Beruflich Dokumente
Kultur Dokumente
Characteristic Values
Applications brochure 10
Characteristic Values
Characteristic Values
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
Characteristic Values
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
Characteristic Values
Characteristic Values
METTLER TOLEDO
M084
Substance Chemicals
Acidic components
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
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
= 0.005091
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!
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
Sample
Substance Chemicals
Acidic components
Titrant
Standard Instruments
Accessories
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
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
STATISTICS Number results R2 Mean value Standard deviation Rel. standard deviation Sample No. 5 deleted
n x s srel
= = = =
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
Sample
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
Standard Instruments
Accessories
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
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
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 . . . . .
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 . . . . . . . .
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 . . .
METTLER TOLEDO
M230
Sample
Substance Chemicals
Titrant
Standard Instruments
Accessories
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
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
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 . . . . . . . .
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 . . .
12
METTLER TOLEDO
M231
Sample
Polyester, 0.2-0.4 g
Substance Chemicals
Acidic components
50 mL tetrahydrofuran
Titrant
Standard Instruments
Accessories
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
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 . . . . .
15:33
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
Sample
Substance Chemicals
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
Standard Instruments
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
Indication Chemistry
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
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!
= = = =
mg KOH/g mg KOH/g
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
Substance Chemicals
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
Standard Instruments
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.
Indication Chemistry
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
Author
K. Mooibroek
19
Results
METTLER DL67 Titrator DL67(1) V3.1 Mettler-Toledo AG Market Support Laboratory 09-Mar-1994 15:28
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
1 2
Araldit 2 Araldit 9
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
21
METTLER TOLEDO
M232
Sample
Substance Chemicals
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
Standard Instruments
Accessories
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
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
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation STATISTICS Number results R2 Mean value Standard deviation Rel. standard deviation
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 . . . . .
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
Sample
Substance Chemicals
50 mL solvent mixture
Titrant
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)
Standard Instruments
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)
Indication Chemistry
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
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
27
METTLER TOLEDO
M233
Sample
Substance Chemicals
Titrant
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)
Standard Instruments
DL38 DL50Graphix, DL53/55/58 with KF Option and DV705 KF titration stand Thermostatable vessel ME-51 107 497 AT261 balance, Printer
Accessories
Calculation
Blank determination (Meth. 111): R1 = VEQ , stored as blank Bromine Index. det. (Meth. 112): R1 = (Consumption-Blank)*Conc*15980/m
Results
Waste disposal
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
Sample
Resin, 3 g
Substance Chemicals
Titrant
Standard Instruments
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
Indication Chemistry
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
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
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
STATISTICS Number results R1 n Mean value x Standard deviation s Rel. standard deviation srel Outlier test: no outliers!
= = = =
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
33
METTLER TOLEDO
M091
Sample
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
Standard Instruments
Accessories
AT261 Balance, printer DL55/58, DL70ES/77: two additional burettes, ev. 1 DU200
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
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
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
= = = = = = = =
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
Sample
Substance Chemicals
Hydroxyl groups
Ethanol:Toluene 1:1
Titrant
Standard Instruments
Accessories
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
Author
37
Results
METTLER DL77 Titrator *114* OH V3.1 Mettler-Toledo AG Market Support Laboratory 31-Jul-1994 13:16
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
STATISTICS Number results R1 n Mean value x Standard deviation s Rel. standard deviation srel Outlier test: no outliers!
= = = =
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
Sample
Substance Chemicals
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
Standard Instruments
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)
Indication Chemistry
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
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
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
n x s srel n x s srel
= = = = = = = =
% 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
Sample
diphenylmethane-4,4-diisocyanate, 0.5 g
Substance Chemicals
20 mL methylethlyketone 10 mL diisobutylamine in isopropanol 50 mL isopropanol Hydrochloric acid, HCl, in isopropanol c(HCl) = 1 mol/L
Titrant
Standard Instruments
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
Indication Chemistry
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
Author
Kees Mooibroek
43
Results
DL40RC: *** 28-JAN-86 *** .5203 12.51 2823 12.51 1 32.718
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
45
METTLER TOLEDO
M236
Substance Chemicals
40 mL methanol
Titrant
Standard Instruments
Accessories
Calculation
Results
Waste disposal
Author
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
NaOH 0.1 mol/L Drive 2 20 mL DG113-SC EQP 1 EQP 2 VEQ1 Q1 EPOT1 VEQ2 Q2 EPOT2 VEX QEX = = = = = = = =
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
Sample
Substance Chemicals
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
Standard Instruments
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
Indication Chemistry
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
. . . . . . . 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
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
Substance Chemicals
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
Standard Instruments
Accessories
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
Waste disposal
Author
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
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
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
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
. . . . Printer . . . . Yes
54
METTLER TOLEDO
M211
Sample
Substance Chemicals
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
Standard Instruments
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
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
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
n x s srel n x s srel
= = = = = = = =
mmol mmol %
Bianco J Bianco J
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
. . . . 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
. . . . 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
Sample
Amorphous PET, 1 g
Substance Chemicals
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
Standard Instruments
Accessories
Calculation
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
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
STATISTICS Number results n Mean value x Standard deviation s Rel. standard deviation srel Outlier test: no outliers!
