Metler Toledo Ttitrator

METTLER TOLEDO Titrators
Dedicated to Mr. Kees Mooibroek
Characteristic Values
Applications brochure 10
METTLER TOLEDO Titrators Characteristic Values
Characteristic Values METTLER TOLEDO Titrators
Contents
M084 Determination of Acid Values in Organic Solvents, Oils, Fats, Polymers ...................... 1
M228 Acid Number of Castor Oil.................................................................................... 4
M229 Acid NUmber of Cosmetic Creams......................................................................... 7
M230 Neutralizing Value of Baking Powder................................................................... 10
M231 Acid Number of Polyester................................................................................... 13
M076 Free Fatty Acid of Oil and Fat .............................................................................. 16
M086 Epoxide Values ................................................................................................. 19

M232 Epoxide Value of 2,3-Epoxypropylene-Phenyl Ether .............................................. 22
M087 Bromine Number of Petroleum Distillates and Aliphatic Olefins ............................... 25

M233 Low Bromine Index Determination of a Standard Solution ...................................... 28
M090 Determination of Saponification Value ................................................................. 31

M091 Determination of Hydroxyl Value ......................................................................... 34
M234 Hydroxyl Value of Polyols .................................................................................. 37
M095 Determination of Isocyanate Content ................................................................... 40
M235 NCO-Content of Isocyanates by Back-Titration ...................................................... 43
M236 Determination of Free HCl and Isocyanates .......................................................... 46
M096 Iodine Value in Resins and Oils According to Wijs ................................................. 49

M051 Iodine Value of Edible OIls and Fats According to Wijs (AOAC Method 28.023) ........ 52
M211 Iodine Value of Cosmetic Fats According to Wijs ................................................... 55
M206 Determination of Carboxyl Groups in PET ............................................................ 58

M237 Peroxide Value of Lecithin .................................................................................. 61
M624 Peroxide Value of Edible Oils and Fats ................................................................. 64
M238 Determination of Permanganate Index in Waste Water .......................................... 67

M239 Chemical Oxygen Demand (COD) of Waste Water ................................................ 70
M517 Blank Determination According to ASTM D664-89 ................................................ 73
M518 Blank Determination According to ASTM D4739-92.............................................. 76
M519 Acid Number (AN) According to ASTM D664-89 .................................................. 79

M520 Base Number (BN) According to ASTM D4739-92 ............................................... 82
M057 TBN According to ASTM D2896-85 .................................................................... 85
M058 TBN According to ASTM D4739-87 .................................................................... 88
M059 TAN According to ASTM D664-89 ....................................................................... 91
M099 Conductometric Base Number Titration of Motor Oil............................................... 94

M100 Standardization of HCl in Isopropanol by Conductometric Titration .......................... 97
M061 pH, Acidity, Lactone and Formol Value of Honey................................................. 100

M240 Formol Number, Acidity and True Brix Value of Orange Juice ............................... 103
M241/1 Carbon Black Surface Area (ASTM D3765-99): Standardization .......................... 106
M241/2 Carbon Black Surface Area (ASTM D3765-99): Linear Regression........................ 109
M241/3 Carbon Black Surface Area (ASTM D3765-99): Sample Titration .......................... 112
M242 Determination of Amine Number ....................................................................... 115

M243 Free Available Chlorine Residual in Water According to ASTM D1253-86 .............. 118
M244 Total Residual Chlorine in Water According to ASTM D1253-86 ........................... 121
M258 Total Base Number According to DIN ISO 3771 .................................................. 124
M259 CTAB Surface Area on Amorphous Silica ............................................................ 127

METTLER TOLEDO M084
Determination of Acid Values in Organic Solvents, Oils, Fats, Polymers

The acid number is the amount of potassium hydroxide used to neutralized acidic components in different
samples (mg KOH/g). Here the determination of the acid value according to DIN 53402 (1973) is
presented.
Sample Organic solvents, resins, oils, fats fatty Preparation and Procedures
acids, softeners, polymers Solvent mixture according to DIN 53402 (1973):
Toluene:ethanol 2:1
Hints:
Substance Acidic components
1) Ensure good stirring. Speed and stirring time can be adapted
iaccording to the viscosity or the bad solubility of the sample.
Chemicals 40 mL solvent mixture: 2) If the dissolution of the sample is not straightforward, heating
Toluene:ethanol 2:1 my be applied to improve it. Ultrasonics can also be applied.
3) The titration can also indicated photometrically by a

phototrode and a color indicator. It can be affected by the
Titrant KOH in Ethanol: limitations of the indicators, by the formation of precipitates, or
c(KOH) = 0.1 mol/L, by change in turbidity.
c(KOH) = 0.01 mol/L
4) Use the same amount of solvent mixture for the blank as well
as for the sample determination.
Standard Potassium hydrogen phthalate
5) Substances which undergo side reactions with the alkaline
Instruments DL50Graphix, DL53/55/58 titrant can not be titrated.
DL70ES, DL77
Accessories 1 additional burette DV1005,

1 additional burette DV1020
100 mL titration beaker ME-101974
AT261 balance, Printer
Remarks
Indication DG113-SC This application describes the determination of the acid value of
resins, oils, fats, fatty acids, solvents, softeners, polymers and
other technical organic products.
Chemistry OH- + H+ = H2O
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.
Calculation The whole acidic components are neutralized, including half of

Blank determination (Meth. 084B):
the acid anhydride. Since the content of free anhydride is small,
R1 = Q this error can be generally neglected. On the other hand, if
R1 is stored as aux. value H8 significant amounts of anhydride are present, an additional
titration with aqueous potassium hydroxide solution must be
Acid value determination (Meth: 084A): performed to determine the second missing half anhydride.
R1 = (Q1 - H8)*C1/m ; C1 = 56.1
Results
Waste Organic solvent waste (chlorinated and

disposal not chlorinated) Literature:
DIN 53402, 51588
ISO 3682
Author Kees Mooibroek
1
Results
Method 084A Acid Values, Solvent Blank 13-Apr-1994 10:38
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
STATISTICS
Number results R1 n = 4
Mean value x = 0.004 mmol Blank Acid No
Standard deviation s = 0.002337 mmol Blank Acid No
Rel. standard deviation srel = 59.191 %
Outlier test : sample No. 1/4
Mean value x = 0.004 mmol Blank Acid No
Standard deviation s = 0.000592 mmol Blank Acid No
AUXILIARY VALUE
New value H8 = 0.005091 Blank Acid No
Method 084B Acid Values (non aqueous) 15-Apr-1994 14:35

