organic phase (lower).
6) Using the methods of this application note the titrations will take about 10 to 15 minutes only. 7) KHP is dissolved externally in 50 mL solvent at 50C using an ultra sonic bath. Literature: ASTM 2896-85 (www.astm.org)
Author
Urs Bchi
85
Results
METTLER DL70 Titrator Mettler-Toledo AG Application Laboratory measured Titrator User 11-11-1991 PT 7 ub 10:08
96d ASTM D 2896-85 (direct) 08-11-1991 13:40 SW Version 2.0
RESULTS No 1/1 1/2 1/3 IDentification Oil Oil Oil 85/06 85/06 85/06 Weight 1.9882 2.0625 2.1691 g g g Results 12.78 12.73 12.70 mg KOH/g base number mg KOH/g base number mg KOH/g base number
n x s srel
= = = =
3 12.74 0.039 0.309
mg KOH/g base number mg KOH/g base number %
Note: The same oil was titrated directly and by back titration. The results differ less than 1%.
Titration curve
86
Method
Method 096A Version ASTM D 2896-85 (direct) 08-Nov-1991 13:40 . . . . 096A . . . . ASTM D 2896-85 (direct) . . . . 08-Nov-1991 13:40 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 ST20 Weight m 0.1 20.0 Oil 56.1 1 Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limits[g] . . . . . Upper limits[g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Pump Auxiliary reagent . . . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . . . Titrant addition . . . . dE(set) [mV] . . . . Limits dV . . . . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . Condition . . . . . . . . . Condition . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . Table of measured values . . E - V curve . . . . . . . . Rinse Auxiliary reagent . . . . . Volume [mL] . . . . . . . . Conditioning Interval . . . . . . . . . Time [s] . . . . . . . . . Rinse . . . . . . . . . . . Auxiliary reagent . . . . Volume [mL] . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Conditioning Interval . . . . . . . . . Time [s] . . . . . . . . . Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Volume[mL] . . . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Pump Auxiliary reagent . . . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Titrant addition . . . . dV(min) [mL] . . . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . Record Output unit . . . . . . . . Raw results last sample . . Rinse Auxiliary reagent . . . . . Volume [mL] . . . . . . . . Conditioning Interval . . . . . . . . . Time [s] . . . . . . . . . Rinse . . . . . . . . . . . Auxiliary reagent . . . . Volume [mL] . . . . . . . Statistics Ri (i=index) . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Conditioning Interval . . . . . . . . . Time [s] . . . . . . . . . Method 096C . . . . 096B . . . . Blank ASTM D2896-85 . . . . 07-11-1991 11:26 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 ST20 Fixed volume U 50.0 Blank 0.0 1
. . . . AcOH-C6H5Cl 1:2 . . . . 50.0 . . . . 60 . . . . 30 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HClO4 0.1 DG113-SC mV EQP INC 0.01 EQU 0.5 6.0 6.0 60.0 500.0 0.5 Yes 1 Standard Blank volume R=VEQ mL 4
. . . . AcOH-C6H5Cl 1:2 . . . . 50.0 . . . . 60 . . . . 60 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HClO4 0.1 DG113-SC mV EQP mL 2.0 DYN 30.0 Absolute 0.05 0.1 EQU 0.5 6.0 6.0 60.0 75.0 10.0 Yes 1 Standard base number R=(Q-H11)*C/m C=M/z mg KOH/g 2 Yes Q>0 Printer Yes Yes Yes
. . . . Printer . . . . Yes . . . . AcOH-C6H5Cl 1:2 . . . . 15.0 . . . . . . . . . . . . . . . . . . . . 1 30 Yes AcOH-C6H5Cl 1:2 15.0
. . . . R1 . . . . Blank volume . . . . H10=x . . . . Printer . . . . Yes . . . . 1 . . . . 1
. . . . AcOH-C6H5Cl 1:2 . . . . 15.0 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 180 Yes AcOH-C6H5Cl 1:2 15.0 R1 Yes Yes Yes
Titer of HClOO4 (0.1mol/L) . . . . . . . . . . . . Titer HClO4 . . . . . . . . . . . . R=m/((VEQ-H10)*c*C) . . . . . . . . . . . . mL . . . . . . . . . . . . Blank . . . . . . . . . . . . R2=H10*0.1*x . . . . . . . . . . . . mmoL . . . . . . . . . . . . Blank . . . . . . . . . . . . H11=R2
. . . . Printer . . . . Yes . . . . 1 . . . . 1
Calculation Result name Formula . . Result unit Calculation Result name Formula . . Result unit Auxiliary value ID text . . Formula . .
87
METTLER TOLEDO
M058
TBN According to ASTM D4739-87

Method for the determination of TBN according to ASTM D 4739-87 in motor oil. This application does not replace the ASTM standard. Sample
Various oil, 0.1-20 g

1) The sample is weighed in a titration beaker and placed on the sample changer rack. 2) The solvent 4739 is automatically added by the pump (Function PUMP). General procedure for direct titration : 1. Titer determination of KOH in isopropanol dissolving 70-100 mg KHP in 50 mL water (example: see M002, M027, M534). 2. Titer determination of HCl in isopropanol using 5 mL of the standardized KOH titrant solution (method 058C) 3. Measurement of the buffer potentials A and B (058B) 4. Blank determination for Base Number BN (with HCl, method 058D) and Strong Base Number SBN (with KOH, 058E). 5. Titration of oil samples (method 058A). Note: 1. The sample has to be homogenized well before weighing. Used oils might be heated to 50-60C and may be filtered if sediments are present. 2. The values for buffer potentials from method 058B have to be entered manually into method 058A. 3. The titration function in method 058A is terminated at a prest potential. The end potentila corresponds to the acidic buffer potential +200 mV (manual entry).
Substance Chemicals
Basic components
50 mL Solvent mixture 4739 Isopropanol:H2O:Toluene:Chloroform (100:3:100:100) HCl in isopropanol, c(HCl)=0.1 mol/L KOH in isopropanol, c(KOH)=0.1mol/L
Titrant
1) KHP; 2) Stand. KOH in isopropanol DL70ES, DL77; Rondo 60 Sample changer Balance, printer 100 mL titration beaker ME-101974, 1 additional DV90 drive 1 additional DV1010 burette, 10 mL syringe ME-71482 DG113-SC at Sensor 1
Accessories
Remarks
1) Standard ATM D4739-87 requires the evaluation o the result at or beyond the acidic buffer potential. Therefoer, an evaluation window "EQP range" is activated. "Limit A" of this window is the potential of the acidic buffer , "Limit B" corresponds to this potential + 100 mV. The limits are entered manually. 2) Calculations in method 058A: R1: Calculation of the SBN if there is a titrant consumption up to the basic buffer (condition: VP1>0). R2: Calculation of the BN based on the titrant consumption up to the acidic buffer, if no EQP was found (condition: VEQ=0). R3: BN based on a found EQP (condition: VEQ>0). 3) A conditioning beaker with water is placed after each sample beaker with 60 mL deionized water. Afterwards the electrode, the stirrer and the burette tip are rinsed with 20 mL solvent 4739 before the analysis of the next sample. 4) If no EQP occurs, the evaluation of the BN is made to the acidic buffer potential. The SBN corresponds to the consumption to the basic buffer potential. The buffer potential determination has to be carried out every day or when using another electrode. 5) At the end of the sample series two conditioning beakers are required to keep the electrode in deionized water. Literature: ASTM 4739-87 (www.astm.org) Application brochure 20, ME-51725020 Applications M576, M577, M584, M585, M586, M587, M588.
Calculation
Base no. determination (058A): R1 = (QP+H19)*C1/m ; mg KOH/g C1 = 56.1 R2 = (QP2-H18)*C2/m ; mg KOH/g C2 = 56.1 R3 = (Q-H18)*C3/m ; mg KOH/g C3 = 56.1
Results
Waste disposal
Halogenated organic waste. Separate the aqueous phase (upper) from the organic phase (lower).
Author
Urs Bchi
88
Results
96d ASTM D 4739-87 13-05-1992 13:36 SW Version 2.0 RESULTS No 1/1 1/2 1/3 Identification Oil Oil Oil SAE 15W-40 SAE 15W-40 SAE 15W-40 Weight 1.2275 1.3951 1.2965 R1 g g g Results 5.24 4.91 4.93 mg KOH/g base number mg KOH/g base number mg KOH/g base number measured Titrator User 14-05-1992 GF121 PT2 ub 12:36
STATISTICS Number results
n = 0 n x s srel = = = = 3 5.03 0.185 3.673
STATISTICS Number results R2 Mean value Standard deviation Rel. standard deviation STATISTICS Number results Sample potential (g) 2 1 0.5 4 2 3 3 2 Weight n R3 Base x
mg KOH/g base number mg KOH/g base number %
n = 0 Number s (BN) srel (%) 1.08 3.67 0.61 1.21 Time (min) 31 27 35 25 1. All tested sample did not have a SBN 2. All evaluation at the acidic buffer Glossar: TBN: Total Base Number SBN: Strong Base Number BN: Base Number
(mg KOH/g) 6.53 0.071 5.03 0.185 10.53 0.064 1.76 0.021
Buffer potential A and B: 5 mL of the corresponding buffer stock solution are pipetted in the beakers on the sample changer. 60 mL solvent are added automatically by a pump. The stock solutions can be kept for maximal two weeks. Buffer stock solution A: 100 mL isopropanol in 1 L volumetric flask, add 24.2 g 2,4,6-trimethyl pyridine ( collidine), add 150 mL alcoholic 0.2 mol/L HCl, fill up to 1 L with isopropyl alcohol. Buffer stock solution B: 100 mL isopropanol in 1 L volumetric flask, add 27.8 g m-nitrophenol and dissolve, add 50 mL alcoholic 0.2 mol/L KOH, fill up to 1 L with isopropyl alcohol.
Titration curve
89
Method
Method 058A Version ASTM D 4739-87 13-05-1992 13:36 . . . . 096A . . . . ASTM D 4739-87 . . . . 13-05-1992 13:36 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 ST20 Weight m 0.1 20.0 Oil 56.1 1 Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limits[g] . . . . . Upper limits[g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Pump Auxiliary reagent . . . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . . . Titrant addition . . . . dV [mL] . . . . . . . Measure mode . . . . . . dt [s] . . . . . . . Threshold . . . . . . . EQP range . . . . . . . Limit A [mV, pH,...] . Limit B [mV, pH,...] . Maximum volume [mL] . . . Termination at potential Potential [mV, pH,...] Evaluation procedure . . Steepest jump only . . . Buffer potential 1 . . . Buffer potential 1 . . Buffer potential 2 . . . Buffer potential 2 . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . Condition . . . . . . . . . Condition . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . Condition . . . . . . . . . Condition . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . Condition . . . . . . . . . Condition . . . . . . . Rinse Auxiliary reagent . . . . . Volume [mL] . . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . Table of measured values . . E - V curve . . . . . . . . dE/dV - V curve . . . . . . Conditioning Interval . . . . . . . . . Time [s] . . . . . . . . . Rinse . . . . . . . . . . . Auxiliary reagent . . . . Volume [mL] . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Conditioning Interval . . . . . . . . . Time [s] . . . . . . . . . . . . . Solvent 4739 . . . . 20.0 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Printer Yes Yes Yes Yes 1 300 Yes Solvent 4739 20.0 R1 Yes Yes Yes R2 Yes Yes Yes R3 Yes Yes Yes
. . . . solvent 4739 . . . . 50.0 . . . . 60 . . . . 60 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HCl in i-PrOH 0.1 DG113-SC mV EQP mL 0.2 INC 0.1 TFIX 90.0 50.0 Yes 151.0 251.0 4.0 Yes 351.0 Standard Yes Yes -153.5 Yes 151.0 SBN R=(QP1+H19)*C/m C=56.1 mg KOH/g 2 Yes VP1>0 BN R2=(QP2-H18)*C2/m C2=56.1 mg KOH/g 2 Yes VEQ=0 Base Number R3=(Q-H18)*C3/m C3=56.1 mg KOH/g 2 Yes VEQ>0
. . . . Printer . . . . Yes . . . . 1 . . . . 10
Buffer determination ASTM D 4739-87: Both buffers can be determined automatically with the sample changer. First buffer A is measured, then buffer B. The electrode is conditioned before measuring the next buffer. Buffer A -> R1 = E[1] = 151.001 mV -> stored as aux. value H16 Buffer B -> R2 = E[2] = -153.5489 mV -> stored as aux. value H17 Blank determination for BN Method 058D: Solvent 4739-87 is dispensed automatically by a pump. Titrant: HCl in isopropanol, R = Q , stored as aux. value H18 Blank determination for SBN Method 058E: Solvent 4739-87 is dispensed automatically by a pump. Titrant: KOH in isopropanol, R = Q , stored as aux. value H19
90
METTLER TOLEDO
M059
TAN According to ASTM D 664-89

Method for the determination of TAN According to ASTM D 664-89, in various oils. This application does not replace the ASTM standard. Sample
Various oils 0.1 - 20 g

1) The sample is weighed in a titration beaker and placed onthe sample changer rack. 2) The solvent 664 is automatically added by the pump. (Function PUMP). General procedure: 1. Titer determination of KOH in isopropanol by dissolving 70-100 mg in 50 mL water (example: M002, M027, M534). 2. Titer determination of HCl in isopropanol using 5 mL of standardized KOH titrant soltuion (Method 059C). 3. Measurement of the buffer potential A and B (059B). 4. Blank determination for Acid Number AN (with KOH, method 059D) and Strong Acid Number SAN (with HCl, method 059E). 5. Titration of samples (method 059A). Note: 1. The sample has to be well homogenized before weighing. Used oils may be heated to 50 - 60 C and filtered if sediments are present. 2. The values for buffer potentials from method 059B have to be entered manually into method 059A. 3. The difference between the two potential values must be at 300 mV, otherwise the electrode must be checked.
Substance Chemicals
Acidic components
50 mL Solvent mixture 664, Toluene:water:isopropanol 500:5:495 KOH in iopropanol (i-PrOH) HCl in i-PrOH c(HCl) = 0.1 mol/L
Titrant
1) KHP, 2) standard. KOH in i-PrOH DL70ES/DL77; Rondo 60 sample changer, Balance, printer Glass beaker ME101446, 1 add. burette drive DV90, 1 add. glas burette Dv1010
Accessories