= = = =
eq/ton eq/ton %
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
60
METTLER TOLEDO
M237
Sample
Lecithin, 5 g
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
Standard Instruments
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
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 ***
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 . . . . .
11:05
. . . . . . . 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
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 . . . . . . . .
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 . . .
63
METTLER TOLEDO
M624
Sample
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
Standard Instruments
Accessories
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 %
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
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
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.
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
Standard Instruments
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.
Indication Chemistry
Calculation
Results
Waste disposal
Author
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
12-Jan-1994
STATISTICS Number results n Mean value x Standard deviation s Rel. standard deviation srel Outlier test: no outliers!
= = = =
mmol/L mmol/L
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
Sample
Substance Chemicals
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
Standard Instruments
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
Indication Chemistry
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
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
n x s srel n x s srel
= = = = = = = =
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
Sample
60 mL Solvent 664
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
Standard Instruments
Potassium hydrogen phthalate DL50Graphix, DL53/55/58, DL70ES/77 Sample changer, Printer Titration beaker ME-101974 Pump ME-65241
Accessories
Calculation
Results
Waste disposal
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
ASTM D664
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation AUXILIARY VALUE New value
n x s srel
= = = =
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
. . . 0 . . . No
75
METTLER TOLEDO
M518
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
Standard Instruments
KOH 0.1 mol/L DL50Graphix, DL53/55/58, DL70ES/77 Rondo 60 Titration beaker ME-101974, Printer
Accessories
Calculation
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
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation AUXILIARY VALUE New value
n x s srel
= = = =
mmol mmol %
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
. . . 0 . . . No
78
METTLER TOLEDO
M519
Sample
1 - 20 g Oil
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.
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
Standard Instruments
Accessories
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
A. Aichert, A. Logean
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
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation
n x s srel
= = = =
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
. . 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
Sample
1 - 20 g Oil
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
Standard Instruments
DL50Graphix, DL53/55/58, Rondo 60 Sample changer
Accessories
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
Literature: ASTM D4739-92 (www.astm.org) Application brochure 3, "TAN and TBN", ME-724559
Author
A. Aichert, A. Logean
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
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation STATISTICS Number results R2 Mean value Standard deviation Rel. standard deviation
n x s srel n x s srel
= = = = = = = =
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
. . 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
Substance Chemicals
Basic components
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
Standard Instruments
Accessories
Calculation
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
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
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation
n x s srel
= = = =
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
. . . . 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
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
Standard Instruments
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.
Indication Chemistry
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 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
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
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
Standard Instruments
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
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
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
93
METTLER TOLEDO
M099
Sample
Substance Chemicals
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
Standard Instruments
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
Indication Chemistry
Calculation
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
STATISTICS Number results Mean value Standard deviation Rel. standard deviation Outlier test: sample No.
n x s srel
= = = =
mg KOH/g mg KOH/g
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
96
METTLER TOLEDO
M100
Sample
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
Standard Instruments
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
Indication Chemistry
Calculation
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
STATISTICS Number results Mean value Standard deviation Rel. standard deviation Outlier test: sample No. Number results Mean value Standard deviation Rel. standard deviation
n x s srel n x s srel
= = = = = = = =
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
99
METTLER TOLEDO
M061
Sample
Honey, approx. 10 g
Substance Chemicals
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
Standard Instruments
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
Indication Chemistry
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
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
mmol/kg mmol/kg %
Acidity Acidity
mmol/kg mmol/kg %
mmol/kg mmol/kg %
n x s srel
= = = =
mmol/kg mmol/kg %
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
102
METTLER TOLEDO
M240
Substance Chemicals
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
Standard Instruments
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.
Indication Chemistry
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!
= = = = = = = = = = = = = = = =
% % %
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 . . . . 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
Substance Chemicals
Titrant
Standard Instruments
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.
Indication Chemistry
Calculation
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
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
. . . . 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
108
METTLER TOLEDO
M241 / 2
Substance Chemicals
Titrant
Standard Instruments
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.
Indication Chemistry
Calculation
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
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
Substance Chemicals
Titrant
Standard Instruments
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.
Indication Chemistry
Calculation
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
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
114
METTLER TOLEDO
M242
Sample
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.
Titrant
Standard Instruments
Accessories
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
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
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 . . . . .
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
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 . . . . . . . .
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 . . .
117
METTLER TOLEDO
M243
Substance Chemicals
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
Standard Instruments
Accessories
KF Option Card ME-51 107 269 250 mL Titration beakers ME-23829 Printer
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
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
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
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
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
Substance Chemicals
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
Standard Instruments
Accessories
KF Option Card ME-51 107 269 250 mL Titration beakers ME-23829 Printer
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
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
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
Sample
0.2-2 g Oil
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
Standard Instruments
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
Indication Chemistry
Calculation
Results
Waste disposal
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
15:40
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation
n x s srel
= = = =
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
126
METTLER TOLEDO
M259
Sample
Substance Chemicals
Amorphous precipitated silica, CTAB surface area: 85-275 m2/g 50 mL distilled water pH buffers 7 and 10.
Titrant
Standard Instruments
--DL50Graphix, DL53/DL55/DL58 DL70ES, DL77 AT261 Balance, printer 100 mL titration beaker ME-101974
Accessories
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
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
STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation
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
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.
Characteristic Values
Characteristic Values
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