User K.M.
RESULTS
1/1 Acid val Terpentine 43.003 g Weight m
R1 = 0.290 mg KOH/g Acid value
................................................................
STATISTICS
Mean value x = 0.298 mg KOH/g Acid value
Standard deviation s = 0.004793 mg KOH/g Acid value
Outlier test: no outliers!
Table of measured values Titration curve
2
Method
Method 084B Acid values (non aqueous) Method 084A Acid Values, Solvent Blank
Version 15-Apr-1994 14:35 Version 13-Apr-1994 10:38
Title Title
Method ID . . . . . . . . . . . . . 084B Method ID . . . . . . . . . . . . . 084A
Title . . . . . . . . . . . . . . . Acid values Title . . . . . . . . . . . . . . . Acid Values,
(non aqueous) Solvent Blank
Date/time . . . . . . . . . . . . . 15-Apr-1994 14:35 Date/time . . . . . . . . . . . . . 13-Apr-1994 10:38
Sample Sample
Number samples . . . . . . . . . . . 7 Number samples . . . . . . . . . . . 4
Titration stand . . . . . . . . . . Stand 1 Titration stand . . . . . . . . . . Stand 1
Entry type . . . . . . . . . . . . . Weight m Entry type . . . . . . . . . . . . . Weight m
Lower limit [g] . . . . . . . . . 0.0 Lower limit [g] . . . . . . . . . 0.0
Upper limit [g] . . . . . . . . . 50.0 Upper limit [g] . . . . . . . . . 50.0
ID1 . . . . . . . . . . . . . . . . Acid val ID1 . . . . . . . . . . . . . . . . SolvBl.
Molar mass M . . . . . . . . . . . . 0.0 Molar mass M . . . . . . . . . . . . 0.0
Equivalent number z . . . . . . . . 1 Equivalent number z . . . . . . . . 1
Temperatur sensor . . . . . . . . . Manual Temperatur sensor . . . . . . . . . Manual
Stir Stir
Speed [%] . . . . . . . . . . . . . 60 Speed [%] . . . . . . . . . . . . . 60
Time [s] . . . . . . . . . . . . . . 60 Time [s] . . . . . . . . . . . . . . 60
Titration Titration
Titrant . . . . . . . . . . . . . . KOH (Isoprop.) Titrant . . . . . . . . . . . . . . KOH (Isoprop.)
Concentration [mol/L] . . . . . . . 0.1 Concentration [mol/L] . . . . . . . 0.1
Sensor . . . . . . . . . . . . . . . DG113-SC Sensor . . . . . . . . . . . . . . . DG113-SC
Unit of meas. . . . . . . . . . . . mV Unit of meas. . . . . . . . . . . . mV
Titration mode . . . . . . . . . . . EQP Titration mode . . . . . . . . . . . EQP
Predispensing 1 . . . . . . . . . mL Titrant addition . . . . . . . . DYN
Volume [mL] . . . . . . . . . 1.0 dE(set) [mV] . . . . . . . . . 8.0
Titrant addition . . . . . . . . DYN Limits dV . . . . . . . . . . Absolute
dE(set) [mV] . . . . . . . . . 8.0 dV(min) [mL] . . . . . . . 0.02
Limits dV . . . . . . . . . . Absolute dV(max) [mL] . . . . . . . 0.2
dV(min) [mL] . . . . . . . 0.02 Measure mode . . . . . . . . . . EQU
dV(max) [mL] . . . . . . . 0.2 dE [mV] . . . . . . . . . . . 0.5
Measure mode . . . . . . . . . . EQU dt [s] . . . . . . . . . . . . 1.0
dE [mV] . . . . . . . . . . . 0.5 t(min) [s] . . . . . . . . . . 3.0
dt [s] . . . . . . . . . . . . 1.0 t(max) [s] . . . . . . . . . . 30.0
t(min) [s] . . . . . . . . . . 3.0 Threshold . . . . . . . . . . . . 500
t(max) [s] . . . . . . . . . . 30.0 EQP range . . . . . . . . . . . . Yes
Threshold . . . . . . . . . . . . 500 Limit A [mV, pH,...] . . . . . +500
EQP range . . . . . . . . . . . . Yes Limit B [mV, pH,...] . . . . . -500
Limit A [mV, pH,...] . . . . . +500 Maximum volume [mL] . . . . . . . 20.0
Limit B [mV, pH,...] . . . . . -500 Termination after n EQPs . . . . Yes
Maximum volume [mL] . . . . . . . 20.0 n = . . . . . . . . . . . . . 1
Termination after n EQPs . . . . Yes Evaluation procedure. . . . . . . Standard
n = . . . . . . . . . . . . . 1 Calculation
Evaluation procedure. . . . . . . Standard Result name . . . . . . . . . . . . Blank Acid No
Calculation Formula . . . . . . . . . . . . . . R1=Q
Result name . . . . . . . . . . . . Acid Value Constant . . . . . . . . . . . . . .
Formula . . . . . . . . . . . . . . R1=(Q1-H8)*C1/m Result unit . . . . . . . . . . . . mmol
Constant . . . . . . . . . . . . . . C1=56.1 Decimal places . . . . . . . . . . . 3
Result unit . . . . . . . . . . . . mg KOH/g Record
Decimal places . . . . . . . . . . . 3 Output unit . . . . . . . . . . . . Printer
Record Results last sample . . . . . . . . Yes
Output unit . . . . . . . . . . . . Printer Table of values . . . . . . . . . . Yes
Results last sample . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes
Table of values . . . . . . . . . . Yes Statistics
E - V curve . . . . . . . . . . . . Yes Ri (i=index) . . . . . . . . . . . . R1
Statistics Standard deviation s . . . . . . . . Yes
Ri (i=index) . . . . . . . . . . . . R1 Rel. standard deviation srel . . . . Yes
Standard deviation s . . . . . . . . Yes Outlier test . . . . . . . . . . . . Yes
Rel. standard deviation srel . . . . Yes Auxiliary value
Outlier test . . . . . . . . . . . . Yes ID text . . . . . . . . . . . . . . Blank Acid No.
Record Formula . . . . . . . . . . . . . . H8=x
Output unit . . . . . . . . . . . . Printer Record
All results . . . . . . . . . . . . Yes Output unit . . . . . . . . . . . . Printer
All results . . . . . . . . . . . . Yes
3
METTLER TOLEDO M228
Acid Number of Castor Oil

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

1 mL hydrochloric acid 0.1 mol/L is added to both solvent and
sample solutions (Spiking)
Chemicals 50 mL toluene
1 mL hydrochloric acid
Titrant KOH in Ethanol:

c(KOH) = 0.1 mol/L,
Instruments DL50Graphix, DL53/55/58

DL70ES, DL77
Accessories 100 mL titration beaker ME-101974

Printer
Balance
Remarks
Indication DG113-SC 1) One mL hydrochloric acid has been added to both 50 mL
solvent and samle solution to test the system (spiking).
Chemistry 2) The first equivalent point is due to the neutralization of 1 mL

hydrochloric acid. The method has been programmed to detect
only the second equivalent point.
Calculation Blank determination (Meth. SZ-bw):

R1 = Q
R1 is stored as auxiliary value H4
Acid value det. (Meth: SZtit):

R1 = (Q1 - H4)*C1/m
C1 = 56.1
Results
Waste Literature:
Organic solvent waste DAB
disposal
Author Dieter Rehwald
4
Results
METTLER TOLEDO DL58 Titrator V2.1 Team Ost:ms/rd 030-35503603
RatzFatz *1999* Help-Hotline: 0172-2727849
Method SZtit Säurezahl Rizinulöl/DAB 22-Feb-1999 19:42

Measured 22-Feb-1999 20:48
User DR
ALL RESULTS
No ID Sample amount and results
1 12.4 g
R1 = 5.308 ml VBR. TM
R2 = 0.601 mg KOH/g Säurezahl
2 9.4 g
R1 = 4.989 ml VBR. TM
3 10.6 g
R1 = 5.131 ml VBR. TM
4 11.6 g
R1 = 5.225 ml VBR. TM
5 9.6 g
R1 = 5.034 ml VBR. TM
STATISTICS
Mean value x = 0.604 mg KOH/g Säurezahl
Standard deviation s = 0.00377 mg KOH/g Säurezahl
Sample No. 5 deleted
5
Method
Method SZtit Säurezahl Rizinusöl/DAB Method SZ-bw Blank value with EQP tit.
Version 22-Feb-1999 19:42 Version 23-Feb-1999 17:09
Title Title
Method ID . . . . . . . . . . . . . SZtit Method ID . . . . . . . . . . . . . SZ-bw
Title . . . . . . . . . . . . . . . Säurezahl Title . . . . . . . . . . . . . . . Blank value
Rizinusöl/DAB with EQP tit.
Date/time . . . . . . . . . . . . . 22-Feb-1999 19:42 Date/time . . . . . . . . . . . . . 23-Feb-1999 17:09
Sample Sample
Sample ID . . . . . . . . . . . . . Sample ID . . . . . . . . . . . . .
Entry type . . . . . . . . . . . . . Weight Entry type . . . . . . . . . . . . . Volume
Lower limit [g] . . . . . . . . . 9.0 Volume [mL] . . . . . . . . . . . 50.0
Upper limit [g] . . . . . . . . . 11.0 Molar mass M . . . . . . . . . . . . 56.1
Molar mass M . . . . . . . . . . . . 56.1 Equivalent number z . . . . . . . . 1
Equivalent number z . . . . . . . . 1 Titration stand . . . . . . . . . . Stand 1
Titration stand . . . . . . . . . . Stand 1 Temperatur sensor . . . . . . . . . Manual
Temperatur sensor . . . . . . . . . Manual Stir
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 20
Time [s] . . . . . . . . . . . . . . 20 EQP Titration
EQP Titration Titrant . . . . . . . . . . . . . . KOH/EtOH
Titrant . . . . . . . . . . . . . . KOH/EtOH Concentration [mol/L] . . . . . . . 0.1
Concentration [mol/L] . . . . . . . 0.1 Sensor . . . . . . . . . . . . . . . DG113
Sensor . . . . . . . . . . . . . . . DG113 Unit of meas. . . . . . . . . . . . mV
Unit of meas. . . . . . . . . . . . mV Predispensing . . . . . . . . . . . No
Predispensing . . . . . . . . . . . No Titrant addition . . . . . . . . . . Dynamic
Titrant addition . . . . . . . . . . Dynamic dE(set) [mV] . . . . . . . . . . 8.0
dE(set) [mV] . . . . . . . . . . 8.0 dV(min) [mL] . . . . . . . . . . 0.02
dV(min) [mL] . . . . . . . . . . 0.02 dV(max) [mL] . . . . . . . . . . 0.3
dV(max) [mL] . . . . . . . . . . 0.3 Measure mode . . . . . . . . . . . . Equilibrium
Measure mode . . . . . . . . . . . . Equilibrium controlled
controlled dE [mV] . . . . . . . . . . . . . 0.5
dE [mV] . . . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . . 1.0
dt [s] . . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . . 3.0
t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . 30.0
t(max) [s] . . . . . . . . . . . 30.0 Recognition
Recognition Threshold . . . . . . . . . . . . 200
Threshold . . . . . . . . . . . . 100 Steepest jump only . . . . . . . Yes
Steepest jump only . . . . . . . Yes Range . . . . . . . . . . . . . . Yes
Range . . . . . . . . . . . . . . Yes Limit A [mV, pH,...] . . . . . -100
Limit A [mV, pH,...] . . . . . -100 Limit B [mV, pH,...] . . . . . -500
Limit B [mV, pH,...] . . . . . -500 Tendency . . . . . . . . . . . . Negative
Tendency . . . . . . . . . . . . Negative Termination
Termination Maximum volume [mL] . . . . . . . 10.0
Maximum volume [mL] . . . . . . . 10.0 at potential . . . . . . . . . . Yes
at potential . . . . . . . . . . Yes Potential [mV, pH,...] . . . . -450
Potential [mV, pH,...] . . . . -450 at slope . . . . . . . . . . . . No
at slope . . . . . . . . . . . . No after number EQPs . . . . . . . . No
after number EQPs . . . . . . . . No comb. termination conditions . . No
comb. termination conditions . . No Evaluation
Evaluation Procedure . . . . . . . . . . . . Standard
Procedure . . . . . . . . . . . . Standard Potential 1 . . . . . . . . . . . No
Potential 1 . . . . . . . . . . . No Potential 2 . . . . . . . . . . . No
Potential 2 . . . . . . . . . . . No Stop for reevaluation . . . . . . No
Stop for reevaluation . . . . . . Yes Calculation
Condition . . . . . . . . . . neq=0 Formula . . . . . . . . . . . . . . R1=Q
Calculation Constant . . . . . . . . . . . . . .
Formula . . . . . . . . . . . . . . R1=VEQ Decimal places . . . . . . . . . . . 3
Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . . mmol
Decimal places . . . . . . . . . . . 3 Result name . . . . . . . . . . . .
Result unit . . . . . . . . . . . . ml Statistics . . . . . . . . . . . . . Yes
Result name . . . . . . . . . . . . VBR. TM Calculation
Statistics . . . . . . . . . . . . . No Formula . . . . . . . . . . . . . .
Formula . . . . . . . . . . . . . . R2=(Q-H4)*C2/m Decimal places . . . . . . . . . . . 0
Constant . . . . . . . . . . . . . . C2=M/z Result unit . . . . . . . . . . . .
Result unit . . . . . . . . . . . . mg KOH/g Statistics . . . . . . . . . . . . .
Result name . . . . . . . . . . . . Säurezahl Auxiliary value
Statistics . . . . . . . . . . . . . Yes ID text . . . . . . . . . . . . . . Blindwert
Calculation Formula . . . . . . . . . . . . . . H4=x
Formula . . . . . . . . . . . . . . Report
Constant . . . . . . . . . . . . . . Output unit . . . . . . . . . . . . Printer
Decimal places . . . . . . . . . . . 0 Results . . . . . . . . . . . . . . No
Result unit . . . . . . . . . . . . All results . . . . . . . . . . . . Yes
Result name . . . . . . . . . . . . Raw results . . . . . . . . . . . . No
Statistics . . . . . . . . . . . . . Table of values . . . . . . . . . . Yes
Report Sample data . . . . . . . . . . . . No
Output unit . . . . . . . . . . . . Printer E - V curve . . . . . . . . . . . . Yes
Results . . . . . . . . . . . . . . No dE/dV - V curve . . . . . . . . . . Yes
All results . . . . . . . . . . . . Yes d2E/dV2 - V curve . . . . . . . . . No
Raw results . . . . . . . . . . . . No log dE/dV - V curve . . . . . . . . No
Table of values . . . . . . . . . . Yes E - t curve . . . . . . . . . . . . No
Sample data . . . . . . . . . . . . No V - t curve . . . . . . . . . . . . No
E - V curve . . . . . . . . . . . . Yes dV/dt - t curve . . . . . . . . . . No
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
6
METTLER TOLEDO M229
Acid Number of Cosmetic Creams