DG113-SC at Sensor 1
1) Standard ASTM 664-89 requires the evaluation of the KOH consumption at acid buffer potential (SAN) or the consumption up to the EQP nearest to buffer B (AN). If no EQP can be found, then the consumption at buffer B (i.e. buffer potential 2) is evaluated (AN). Therefore, an evaluation window "EQP range" is activated. Within this range, the most significant EQP only is evaluated ("steepest jump only yes"). 2) The limits of the EQP range in method 059A are set to 100 mV of the buffer B (manual entry). The window can be modified as required by the user. The limits are entered manually. 3) Calculations in method 059A: R1: Calculation of the SAN if there is a titrant consumption up to the acidic buffer A (Condition: "VP1>0). R2: Calculation of the BN based on the titrant consumption up to basic baffer B , if no EQP was found (Condition: "VEQ=0"). R3: BN based on a found EQP (Condition: "VEQ>0"). 4) A conditioning beaker with 60 mL deion. water is placed after each sample on the sample tray ("conditioning interval = 1"). 5) The electrode, stirrer and burette tip are rinsed with 20 mL solvent 664 before next sample. At the end of a series two conditioning beakers are placed to store the electrode in water. Literature: ASTM D664-89 (www.atm.org) Application brochure 20, ME51725020 Applications M576, M577, M578, M579, M580, M581, M582
Calculation
Method 059A (Sample determination): R1=(QP1+H15)*C/m , C=56.1 SAN (Strong acid number), mg KOH/g R2=(QP2-H14)*C2/m , C2=56.1 AN (Acid number), mg KOH/g R3=(Q-H14)*C/m, C3=56.1 AN (acid number), mg KOH/g
Results
Waste disposal
Separate organic phase from water. Disposal as aromatic organic solvent.
Author
Urs Bchi
91
Results
Sample Motor Oil new Motor Oil I used Motor Oil II used Arabian light Hydraulic Oil I Hydraulic Oil II Hydraulic Oil III Weight [g] ~5 ~1 ~5 15-20 15-20 15-20 15-20 3 3 3 3 3 3 3 n Strong Acid Number (SAN) mg KOH/g sabs RSD[%] no SAN 1.06 no SAN no SAN 0.11 no SAN no SAN 0.002 0.023 2.15 1.97 Acid Number (AN) mg KOH/g sabs RSD[%] 1.33 1) 8.73 1) 2.93 1) 0.09 2) 0.25 1) 0.06 2) 0.12 1) 0.036 0.032 0.054 0.005 0.004 0.005 0.001 2.71 0.36 1.86 5.12 1.56 7.92 0.85 Time [min] 31 27 35 25 15 13 18
Remarks 1) Evaluation at the basic buffer potential; 2) Evaluation at found equivalence point; 3) i-PrOH isopropylalcohol expected AN recommended sample weight [mg KOH/g] [g] 0.05 1.9 20 1.0 4.9 5 5 4.9 1 100 250 0.1 Buffer Stock Solution A (Acid buffer) Add 100 mL of i-PrOH in 1 L volumetric flask, add 24.2 g 2,4,6-trimethyl pyridine( -collidine), add 150 mL alcoholic HCl (c(HCl) = 0.2 mol/L), and fill up with i-PrOH to 1 L. Buffer Stock Solution B (Basic buffer) Add 100 mL of i-PrOH in 1 L volumetric flask, add 27.8 g m-nitrophenol and dissolve, add 50 mL alcoholic KOH (c(KOH) = 0.2 mol/L), and fill up with i-PrOH to 1 L. Both stock solutions keep for maximal 2 weeks.
Titration curve
92
Method
Method 059A Version ASTM D 664-89 07-May-1992 09:32 . . . . . 059A . . . . . ASTM D 664-89 . . . . . 07-May-1992 09:32 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 ST20 Weight m 0.1 20.0 Oil 56.1 1 Title Method ID . . . . . . . . Title . . . . . . . . . . Date/time . . . . . . . . Sample Number samples . . . . . . Titration stand . . . . . Entry type . . . . . . . . Lower limits[g] . . . . Upper limits[g] . . . . ID1 . . . . . . . . . . . Molar mass M . . . . . . . Equivalent number z . . . Pump Auxiliary reagent . . . . Volume [mL] . . . . . . . Stir Speed [%] . . . . . . . . Time [s] . . . . . . . . . Titration Titrant . . . . . . . . . Concentration [mol/L] . . Sensor . . . . . . . . . . Unit of meas. . . . . . . Titration mode . . . . . . Predispensing 1 . . . . Volume [mL] . . . Titrant addition . . . dE(set) [mV] . . . Limits dV . . . . . dV(min) [mL] . . . . dV(max) [mL] . . . . Measure mode . . . . . dE [mV] . . . . . . dt [s] . . . . . . . t (min) [s] . . . t (max) [s] . . . Threshold . . . . . . . EQP range . . . . . . . Limit A [mV,pH..] Limit B [mV,pH..] Maximum volume [mL] . . Termination at slope . Slope [mV,pH../mL] Evaluation prodedure . Steepest jump only . . Buffer potential 1 . . Buffer potential 1 Buffer potential 2 . . Buffer potential 2 Calculation Result name . . . . . . . Formula . . . . . . . . . Constant . . . . . . . . . Result unit . . . . . . . Decimal places . . . . . . Condition . . . . . . . . Condition . . . . . . Calculation Result name . . . . . . . Formula . . . . . . . . . Constant . . . . . . . . . Result unit . . . . . . . Decimal places . . . . . . Condition . . . . . . . . Condition . . . . . . Calculation Result name . . . . . . . Formula . . . . . . . . . Constant . . . . . . . . . Result unit . . . . . . . Decimal places . . . . . . Condition . . . . . . . . Condition . . . . . . Rinse Auxiliary reagent . . . . Volume [mL] . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . E - V curve . . . . . . . . Table of measured samples . dE/dV - V curve . . . . . . Conditioning Interval . . . . . . . . . Time [s] . . . . . . . . . Rinse . . . . . . . . . Auxiliary reagent . . . . Volume [mL] . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Conditioning Interval . . . . . . . . . Time [s] . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Printer Yes Yes Yes Yes 1 300 Yes Solvent 664 20.0 R1 Yes Yes Yes R2 Yes Yes Yes R3 Yes Yes Yes
. . . . . solvent 664 . . . . . 50.0 . . . . . 60 . . . . . 60 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . KOH in i-PrOH 0.1 DG113-SC mV EQP mL 0.2 DYN 30.0 Absolute 0.05 0.2 EQU 0.5 6.0 30.0 90.0 300 yes -44.7 -244.7 10.0 Yes 50.0 Standard Yes Yes 166.4 Yes -144.7 SAN R=(QP1+H15)*C/m C=56.1 mg KOH/g 2 Yes VP1>0 Acid number R2=(QP2+H14)*C2/m C2=56.1 mg KOH/g 2 Yes VEQ=0 Acid number R3=(Q+H14)*C/m C3=56.1 mg KOH/g 2 Yes VEQ]0
. . . . Printer . . . . Yes . . . . 1 . . . . 10
Buffer determination ASTM D 664-89: Both buffers can be determined automatically with the sample changer. First buffer A is measured, then buffer B. The electrode is conditioned before measuring the next buffer. Buffer A -> R1 = E[1] = 166.4147 mV -> stored as aux. value H12 Buffer B -> R2 = E[2] = -144.7011 mV -> stored as aux. value H13
Blank determination for AN Method 059D: Solvent 664-89 is dispensed automatically by a pump. Titrant: KOH in isopropanol, R = Q , stored as aux. value H14 Blank determination for SAN Method 059E: Solvent 664-89 is dispensed automatically by a pump. Titrant: HCl in isopropanol, R = Q , stored as aux. value H15
. . . . . Solvent 664 . . . . . 20.0
93
METTLER TOLEDO
M099
Conductometric Base Number Titration of Motor Oil

Determination of the base number in motor oils by conductometric titration according to IP400/94
Sample
Motor oil, 2-4 g

1) Titrant preparation: The titrant can be prepared manually by adding 9 mL 37% v/v HCl and filling up to 1 L with isopropanol (2-propanol).
Substance Chemicals
Basic components, expressed as KOH
50 mL solvent mixture Toluene:isopropanol:distilled water (50% (v/v):49.5%(v/v):0.5%(v/v) ) HCl in isopropanol: c(HCl) = 0.1 mol/L
2) The titrant is standardized with a solution of potassium hydrogen phtalate of known concentration (see application M100). 3) MCP227 calibration: 3.1 The conductivity meter is calibrated before titration using air (0 S/cm) and 1413 S/cm. 3.2 The linear output range of the MPC227 conductivity meter has to be appropriate to the measuring range during the titration. The range can be set accordingly: a. Press "Read" to stop measuring if necessary. The dor must not flash anymore. b. Press "Mode" for 2 seconds. prog appears on the display. c. Keep pressing "Mode" until P5 is reached. d. Select the lowest millivolt output range /midpoint: 20 S/cm. e. Confirm it by pressing "Mode". e. Return to normal measuring by pressing "Read". f. Check whether you have turned the automatic endpoint off. 4) If the sample contains insoluble material it must be shaken thoroughly in the original container before it is taken.
Titrant
Potassium hydrogen phthalate DL50Graphix, DL53/55/58 DL70ES, DL77 MPC227 conductivity meter 100 mL titration beaker ME-101974 Connection cable 51302258 1 additional burette drive DV90, 1 additional DV1010, Printer, balance InLab717 conductivity probe
Accessories
Remarks
1) This application is based on the IP400/94 standard published by the Institute of Petroleum, London. The following modifications to the standard IP method were made: 1.1 INC = 0.1 mL at TFIX = 5 s instead of 10 s. The analysis is speeded up. 1.2 Solvent mixture instead of nitric acid is used to rinse the conductivity probe. 2) Most oil samples create sticky residues. The conductivity probe is cleaned with a paper tissue soaked in solvent mixture. Afterwards, the probe is rinsed again with solvent mixture to remove the last impurities. Therefore, an automatic procedure using a sample changer is not recommended. 3) If you want to monitor the conductivity values at the titrator, the appropriate slope and unit have to be installed in the sensor setup of the titrator. For instance, for the selected MPC227 range with a midpoint of 20 S/cm the slope is 9.00 S/cm, and the unit is S/cm (Check MPC227 op. instructions p. 17). Literature: IP 400/94, "Determination of Base Number of Petroleum Products - Conductimetric titration method" The Institute of Petroleum, London, 1994
Calculation
Base number determination (BN 1): R1 = Q*C/m ; mg KOH/g C1 = M/z M = 56.1, z =1
Results
Waste disposal
Author
K. Saegesser
94
Results
METTLER TOLEDO DL77 Method User Measured RESULTS No 1/1 1/2 1/3 1/4 1/5 1/6 ID1 Oil Oil Oil Oil Oil Oil ID2 Sample amount and results 1.009 R1 = 10.338 0.961 R1 = 0.000 0.974 R1 = 10.639 1.023 R1 = 10.569 1.0 R1 = 10.368 0.974 R1 = 10.581 g mg g mg g mg g mg g mg g mg Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g m base m base m base m base m base m base number number number number number number Titrator 23 V3.1 Mettler-Toledo GmbH Market Support Laboratory 23-Apr-1998 9:50
BN 1 BN conductometric K Sgesser 23-Apr-1998 10:23
STATISTICS Number results Mean value Standard deviation Rel. standard deviation Outlier test: sample No.
n x s srel
= = = =
6 8.7492 4.2879 49.01 1/2
mg KOH/g mg KOH/g
base number base number
Statistics without sample No. 1/2 Number results n = 5 Mean value x = 10.499 Standard deviation s = 0.136165 Rel. standard deviation srel = 1.297
mg KOH/g mg KOH/g
Titration curve
95
Method
Method BN 1 Version BN conductometric 23-Apr-1998 9:50 . . . . BN 1 . . . . BN conductometric . . . . 23-Apr-1998 9:50 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Stand 1 Weight m 0.5 2.0 Oil 56.1 1 Manual Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperature sensor . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [m%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing . . . . . . Volume [mL] . . . . . Titrant addition . . . . dV [mL] . . . . . . . Measure mode . . . . . . dt [s] . . . . . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Table of values . . . . . . E - V curve . . . . . . . . dE/dV - V curve . . . . . . d2E/dV2 - V curve . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . Sample data . . . . . . . . All results . . . . . . . .
. . . . BN solvent . . . . 1.0 . . . . 50 . . . . 45 . . . . 120 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HCl (2-prop) 0.1 Cond mV EQP mL 0.6 INC 0.1 TFIX 5.0 50.0 10.0 Yes 1 Segmented base number R=Q*C/m C=M/z mg KOH/g 3 Printer Yes Yes Yes Yes Yes R1 Yes Yes Yes
. . . . Printer . . . . Yes . . . . Yes
96
METTLER TOLEDO
M100
Standardization of HCl in Isopropanol by Conductometric Titration

Standardization of alcoholic HCl by conductometric titration.
Sample
5 mL 0.1 mol/L potassium hydrogen phtalate solution (KHP)