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

1) A ethanol:toluene 1.1 mixture is used to dissolve the
cosmetic creams.
2) To ensure complete dissolution, the sample solution is

dissolved under stirring at 40°C.
Chemicals 25 mL ethanol
25 mL toluene

c(KOH) = 0.1 mol/L

DL70ES, DL77

Printer
Balance
Remarks
Indication DG113-SC 1) The customer always titrates manually to the phenolphtalein
colour change. Therefore an endpoint titration was performed to
an absolute Ep value of -310 mV, although this point has no
Chemistry real meaning.
2) In addition, an EQP titration was performed. Two equivalence

points have been found.
3) The arrows in the titration curve indicate two equivalence

points due to the presence of at least two acids of different
Calculation strength.
Blank determination (Meth. blv):
R1 = Q
Acid value det. (Meth: 40012):

R1 = (Q1 - H5)*C1/m
C1 = 56.1
Results
Waste Organic solvent waste Literature:

disposal Application DL40RC No. 117.
Author U. Büchi/P. Schauwecker
7
Results
Results from endpoint titration to EPA = -310 mV (phenolphtalien colour change):
DL40RC:
*** 17-NOV-81 ***
PROV. 11321 1321

IDENT. 81596
SAMPLE NO. 2
*R * TAN 5.8836
STATISTICS:
N 2
MEAN 5.9188
STAND.DEV.% .84
8
Method
Method 40012 Acid No. Cosm. Cream Method blv Blank value
Version 11-Dec-2001 10:00 Version 11-Dec-2001 10:05
Title Title
Method ID . . . . . . . . . . . . . 40012 Method ID . . . . . . . . . . . . . blv
Title . . . . . . . . . . . . . . . Acid No. Cosm. Cream Title . . . . . . . . . . . . . . . Blank value
Date/time . . . . . . . . . . . . . 11-Dec-2001 10:00 Date/time . . . . . . . . . . . . . 11-Dec-2001 10:05
Sample Sample
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 90
dE(set) [mV] . . . . . . . . . . 8.0 dV(min) [mL] . . . . . . . . . . 0.02
dV(min) [mL] . . . . . . . . . . 0.02 dV(max) [mL] . . . . . . . . . . 0.3
controlled dE [mV] . . . . . . . . . . . . . 0.5
dE [mV] . . . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . . 1.0
dt [s] . . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . . 3.0
t(min) [s] . . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . . 30.0
Threshold . . . . . . . . . . . . 100 Steepest jump only . . . . . . . No
Steepest jump only . . . . . . . No Range . . . . . . . . . . . . . . No
Range . . . . . . . . . . . . . . No Tendency . . . . . . . . . . . . Negative
Maximum volume [mL] . . . . . . . 10.0 at potential . . . . . . . . . . No
at potential . . . . . . . . . . No at slope . . . . . . . . . . . . No
Potential 2 . . . . . . . . . . . No Stop for reevaluation . . . . . . Yes
Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0
Condition . . . . . . . . . . neq=0 Calculation
Formula . . . . . . . . . . . . . . R1=VEQ Constant . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . . Decimal places . . . . . . . . . . . 3
Decimal places . . . . . . . . . . . 3 Result unit . . . . . . . . . . . . mmol
Result unit . . . . . . . . . . . . ml Result name . . . . . . . . . . . .
Result name . . . . . . . . . . . . Consumption Statistics . . . . . . . . . . . . . Yes
Statistics . . . . . . . . . . . . . No Calculation
Calculation Formula . . . . . . . . . . . . . .
Formula . . . . . . . . . . . . . . R2=(Q-H5)*C2/m Constant . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . . C2=M/z Decimal places . . . . . . . . . . . 0
Decimal places . . . . . . . . . . . 3 Result unit . . . . . . . . . . . .
Result unit . . . . . . . . . . . . mg KOH/g Result name . . . . . . . . . . . .
Result name . . . . . . . . . . . . Acid No. Statistics . . . . . . . . . . . . .
Statistics . . . . . . . . . . . . . Yes Auxiliary value
Calculation ID text . . . . . . . . . . . . . . Blindwert
Formula . . . . . . . . . . . . . . Formula . . . . . . . . . . . . . . H5=x
Constant . . . . . . . . . . . . . . Report
Result unit . . . . . . . . . . . . Results . . . . . . . . . . . . . . No
Result name . . . . . . . . . . . . All results . . . . . . . . . . . . Yes
Statistics . . . . . . . . . . . . . Raw results . . . . . . . . . . . . No
Report Table of values . . . . . . . . . . Yes
Output unit . . . . . . . . . . . . Printer Sample data . . . . . . . . . . . . No
Results . . . . . . . . . . . . . . No E - V curve . . . . . . . . . . . . Yes
All results . . . . . . . . . . . . Yes dE/dV - V curve . . . . . . . . . . Yes
Raw results . . . . . . . . . . . . No d2E/dV2 - V curve . . . . . . . . . No
Table of values . . . . . . . . . . Yes log dE/dV - V curve . . . . . . . . No
Sample data . . . . . . . . . . . . No E - t curve . . . . . . . . . . . . No
E - V curve . . . . . . . . . . . . Yes V - t curve . . . . . . . . . . . . No
dE/dV - V curve . . . . . . . . . . Yes dV/dt - t curve . . . . . . . . . . No
d2E/dV2 - V curve . . . . . . . . . No
E - t curve . . . . . . . . . . . . No
V - t curve . . . . . . . . . . . . No
dV/dt - t curve . . . . . . . . . . No
9
METTLER TOLEDO M230
Neutralizing Value of Baking Powder

Determination of the neutralizing value of baking powder by titration with sodium hydroxide.
Sample Baking powder, 10 g Preparation and Procedures

Use 5 mL aliquots 1) 100 mL sulphuric acid c(1/2 H2SO4) = 0.5 mol/L are added
carefully to the weighed sample and stirred during 10 min.
Substance Acidic / basic components 2) The sample solution is subsequently filtered. CO2 is then
removed from the filtrate in an ultrasonic bath. (CO2 can also be
removed by heating the solution prior titration).
Chemicals 100 mL Sulphuric acid, H2SO4 , 3) For the titration, 5 mL aliquot samples are taken.
c(1/2 H2SO4) = 0.5 mol/L
Procedure:
1) A known amount of sulphuric acid is added to the sample.
2) Baking powder kan be either acidic or alkaline. Therefore, the
Titrant Sodium hydroxide, NaOH result in mmol/g can be negative or positive:
c(NaOH) = 0.25 mol/L
Negative result:
Baking powder is alkaline (Sulphuric acid amount higher than
equivalent value of titrant)
Positive result:
Instruments DL50Graphix, DL53/55/58 Baking powder is acidic (Sulphuric acid amount lower than
DL70ES, DL77 equivalent value of titrant)
For a final result in %, multiply with M/(10*z), where M/z is the
equivalent mass of the acidic or alkaline compound.
Printer
Balance
Remarks
Indication DG111-SC 1) The method can be used for both alkaline and acidic baking
powders.
Chemistry Method "back": 2) The amount of sulphuric acid added before titration,
H2SO4 + 2 NaOH = Na2SO4 + 2 H2O expressed in mmol, is introduced as auxiliary value H6 in the
titrator.
Method 40013: 3) The exact amount of sulphuric acid is determined by a
Acidic/alkaline components similar method using only 5 mL of sulphuric acid (see method
"back"). In this way, it is not necessary to perform a
Calculation standardization of the sulphuric acid solution.
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 Literature:
Results Application DL40RC No. 118.
Waste Aqueous waste (after neutralization)

disposal
Author K. Mooibroek/P. Schauwecker
10
Results
DL40RC:
*** 20-NOV-81 ***
INPUT:
WEIGHT 0.527
IDENT. 85.09
BLANK MEQ 2.5067
METHOD 118 1521

IDENT. 85.09
SAMPLE NO. 8
*R * /G .13275
STATISTICS:
N 8
MEAN 0.12 /G
STAND.DEV.% 10.0
11
Method
Method 40013 Neutr.Value Method back Back value
Version 11-Dec-2001 11:00 Version 11-Dec-2001 11:05
Title Title
Method ID . . . . . . . . . . . . . 40013 Method ID . . . . . . . . . . . . . Back
Title . . . . . . . . . . . . . . . Neutr.Value Title . . . . . . . . . . . . . . . Back value
Date/time . . . . . . . . . . . . . 11-Dec-2001 11:00 Date/time . . . . . . . . . . . . . 11-Dec-2001 11:05
Sample Sample
Sample ID . . . . . . . . . . . . . Baking Pwd. Sample ID . . . . . . . . . . . . . H2SO4
Entry type . . . . . . . . . . . . . Fixed volume Entry type . . . . . . . . . . . . . Volume
Volume [mL] . . . . . . . . . . . 5.0 Volume [mL] . . . . . . . . . . . 5.0
Stir Stir
Speed [%] . . . . . . . . . . . . . 50 Speed [%] . . . . . . . . . . . . . 50
Time [s] . . . . . . . . . . . . . . 10 Time [s] . . . . . . . . . . . . . . 10
EQP Titration EQP Titration
Titrant . . . . . . . . . . . . . . NaOH Titrant . . . . . . . . . . . . . . NaOH
Sensor . . . . . . . . . . . . . . . DG111 Sensor . . . . . . . . . . . . . . . DG111
Predispensing . . . . . . . . . . . No Predispensing . . . . . . . . . . . No
Titrant addition . . . . . . . . . . Dynamic Titrant addition . . . . . . . . . . Dynamic
dE(set) [mV] . . . . . . . . . . 8.0 dE(set) [mV] . . . . . . . . . . 8.0
dV(min) [mL] . . . . . . . . . . 0.02 dV(min) [mL] . . . . . . . . . . 0.02
dV(max) [mL] . . . . . . . . . . 0.3 dV(max) [mL] . . . . . . . . . . 0.3
Measure mode . . . . . . . . . . . . Equilibrium Measure mode . . . . . . . . . . . . Equilibrium
controlled controlled
dE [mV] . . . . . . . . . . . . . 1.0 dE [mV] . . . . . . . . . . . . . 1.0
dt [s] . . . . . . . . . . . . . 4.0 dt [s] . . . . . . . . . . . . . 4.0
t(min) [s] . . . . . . . . . . . 3.0 t(min) [s] . . . . . . . . . . . 3.0
t(max) [s] . . . . . . . . . . . 30.0 t(max) [s] . . . . . . . . . . . 30.0
Recognition Recognition
Threshold . . . . . . . . . . . . 60 Threshold . . . . . . . . . . . . 60
Steepest jump only . . . . . . . No Steepest jump only . . . . . . . No
Range . . . . . . . . . . . . . . No Range . . . . . . . . . . . . . . No
Tendency . . . . . . . . . . . . Negative Tendency . . . . . . . . . . . . Negative
Termination Termination
Maximum volume [mL] . . . . . . . 10.0 Maximum volume [mL] . . . . . . . 10.0
at potential . . . . . . . . . . No at potential . . . . . . . . . . No
at slope . . . . . . . . . . . . No at slope . . . . . . . . . . . . No
after number EQPs . . . . . . . . No after number EQPs . . . . . . . . No
comb. termination conditions . . No comb. termination conditions . . No
Evaluation Evaluation
Procedure . . . . . . . . . . . . Standard Procedure . . . . . . . . . . . . Standard
Stop for reevaluation . . . . . . Yes Stop for reevaluation . . . . . . Yes
Condition . . . . . . . . . . neq=0 Condition . . . . . . . . . . neq=0
Calculation Calculation
Formula . . . . . . . . . . . . . . R1=VEQ Formula . . . . . . . . . . . . . . R1=Q*C1
Constant . . . . . . . . . . . . . . Constant . . . . . . . . . . . . . . C1=1/z
Decimal places . . . . . . . . . . . 3 Decimal places . . . . . . . . . . . 3
Result unit . . . . . . . . . . . . ml Result unit . . . . . . . . . . . . mmol
Result name . . . . . . . . . . . . Consumption Result name . . . . . . . . . . . . mmol H2SO4
Statistics . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . Yes
Formula . . . . . . . . . . . . . . R2=(H6-Q)*C2/m Formula . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . . C2=1/z Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . mmol/g Result unit . . . . . . . . . . . .
Result name . . . . . . . . . . . . Neutral. value Result name . . . . . . . . . . . .
Statistics . . . . . . . . . . . . . Yes Statistics . . . . . . . . . . . . .
Calculation Auxiliary value
Formula . . . . . . . . . . . . . . ID text . . . . . . . . . . . . . . Back value
Constant . . . . . . . . . . . . . . Formula . . . . . . . . . . . . . . H6=x
Decimal places . . . . . . . . . . . 0 Report
Result unit . . . . . . . . . . . . Output unit . . . . . . . . . . . . Printer
Result name . . . . . . . . . . . . Results . . . . . . . . . . . . . . No
Statistics . . . . . . . . . . . . . All results . . . . . . . . . . . . Yes
Report Raw results . . . . . . . . . . . . No
Results . . . . . . . . . . . . . . No Sample data . . . . . . . . . . . . No
All results . . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes
Raw results . . . . . . . . . . . . No dE/dV - V curve . . . . . . . . . . Yes
Table of values . . . . . . . . . . Yes d2E/dV2 - V curve . . . . . . . . . No
Sample data . . . . . . . . . . . . No log dE/dV - V curve . . . . . . . . No
E - V curve . . . . . . . . . . . . Yes E - t curve . . . . . . . . . . . . No
dE/dV - V curve . . . . . . . . . . Yes V - t curve . . . . . . . . . . . . No
d2E/dV2 - V curve . . . . . . . . . No dV/dt - t curve . . . . . . . . . . No
E - t curve . . . . . . . . . . . . No
V - t curve . . . . . . . . . . . . No
dV/dt - t curve . . . . . . . . . . No
12
METTLER TOLEDO M231
Acid Number of Polyester

Determination of the acid number of polyester
Sample Polyester, 0.2-0.4 g Preparation and Procedures
Chemicals 50 mL tetrahydrofuran

c(KOH) = 0.1 mol/L

DL70ES, DL77

Printer
Balance
Remarks
Indication DG113-SC If needed, a blank value determination is performed. The blank
value is stored as auxiliary value H7.
Chemistry
Calculation Blank determination (Meth. blk):

R1 = Q

R1 = (Q1 - H7)*C1/m
C1 = 56.1
Results
Waste Organic solvent waste

disposal
Author R. Boehlen, MT-CH
13
Results
METTLER TOLEDO DL58 Titrator V2.4
5121086246
Method 2 Säurezahl 05-04-2001 15:33