1) Titrant preparation: The titrant can be prepared manually by adding 9 mL 37% v/v HCl and filling up to 1 L with isopropanol (2-propanol). 2) 0.1 mol/L KHP solution: Dissolve KHP in 200 mL water by means of an ultrasonic bath and fill up to 1 L with isopropanol. 3) MCP227 calibration: 3.1 The conductivity meter is calibrated before titration using air (0 S/cm) and 1413 S/cm. 3.2 The linear output range of the MPC227 conductivity meter has to be appropriate to the measuring range during the titration. The range can be set accordingly: a. Press "Read" to stop measuring if necessary. The dor must not flash anymore. b. Press "Mode" for 2 seconds. prog appears on the display. c. Keep pressing "Mode" until P5 is reached. d. Select the lowest millivolt output range /midpoint: 20 S/cm. e. Confirm it by pressing "Mode". e. Return to normal measuring by pressing "Read". f. Check whether you have turned the automatic endpoint off.
Substance Chemicals
KHP
45 mL solvent mixture Toluene:isopropanol:distilled water (50% (v/v):49.5%(v/v):0.5%(v/v) ) HCl in isopropanol: c(HCl) = 0.1 mol/L
Titrant
DL50Graphix, DL53/55/58 DL70ES, DL77 MPC227 conductivity meter 100 mL titration beaker ME-101974 Connection cable 51302258 1 additional burette drive DV90, 1 additional DV1010, Printer, balance InLab717 conductivity probe
Accessories
Remarks
1) If you want to monitor the conductivity values at the titrator, the appropriate slope and unit have to be installed in the sensor setup of the titrator. For instance, for the selected MPC227 range with a midpoint of 20 S/cm the slope is 9.00 S/cm, and the unit is S/cm (Check MPC227 op. instructions p. 17). 2) MPC227 Linear ranges: Range 1: 2-200 S/cm Midpoint: 20 S/cm; Slope: 9.00 mV/(S/cm); Unit: S/cm
Calculation
Titer determination (BN 2): R1 = U/(VEQ*c*C) C1 = 1/(0.1*z)
Range 2: 20-2000 S/cm Midpoint: 200 S/cm Slope: 0.90 mV/(S/cm), Unit: S/cm Range 3: 0.2-20 mS/cm Midpoint: 2.0 mS/cm; Slope: 90.00 mV/(S/cm); Unit: mS/cm
Results
Range 4: 2-200 mS/cm Midpoint: 20 mS/cm Slope: 9.00 mV/(S/cm), Unit: mS/cm
Waste disposal
Range 5: 20-2000 mS/cm Midpoint: 200 mS/cm Slope: 0.90 mV/(S/cm), Unit: mS/cm
Author
K. Saegesser
97
Results
METTLER TOLEDO DL77 Method User Measured RESULTS No 1/1 1/2 1/3 1/4 1/5 1/6 ID1 Oil Oil Oil Oil Oil Oil ID2 Sample amount and results 1.009 R1 = 10.338 0.961 R1 = 0.000 0.974 R1 = 10.639 1.023 R1 = 10.569 1.0 R1 = 10.368 0.974 R1 = 10.581 g mg g mg g mg g mg g mg g mg Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g Weight KOH/g m base m base m base m base m base m base number number number number number number Titrator 23 V3.1 Mettler-Toledo GmbH Market Support Laboratory 23-Apr-1998 9:50
BN 1 BN conductometric K Sgesser 23-Apr-1998 10:23
STATISTICS Number results Mean value Standard deviation Rel. standard deviation Outlier test: sample No. Number results Mean value Standard deviation Rel. standard deviation
= = = = = = = =
6 8.7492 4.2879 49.01 1/2 5 10.499 0.136165 1.297
mg KOH/g mg KOH/g
mg KOH/g mg KOH/g
Titration curve
98
Method
Method BN 1 Version BN conductometric 23-Apr-1998 9:50 . . . . BN 1 . . . . BN conductometric . . . . 23-Apr-1998 9:50 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 Stand 1 Weight m 0.5 2.0 Oil 56.1 1 Manual Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperature sensor . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [m%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing . . . . . . Volume [mL] . . . . . Titrant addition . . . . dV [mL] . . . . . . . Measure mode . . . . . . dt [s] . . . . . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Table of values . . . . . . E - V curve . . . . . . . . dE/dV - V curve . . . . . . d2E/dV2 - V curve . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . Sample data . . . . . . . . All results . . . . . . . .
. . . . BN solvent . . . . 1.0 . . . . 50 . . . . 45 . . . . 120 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HCl (2-prop) 0.1 Cond mV EQP mL 0.6 INC 0.1 TFIX 5.0 50.0 10.0 Yes 1 Segmented base number R=Q*C/m C=M/z mg KOH/g 3 Printer Yes Yes Yes Yes Yes R1 Yes Yes Yes
. . . . Printer . . . . Yes . . . . Yes
99
METTLER TOLEDO
M061
pH, Acidity, Lactone and Formol Value of Honey

Method for the determination of the pH, acidity, lactone and formol value of honey.
Sample
Honey, approx. 10 g

1) The sample is weighed in the titration beaker and mounted at the titration head.
Substance Chemicals
Organic acids, lactone, free amino acids 40 mL deionized water
2) Deionized water is automatically added by the peristaltic pump. 3) First the pH value and the acidity content are determined. 4) Then the lactone value is determined by means of two titration. 5) Finally, the formol value is determined after addition of formol solution which is neutralized to pH 8.
Titrant
0.1mol/L HCl; 0.1 mol/L NaOH; 36.5% Formol to pH 8.0 with NaOH
1) THAM (NaOH), 2) KHP (HCl) DL70ES/DL77, balance
Note: A blank value determination is performed before sample analysis. This is used in calculation R3 (Lactone content). The blank value is stored as auxiliary value H11.
Accessories
Beakers ME-101974; 2 additional burette drives DV90; 2 burettes DV1010; 1 Pump ME-51108016 with adapter ME-51108350 DG111-SC at Sensor 1
Remarks
Honey is one of the richest natural products and the oldest sweetener. It contains sugars, water, amino acids, minerals, vitamins, ferments, hormones, inhibitors, other compounds. 1) pH and acidity: Pure blossom honey has generally a pH value of 3.3 - 4.6. The acid content is usually between 7.4 and 30 mmol/kg. If it exceeds 30 mmol/kg , then honey has undergone deterioration by fermentation/acidification. Organic acids such as tartaric, succinic, citric and oxalic are present in honey. Clover honey may further contain butyric, acetic, formic and lactic acid. 2) Formol value: The formol value is a measure of the free amino acids. Its usual level is between 4.5 and 15.5 mmol/kg. A low formol value indicates adulteration with artificial honey or additional feeding of the bees with sugar. The formol value is determined by adding a formol solution which must be neutralized prior determination. 3) Lactone value: The lactone content varies between 2-20 mmol/kg. Literature: Schweizerisches Lebensmittelbuch, Band II, Chap. 23 AOAC Official Methods of Analysis, 1984, pages 595-596
Free amino acids (formol no.): R-COOH-NH2 + HCHO = H2O + R-COOH-N=CH2 R-COOH-N=CH2 + OH- = R-COO--N=CH2 + H2O
Calculation
pH (R1) & Acidity (R2): R1=E ; R2=Q[1]*C2/m, C2=1000; Lactone content: R3=(Q[2]+Q[3]-H11)*C3, C3=1000/m Formol value: R4=Q[5]*C4/m, C4=1000
Results
Waste disposal
Aqueous solutions
Author
Ruth von Rotz
100
Results
RESULTS 1/1 Ex.honey 10.3302 g 3.819 21.869 15.010 8.539 3.782 21.539 14.713 8.947 3.768 21.689 14.879 8.982 3.766 21.536 14.981 9.095 3.764 21.577 14.683 9.079 = = = = = = = = = = = = 5 21.642 0.1413 0.653 5 14.853 0.1504 1.013 5 21.642 0.1413 0.653 1/1 1/1 4 9.026 0.0723 0.801 mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg mmol/kg pH Acidity Lactone cont. Formol value pH Acidity Lactone cont. Formol value pH Acidity Lactone cont. Formol value pH Acidity Lactone cont. Formol value pH Acidity Lactone cont. Formol value
1/2
Ex.honey
10.287
1/3
Ex.honey
10.3434
1/4
Ex.honey
10.3955
1/5
Ex.honey
10.3756
STATISTICS Number results R2 Mean value Standard deviation Rel. standard deviation Outlier test: no outliers! STATISTICS Number results R3 Mean value Standard deviation Rel. standard deviation Outlier test: no outliers! STATISTICS Number results R4 Mean value Standard deviation Rel. standard deviation Outlier test: Sample No. Statistics without sample No Number results R4 Mean value Standard deviation Rel. standard deviation Outlier test: no outliers! Sample Mountain honey French honey Swiss honey 1 Swiss honey 2 pH Result 3.78 4.01 4.37 3.98
n x s srel n x s srel n x s srel
mmol/kg mmol/kg %
Acidity Acidity
mmol/kg mmol/kg %
Lactone cont. Lactone cont.
mmol/kg mmol/kg %
Formol value Formol value
n x s srel
= = = =
mmol/kg mmol/kg %
Formol value Formol value
RSD (%) 0.61 0.33 0.33 0.69
Acidity Lactone Result RSD Result RSD (mmol/kg) (%) (mmol/kg) (%) 21.64 0.65 14.85 17.11 0.70 10.16 11.59 0.75 6.39 8.51 0.81 3.95
Formol value Result RSD mmol/kg) (%) 1.01 8.93 2.54 1.65 4.27 1.95 2.57 2.36 3.56 4.85 2.77 0.30
Titration curve
101
Method
Method R1 Version pH,ac.,lact.,form. No Honey 11-July-1991 1:23 pm Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Titrant addition . . . . Control band[mV,pH..] Delay [s] . . . . . . End point mode . . . . . Potential [mV,pH..] Tendency . . . . . . . . Maximum volume [mL] . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . Results last sample . . . . Table of measured values . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Method R1a Version . . . . Formol 36.5% . . . . 36.5 . . . . 15.0 . . . . 50 . . . . 60 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . NaOH 0.1 DG111-SC As installed EP Continuous 3.0 10 EPA 8.0 Positive 10.0
Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Pump Auxiliary reagent . . . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Measure Sensor . . . . . . . . . . . Unit of meas. . . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t(min) mode . . . . . t (min) [s] . . . . t (max) [s] . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . Titrant addition . . . . dV (set)[mV] . . . dV(min) [mL] . . . dV(max) [mL] . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t (min) [s] . . . . t (max) [s] . . . . End point mode . . . . . Potential [mV,pH..] Tendency . . . . . . . . Maximum volume [mL] . . . Record Output unit . . . . . . . . Table of measured values . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . Titrant addition . . . . dV (set)[mV] . . . dV(min) [mL] . . . dV(max) [mL] . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t (min) [s] . . . . t (max) [s] . . . . End point mode . . . . . Potential [mV,pH..] Tendency . . . . . . . . Maximum volume [mL] . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Titrant addition . . . . Control band[mV,pH..] Delay [s] . . . . . . End point mode . . . . . Potential [mV,pH..] Tendency . . . . . . . . Maximum volume [mL] . . . Record Output unit . . . . . . . . Table of measured values . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Titrant addition . . . . Control band[mV,pH..] Delay [s] . . . . . . End point mode . . . . . Potential [mV,pH..] Tendency . . . . . . . . Maximum volume [mL] . . .
. . . . R1 . . . . pH,ac.,lact.,form. No Honey . . . . 11-July-1991 1:23 pm . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Stand 1 Weight m 9.0 11.0 CH honey 0.0 1
. . . . H2O . . . . 40.0 . . . . 90 . . . . 150 . . . . 50 . . . . 30 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . DG111-SC As installed 0.5 1.5 Fix 10.0 30.0 NaOH 0.1 DG111-SC As installed EP mL 0.7 Dynamic 8.0 0.02 0.1 0.5 0.5 2.0 20.0 EPA 7.0 Positive 10.0
. pH . R=E . . . 3 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Acidity R2=Q[1]*C2/m C2=1000 mmol/kg 3 Lactone cont. R3=(Q[2]+Q[3]-H11)*C3 C3=1000/m mmol/kg 3 Formol value R4=Q[5]*C4/m C4=1000 mmol/kg 3 Printer Yes Yes Yes R2 Yes Yes Yes R3 Yes Yes Yes R4 Yes Yes Yes
. . . . Printer . . . . Yes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . NaOH 0.1 DG111-SC As installed EP mL 3.0 Dynamic 8.0 0.02 0.3 0.5 0.5 2.0 20.0 EPA 9.8 Positive 10.0
. . . . Printer . . . . Yes
Blank for Honey 11-07-1991 11:25 am . . . . R1a . . . . Blank for Honey . . . . 11-07-1991 11:25 am . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Stand 1 Fixed volume U 5.0 Blank 0.0 1
. . . . 50 . . . . 60 . . . . HC1 . . . . 0.1 . . . . 5.0 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . NaOH 0.1 DG111-SC As installed EP Continuous 3.0 10 EPA 7.0 Positive 10.0
. . . . Printer . . . . Yes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . NaOH 0.1 DG111-SC As installed EP Continuous 2.0 10 EPA 8.0 Positive 10.0
Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Volume [mL] . . . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . Titrant addition . . . . dV (set)[mV] . . . dV(min) [mL] . . . dV(max) [mL] . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t (min) [s] . . . . t (max) [s] . . . . End point mode . . . . . Potential [mV,pH..] Tendency . . . . . . . . Maximum volume [mL] . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Table of measured values . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Auxiliary value ID t t
. . . . 50 . . . . 30 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . NaOH 0.1 DG111-SC As installed EP mL 3.0 Dynamic 8.0 0.02 0.2 0.5 0.5 2.0 20.0 EPA 7.0 Positive 10.0
. . R=Q[1] . . mmol . 3
. . . . Printer . . . . Yes . . . . . . . . . . . . . . . . R1 Yes Yes Yes Bl k l t
102
METTLER TOLEDO
M240
Formol Number, Acidity and True Brix Value of Orange Juice

Method for the determination of the formol number, acidity and true Brix value of orange juice according to NEN 2843 and NEN 2861 (Dutch standards). Sample
Concentarted orange juice, 1-4 g

1) The DG111 electrode must be calibrated with pH buffers. 2) The sample is weighed in the titration beaker and mounted at the titration head. If drinkable orange juice is used, then weigh in approximately 20 g. The sample is diluted using the second pump of the sample changer (DOSE). 3) First the acidity content is determined by performing an EP titration to pH 8.2 with NaOH. This is given as citric acid content. 4) Formol is dispensed by the second burette. After 1 minute reaction time, an EP titration to pH 8.2 with NaOH is started. 5) The formol number is defined in calculation R4 as mmol NaOH/10g sample, normalized to 65 True Brix: FN = (mmol NaOH*10*10*65)/(m*True Brix). 6) A blank is run and stored as auxiliary value H2.
Substance Chemicals
Organic acids, free amino acids
50 mL deionized water
Titrant
NaOH, c(NaOH) = 0.5 mol/L Formol , c(Formol) = 36.5% Adjusted to pH 8.2 with NaOH THAM (NaOH) DL70ES/DL77 Rondo 60 sample changer Balance, printer Beakers ME-101974; 1 additional burette drive DV90; 1 burette DV1010; 1 additional diaphragma pump (DOSE) DG111-SC at Sensor 1
Accessories
Note: 1. The molar mass M is set to 1.0 and is not used. 2. Prior titration the Brix value of the sample is measured with a refractometer. The value is stored as auxiliary value H1and usd in calculation R3 (correction for true brix).
Remarks
1) Formol value: The formol value is a measure of the free amino acids and allows an estimation of of the protein content. Amino acids can not be titrated directly with a base since the dissociation constant of the -COOH group is too weak. By adding formaldehyde, the amino group -NH2 of the amino acids reacts forming to -N=CH2 . As a consequence, the dissociation strength of the hydrogen atom present in the carboxylic group -COOH of the amino acid i increased. The amino acid can be directly titrated with sodium hydroxide. 2) The formol value is generally given as the titrant consumption of 0.1 mol/L NaOH needed for 10 g or sample. 3) True Brix: correction of the measured refrative index for the citric acid concentration (given in R1): Corrected value = (-0.00035)*R12 + 0.191*R1 + 0.024 (According to Stevens and Baier, 1959) Literature: NEN 2843, NEN 2861 J. Stevens, W.Baier, Die Fruchtsaftindustrie, 4 (1959), p. 28. (See also: C.W. Lindsay, J. of AOAC International, Vol. 76, NO.2, 1993, page 424). AOAC Official Methods of Analysis, 1984.
Free amino acids (formol no.): R-COOH-NH2 + HCHO = H2O + R-COOH-N=CH2 R-COOH-N=CH2 + OH- = R-COO--N=CH2 + H2O
Calculation
Results
Citric acid (R1): R1 = Q[1]*C1/m, C1= 192/(10*3); True Brix correction (R2): R2 = R1*R1*(-0.000035)+C2, C2 = (R1*0.191)+0.024 True Brix (R3): R3 = H1+R2 Formol No. R4 = 6500*C4/(m*R3), C4=Q[2]-H2+QEX[1] Aqueous solution
Waste disposal
Author
Ko Schaap, MT-NL
103
Results
METTLER DL70 Titrator Quest Naarden Analytical Laboratory measured Titrator User 30-Oct-1991 jan 11:13
4 F.N./Acid./True Brix 11-Oct-1991 9:00 SW Version 2.0 RESULTS No 1/1 Identification 11570 03500 Weight 1.5503 g
Results 31.3 5.66 57.76 18.35 31.4 5.67 57.77 18.35 % Citric acid True Bx corr. True brix mmol NaOH/10g(65wBx) Citric acid True Bx corr. True brix mmol NaOH/10g(65wBx)
1/2
11570
03500
1.5503
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation STATISTICS Number results R2 Mean value Standard deviation Rel. standard deviation STATISTICS Number results R3 Mean value Standard deviation Rel. standard deviation STATISTICS Number results R4 Mean value Standard deviation Rel. standard deviation Outlier test: no outliers!
n x s srel n x s srel n x s srel n x s srel
= = = = = = = = = = = = = = = =
2 31.3 0.04 0.138
% % %
Citric acid Citric acid
2 5.67 0.1504 1.013 % 2 57.77 0.007 0.013 2 18.66 0.443 2.374
True Bx. corr. True Bx. corr.
True brix True brix
mmol NaOH/10g(65wBx) mmol NaOH/10g(65wBx)
Titration curve
104
Method
Method 4 Version F.N./Acid./True Brix 11-Oct-1991 9:00 Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Record Output unit . . . . . . . . All results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . True brix . R3=H1+R2 . . . 2 . . . . . mmol NaOH/10g(65wBx) R4=6500*C4/(m*R3) C4=Q[2]-H2+QEX[1] 2
Title Method ID . . . . . . . . . . Title . . . . . . . . . . . . Date/time . . . . . . . . . . Conditioning Interval . . . . . . . . . . . Time [s] . . . . . . . . . . . Sample Number samples . . . . . . . . Titration stand . . . . . . . Entry type . . . . . . . . . . Lower limit [g] . . . . . . Upper limit [g] . . . . . . ID1 . . . . . . . . . . . . . Molar mass M . . . . . . . . . Equivalent number z . . . . . Stir Speed [%] . . . . . . . . . . Time [s] . . . . . . . . . . . Auxiliary instrument Name . . . . . . . . . . . . . Time [s] . . . . . . . . . . . Titration Titrant . . . . . . . . . . . Concentration [mol/L] . . . . Sensor . . . . . . . . . . . . Unit of meas. . . . . . . . . Titration mode . . . . . . . . Titrant addition . . . . . dE(set)[mV] . . . . . . dV(min) [mL] . . . . . . dV(max) [mL] . . . . . . dE [mV] . . . . . . . . dt [s] . . . . . . . . . t(min) [s] . . . . . . . t(max) [s] . . . . . . . End point mode . . . . . . Potential [mV,pH..] . Tendency . . . . . . . . . Maximum volume [mL] . . . . Dispense Titrant . . . . . . . . . . . Concentration [mol/L] . . . . Volume . . . . . . . . . . . Stir Speed [%] . . . . . . . . . . Time [s] . . . . . . . . . . . Titration Titrant . . . . . . . . . . . Concentration [mol/L] . . . . Sensor . . . . . . . . . . . . Unit of meas. . . . . . . . . Titration mode . . . . . . . . Titrant addition . . . . . Control band [mV,pH,...] Delay [s] . . . . . . . End point mode . . . . . . Potential [mV,pH..] . Tendency . . . . . . . . . Maximum volume [mL] . . . . Rinse Auxiliary reagent . . . . . . Volume [mL] . . . . . . . . . Conditioning Interval . . . . . . . . . . . Time [s] . . . . . . . . . . . Calculation Result name . . . . . . . . . Formula . . . . . . . . . . . Constant . . . . . . . . . . . Result unit . . . . . . . . . Decimal places . . . . . . . . Calculation Result name . . . . . . . . . Formula . . . . . . . . . . . Constant . . . . . . . . . . . Result unit . . . . . . . . . Decimal places . . . . . . . .
. . . R1 . . . F.N./Acid./True Brix . . . 11-Oct-1991 9:00 . . . 1 . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . 2 ST20 Weight m 1.0 4.0 1.0 1
. . . . R1 . . . . Yes . . . . Yes . . . . R2 . . . . Yes . . . . Yes . . . . R3 . . . . Yes . . . . Yes . . . . R4 . . . . Yes . . . . Yes . . . . Printer . . . . Yes
. . . 70 . . . 15 . . . DOSE . . . 5.0 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . NaOH 0.5 DG111-SC As installed EP Dynamic 4.0 0.005 0.5 0.5 0.5 2.0 20.0 EPA 8.2 Positive 30.0
. . . Formol . . . 36.5% . . . 10 mL . . . 70 . . . 60 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . NaOH 0.5 DG111-SC As installed EP Continuous 3.0 10 EPA 8.2 Positive 20.0
. . . H2O . . . 10.0 . . . 1 . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Citric acid R1=Q[1]*C1/m C1=192/(m*3) % 1 True Bx corr. R2=R1*R1*(-0.00035)+C2 C2=(R1*0.191)+0.024 2
105
METTLER TOLEDO
M241 / 1
Carbon Black Surface Area (ASTM D3765-99): Standardization

Titration of unadsorbed CTAB (cetyltrimethylammonium bromide) on the ITRB standards for the carbon black surface area determination according to ASTM D3765-99 (see also 241 / 2, and 241 / 3). Sample
5 Standard samples with ITRB 5 samples (0.2-0.6 g, with 0.1 g diff.) ITRB (Industry Tint Reference Black) ITRB, accessible surface area: 83.0 x103 m2/kg 45 mL deionized water 5 mL 0.15% Triton X-100 10 mL 0.01 mol/L CTAB (Cetyltrimethylammonium bromide) Dioctyl sodium sulfosuccinate (Aerosol OT) c(Aerosol OT) = 0.1 mol/L --DL70ES, DL77 Rondo 60 sample changer AT261 Balance, printer 2 additional burette drive DV90, 2 additional burette DV1010 100 mL titration beaker ME-101974 DT120 Temperature sensor DP550 with adapter cable ME-89600

The sample must be prepared according to ASTM D3765-99. After filtration, the standard samples are ready for titration: 1) Add 45 mL deionized water 2) Mount the beaker on the titration stand, start method ALG1. 3) 5 mL 0.15% Triton X-100 solution are added by a burette, 4) 10 mL 0.01 CTAB solution are added by a second burette. CTAB Standard solution (0.01 mol/L): Dissolve 3.64 g of reagent-grade CTAB (Cetyltrimethylammonim bromide, available from e.g. J.T. Baker, Cat. No. 7N121) in 900 mL distilled or deionized water. Add 100 mL of the pH 7.0 0.05 mol/L buffer solution. Warm the solution to a temperature of 27-37C to facilitate the dissolution. Cool to a temperature between 22 and 25C before using. Aerosol OT (Dioctyl sodium sulfosuccinate): Dissolve 1g/L of Aerosol OT solution in distilled or deionized water containing 2.5 mL/L of 37% formaldehyde, by swirling vogourously with a magnetic stirrer for 48 h. Allow to stand an additional twelve days before standardization and use. The solution should be capped tightly and stored in a cool place (once opened, the solution should be store in a dessiccator).
Substance Chemicals
Titrant
Accessories
Remarks
This method covers the measurement of the specific surface area of carbon black exclusive of area contained in micropores too small to admit CTAB molecules. This test method is suitable for characterizing rubber-grade carbon blacks of all types. The CTAB adsorption by carbon black is independent of residual tars and functional groups containing hydrogen and oxygen, etc. Rapid equilibration is achieved by mechanical stirring and ultrasonic vibration. The CTAB molecule is relatively large; so it is not adsorped in micropores or on surface roughness. Thus, the CTAB surface area reflects only the surface f the carbon black that is available for interaction with rubber molecules. Titration with Aerosol OT solution to a turbidity maximum endpoint is used to determine the unadsorped CTAB after removal of the colloidally dispersed carbon black by ultrafiltration.
Calculation
See method below
Results
Waste disposal
Aqueous waste
All results are scaled by using the Industry Tint reference Black (ITRB) as a primary standard and taking its accessible surface area to be exactly 83.0 x 103 m2/kg. Literature: ASTM D3765 (www.astm.org)
Author
K. Mooibroek/C. Gordon/Ch. Walter
106
Results
Titration curve
107
Method
Method ALG1 Version ASTM3765: Standards 22-Feb-2002 10:30 . . . . ALG1 . . . . ASTM3765: Standards . . . . 22-Feb-2002 10:30 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 ST20 1 Weight m 0.2 0.6 ITRB 0.0 1 TEMP A Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperatur sensor . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Titrant addition . . . . dV[mL] . . . . . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure. . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Condition . . . . . . . . . Condition . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Condition . . . . . . . . . Condition . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Condition . . . . . . . . . Condition . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Condition . . . . . . . . . Condition . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Condition . . . . . . . . . Condition . . . . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Record Output unit . . . . . . . . All results . . . . . . . . . . . . H17 4. standard . . . . H17=m . . . . . . . . . . . . . . . . ITBR(4) H4=R1 Yes f=4
. . . . H16 5. standard . . . . H16=m . . . . . . . . . . . . . . . . ITBR(5) H5=R1 Yes f=5
. . . . Triton X-100 . . . . 0.15 . . . . 5.0 . . . . CTAB . . . . 0.01 . . . . 10.0 . . . . 50 . . . . 30 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Aerosol OT 0.1 DP550 mV EQP INC 0.1 EQU 1.0 2.0 3.0 30.0 500 10.0 Yes 1 Minimum Volume/gram R1=VEQ/m cm3/g 4
. . . . R1 . . . . Yes . . . . Yes . . . . Printer . . . . Yes
108
METTLER TOLEDO
M241 / 2
Carbon Black Surface Area (ASTM D3765-99): Linear regression

Linear regression for calibration line of Carbon Black Area Determination according to ASTM D3765-99. Five ITRB standards have been determined in Application 241/1, while sample titration is described in 241/3 . Sample
CTAB Standard solution (0.01 mol/L): Dissolve 3.64 g of reagent-grade CTAB (Cetyltrimethylammonim bromide, available from e.g. J.T. Baker, Cat. No. 7N121) in 900 mL distilled or deionized water. Add 100 mL of the pH 7.0 0.05 mol/L buffer solution. Warm the solution to a temperature of 27-37C to facilitate the dissolution. Cool to a temperature between 22 and 25C before using. Aerosol OT (Dioctyl sodium sulfosuccinate): Dissolve 1g/L of Aerosol OT solution in distilled or deionized water containing 2.5 mL/L of 37% formaldehyde, by swirling vogourously with a magnetic stirrer for 48 h. Allow to stand an additional twelve days before standardization and use. The solution should be capped tightly and stored in a cool place (once opened, the solution should be store in a dessiccator).

For the calculation of the calibration line starts method ALG2.
Substance Chemicals
Titrant
Accessories
Remarks
This method covers the measurement of the specific surface area of carbon black exclusive of area contained in micropores too small to admit CTAB molecules. This test method is suitable for characterizing rubber-grade carbon blacks of all types. The CTAB adsorption by carbonn black is independent of residual tars and functional groups containing hydrogen and oxygen, etc. Rapid equilibration is achieved by mechanical stirring and ultrasonic vibration. The CTAB molecule is relatively large; so it is not adsorped in micropores or on surface roughness. Thus, the CTAB surface area reflects only the surface f the carbon black that is available for interaction with rubber molecules. Titration with Aerosol OT soltuion to a turbidity maximum endpoint is used to determine the unadsorped CTAB after removal of the colloidally dispersed carbon black by ultrafiltration.
Calculation
Calculation of linear regression: see below
Results
Waste disposal
Aqueous waste
Author
109
Results
Titration curve
110
Method
Method ALG2 Version ASTM3765: Lin. regr. 22-Feb-2002 11:30 . . . . . . . . ALG2 . . . . . . . . ASTM3765: Lin. regr. . . . . . . . . 22-Feb-2002 11:30 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 Stand 1 Fixed volume U 1.0 ITRB 0.0 1 TEMP A Title Method ID . . . . . Title . . . . . . . Date/time . . . . . Sample Number samples . . . Titration stand . . Entry type . . . . . Volume [mol/L] . ID1 . . . . . . . . Molar mass M . . . . Equivalent number z Temperatur sensor . Auxiliary value ID text . . . . . . Formula . . . . . . Auxiliary value ID text . . . . . . Formula . . . . . . Auxiliary value ID text . . . . . . Formula . . . . . . Auxiliary value ID text . . . . . . Formula . . . . . . Auxiliary value ID text . . . . . . Formula . . . . . . Auxiliary value ID text . . . . . . Formula . . . . . . Auxiliary value ID text . . . . . . Formula . . . . . . Auxiliary value ID text . . . . . . Formula . . . . . . Auxiliary value ID text . . . . . . Formula . . . . . . Auxiliary value ID text . . . . . . Formula . . . . . . Calculation Result name . . . . Formula . . . . . . Constant . . . . . . Result unit . . . . Decimal places . . . Calculation Result name . . . . Formula . . . . . . Constant . . . . . . Result unit . . . . Decimal places . . . Calculation Result name . . . . Formula . . . . . . Constant . . . . . . Result unit . . . . Decimal places . . . Calculation Result name . Formula . . . Constant . . . Result unit . Decimal places Calculation Result name . Formula . . . Constant . . . Result unit . Decimal places Calculation Result name . Formula . . . Constant . . . Result unit . Decimal places Calculation Result name . Formula . . . Constant . . . Result unit . Decimal places Calculation Result name . Formula . . . Constant . . . Result unit . Decimal places Calculation Result name . Formula . . . Constant . . . Result unit . Decimal places Calculation Result name . Formula . . . Constant . . . Result unit . Decimal places Record Output unit . All results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Bottom line calc. (1) . R4=-sq(H7) . . . 4 . Bottom line calc. (2) . R5=4*H15 . . . 4 . Bottom line calc. (3) . R6=R4+R5 . . . 4 . . . . . . . . . . . . . . . . . . . . Slope b R7=R3/R6 cm3/g 4 Intercept, V0 (1) R8=H8/4 cm3 4 Intercept, V0(2) R9=(R7*H7)/4 cm3 4 Intercept, V0 (3) R10=R8-R9 cm3 4
. . . . . . . . Sum of masses (1) . . . . . . . . H6=H20+H19+H18 . . . . . . . . Sum of masses (2) . . . . . . . . H7=H6+H17+H16 . . . . . . . . Sum of volumes . . . . . . . . H8=H1+H2+H3+H4+H5 . . . . . . . . Products (1) . . . . . . . . H9=H20*H1+H19*H2 . . . . . . . . Products (2) . . . . . . . . H10=H18*H3+H17*H4 . . . . . . . . Products (3) . . . . . . . . H11=H16*H5 . . . . . . . . Sum of products . . . . . . . . H12=H9+H10+H11 . . . . . . . . Sum of squares (1) . . . . . . . . H13=sq(H20)+sq(H19) . . . . . . . . Sum of squares (2) . . . . . . . . H14=sq(H18)+sq(H17) . . . . . . . . Sum of squares (3) . . . . . . . . H15=H13+H14+sq(H16) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Top line calc. (1) . R1=4*H12 . . . 4 . Top line calc. (2) . R2=-H7*H8 . . . 4 . Top line calc. (3) . R3=R1+R2 . . . 4
. . . . . . . . . . . Printer . . . . . . . . . . . Yes
111
METTLER TOLEDO
M241 / 3
Carbon Black Surface Area (ASTM D3765-99): Sample Titration