Measured 05-04-2001 15:44
User RB
ALL RESULTS
1 0.3113 g
R1 = 26.78 mg/g Säurezahl
R2 = 2.08 mL Verbrauch
14
Method
Method 2 Saeurezahl Method blk Blindwert
Version 05-04-2001 15:53 Version 05-04-2001 15:05
Title Title
Method ID . . . . . . . . . . . . . 2 Method ID . . . . . . . . . . . . . blk
Title . . . . . . . . . . . . . . . Saeurezahl Title . . . . . . . . . . . . . . . Blindwert
Date/time . . . . . . . . . . . . . 05-04-2001 15:33 Date/time . . . . . . . . . . . . . 05-04-2001 15:05
Sample Sample
Sample ID . . . . . . . . . . . . . Polyester Sample ID . . . . . . . . . . . . . THF
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 70 Time [s] . . . . . . . . . . . . . . 10
dE(set) [mV] . . . . . . . . . . 8.0 dV(min) [mL] . . . . . . . . . . 0.02
dV(min) [mL] . . . . . . . . . . 0.1 dV(max) [mL] . . . . . . . . . . 0.5
controlled dE [mV] . . . . . . . . . . . . . 0.5
dE [mV] . . . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . . . 1.0
dt [s] . . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . . 2.0
t(min) [s] . . . . . . . . . . . 2.0 t(max) [s] . . . . . . . . . . . 20.0
at slope . . . . . . . . . . . . No after number EQPs . . . . . . . . Yes
after number EQPs . . . . . . . . Yes n = . . . . . . . . . . . . . 1
n = . . . . . . . . . . . . . 1 comb. termination conditions . . No
Stop for reevaluation . . . . . . No Calculation
Formula . . . . . . . . . . . . . . R=(Q-H7)*C/m Constant . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . . C=M/z Decimal places . . . . . . . . . . . 3
Result unit . . . . . . . . . . . . mg/g Result name . . . . . . . . . . . .
Result name . . . . . . . . . . . . Saeurezahl Statistics . . . . . . . . . . . . . Yes
Statistics . . . . . . . . . . . . . Yes Calculation
Formula . . . . . . . . . . . . . . R2=VEQ Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . mL Result name . . . . . . . . . . . .
Result name . . . . . . . . . . . . Verbrauch Statistics . . . . . . . . . . . . .
Calculation ID text . . . . . . . . . . . . . . Blindwert
Constant . . . . . . . . . . . . . . Report
d2E/dV2 - V curve . . . . . . . . . No
E - t curve . . . . . . . . . . . . No
V - t curve . . . . . . . . . . . . No
dV/dt - t curve . . . . . . . . . . No
15
METTLER TOLEDO M076
Free Fatty Acid of Oil and Fat

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

1) For oil, fat and butter a 1:1 mixture of ether and ethanol is
generally usedas a solvent. It can be added automatically with a
function DISPENSE.
Substance Free fatty acids
2) To achieve a complete dissolution of the sample, an
additional stirring with higher stirrer speed during 1-2 minutes is
used.
Chemicals 40 mL 1:1 ethanol:ether
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
Titrant KOH in ethanol: free acidity:
c(KOH) = 0.05 mol/L
Acid number AN = 5.61*a*t/m mg KOH/g
Free Fatty acid FFA = a*t*M/(100*m) %

Standard Benzoic acid
Instruments DL50Graphix, DL53/55/58 M = Molecular mass of the fatty acid involved:

M = 288 (oleic acid)
DL70ES, DL77
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)
Accessories 1 additional burette drive DV90 a = KOH consumption (mL)
1 additional burette DV1020 t =Titer (KOH)
100 mL beaker ME-101974
Printer, Balance
Remarks
Indication DG113-SC 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
Chemistry R-COOH + OH- = R-COO- + H2O 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
Calculation 3) Electrode conditioning:

Blank determination (Meth. 076b):
To ensure hydration of the membrane glass, the Dg113
R1 = Q electrode is stoed over night in water. Before titraiton, clean the
R1 is stored as auxiliary value H8 electrode with solvent.
Acid value det. (Meth: 076a): 4) Butter and coconut fats: For a complete dissolution 5 minutes
R1 = (Q1 - H8)*C1/m high speed stirring is required. After each sample, the fatty layer
C1 = M/z on the electrode must be removed by rinsing it with solvent. The
Results titration curve of butter is flat. The threshold hs to lowered to 400
mV.
Waste Organic solvent waste 5) Difficult samples:
disposal 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.
Author A. Aichert
16
Results
METTLER DL77 Titrator V3.1 Mettler-Toledo AG
*114* Market Support Laboratory
Method 076a FFA in Oil and Fat 28-Sep-1994 12:18

User dw
Measured 28-Sep-1994 16:16
RESULTS
1/1 Thistle oil 6.444 g Weight m

R1 = 0.477 mg KOH/g Acid Value
STATISTICS
Mean value x = 0.480 mg KOH/g Acid Value
Standard deviation s = 0.0022 mg KOH/g Acid Value
17
Method
Method 076a FFA in Oil and Fat Method 076b FFA in Oil and Fat / Blank
Version 28-Sep-1994 12:18 Version 28-Sep-1994 11:33
Title Title
Method ID . . . . . . . . . . . . . 076a Method ID . . . . . . . . . . . . . 076b
Title . . . . . . . . . . . . . . . FFA in Oil and Fat Title . . . . . . . . . . . . . . . FFA in Oil and Fat
Date/time . . . . . . . . . . . . . 28-Sep-1994 12:18 / Blank
Sample Date/time . . . . . . . . . . . . . 28-Sep-1994 11:33
Number samples . . . . . . . . . . . 6 Sample
Titration stand . . . . . . . . . . Stand 1 Number samples . . . . . . . . . . . 6
Entry type . . . . . . . . . . . . . Weight m Titration stand . . . . . . . . . . Stand 1
Lower limit [g] . . . . . . . . . 0.5 Entry type . . . . . . . . . . . . . Weight m
Upper limit [g] . . . . . . . . . 10.0 Lower limit [g] . . . . . . . . . 0.5
ID1 . . . . . . . . . . . . . . . . Thistle Upper limit [g] . . . . . . . . . 5.0
Molar mass M . . . . . . . . . . . . 56.11 ID1 . . . . . . . . . . . . . . . . Blank
Equivalent number z . . . . . . . . 1 Molar mass M . . . . . . . . . . . . 56.11
Temperatur sensor . . . . . . . . . Manual Equivalent number z . . . . . . . . 1
Stir Temperatur sensor . . . . . . . . . Manual
Speed [%] . . . . . . . . . . . . . 0 Stir
Time [s] . . . . . . . . . . . . . . 0 Speed [%] . . . . . . . . . . . . . 0
Dispense Time [s] . . . . . . . . . . . . . . 0
Titrant . . . . . . . . . . . . . . EtOH/Ether Dispense
Concentration [mol/L] . . . . . . . 1.0 Titrant . . . . . . . . . . . . . . EtOH/Ether
Volume [mL] . . . . . . . . . . . . 40.0 Concentration [mol/L] . . . . . . . 1.0
Stir Volume [mL] . . . . . . . . . . . . 40.0
Speed [%] . . . . . . . . . . . . . 70 Stir
Time [s] . . . . . . . . . . . . . . 60 Speed [%] . . . . . . . . . . . . . 50
Stir Time [s] . . . . . . . . . . . . . . 5
Speed [%] . . . . . . . . . . . . . 50 Titration
Time [s] . . . . . . . . . . . . . . 5 Titrant . . . . . . . . . . . . . . KOH/EtOH
Titration Concentration [mol/L] . . . . . . . 0.05
Titrant . . . . . . . . . . . . . . KOH/EtOH Sensor . . . . . . . . . . . . . . . DG113-SC
Concentration [mol/L] . . . . . . . 0.05 Unit of meas. . . . . . . . . . . . mV
Sensor . . . . . . . . . . . . . . . DG113-SC Titration mode . . . . . . . . . . . EQP
Unit of meas. . . . . . . . . . . . mV Titrant addition . . . . . . . . DYN
Titration mode . . . . . . . . . . . EQP dE(set) [mV] . . . . . . . . . 10.0
Predispensing 1 . . . . . . . . . mL Limits dV . . . . . . . . . . Absolute
Volume [mV] . . . . . . . . . 0.5 dV(min) [mL] . . . . . . . 0.005
Titrant addition . . . . . . . . DYN dV(max) [mL] . . . . . . . 0.04
dE(set) [mV] . . . . . . . . . 8.0 Measure mode . . . . . . . . . . EQU
Limits dV . . . . . . . . . . Absolute dE [mV] . . . . . . . . . . . 1.0
dV(min) [mL] . . . . . . . 0.01 dt [s] . . . . . . . . . . . 1.5
dV(max) [mL] . . . . . . . 0.2 t(min) [s] . . . . . . . . . . 2.0
Measure mode . . . . . . . . . . EQU t(max) [s] . . . . . . . . . . 20.0
dE [mV] . . . . . . . . . . . 1.0 Threshold . . . . . . . . . . . . 800.0
dt [s] . . . . . . . . . . . 1.5 Maximum volume [mL] . . . . . . . 0.3
t(min) [s] . . . . . . . . . . 2.0 Evaluation procedure . . . . . . Standard
t(max) [s] . . . . . . . . . . 20.0 Calculation
Threshold . . . . . . . . . . . . 1000.0 Result name . . . . . . . . . . . . Blank FFA
Maximum volume [mL] . . . . . . . 5.0 Formula . . . . . . . . . . . . . . R=Q
Termination after n EQPs . . . . Yes Constant . . . . . . . . . . . . . .
n = . . . . . . . . . . . . . 1 Result unit . . . . . . . . . . . . mmol
Evaluation procedure . . . . . . Standard Decimal places . . . . . . . . . . . 3
Calculation Record
Result name . . . . . . . . . . . . Acid Value Output unit . . . . . . . . . . . . Printer
Formula . . . . . . . . . . . . . . R=(Q-H8)*C/m Raw results last sample . . . . . . Yes
Constant . . . . . . . . . . . . . . C=M/z Table of values . . . . . . . . . . Yes
Result unit . . . . . . . . . . . . mg KOH/g E - V curve . . . . . . . . . . . . Yes
Decimal places . . . . . . . . . . . 3 Statistics
Record Ri (i=index) . . . . . . . . . . . . R1
Output unit . . . . . . . . . . . . Printer Standard deviation s . . . . . . . . Yes
Raw results last sample . . . . . . Yes Rel. standard deviation srel . . . . Yes
Table of values . . . . . . . . . . Yes Outlier test . . . . . . . . . . . . Yes
E - V curve . . . . . . . . . . . . Yes Auxiliary value
Statistics ID text . . . . . . . . . . . . . . FFA Blank
Ri (i=index) . . . . . . . . . . . . R1 Formula . . . . . . . . . . . . . . H8=x
Standard deviation s . . . . . . . . Yes Record
Rel. standard deviation srel . . . . Yes Output unit . . . . . . . . . . . . Printer
Outlier test . . . . . . . . . . . . Yes All results . . . . . . . . . . . . Yes
Record
Output unit . . . . . . . . . . . . Printer
All results . . . . . . . . . . . . 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 Preparation and Procedures