Sample titraiton according to Carbon Black Area Determination according to ASTM D3765-99. Five ITRB standards have been determined in Application 241/1, the calibration line is described in 241 / 2 . Sample

The sample must be prepared according to ASTM D3765-99. 1) Dry an adequate sample of carbon black at 125C for 1 hour and cool in dessiccator. 2) Weigh to 0.1 mg a suitable sample into a glass vial, and proceed according to ASTM D3765-99, chap. 9. After filtration, the samples are ready for titration: 1) Add 45 mL deionized water 2) Mount the beaker on the titration stand, start method ALG3. 3) 5 mL 0.15% Triton X-100 solution are added by a burette, 4) 10 mL 0.01 CTAB solution are added by a second burette. CTAB Standard solution (0.01 mol/L): Dissolve 3.64 g of reagent-grade CTAB (Cetyltrimethylammonim bromide, available from e.g. J.T. Baker, Cat. No. 7N121) in 900 mL distilled or deionized water. Add 100 mL of the pH 7.0 0.05 mol/L buffer solution. Warm the solution to a temperature of 27-37C to facilitate the dissolution. Cool to a temperature between 22 and 25C before using. Aerosol OT (Dioctyl sodium sulfosuccinate): Dissolve 1g/L of Aerosol OT solution in distilled or deionized water containing 2.5 mL/L of 37% formaldehyde, by swirling vogourously with a magnetic stirrer for 48 h. Allow to stand an additional twelve days before standardization and use. The solution should be capped tightly and stored in a cool place (once opened, the solution should be store in a dessiccator).
Substance Chemicals
Titrant
Accessories
Remarks
This method covers the measurement of the specific surface area of carbon black exclusive of area contained in micropores too small to admit CTAB molecules. This test method is suitable for characterizing rubber-grade carbon blacks of all types. The CTAB adsorption by carbonn black is independent of residual tars and functional groups containing hydrogen and oxygen, etc. Rapid equilibration is achieved by mechanical stirring and ultrasonic vibration. The CTAB molecule is relatively large; so it is not adsorped in micropores or on surface roughness. Thus, the CTAB surface area reflects only the surface f the carbon black that is available for interaction with rubber molecules. Titration with Aerosol OT soltuion to a turbidity maximum endpoint is used to determine the unadsorped CTAB after removal of the colloidally dispersed carbon black by ultrafiltration.
Calculation
Results
Waste disposal
Aqueous waste
Author
112
Results
Titration curve
113
Method
Method ALG3 Version ASTM3765: Sample det. 24-Jan-1995 11:13 . . . . AL3 . . . . ASTM3765: Sample det. . . . . 24-Jan-1995 11:13 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Stand 1 Weight m 0.15 0.25 100.0 1 TEMP A Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Temperatur sensor . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . . . . Titrant addition . . . . dV[mL] . . . . . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t(min) [s] . . . . . . t(max) [s] . . . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure. . . Stop for reevaluation . . Condition . . . . . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Result last sample . . . . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . .
. . . . 50 . . . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Aerosol OT 0.1 DP550 mV EQP mL 1.0 INC 0.1 EQU 1.0 2.0 3.0 30.0 500.0 10.0 Yes 1 Minimum Yes neq=0 Consumption R=VEQ mL 3
. . . . Printer . . . . Yes . . . . . . . . . . . . . . . . R1 Yes Yes Yes
. . . . Printer . . . . Yes
114
METTLER TOLEDO
M242
Determination of Amine Number

Determination of the acid number in several polymers by titration with perchloric acid.
Sample
MOCA, PPG, FCA-504 polymers

1) The sample mass depends on the amine number. 2) Recommended titrant consumption: 5-10 mL
Substance Chemicals
Basic components
Electrode cleaning: 1) Rinse the electrode after each titration withacetone 2) Soak it in water for at least 2 minutes to allow hydratation of the pH sensitive membrane glass. 3) Rinse again with acetone or glacial acetic acid before next titration.
60 mL glacial acetic acid
Titrant
Perchloric acid in glacial acetic acid: c(HClO4) = 0.1 mol/L
THAM, 50-100 mg DL50Graphix, DL53/55/58 DL70ES, DL77
Accessories
100 mL glass titration beaker ME-101446, DV1010 burette, printer, balance

If necessary , perform a blank value titration of the solvent. Literature: Application DL40RC No. 84-05.
DG113-SC
The amine value is the amount of substance of perchloric acid used for sample titration. It is expressed as mg KOH / g sample.
Calculation
Blank determination (Meth. blv): R1 = Q R1 is stored as auxiliary value H5 Acid value det. (Meth: 40012): R1 = (Q1 - H5)*C1/m C1 = 56.1
Results
Waste disposal
Author
MSG
115
Results
DL40RC: *** 17-FEB-84 *** 2114 530 3 198.71
METHOD 8405 IDENT. SAMPLE NO. *R * MG/G
Results: Sample MOCA ML-530 FCA-504 Weight in g ca. 0.1 ca. 0.2 ca. 0.3 Result mg KOH/g 415.58 200.32 143.79 St.Dev. in % 0.11 0.80 0.71 n 2 3 2
Statistics: n 3 Mean: 200.32 Stand. dev% .80
Titration curve
116
Method
Method 40016 Version Amine number det. 25-Mar-2002 10:00 . . . . . . . 40016 . . . . . . . Amine number det. . . . . . . . 25-Mar-2002 10:00 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Weight 0.0 2.0 56.1 1 Stand 1 Manual Method bv Version Blank value 25-Mar-2002 10:30 Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Lower limit [g] . . Upper limit [g] . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Volume [mL] . . . . Titrant addition . . . dV [mL] . . . . . . Measure mode . . . . . Title Method ID . . . . . . Title . . . . . . . . Date/time . . . . . . Sample Sample ID . . . . . . Entry type . . . . . . Volume [mL] . . . . Molar mass M . . . . . Equivalent number z . Titration stand . . . Temperatur sensor . . Stir Speed [%] . . . . . . Time [s] . . . . . . . EQP Titration Titrant . . . . . . . Concentration [mol/L] Sensor . . . . . . . . Unit of meas. . . . . Predispensing . . . . Titrant addition . . . dE(set) [mV] . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . .
. . . . . . . bl . . . . . . . Blank value . . . . . . . 25-Mar-2002 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Volume 60.0 56.1 1 Stand 1 Manual
10:30
. . . . . . . 50 . . . . . . . 120 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HClO4 0.1 DG113 mV Yes 5.0 INC 0.25 Equilibrium controlled 1.0 2.0 3.0 30.0 40 No No Positive 20.0 No No No No Standard No No Yes neq=0 R1=VEQ 3 ml Consumption No R2=(Q-H5)*C2/m C2=M/z 3 mg KOH/g Amine Number Yes
. . . . . . . 50 . . . . . . . 120 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HClO4 0.1 DG113 mV No Dynamic 8.0 0.02 0.3 Equilibrium controlled 0.5 1.0 3.0 30.0 40 No No Positive 10.0 No No No No Standard No No Yes neq=0 R1=Q 3 mmol Yes
. . . 0 . . .
117
METTLER TOLEDO
M243
Free available chlorine residual in water according to ASTM D 1253 - 86

Determination of free available chlorine residual (residual consisting of hypochlorite ions (OCl-), hypochlorous acid (HOCl) or combination thereof) in chlorine treated water by direct amperometric titration Sample
Chlorine treated waste water

1) 250 mL 0.4 M phosphate buffer pH 7.0: Weight in 6.35 g KH 2PO4 and 21.5 g Na2HPO4 * 12 H2O and fill up to 250 mL with dest. water.
Substance Chemicals
OCl- and HOCl
2) 250 mL 0.3 M KI: Weight in 12.5 g KI and fill up to 250 mL with dest. water. 3) 150 mL 0.3 M NaOH: Take 45 mL 1 M NaOH and add 105 mL of dest. water. 4) 100 mL 0.1 M HCl: Take 10 mL 1 M HCl and fill up to 100 mL with dest. water. 5) 1L 0.0047 M KIO 3: Weight in 1.0058 g KIO 3 and fill up to 1L with dest. water. 6) 1L 0.00282 M Phenylarsine Oxide (PAO): Weight in 0.8 g PAO and add 150 mL 0.3 M NaOH. Even upon fast stirring not all the PAO will dissolve. After settling, transfer 110 mL of the saturated solution into a 1L measuring cylinder, add 800 mL dest. water and adjust the pH between 6 and 7 using 0.1 M HCl. Fill up to 1L with dest. water and add 1 mL of CHCl 3 for preservation. Standardize the resulting solution to 0.00282 M (0.00564 N) against 0.0047 M (0.0282 N) KIO3 in the following way: Take 0.5 mL 0.0047 M KIO3, add 150 mL dest. water, 5 mL 0.3 M KI and (shortly before the titration) 1 pipette of concentrated acedic acid. Titrate this sample with the prepared PAO-solution using the titer-determination-method described in the method section. 7) Sample preparation: Take 200 mL sample and add 1 mL 0.4 M phosphate buffer pH 7.0.
KH2PO4 (Merck pro analysi, 136.09 g*mol-1) Na2HPO4*12 H2O (Merck pro analysi, 358.14 g*mol-1) KI (Fluka puriss, 166.01 g*mol-1); KIO3 (Fluka puriss, 214 g*mol-1) NaOH (Merck Titrisol, 1 M); Acedic acid (Fluka puriss, 60.05 g*mol-1) Phenylarsine Oxide (Sigma, min. 97%, 168.0 g*mol-1) CHCl3 (Fluka purum, 119.38 g*mol-1); HCl (Merck Titrisol, 1 M)
Titrant
0.00282 M Phenylarsine Oxide (PAO) (= 0.00564 N PAO)
0.0047 M KIO3 (= 0.0282 N KIO3) DL5x Rondo 60 with diaphragm pump
Accessories
KF Option Card ME-51 107 269 250 mL Titration beakers ME-23829 Printer