1) Epoxide resins are dissolved in a mixture consisting of four
parts dichloromethane (water content <0.02%) and one part
glacial acetic acid (water content <0.5%).
Substance Epoxide end groups
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
Chemicals 50 mL Dichloromethane:glacial acetic consumption in the order of 10-20 mL.
acid 4:1 ;
2 g Tetra-n-butylammonium iodide 3) The solution can be warmed up to 50°C to improve
dissolution, and cooled to room temperature before starting
tiration. Generally, solid resins are completely dissolved after ten
Titrant Perchloric acid in acetic acid, HClO4 minutes stirring time (see method 086).
c(HClO4) = 0.1 mol/L
4) 2 g Tetra-n-butylammonium iodide are added to the sample
solution, and the titration method is started.
Standard Tris(hydroxymethyl)aminomethane

DL70ES, DL77
Accessories 1 additional burette drive DV90

100 mL glass beaker ME-101974
Printer, Balance
Remarks
Indication DG113-SC 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.
Chemistry
2) Water in the solvent can affect the results. Therefore, only
anhydrous reagents should be used.
3) This application can not be used for epoxide resins

containing alkaline groups.
Calculation 4) Perchloric acid reacts stoichiometrically with epoxide end

Blank determination (method 086b):
groups.
R1 = Q ; mmol
R1 is stored as auxiliary value H9. 5) Calculations:
Epoxide value det. (Method 086a): The epoxide equivalent weight (EEW) is the amount of epoxide
R1 = (Q-H9)/(10*m) ; mg Mol/100g resin in g which contains 16 g of oxigen bound as epoxide:
R2 = (m*1000)/(Q1-H9) ; g/Mol EEM = m * 1000 / Q g/Mol
R3 = (Q1-H9)*1.6/m ; %
Results The epoxide value (EV) indicates the amount-of-substance of
epoxide groups in 100 g of an epoxide resin:
Waste EV = 100 / EEM Mol/100 g sample
Halogenated, organic solvent waste
disposal The content of oxirane oxigen in % = 1.6*Q/m
Literature:
ASTM D 1652-80, DIN 53188
Author K. Mooibroek
19
Results
DL67(1) Market Support Laboratory
Method 086a Epoxy Content 09-Mar-1994 15:28

User K.M.
Measured 10-Mar-1994 11:10
RESULTS LAST SAMPLE
1/2 Polymer 2.0734 g Weight m

R1 = 0.069 Mol/100g Epoxy Content
R2 = 1439.246 g/Mol Epoxide Eq.W.
R3 = 1.112 % Oxirane O 2
No. Probe Einwaage (g) n Epoxide equiv. Epoxide Oxiran srel

weight value oxygen
(g) (g/mol) (mol/100 g) (%) (%)
1 Araldit 2 0.4973 - 0.5562 6 1482.188 0.068 1.084 6.632
2 Araldit 9 2.0 - 2.5053 4 1440.431 0.069 1.111 0.1062
20
Method
Method 086a Epoxy Content Method 086b Blank
Version 09-Mar-1994 15:28 Version 17-Dec-2001 10:15
Title Title
Method ID . . . . . . . . . . . . . 086a Method ID . . . . . . . . . . . . . 086a
Title . . . . . . . . . . . . . . . Epoxy Content Title . . . . . . . . . . . . . . . Blank
Date/time . . . . . . . . . . . . . 09-Mar-1994 15:28 Date/time . . . . . . . . . . . . . 17-Dec-2001 10:15
Sample Sample
Lower limit [g] . . . . . . . . . 0.0 Lower limit [g] . . . . . . . . . 0.0
Upper limit [g] . . . . . . . . . 2.0 Upper limit [g] . . . . . . . . . 2.0
ID1 . . . . . . . . . . . . . . . . Polymer ID1 . . . . . . . . . . . . . . . . Polymer
Molar mass M . . . . . . . . . . . . 0 Molar mass M . . . . . . . . . . . . 0
Stir Stir
Speed [%] . . . . . . . . . . . . . 75 Speed [%] . . . . . . . . . . . . . 50
Time [s] . . . . . . . . . . . . . . 600 Time [s] . . . . . . . . . . . . . . 15
Titration Titration
Titrant . . . . . . . . . . . . . . HClO4 Titrant . . . . . . . . . . . . . . HClO4
Titrant addition . . . . . . . . DYN Titrant addition . . . . . . . . DYN
dE(set) [mV] . . . . . . . . . 8.0 dE(set) [mV] . . . . . . . . . 8.0
Limits dV . . . . . . . . . . Absolute Limits dV . . . . . . . . . . Absolute
dV(min) [mL] . . . . . . . 0.02 dV(min) [mL] . . . . . . . 0.005
dV(max) [mL] . . . . . . . 0.2 dV(max) [mL] . . . . . . . 0.2
Measure mode . . . . . . . . . . EQU Measure mode . . . . . . . . . . EQU
dE [mV] . . . . . . . . . . . 0.1 dE [mV] . . . . . . . . . . . 0.1
dt [s] . . . . . . . . . . . 5.0 dt [s] . . . . . . . . . . . 5.0
t(min) [s] . . . . . . . . . . 5.0 t(min) [s] . . . . . . . . . . 5.0
t(max) [s] . . . . . . . . . . 20.0 t(max) [s] . . . . . . . . . . 20.0
Threshold . . . . . . . . . . . . 75.0 Threshold . . . . . . . . . . . . 75.0
EQP range . . . . . . . . . . . . Yes EQP range . . . . . . . . . . . . Yes
Limit A . . . . . . . . . . . -1000 Limit A . . . . . . . . . . . -1000
Limit B . . . . . . . . . . . 1000 Limit B . . . . . . . . . . . 1000
Termination after n EQPs . . . . Yes Termination after n EQPs . . . . Yes
n = . . . . . . . . . . . . . 1 n = . . . . . . . . . . . . . 1
Evaluation procedure . . . . . . Standard Evaluation procedure . . . . . . Standard
Result name . . . . . . . . . . . . Epoxy Content Result name . . . . . . . . . . . . Blank
Formula . . . . . . . . . . . . . . R1=(Q1-H9)/(10*m) Formula . . . . . . . . . . . . . . R=Q
Constant . . . . . . . . . . . . . . Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . Mol/100g Result unit . . . . . . . . . . . . mmol
Calculation Record
Result name . . . . . . . . . . . . Epoxide Eq.W. Output unit . . . . . . . . . . . . Printer
Formula . . . . . . . . . . . . . . R1=(m*1000)/(Q1-H9) Raw results last sample . . . . . . Yes
Constant . . . . . . . . . . . . . . Table of values . . . . . . . . . . Yes
Result unit . . . . . . . . . . . . g/Mol E - V curve . . . . . . . . . . . . Yes
Calculation Ri (i=index) . . . . . . . . . . . . R1
Result name . . . . . . . . . . . . Oxirane O2 Standard deviation s . . . . . . . . Yes
Formula . . . . . . . . . . . . . . R3=(Q1-H9)*1.6/m Rel. standard deviation srel . . . . Yes
Constant . . . . . . . . . . . . . . Outlier test . . . . . . . . . . . . Yes
Result unit . . . . . . . . . . . . % Auxiliary value
Decimal places . . . . . . . . . . . 3 ID text . . . . . . . . . . . . . . Epoxide Blank
Raw results last sample . . . . . . Yes Output unit . . . . . . . . . . . . Printer
Results last sample . . . . . . . . Yes All results . . . . . . . . . . . . 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
Statistics
Ri (i=index) . . . . . . . . . . . . R2
Statistics
Ri (i=index) . . . . . . . . . . . . R3
Outlier test . . . . . . . . . . . . Yes
Record
Short-form method . . . . . . . . . Yes
All results . . . . . . . . . . . . Yes
21
METTLER TOLEDO M232
Epoxide Value of 2,3-Epoxypropylene-Phenyl Ether