DM 143
The method is reliable down to a Cl2-concentration of about 100 ppb. Below this concentration the relative standard deviation (rsd) of a sample series increases dramatically. However, the method is well suitable to (qualitatively) detect traces of free available chlorine in waste water. Measured sample series: 2 ppm Cl2: rsd = 0.082 % (3 samples) 500 ppb Cl2: rsd = 7.402 % (3 samples, see results) 100 ppb Cl2: rsd = 3.442 % (4 samples) 50 ppb Cl2: rsd = 31.242 % (3 samples)
Titer: KIO3 + 5 KI + 6H+ --> 3 I2 + 6 K+ + 3 H2O C6H5AsIIIO + I2 + 2 H2O --> C6H7AsVO3 + 2 HI Sample: Cl2 in waste water --> HOCl, OCl-, Cl-, ClNR2, ... C6H5AsIIIO + OCl- (HOCl) + H2O --> C6H7AsVO3 + Cl- (HCl)
Calculation
free available chlorine - conc. in mmol / L
R1 = Q * C1 / m; C1 = 1000 / z
free available chlorine - conc. in mg / L
R2 = Q * C2 / m; C2 = 1000 * M / z
Method adjustment for different Cl2-Concentrations: Titrant addition dV [mL] Termination at maximum volume [mL] 3.0 1.2 (see method) 0.2 0.1
Results
Waste disposal
Collect all arsine containinig solutions in a separate, designated tank
2 ppm Cl2: 0.3 500 ppb Cl2: 0.06 100 ppb Cl2: 0.012 50 ppb Cl2: 0.006
Author
Mike Treyer
118
Results
Method Measured User ALL RESULTS No. ID 1 2 3 4 KIO3 KIO3 KIO3 KIO3 3333 Titer 0.00564 N PAO 31-May-2002 12:50 pm 31-May-2002 1:07 pm Mike Treyer Sample size and results 0.5 mL R1 = 1.21625 0.5 mL R1 = 1.21086 0.5 mL R1 = 1.21383 0.5 mL R1 = 1.21313 n x s srel = = = = Titer Titer Titer Titer 4 1.21352 Titer 0.00222 Titer 0.183 %
STATISTICS Number of results R1 Mean value Standard deviation Rel. standard deviation TITER Titrant PAO New titer Method Measured User ALL RESULTS No. ID 1 2 3 Waste water Waste water Waste water
0.00564 mol/L t = 1.21352
3341 free available chlorine residual 06-Jun-2002 2:50 pm 06-Jun-2002 3:20 pm Mike Treyer Sample size and results 200.0 mL R1 = 0.007 R2 = 0.521 200.0 mL R1 = 0.008 R2 = 0.585 200.0 mL R1 = 0.007 R2 = 0.512 n x s srel n x s srel = = = = = = = = mmol/L mg/L mmol/L mg/L mmol/L mg/L 3 0.008 0.00056 7.407 % 3 0.540 0.03997 7.407 % Cl2-Concentration Cl2-Concentration Cl2-Concentration Cl2-Concentration Cl2-Concentration Cl2-Concentration
STATISTICS Number of results R1 Mean value Standard deviation Rel. standard deviation Number of results R2 Mean value Standard deviation Rel. standard deviation
mmol/L mmol/L mg/L mg/L
Cl2-Concentration Cl2-Concentration Cl2-Concentration Cl2-Concentration
Titration curve
119
Method
Method 3333 Version Titer 0.00564 N PAO 31-May-2002 12:50 pm Method 3341 Version free available cholorine residual 06-Jun-2002 2:50 pm Title Method ID . . . . . . . . . . . .3333 Title . . . . . . . . . . . . . Titer 0.00564 N PAO Date/time . . . . . . . . . . . .31-May-2002 12:50 Sample Sample ID . . . . . . . . . . . . KIO3 Entry type . . . . . . . . . . . . Fixed volume Volume [mL] . . . . . . . . . .0.5 Molar mass M . . . . . . . . . . . 214.00 Equivalent number z . . . . . . . 6 Titration stand . . . . . . . . . ST20A Pump . . . . . . . . . . . . . No Pump . . . . . . . . . . . . . No Rinse . . . . . . . . . . . . .Yes Solvent . . . . . . . . . .H2O Volume[mL] . . . . . . . . 20.0 Conditioning . . . . . . . . . No Temperatur sensor . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . 30 EQP Titration (Ipol/Upol) Titrant/Sensor Titrant . . . . . . . . . . . .PAO Concentration [mol/L] . . . . 0.00564 Sensor . . . . . . . . . . . . DM143 Indication . . . . . . . . . . . . Amperometric Upol [mV] . . . . . . . . . . .500.0 Predispensing . . . . . . . . . . to volume Volume [mL] . . . . . . . . . . 1.5 Wail time [s] . . . . . . . . . 20 Titrant addition dV [mL] . . . . . . . . . . . . 0.05 Measure mode . . . . . . . . . . . Equilibrium controlled dE [mV, A] . . . . . . . . . . 0.2 dt [s] . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0 Recognition Threshold . . . . . . . . . . . 5.0 Steepest jump only . . . . . . .No Range . . . . . . . . . . . . . .No Tendency . . . . . . . . . . . .None Termination at maximum volume [mL] . . . . . 5.0 at potential . . . . . . . . . .No at slope . . . . . . . . . . . .No after number EQPs . . . . . . . .Yes n = . . . . . . . . . . . . 1 comb. termination conditions . .No Evaluation Procedure . . . . . . . . . . . .Minimum Potential 1 . . . . . . . . . . .No Potential 2 . . . . . . . . . . .No Stop for reevaluation . . . . . .Yes Condition . . . . . . . . . .neq=0 Calculation Formula . . . . . . . . . . . . . .R1=m/(VEQ*c*C1) Constant . . . . . . . . . . . . . .C1=1/(H1*z)
{H1 = 0.0047 M = Conc. of standard KIO3-solution}
Decimal places . . . . . . . . . . .5 Result unit . . . . . . . . . . . . Result name . . . . . . . . . . . .Titer Statistics . . . . . . . . . . . . .Yes Titer Titrant . . . . . . . . . . . . . .PAO Concentration [mol/L] . . . . . . . 0.00564 Formula t = . . . . . . . . . . . . x Report Output . . . . . . . . . . . . . . .Printer Results . . . . . . . . . . . . . .Yes All results . . . . . . . . . . . .Yes Raw results . . . . . . . . . . . .No Table of values . . . . . . . . . .No Sample data . . . . . . . . . . . .No E - V curve . . . . . . . . . . . .Yes dE/dV - V curve . . . . . . . . . .No d2E/dV2 - V curve . . . . . . . . .No log dE/dV - V curve . . . . . . . .No E - t curve . . . . . . . . . . . .No V - t curve . . . . . . . . . . . .No dV/dt - t curve . . . . . . . . . .No
Title Method ID . . . . . . . . . . . .3341 Title . . . . . . . . . . . . . free av. chl. rs. Date/time . . . . . . . . . . . .06-Jun-2002 2:50 Sample Sample ID . . . . . . . . . . . . Waste water Entry type . . . . . . . . . . . . Fixed volume Volume [mL] . . . . . . . . . .200.0 Molar mass M . . . . . . . . . . . 70.90 Equivalent number z . . . . . . . 2 Titration stand . . . . . . . . . ST20A Pump . . . . . . . . . . . . . No Pump . . . . . . . . . . . . . No Rinse . . . . . . . . . . . . .Yes Solvent . . . . . . . . . .H2O Volume[mL] . . . . . . . . 20.0 Conditioning . . . . . . . . . No Temperatur sensor . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . 20 EQP Titration (Ipol/Upol) Titrant/Sensor Titrant . . . . . . . . . . . .PAO Concentration [mol/L] . . . . 0.00564 Sensor . . . . . . . . . . . . DM143 Indication . . . . . . . . . . . . Amperometric Upol [mV] . . . . . . . . . . .500.0 Predispensing . . . . . . . . . . No Titrant addition dV [mL] . . . . . . . . . . . . 0.06 Measure mode . . . . . . . . . . . Timed increment dt [s] . . . . . . . . . . . . .20.0 Recognition Threshold . . . . . . . . . . . 0.0 Steepest jump only . . . . . . .Yes Range . . . . . . . . . . . . . .No Tendency . . . . . . . . . . . .None Termination at maximum volume [mL] . . . . . 1.2 at potential . . . . . . . . . .No at slope . . . . . . . . . . . .No after number EQPs . . . . . . . .No comb. termination conditions . .No Evaluation Procedure . . . . . . . . . . . .Segmented Potential 1 . . . . . . . . . . .No Potential 2 . . . . . . . . . . .No Stop for reevaluation . . . . . .No Calculation Formula . . . . . . . . . . . . . .R1=Q*C1/m Constant . . . . . . . . . . . . . .C1=1000/z Decimal places . . . . . . . . . . .3 Result unit . . . . . . . . . . . .mmol/L Result name . . . . . . . . . . . .Cl2-Concentration Statistics . . . . . . . . . . . . .Yes Calculation Formula . . . . . . . . . . . . . .R2=Q*C2/m Constant . . . . . . . . . . . . . .C2=1000*M/z Decimal places . . . . . . . . . . .3 Result unit . . . . . . . . . . . .mg/L Result name . . . . . . . . . . . .Cl2-Concentration Statistics . . . . . . . . . . . . .Yes Report Output . . . . . . . . . . . . . . .Printer Results . . . . . . . . . . . . . .Yes All results . . . . . . . . . . . .Yes Raw results . . . . . . . . . . . .No Table of values . . . . . . . . . .Yes Sample data . . . . . . . . . . . .No E - V curve . . . . . . . . . . . .Yes dE/dV - V curve . . . . . . . . . .Yes d2E/dV2 - V curve . . . . . . . . .Yes log dE/dV - V curve . . . . . . . .No E - t curve . . . . . . . . . . . .No V - t curve . . . . . . . . . . . .No dV/dt - t curve . . . . . . . . . .No
120
METTLER TOLEDO
M244
Total residual chlorine in water according to ASTM D 1253 - 86

Determination of total residual chlorine (amount of available chlorine-induced oxidants present in water at any specified period, subsequent to the addition of chlorine) in chlorine treated water by direct amperometric titration Sample
Chlorine treated waste water

1) 250 mL 9.8 M Acetate buffer pH 4.0 Weight in 36.625 g Sodium Acetate and 120 g Acedic acid and fill up to 250 mL with dest. water
Substance Chemicals
OCl-, HOCl, Cl3N, Cl2NR, ClNRR', ClNR2

Sodium acetate (anhydr., Fluka puriss, 82.04 g*mol-1) Acedic acid (Fluka puriss, 60.05 g*mol-1) KI (Fluka puriss, 166.01 g*mol-1); KIO3 (Fluka puriss, 214 g*mol-1) NaOH (Merck Titrisol, 1 M); HCl (Merck Titrisol, 1 M) Phenylarsine Oxide (Sigma, min. 97%, 168.0 g*mol-1) CHCl3 (Fluka purum, 119.38 g*mol-1)
2) 250 mL 0.3 M KI: Weight in 12.5 g KI and fill up to 250 mL with dest. water. 3) 150 mL 0.3 M NaOH: Take 45 mL 1 M NaOH and add 105 mL of dest. water. 4) 100 mL 0.1 M HCl: Take 10 mL 1 M HCl and fill up to 100 mL with dest. water. 5) 1L 0.0047 M KIO 3: Weight in 1.0058 g KIO 3 and fill up to 1L with dest. water. 6) 1L 0.00282 M Phenylarsine Oxide (PAO): Weight in 0.8 g PAO and add 150 mL 0.3 M NaOH. Even upon fast stirring not all the PAO will dissolve. After settling, transfer 110 mL of the saturated solution into a 1L measuring cylinder, add 800 mL dest. water and adjust the pH between 6 and 7 using 0.1 M HCl. Fill up to 1L with dest. water and add 1 mL of CHCl 3 for preservation. Standardize the resulting solution to 0.00282 M (0.00564 N) against 0.0047 M (0.0282 N) KIO3 in the following way: Take 0.5 mL 0.0047 M KIO3, add 150 mL dest. water, 5 mL 0.3 M KI and (shortly before the titration) 1 pipette of concentrated acedic acid. Titrate this sample with the prepared PAO-solution using the titer-determination-method described in the method section of application M 243. 7) Sample preparation: Take 200 mL sample and add shortly before the titration both 1 mL 9.8 M acetate buffer pH 4.0 and 1 mL 0.3 M KI solution. To add one or both solutions long before the titration starts will falsify the results.
Titrant
0.00282 M Phenylarsine Oxide (PAO) (= 0.00564 N PAO)
0.0047 M KIO3 (= 0.0282 N KIO3) DL5x Rondo 60 with diaphragm pump
Accessories
KF Option Card ME-51 107 269 250 mL Titration beakers ME-23829 Printer

DM 143
The method is reliable down to a Cl2-concentration of about 100 ppb. Below this concentration the relative standard deviation (rsd) of a sample series increases dramatically. However, the method is well suitable to (qualitatively) detect traces of chlorine in waste water. Method adjustment for different Cl2-Concentrations: Titrant addition dV [mL] 2 ppm Cl2: 0.3 500 ppb Cl2: 0.06 100 ppb Cl2: 0.012 50 ppb Cl2: 0.006 Termination at maximum volume [mL] 3.0 1.2 (see method) 0.2 0.1
Cl2 in waste water --> OCl-, HOCl, Cl3N, Cl2NR, ClNRR', ClNR2,ClClIxNR3-x + 2 x KI-I + x H+ --> x KCl-I + x I20 + HxNR3-x + x K+ and HOClI (OCl-) + 2 KI-I + H+ --> KCl-I + I20 + K+ + H2O (OH-) 1 mol Cl 2 corresponds to 1 mol I 2 C6H5AsIIIO + I2 + 2 H2O --> C6H7AsVO3 + 2 HI
Calculation
free available chlorine - conc. in mmol / L
R1 = Q * C1 / m; C1 = 1000 / z
free available chlorine - conc. in mg / L
R2 = Q * C2 / m; C2 = 1000 * M / z
Results
Waste disposal
Collect all arsine containinig solutions in a separate, designated tank
Author
Mike Treyer
121
Results
Method Measured User ALL RESULTS No. 1 2 3 ID Waste water Waste water Waste water Sample size and results 200.0 mL R1 = 0.007 R2 = 0.523 200.0 mL R1 = 0.007 R2 = 0.513 200.0 mL R1 = 0.007 R2 = 0.513 mmol/L mg/L mmol/L mg/L mmol/L mg/L Cl2-Concentration Cl2-Concentration Cl2-Concentration Cl2-Concentration Cl2-Concentration Cl2-Concentration 3340 total chlorine residual 06-Jun-2002 1:50 pm 06-Jun-2002 5:20 pm Mike Treyer
STATISTICS Number of results R1 Mean value Standard deviation Rel. standard deviation Number of results R2 Mean value Standard deviation Rel. standard deviation n x s srel n x s srel = = = = = = = = 3 0.007 mmol/L 0.00008 mmol/L 1.118 % 3 0.516 mg/L 0.00577 mg/L 1.118 % Cl2-Concentration Cl2-Concentration
Cl2-Concentration Cl2-Concentration
Titration curve
122
Method
Method 3340 Version total cholorine residual 06-Jun-2002 1:50 pm Title Method ID . . . . . . . . . . . .3340 Title . . . . . . . . . . . . . total chlorine residual Date/time . . . . . . . . . . . .06-Jun-2002 1:50 Sample Sample ID . . . . . . . . . . . . Waste water Entry type . . . . . . . . . . . . Fixed volume Volume [mL] . . . . . . . . . .200.0 Molar mass M . . . . . . . . . . . 70.90 Equivalent number z . . . . . . . 2 Titration stand . . . . . . . . . ST20A Pump . . . . . . . . . . . . . No Pump . . . . . . . . . . . . . No Rinse . . . . . . . . . . . . .Yes Solvent . . . . . . . . . .H2O Volume[mL] . . . . . . . . 20.0 Conditioning . . . . . . . . . No Temperatur sensor . . . . . . . . Manual Stir Speed [%] . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . 20 EQP Titration (Ipol/Upol) Titrant/Sensor Titrant . . . . . . . . . . . .PAO Concentration [mol/L] . . . . 0.00564 Sensor . . . . . . . . . . . . DM143 Indication . . . . . . . . . . . . Amperometric Upol [mV] . . . . . . . . . . .500.0 Predispensing . . . . . . . . . . No Titrant addition dV [mL] . . . . . . . . . . . . 0.06 Measure mode . . . . . . . . . . . Timed increment dt [s] . . . . . . . . . . . . .20.0 Recognition Threshold . . . . . . . . . . . 0.0 Steepest jump only . . . . . . .Yes Range . . . . . . . . . . . . . .No Tendency . . . . . . . . . . . .None Termination at maximum volume [mL] . . . . . 1.2 at potential . . . . . . . . . .No at slope . . . . . . . . . . . .No after number EQPs . . . . . . . .No comb. termination conditions . .No Evaluation Procedure . . . . . . . . . . . .Segmented Potential 1 . . . . . . . . . . .No Potential 2 . . . . . . . . . . .No Stop for reevaluation . . . . . .No Calculation Formula . . . . . . . . . . . . . .R1=Q*C1/m Constant . . . . . . . . . . . . . .C1=1000/z Decimal places . . . . . . . . . . .3 Result unit . . . . . . . . . . . .mmol/L Result name . . . . . . . . . . . .Cl2-Concentration Statistics . . . . . . . . . . . . .Yes Calculation Formula . . . . . . . . . . . . . .R2=Q*C2/m Constant . . . . . . . . . . . . . .C2=1000*M/z Decimal places . . . . . . . . . . .3 Result unit . . . . . . . . . . . .mg/L Result name . . . . . . . . . . . .Cl2-Concentration Statistics . . . . . . . . . . . . .Yes Report Output . . . . . . . . . . . . . . .Printer Results . . . . . . . . . . . . . .Yes All results . . . . . . . . . . . .Yes Raw results . . . . . . . . . . . .No Table of values . . . . . . . . . .Yes Sample data . . . . . . . . . . . .No E - V curve . . . . . . . . . . . .Yes dE/dV - V curve . . . . . . . . . .Yes d2E/dV2 - V curve . . . . . . . . .Yes log dE/dV - V curve . . . . . . . .No E - t curve . . . . . . . . . . . .No V - t curve . . . . . . . . . . . .No dV/dt - t curve . . . . . . . . . .No
123
METTLER TOLEDO
M258
Total Base Number according to DIN ISO 3771