Determination of the epoxide value by titration with HClO4
Sample 0.1 g Preparation and Procedures

2,3-epoxypropylene-phenyl ether, 99% 1) 0.1 g sample are dissolved in 50 mL 0.4 mol/L TEAB
solution
2) TEAB: tetraethylammonium bromide

Substance Epoxide end groups
Chemicals 50 mL 0.4 mol/L TEAB solution

(Tetraethylammonium bromide in
glacial acetic acid), M(TEAB)= 210.16
Titrant Perchloric acid in acetic acid, HClO4

Standard Tris(hydroxymethyl)aminomethane

DL70ES, DL77
Accessories 100 mL glass beaker ME-101974

Printer, Balance
Remarks
Indication DG113-SC 1) Water in the solvent can affect the results. Therefore, only
anhydrous reagents should be used.
Chemistry 2) Perchloric acid reacts stoichiometrically with epoxide end

groups.
3) After each meausrement the electrode was placed in water for

approximately 5 minutes.
Calculation Blank determination (method vsb):

R1 = Q ; mmol
R1 is stored as auxiliary value H10.
Epoxide value det. (Method vsa):
R1 = (Q-H10)*C/m ; C=1/z ; mol/kg
R2 = VEQ ; mL
R3 = 1000/R1 ; Epoxide value
Results
Waste Halogenated, organic solvent waste

disposal
Author Viola Mueller-Schindler
22
Results
METTLER TOLEDO DL58 Titrator V2.0 Titrations-Kurs
20.-29. Mai 1997
Method vsa Epoxid Bestimmung 27-Mai-1997 14:58

Measured 27-Mai-1997 15:59
User VS
ALL RESULTS
1 0.116 g
R1 = 6.6592 mol/kg Gehalt
R2 = 7.7246 mL
R3 = 150.2 Epoxyd Wert
2 0.0955 g
R2 = 6.3935 mL
3 0.1035 g
R2 = 6.9026 mL
4 0.0964 g
R2 = 6.4363 mL
STATISTICS
Mean value x = 6.6750 mol/kg Gehalt
Standard deviation s = 0.01504 mol/kg Gehalt
STATISTICS
Mean value x = 6.8643 mL
Standard deviation s = 0.61818 mL
23
Method
Method vsa Epoxid Bestimmung Method vsb Blank
Version 27-Mai-1997 14:58 Version 27-Mai-1997 14:30
Title Title
Method ID . . . . . . . . . . . . . Method ID . . . . . . . . . . . . . vsb
Title . . . . . . . . . . . . . . . Epoxid Bestimmung Title . . . . . . . . . . . . . . . Blank
Date/time . . . . . . . . . . . . . 27-Mai-1997 14:58 Date/time . . . . . . . . . . . . . 27-Mai-1997 14:30
Sample Sample
Upper limit [g] . . . . . . . . . 5.0 Molar mass M . . . . . . . . . . . . 1
Molar mass M . . . . . . . . . . . . 1 Equivalent number z . . . . . . . . 1
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 20
EQP Titration Titrant . . . . . . . . . . . . . . HClO4
Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1
Predispensing . . . . . . . . . . . Yes Titrant addition . . . . . . . . . . Incremental
Volume [mL] . . . . . . . . . . . 1.0 dV [mL] . . . . . . . . . . . . . 0.02
Wait time [s] . . . . . . . . . . 0 Measure mode . . . . . . . . . . . . Equilibrium
Titrant addition . . . . . . . . . . Incremental controlled
dV [mL] . . . . . . . . . . . . . 0.1 dE [mV] . . . . . . . . . . . . . 0.5
Measure mode . . . . . . . . . . . . Equilibrium dt [s] . . . . . . . . . . . . . 3.0
controlled t(min) [s] . . . . . . . . . . . 2.0
dE [mV] . . . . . . . . . . . . . 0.5 t(max) [s] . . . . . . . . . . . 30.0
dt [s] . . . . . . . . . . . . . 3.0 Recognition
t(min) [s] . . . . . . . . . . . 2.0 Threshold . . . . . . . . . . . . 170
t(max) [s] . . . . . . . . . . . 30.0 Steepest jump only . . . . . . . Yes
Recognition Range . . . . . . . . . . . . . . No
Threshold . . . . . . . . . . . . 170 Tendency . . . . . . . . . . . . Positive
Steepest jump only . . . . . . . Yes Termination
Range . . . . . . . . . . . . . . No Maximum volume [mL] . . . . . . . 20.0
Tendency . . . . . . . . . . . . Positive at potential . . . . . . . . . . No
Termination at slope . . . . . . . . . . . . No
Maximum volume [mL] . . . . . . . 20.0 after number EQPs . . . . . . . . Yes
at potential . . . . . . . . . . No n = . . . . . . . . . . . . . 1
at slope . . . . . . . . . . . . No comb. termination conditions . . No
after number EQPs . . . . . . . . Yes Evaluation
n = . . . . . . . . . . . . . 1 Procedure . . . . . . . . . . . . Standard
comb. termination conditions . . No Potential 1 . . . . . . . . . . . No
Evaluation Potential 2 . . . . . . . . . . . No
Procedure . . . . . . . . . . . . Standard Stop for reevaluation . . . . . . No
Potential 2 . . . . . . . . . . . No Calculation
Stop for reevaluation . . . . . . No Formula . . . . . . . . . . . . . . R1=Q
Formula . . . . . . . . . . . . . . R=(Q-H10)*C/m Decimal places . . . . . . . . . . . 3
Constant . . . . . . . . . . . . . . C=1/z Result unit . . . . . . . . . . . . mmol
Result unit . . . . . . . . . . . . mol/kg Statistics . . . . . . . . . . . . . Yes
Result name . . . . . . . . . . . . Gehalt Calculation
Statistics . . . . . . . . . . . . . Yes Formula . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . .
Result unit . . . . . . . . . . . . mL Statistics . . . . . . . . . . . . .
Result name . . . . . . . . . . . . Auxiliary value
Statistics . . . . . . . . . . . . . Yes ID text . . . . . . . . . . . . . . Blindwert
Formula . . . . . . . . . . . . . . R3=1000/R1 Report
Decimal places . . . . . . . . . . . 1 Results . . . . . . . . . . . . . . No
Result name . . . . . . . . . . . . Epoxid Wert Raw results . . . . . . . . . . . . No
Statistics . . . . . . . . . . . . . No Table of values . . . . . . . . . . Yes
Results . . . . . . . . . . . . . . Yes dE/dV - V curve . . . . . . . . . . Yes
Raw results . . . . . . . . . . . . Yes log dE/dV - V curve . . . . . . . . No
Table of values . . . . . . . . . . Yes E - t curve . . . . . . . . . . . . No
dE/dV - V curve . . . . . . . . . . Yes
d2E/dV2 - V curve . . . . . . . . . No
E - t curve . . . . . . . . . . . . No
V - t curve . . . . . . . . . . . . No
dV/dt - t curve . . . . . . . . . . No
24
METTLER TOLEDO M087
Bromine Number of Petroleum Distillates and Aliphatic Olefins

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

olefins 1) Solvent mixture according to ASTM D1159-89:
714 mL glacial acetic acid, 134 mL 1,1,1-trichloroethane
134 mL methanol, and 18 mL 1+5 H2SO4 (16%)
Substance Carbon-Carbon double bounds
Preparation of 1+5 H2SO4 solution:
Add 1 volume concentrated H2SO4 (specific gravity 1.84) to 5
volumes deionized water.
Chemicals 50 mL solvent mixture
2) Cool the solvent to 0-5°C before starting titration by setting
the temperature of the thermostate.
3) The DK102A polrization current is set to 0.5 µA, and it is

Titrant Bromide-Bromate, Br-/BrO3- connected to sensor input 1. Voltametric end point indication
c(Br2) = 0.05 mol/L 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

Standard
as a titrant. It is stable and does not need a standardization. If
necessary (e.g. by home-made titrant) reagents and titrant are
Instruments DL70ES, DL77 checked by titrating standards as given in ASTM D1159-89.
5) A blank is determined for every new batch of solvent mixture