Method for the determination of TBN (Total Base Number) according to DIN ISO 3771
Sample
0.2-2 g Oil

General procedure: 1. Blank determ. of solvent 3771. The blank is stored as auxiliary value H3 in mL (method b TBN). Therefore, it is not necessary to determine the titer before running the blank determination. 2. Titer determination of 0.1 mol/L HClO4 in acetic acid with THAM (M524). 3. Determination of the total base number, TBN (Method TBN) Sample determination: 1) Weigh in a well homogenized oil sample in the titration beaker. The sample size is selected according to the expected base number: BN until 1: 2g BN 15-30: 1g BN more than 30: 0.25 g 2) 60 mL solvent 3771 needed to dissolve the sample are added automatically with a second burette. 3) The electrolyte for the DG113 sensor is TEAB (Tetraethyl ammonium bromide)in ethylene glycol (EtG).To proceed with this determination, the following steps are needed: 1. Titer determination of perchloric acid (application M524) 2. Blank of solvent 3771 (method ) 3. Sample titration.
Substance Chemicals
Basic components
DIN ISO 3771 solvent Toluene/acetic acid/acetone 600:300:100 mL in 1 L Perchloric acid, HClO4 in acetic acid, c(HClO4) = 0.1 mol/L; THAM, see application M524 DL55, DL58 DL70ES, DL77
Titrant
Accessories
Glass titration beaker ME-101446 1 additional burette DV90 1 additional burette drive DV1010 AT261 Balance, Olivetti Artjet 20 printer DG113-SC with 0.4 mol/L TEAB in EtG
Remarks
Total base number according to DIN ISO 3771 Consumption of mg KOH/g oil to the EQP. Conditioning After every titration the electrode is conditioned in DIN ISO 3771. Note: This application does not replace the standard DIN ISO 3771
Calculation
Base Number: R1 = (VEQ-H3)*c*t*C/m ; C1 = 56.1 BN: mg KOH/g R2 = VEQ ; mL
Results
Waste disposal
Special waste (aromatic compounds)
Author
C. De Caro
124
Results
METTLER TOLEDO DL58 Method Measured User RESULTS No. 1 2 3 ID 01201 01201 01201 Sample size and results 0.25725 R1 = 74.18 R2 = 3.407 0.2323 R1 = 74.03 R2 = 3.071 0.29195 R1 = 74.11 R2 = 3.862 g mg mL g mg mL g mg mL KOH/g TBN Consumption KOH/g TBN Consumption KOH/g TBN Consumption Titrator V2.4 Mettler-Toledo GmbH Market Support Laboratory 30-04-2002 14:35
TBN TBN 30-04-2002 C. De Caro
15:40
n x s srel
= = = =
3 74.10 0.07412 0.100
mg KOH/gTBN mg KOH/gTBN %
Additional results: Oil 01204 02301 02302 01201 01202 01206 n 3 2 2 3 2 3 TBN 9.85 9.38 10.90 74.10 17.13 13.92 srel 0.20 --0.10 -0.18
Titration curve
125
Method
Method TBN Version TBN 30-04-2002 Method 14:35 . . TBN . . TBN . . 30-04-2002 . . . . . . . . . . . . . . . . 01201 Weight 0.2 0.3 100 1 Stand 1 Manual b TBN Version Blank with EQP 30-04-2002 9:59 . . b TBN . . Blank with EQP . . 30-04-2002 9:59 . . . . . . . . . . . . . . DIN ISO 3771 Fixed volume 60.0 100 1 Stand 1 Manual Title Method ID . . . . . . . . . . . Title . . . . . . . . . . . . . Date/time . . . . . . . . . . . Sample Sample ID . . . . . . . . . . . Entry type . . . . . . . . . . . Lower limit [g] . . . . . . . Upper limit [g] . . . . . . . Molar mass M . . . . . . . . . . Equivalent number z . . . . . . Titration stand . . . . . . . . Temperature sensor . . . . . . . Dispense Titrant . . . . . . . . . . . . Concentration [mol/L] . . . . . Volumen [mL] . . . . . . . . . . Stir Speed [%] . . . . . . . . . . . Time [s] . . . . . . . . . . . . EQP titration Titrant/Sensor Titrant . . . . . . . . . . . Concentration [mol/L] . . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . . Predispensing . . . . . . . . . Titrant addition . . . . . . . . dE(set) [mV] . . . . . . . . dV(min) [mL] . . . . . . . . dV(max) [mL] . . . . . . . . Measure mode . . . . . . . . . . dE [mV] . . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . . Limit A [mV,pH,...] . . . Limit B [mV,pH,...] . . . Tendency . . . . . . . . . . Termination at maximum volume [mL] . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs . . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . . Potential 1 . . . . . . . . . Potential 2 . . . . . . . . . Stop for reevaluation . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Report Output unit . . . . . . . . . . Results . . . . . . . . . . . . All results . . . . . . . . . . Raw results . . . . . . . . . . Table of measured values . . . . Sample data . . . . . . . . . . E - V curve . . . . . . . . . . dE/dV - V curve . . . . . . . . d2E/dV2 - V curve . . . . . . . log dE/dV - V curve . . . . . . E - t curve . . . . . . . . . . V - t curve . . . . . . . . . . dV/dt - t curve . . . . . . . . Title Method ID . . . . . . . . . . . Title . . . . . . . . . . . . . Date/time . . . . . . . . . . . Sample Sample ID . . . . . . . . . . . Entry type . . . . . . . . . . . Volume [mL] . . . . . . . . . Molar mass M . . . . . . . . . . Equivalent number z . . . . . . Titration stand . . . . . . . . Temperature sensor . . . . . . . Dispense Titrant . . . . . . . . . . . . Concentration [mol/L] . . . . . Volumen [mL] . . . . . . . . . . Stir Speed [%] . . . . . . . . . . . Time [s] . . . . . . . . . . . . EQP titration Titrant/Sensor Titrant . . . . . . . . . . . Concentration [mol/L] . . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . . Predispensing . . . . . . . . . Titrant addition . . . . . . . . dE(set) [mV] . . . . . . . . dV(min) [mL] . . . . . . . . dV(max) [mL] . . . . . . . . Measure mode . . . . . . . . . . dE [mV] . . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . . Tendency . . . . . . . . . . Termination at maximum volume [mL] . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs . . . . . . n = . . . . . . . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . . Potential 1 . . . . . . . . . Potential 2 . . . . . . . . . Stop for reevaluation . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . Constant . . . . . . . . . . . . Decimal places . . . . . . . . . Result unit . . . . . . . . . . Result name . . . . . . . . . . Statistics . . . . . . . . . . . Auxiliary value ID . . . . . . . . . . . . . . . Formula . . . . . . . . . . . . Report Output unit . . . . . . . . . . Results . . . . . . . . . . . . All results . . . . . . . . . . Raw results . . . . . . . . . . Table of measured values . . . . Sample data . . . . . . . . . . E - V curve . . . . . . . . . . dE/dV - V curve . . . . . . . . d2E/dV2 - V curve . . . . . . . log dE/dV - V curve . . . . . . E - t curve . . . . . . . . . . V - t curve . . . . . . . . . . dV/dt - t curve . . . . . . . .
14:35
. . TBN DIN 3771 . . 0.1 . . 60 . . 50 . . 240 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HClO4 0.1 DG113 mV No Dynamic 8.0 0.02 0.5 Equilibrium controlled 1.0 5.0 10.0 45.0 200.0 Yes Yes 550 900 Positive 8.0 No No No No Standard No No No R1=(VEQ-H3)*c*t*C/m C1=56.1 2 mg KOH/g TBN Yes R2=VEQ 3 mL Consumption No
. . TBN DIN 3771 . . 0.1 . . 60 . . 50 . . 10 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . HClO4 0.1 DG113 mV No Dynamic 8.0 0.002 0.1 Equilibrium controlled 0.5 6.0 10.0 60.0 200.0 Yes No Positive 0.1 No No Yes 1 No Standard No No No R1= VEQ 3 mL Blank Yes
. . . 0 . . . No
. . Blank . . H3=x . . . . . . . . . . . . . . . . . . . . . . . . . . Printer Yes Yes No Yes No Yes Yes No No No No No
. . . 0 . . . No . . . . . . . . . . . . . Printer Yes Yes No Yes No Yes Yes No No No No No
126
METTLER TOLEDO
M259
CTAB Surface Area on Amorphous Silica

Titration of unadsorbed CTAB (cetyltrimethylammonium bromide) on amorphous precipitated silica.
Sample
1 mL of silica-CTAB sample solution

General procedure: 1) Titration of a known amount of CTAB solution (meth. 00032) 2) The silica sample is prepared as indicated in the patent, and unadsorbed CTAB is titrated (1 mL sample size, meth. 00033). 3) Calculation of the surface area, ACTAB (m2/g) CTAB Standard solution (Cetyltrimethylammonium bromide, CAS 57-09-0) Dissolve 11.000 +/- 0.001 g of reagent-grade CTAB in distilled water in a 2 L volumetric flask. record the value as C. Aerosol OT titrant solution (Sodium di(2-ethylhexyl) sulfosuccinate, CAS 577-11-7): Dissolve 3.70 g of Aerosol OT in distilled water in a 2 L flask. Both solutions are kept in the dark for at least 12 days before use (storage lives of the solutions: 2 months after preparation) Sample preparation: The sample must be prepared according to the procedure by Swift at al. indicated in the US Patent 5.888.467 (1999). For more details, see under remarks.
Substance Chemicals
Amorphous precipitated silica, CTAB surface area: 85-275 m2/g 50 mL distilled water pH buffers 7 and 10.
Titrant
Aerosol OT, c(Aerosol OT) = 3.7 g / 2 L
--DL50Graphix, DL53/DL55/DL58 DL70ES, DL77 AT261 Balance, printer 100 mL titration beaker ME-101974
Accessories

DP550 with adapter cable ME-89600 DG111
Silica sample preparation: 1) Add 0.500+/- 0.001 g silica as received in a 200 mL wide mouth glass bottle. Record the value as S (g). 2) 100 mL standard CTAB solution is added into the bottle. 3) Add a stirring bar, close the bottle, stir gently for 15 minutes 4) Place a calibrated pH electrode into the bottle and adjust the pH value to between 9.0 and 9.5. 5) Cover the bottle with aluminium foil, and stir for 1 hour. 6) The mixture is filtrated (0.2 or 0.45 m filter). Note: the original patent indicates to filtrate the sample for 30 minutes. 7) 1 mL from the filtrated clear solution is taken and diluted with 50 mL distilled water in a titration beaker. 8) The sample is titrated with Aerosol OT solution to a turbidity maximum endpoint ito determine the unadsorbed CTAB after removal of the colloidally dispersed silica. The method has been modified with respect to the original titration procedure: Instead of performing a two-phase titration as described by the patent, a direct turbidimetric titration was done. Automated two-phase titration did not provide any result, since the samples were too milky for an efficient EP recognition by the photometric sensor. Literature: US Patent 5.888.467, 30th March 1999, Swift et al.
Calculation
Results
ACTAB = (V1-V2)*C*A*28.92/(V1*S*B) V1 = Titr. consumption for CTAB V2 = Titr. consumption for CTAB-Silica C = CTAB mass for standard sol. (g) A, B = Mass of a 1 g silica sample before/after drying (2 hours, 105C). S = Silica sample mass (g) Aqueous waste
Waste disposal
Author
C. De Caro
127
Results
Method Measured User ALL RESULTS No. ID 1 2 3 4 CTAB CTAB CTAB CTAB Sample amount and results 1.0 R1 = 3.707 1.0 R1 = 3.612 1.0 R1 = 3.645 1.0 R1 = 3.649 n x s srel = = = = mL ml mL ml mL ml mL ml 3 3.636 0.02019 0.555 Consumption Consumption Consumption Consumption 00032 CTAB 15-04-2002 Cosimo 18:06 15-04-2002 17:13
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation Sample No. 1 deleted
mL mL %
Comsumption Comsumption
--> V 1
Method Measured User ALL RESULTS No. ID 1 2 3 4
00033 Silica 2 + CTAB 19-04-2002 11:54 Cosimo
19-04-2002
10:47
Sample amount and results 1.0 R1 = 3.045 1.0 R1 = 3.071 1.0 R1 = 3.054 1.0 R1 = 3.017 n x s srel = = = = mL ml mL ml mL ml mL ml 4 3.047 0.02255 0.740 Consumption Consumption Consumption Consumption
Silica2CTAB Silica2CTAB Silica2CTAB Silica2CTAB
mL mL %
Comsumption Comsumption
--> V 2
Titration curve
128
Method
Method 00032 Version CTAB 15-04-2003 Method 17:13 . 00032 . CTAB . 15-04-2003 . . . . . . . CTAB Weight m 1.0 1.0 1 Stand 1 Manual 00033 Version Silica 2 + CTAB 19-04-2003 10:47 . 00033 . Silica 2 + CTAB . 19-04-2003 17:13 . . . . . . . Silica2CTAB Weight m 1.0 1.0 1 Stand 1 Manual Title Method ID . . . . . . . . . . . . Title . . . . . . . . . . . . . . Date/time . . . . . . . . . . . . Sample Sample ID . . . . . . . . . . . . Entry type . . . . . . . . . . . . Volume [mL] . . . . . . . . . . Molar mass M . . . . . . . . . . . Equivalent nuber z . . . . . . . . Titration stand . . . . . . . . . Temperatur sensor . . . . . . . . Stir Speed [%] . . . . . . . . . . . . Time [s] . . . . . . . . . . . . . EQP Titration Titrant/Sensor Titrant . . . . . . . . . . . . Concentration [mol/L] . . . . . Sensor . . . . . . . . . . . . Unit of meas. . . . . . . . . Predispensing . . . . . . . . . . Titrant addition Titrant addition . . . . . . . dE(set) [mV] . . . . . . . dV(min) [mL] . . . . . . . dV(max) [mL] . . . . . . . Measure mode . . . . . . . . . dE [mV] . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . Tendency . . . . . . . . . . Termination at maximum volume [mL] . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . Potential 1 . . . . . . . . Potential 2 . . . . . . . . Stop for reevaluation . . . Condition . . . . . . . . Calculation Formula . . . . . . . . . . . . . Constant . . . . . . . . . . . . . Decimal places . . . . . . . . . . Result unit . . . . . . . . . . . Result name . . . . . . . . . . . Statistics . . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . . Constant . . . . . . . . . . . . . Decimal places . . . . . . . . . . Result unit . . . . . . . . . . . Result name . . . . . . . . . . . Statistics . . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . . Constant . . . . . . . . . . . . . Decimal places . . . . . . . . . . Result unit . . . . . . . . . . . Result name . . . . . . . . . . . Statistics . . . . . . . . . . . . Report Output . . . . . . . . . . . . . . Results . . . . . . . . . . . . . All results . . . . . . . . . . . Raw results . . . . . . . . . . . Tables of measured values . . . . Sample data . . . . . . . . . . . E - V curve . . . . . . . . . . . dE/dV - V curve . . . . . . . . . d2E/dv2 - V curve . . . . . . . . log dE/dV -V curve . . . . . . . . E - t curve . . . . . . . . . . . V - t curve . . . . . . . . . . . dv/dt - t curve . . . . . . . . . Title Method ID . . . . . . . . . . . . Title . . . . . . . . . . . . . . Date/time . . . . . . . . . . . . Sample Sample ID . . . . . . . . . . . . Entry type . . . . . . . . . . . . Volume [mL] . . . . . . . . . . Molar mass M . . . . . . . . . . . Equivalent nuber z . . . . . . . . Titration stand . . . . . . . . . Temperatur sensor . . . . . . . . Stir Speed [%] . . . . . . . . . . . . Time [s] . . . . . . . . . . . . . EQP Titration Titrant/Sensor Titrant . . . . . . . . . . . . Concentration [mol/L] . . . . . Sensor . . . . . . . . . . . . Unit of meas. . . . . . . . . Predispensing . . . . . . . . . . Titrant addition Titrant addition . . . . . . . dE(set) [mV] . . . . . . . dV(min) [mL] . . . . . . . dV(max) [mL] . . . . . . . Measure mode . . . . . . . . . dE [mV] . . . . . . . . . . dt [s] . . . . . . . . . . . t(min) [s] . . . . . . . . . t(max) [s] . . . . . . . . . Recognition Threshold . . . . . . . . . Steepest jump only . . . . . Range . . . . . . . . . . . Tendency . . . . . . . . . . Termination at maximum volume [mL] . . . at potential . . . . . . . . at slope . . . . . . . . . . after number EQPs . . . . . comb. termination conditions Evaluation Procedure . . . . . . . . . Potential 1 . . . . . . . . Potential 2 . . . . . . . . Stop for reevaluation . . . Condition . . . . . . . . Calculation Formula . . . . . . . . . . . . . Constant . . . . . . . . . . . . . Decimal places . . . . . . . . . . Result unit . . . . . . . . . . . Result name . . . . . . . . . . . Statistics . . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . . Constant . . . . . . . . . . . . . Decimal places . . . . . . . . . . Result unit . . . . . . . . . . . Result name . . . . . . . . . . . Statistics . . . . . . . . . . . . Calculation Formula . . . . . . . . . . . . . Constant . . . . . . . . . . . . . Decimal places . . . . . . . . . . Result unit . . . . . . . . . . . Result name . . . . . . . . . . . Statistics . . . . . . . . . . . . Report Output . . . . . . . . . . . . . . Results . . . . . . . . . . . . . All results . . . . . . . . . . . Raw results . . . . . . . . . . . Tables of measured values . . . . Sample data . . . . . . . . . . . E - V curve . . . . . . . . . . . dE/dV - V curve . . . . . . . . . d2E/dv2 - V curve . . . . . . . . log dE/dV -V curve . . . . . . . . E - t curve . . . . . . . . . . . V - t curve . . . . . . . . . . . dv/dt - t curve . . . . . . . . .
17:13
. 40 . 5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Aerosol OT 1.0 DP550 mV No Dynamic 8.0 0.02 0.2 Equilibrium controlled 0.5 2.0 10.0 30.0 600.0 Yes No Negative 5.0 No No No No Minimum No No Yes neq=0 R1=VEQ 3 mL Consumption Yes
. 40 . 5 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Aerosol OT 1.0 DP550 mV No Dynamic 8.0 0.02 0.2 Equilibrium controlled 0.5 1.0 10.0 30.0 600.0 Yes No Negative 3.5 No No No No Minimum No No Yes neq=0 R1=VEQ 3 mL Consumption Yes
. . . 0 . . . . . . 0 . . . . . . . . . . . . . . . . Printer No Yes Yes Yes No Yes Yes No No No No No
. . . 0 . . . . . . 0 . . . . . . . . . . . . . . . . Printer No Yes Yes Yes No Yes Yes No No No No No
129
This application bulletin represents selected, possible application examples. These have been tested with all possible care in our lab with the analytical instrument mentioned in the bulletin. The experiments were conducted and the resulting data evaluated based on our current state of knowledge. However, the application bulletin does not absolve you from personally testing its suitability for your intended methods, instruments and purposes. As the use and transfer of an application example are beyond our control, we cannot accept responsibility therefore. When chemicals and solvents are used, the general safety rules and the directions of the producer must be observed.
Mettler-Toledo GmbH Analytical CH-8603 Schwerzenbach, Schweiz Telefon (01) 806 77 11, Fax (01) 806 73 50 Internet: http://www.mt.com
AT Mettler-Toledo GmbH., A-1100 Wien Tel. +43-1-604 19 80, Fax +43-1-604 28 80 AU Mettler-Toledo Ltd., Port Melbourne, Victoria 3207 Tel. +61-3-9644 5700, Fax +61-3-9645 3935 BE N.V. Mettler-Toledo S.A., B-1932 Zaventem Tel. +32-2-334 02 11, Fax +32-2-334 03 34 CH Mettler-Toledo (Schweiz) AG, CH-8606 Greifensee Tel. +41-1-944 45 45, Fax +41-1-944 45 10 CN Mettler-Toledo (Shanghai) Ltd., Shanghai 200233 Tel. +86-21-6485 0435, Fax +86-21-6485 3351 CZ Mettler-Toledo, spol, s.r.o., CZ-12000 Praha 2 Tel. +420-2-25 49 62, Fax +420-2-2424 7583 DE Mettler-Toledo GmbH, D-35353 Giessen Tel. +49-6-41 50 70, Fax +49-6-41 507 128 DK Mettler-Toledo A/S, DK-2600 Glostrup Tel. +45-4327 0800, Fax +45-4327 0828 ES Mettler-Toledo S.A.E., E-08038 Barcelona Tel. +34-3-223 22 22, Fax +34-3-223 02 71 FR Mettler-Toledo s.a., F-78222 Viroflay Tel. +33-1-3097 1717, Fax +33-1-3097 1616 HK Mettler-Toledo (HK) Ltd., Kowloon Tel. +852-2744 1221, Fax +852-2744 6878 HR Mettler-Toledo, d.o.o., HR-10000 Zagreb Tel. +385-1-230 41 47, Fax +385-1-233 63 17 HU Mettler-Toledo, KFT, H-1139 Budapest Tel. +36-1-288 40 40, Fax +36-1-288 40 50 IT Mettler-Toledo S.p.A., I-20026 Novate Milanese Tel. +39-2-333 321, Fax +39-2-356 29 73 JP Mettler-Toledo K.K., Tokyo 143-0006 Tel. +81-3-5762-0606, Fax +81-3-5762-0756 KR Mettler-Toledo (Korea) Ltd., Seoul (135-090) Tel. +82-2-518 20 04, Fax +82-2-518 08 13 KZ Mettler-Toledo CA, 480009 Almaty Tel. +7- 3272-608 834, Fax +7-3272-608 835 MY Mettler-Toledo (M) Sdn. Bhd. 47301 Petaling Jaya Tel. +60-3-703 27 73, Fax +60-3-703 17 72 MY Mettler-Toledo (S.E.A.), 47301 Petaling Jaya Tel. +60-3-704 17 73, Fax +60-3-703 17 72 MX Mettler-Toledo S.A. de C.V., Mxico C.P. 06430 Tel. +52-5-547 57 00, Fax +52-5-541 22 28 NL Mettler-Toledo B.V., NL-4000 HA Tiel Tel. +31-3-4463 8363, Fax +31-3-4463 8390 PL Mettler-Toledo, Sp. z o.o., PL-02-929 Warszawa Tel. +48-22-651 92 32, Fax +48-22-651 71 72 RU Mettler-Toledo C.I.S. AG, 10 1000 Moscow Tel. +7-095-921 92 11, Fax +7-095-921 63 53 SE Mettler-Toledo AB, S-12008 Stockholm Tel. +46-8-702 50 00, Fax +46-8-642 45 62 SG Mettler-Toledo (S) Pte. Ltd., Singapore 139944 Tel. +65-7786 779, Fax +65-7786 639 SK Mettler-Toledo, SK-82104 Bratislava Tel. +421-7-4342 7496, Fax +421-7-4333 7190 SI Mettler-Toledo, d.o.o., SI-1236 Trzin Tel. +386-61-162 18 01, Fax +386-61-162 17 89 TH Mettler-Toledo (Thailand) Ltd., Bangkok 10310 Tel. +66-2-719 64 80, Fax +66-2-719 64 79 TW Mettler-Toledo Pac Rim AG, Taipei Tel. +886-2-2579 5955, Fax +886-2-2579 5977 UK Mettler-Toledo Ltd., Leicester, LE4 1AW Tel. +44-116-235 70 70, Fax +44-116-236 63 99 US Mettler-Toledo, Inc., Columbus, OH 43240 Tel. +1-614-438 4511, Fax +1-614-438 4900
METTLER TOLEDO on the WWW You can also reach us on the World Wide Web. There you will find information on other products and services of METTLER TOLEDO and interesting information about our company. The address is http://www.mt.com
For all other countries: Mettler-Toledo GmbH PO Box, VI-400, CH-8606 Greifensee, Schweiz Tel. (01) 944 22 11, Fax (01) 944 31 70
Subject to technical changes 12/03 Mettler-Toledo GmbH

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Determination of Acid Values in Organic Solvents, Oils, Fats, Polymers

Preparation and Procedures

40 mL solvent mixture: Toluene:ethanol 2:1

Organic solvent waste (chlorinated and not chlorinated)

Literature: DIN 53402, 51588 ISO 3682

mmol mmol % mmol mmol %

Blank Acid No Blank Acid No

Blank Acid No Blank Acid No

Blank Acid No 15-Apr-1994 14:35

084B Acid Values (non aqueous) K.M. 15-Apr-1994 16:18

Table of measured values

Acid Number of Castor Oil

Castor oil, 9-11 g

Preparation and Procedures

50 mL toluene 1 mL hydrochloric acid

KOH in Ethanol: c(KOH) = 0.1 mol/L,

Potassium hydrogen phthalate DL50Graphix, DL53/55/58 DL70ES, DL77

100 mL titration beaker ME-101974 Printer Balance

Remarks Indication Chemistry

Organic solvent waste

SZtit Surezahl Rizinull/DAB 22-Feb-1999 20:48 DR

KOH/g KOH/g KOH/g KOH/g KOH/g

4 0.604 0.00377 0.625

mg KOH/g Surezahl mg KOH/g Surezahl %

Table of measured values

Acid Number of Cosmetic Creams

Cosmetic creams, 1-2 g

Preparation and Procedures

KOH in Ethanol: c(KOH) = 0.1 mol/L

Potassium hydrogen phthalate DL50Graphix, DL53/55/58 DL70ES, DL77

100 mL titration beaker ME-101974 Printer Balance

Remarks Indication Chemistry

Organic solvent waste

Literature: Application DL40RC No. 117.

PROV. 11321 IDENT. SAMPLE NO. *R * TAN STATISTICS: N MEAN STAND.DEV.%

Table of measured values

. . . . . . . blv . . . . . . . Blank value . . . . . . . 11-Dec-2001 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Volume 50.0 56.1 1 Stand 1 Manual

. . . 0 . . . . . . . . . . . . . . . . Printer No Yes No Yes No Yes Yes No No No No No

. . Blindwert . . H5=x . . . . . . . . . . . . . . . . . . . . . . . . . . Printer No Yes No Yes No Yes Yes No No No No No

Neutralizing Value of Baking Powder

Baking powder, 10 g Use 5 mL aliquots

Preparation and Procedures

Acidic / basic components

100 mL Sulphuric acid, H2SO4 , c(1/2 H2SO4) = 0.5 mol/L

Sodium hydroxide, NaOH c(NaOH) = 0.25 mol/L

Potassium hydrogen phthalate DL50Graphix, DL53/55/58 DL70ES, DL77

100 mL titration beaker ME-101974 Printer Balance

Remarks Indication Chemistry

Literature: Application DL40RC No. 118.

STATISTICS: N MEAN STAND.DEV.% 8 0.12 /G 10.0

Table of measured values

. . . 0 . . . . . . . . . . . . . . . . Printer No Yes No Yes No Yes Yes No No No No No

. . Back value . . H6=x . . . . . . . . . . . . . . . . . . . . . . . . . . Printer No Yes No Yes No Yes Yes No No No No No

Acid Number of Polyester

Preparation and Procedures

KOH in Ethanol: c(KOH) = 0.1 mol/L

PROV. 11321 IDENT. SAMPLE NO. R TAN STATISTICS: N MEAN STAND.DEV.%