(Method 087B)
Accessories 1 additional burette drive DV90
Thermostatable vessel ME-23517
DT120 Temperature sensor (Pt100)
Remarks
Indication DM143-SC with DK102A, cables Ban. 1) The bromine number is the number of grams of bromine
-SC 51108061, LEMO-SC 89601 which react completely with 100 g of the sample under the
conditions indicated by the standard ASTM 1159-89.
Chemistry Bromine generation:
BrO3- + 5Br- + 6H+ = 3Br2 + 3H2O It gives the quantity of bromine reactive components, and it also
characterizes the degree of unsaturation of the sample, based
only the addition reaction.
Bromine addition to C=C double bond:
R-CH=CH-R2 + Br2 = R-CHBr-CHBr-R2 2) By choosing the appropriate reaction conditions -i.e. the
composition of the solvent and a reaction temperature between
Calculation 0-5°C- only the additoon reaction takes place, while
Blank determination (Meth. 087B):
substitution and oxidation reactions are suppressed.
R1 = Q
R1 is stored as aux. value H11 3) Method 087A is especially designed for fast voltametric end
point titration with continuous titrant addtion according to ASTM
Bromine No. det. (Meth: 087A): D1159-89 (delay time 30 s, increment 0.1 mL)
R1 = (Q-H11)*15.98/m
Results
Literature:
Waste ASTM D1159-89, IP130/85
Chlorinated organic solvents
disposal
25
Results
No. Sample Weight n Bromine srel time

Number
(g) (g/100g) (%) (min)
1 Gasoline A 0.2165 6 55.4 3.03 3
2 Gasoline B 0.2 - 0.5 8 25.9 1.56 4
3 1-Decene 0.03296 6 106 1.82 8
4 Cyclopentene 0.03033 6 232 1.43 2
5 Cyclohexene 0.0518 6 198 2.57 3
26
Method
Method 087A Bromine number Method 087B Bromine Number:Blank
Version 25-Oct-1993 4:07 pm Version 21-Oct-1993 6:31 pm
Title Title
Method ID . . . . . . . . . . . . . 087A Method ID . . . . . . . . . . . . . 087B
Title . . . . . . . . . . . . . . . Bromine number Title . . . . . . . . . . . . . . . Bromine Number:Blank
Date/time . . . . . . . . . . . . . 25-Oct-1993 4:07 pm Date/time . . . . . . . . . . . . . 21-Oct-1993 6:31 pm
Sample Sample
Entry type . . . . . . . . . . . . . Weight m Entry type . . . . . . . . . . . . . Fixed volume U
Upper limit [g] . . . . . . . . . 2.0 ID1 . . . . . . . . . . . . . . . . Blank
ID1 . . . . . . . . . . . . . . . . Bromine Molar mass M . . . . . . . . . . . . 159.8
Equivalent number z . . . . . . . . 1 Temperatur sensor . . . . . . . . . TEMP A
Temperatur sensor . . . . . . . . . TEMP A Stir
Stir Speed [%] . . . . . . . . . . . . . 60
Speed [%] . . . . . . . . . . . . . 60 Time [s] . . . . . . . . . . . . . . 120
Time [s] . . . . . . . . . . . . . . 120 Temperature
Temperature Sensor . . . . . . . . . . . . . . . TEMP A
Sensor . . . . . . . . . . . . . . . TEMP A Unit of meas. . . . . . . . . . . . °C
Unit of meas. . . . . . . . . . . . °C dT [°C,°F,K] . . . . . . . . . . . . 1.0
dT [°C,°F,K] . . . . . . . . . . . . 1.0 dt [s] . . . . . . . . . . . . . . . 2.0
dt [s] . . . . . . . . . . . . . . . 2.0 t(min) mode . . . . . . . . . . . . T < set value
t(min) mode . . . . . . . . . . . . T < set value Set value [°C,°F,K] . . . . . . . 5.0
Set value [°C,°F,K] . . . . . . . 5.0 t(max) [s] . . . . . . . . . . . . . 600.0
t(max) [s] . . . . . . . . . . . . . 600.0 Titration
Titration Titrant . . . . . . . . . . . . . . Bromide-Bromate
Titrant . . . . . . . . . . . . . . Bromide-Bromate Concentration [mol/L] . . . . . . . 0.05
Concentration [mol/L] . . . . . . . 0.05 Sensor . . . . . . . . . . . . . . . DK102A/DM143
Sensor . . . . . . . . . . . . . . . DK102A/DM143 Unit of meas. . . . . . . . . . . . mV
Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EP
Titration mode . . . . . . . . . . . EP Titrant addition . . . . . . . . Continuous
Titrant addition . . . . . . . . Continuous Control band [mV,pH,...] . . . 3500
Control band [mV,pH,...] . . . 3000 Delay [s] . . . . . . . . . . 30
Delay [s] . . . . . . . . . . 30 dV(min) [mL] . . . . . . . . . 0.001
dV(min) [mL] . . . . . . . . . 0.02 End point mode . . . . . . . . . EPA
End point mode . . . . . . . . . EPA Potential [mV,pH,...] . . . . -150.0
Potential [mV,pH,...] . . . . -150.0 Tendency . . . . . . . . . . . . Positive
Tendency . . . . . . . . . . . . Positive Maximum volume [mL] . . . . . . . 5.0
Maximum volume [mL] . . . . . . . 20.0 Calculation
Calculation Result name . . . . . . . . . . . . Blank
Result name . . . . . . . . . . . . Bromine Number Formula . . . . . . . . . . . . . . R1=H11
Formula . . . . . . . . . . . . . . R=(Q-H11)*C/m Constant . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . . C=M/(10*z) Result unit . . . . . . . . . . . . mmol/50 mL
Result unit . . . . . . . . . . . . g Br2/100g Decimal places . . . . . . . . . . . 3
Decimal places . . . . . . . . . . . 2 Record
Record Output unit . . . . . . . . . . . . Printer
Output unit . . . . . . . . . . . . Printer Results last sample . . . . . . . . Yes
Results last sample . . . . . . . . Yes Statistics
Table of values . . . . . . . . . . Yes Ri (i=index) . . . . . . . . . . . . R1
E - V curve . . . . . . . . . . . . Yes Standard deviation s . . . . . . . . Yes
Statistics Rel. standard deviation srel . . . . Yes
Ri (i=index) . . . . . . . . . . . . R1 Outlier test . . . . . . . . . . . . Yes
Standard deviation s . . . . . . . . Yes Auxiliary value
Rel. standard deviation srel . . . . Yes ID text . . . . . . . . . . . . . . Blank value Bromine
Outlier test . . . . . . . . . . . . Yes Formula . . . . . . . . . . . . . . H11=x
Record Record
Output unit . . . . . . . . . . . . Printer Output unit . . . . . . . . . . . . Printer
All results . . . . . . . . . . . . Yes All results . . . . . . . . . . . . Yes
27
METTLER TOLEDO M233
Low Bromine Index Determination of a Standard Solution

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

5-10 ppm 1) Solvent mixture according to ASTM D2710-89:
714 mL glacial acetic acid, 134 mL 1,1,1-trichloroethane
134 mL methanol, and 18 mL 1+5 H2SO4 (16%)
Substance Carbon-Carbon double bounds
Preparation of 1+5 H2SO4 solution:
(Cyclohexene)
Add 1 volume concentrated H2SO4 (specific gravity 1.84) to 5
volumes deionized water.
2) Cool the solvent to 0-5°C before starting titration by setting
the temperature of the thermostate.
3) Voltametric end point indication allows a fast and accurate

Titrant Bromide-Bromate, Br-/BrO3- deterimantion. At the appearance of unreacted bromine a
c(Br2) = 0.05 mol/L 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
Standard standardization. If necessary (e.g. by home-made titrant)
reagents and titrant are checked by titrating standards as given
Instruments DL38 in ASTM D2710-99.
DL50Graphix, DL53/55/58 with KF
Option and DV705 KF titration stand 5) A blank is determined for every new batch of solvent mixture
(Method 111)
Accessories Thermostatable vessel ME-51 107 497
Remarks
Indication DM143-SC, or Pt885-NS-S7/105 1) The bromine index is the number of milligrams of bromine
(ME-59 904 435) which react completely with 100 g of the sample under the
conditions indicated by the standard ASTM 2710-99.
Chemistry Bromine generation:
BrO3- + 5Br- + 6H+ = 3Br2 + 3H2O It gives the quantity of bromine reactive components, and it also
characterizes the degree of unsaturation of the sample, based
only the addition reaction.
Bromine addition to C=C double bond:
R-CH=CH-R + Br2 = R-CHBr-CHBr-R 2) By choosing the appropriate reaction conditions -i.e. the
composition of the solvent and a reaction temperature between
Calculation 0-5°C- only the addition reaction takes place, while substitution
Blank determination (Meth. 111):
and oxidation reactions are suppressed.
R1 = VEQ , stored as blank
3) For very low bromine index values the platinum double ring
Bromine Index. det. (Meth. 112): electrode Pt885-NS-S7/105 (ME-59 904 435) was found to be
R1 = very suitable. In this case, it is recommended to replace the
(Consumption-Blank)*Conc*15980/m DM143 electrode with the Pt885 electrode.
Results
Waste Literature:
Chlorinated organic solvents ASTM D2710-99, IP299/92
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

RESULTS Br No. determination
No. Sample-ID Sample size and results
1 10mL4.724E-5g/mL 10.5 g
Bromine index = 9.09
R2 = 0.292 mL
R3 = 0.0146 mmol
2 5mL4.724E-5g/mL 5.25 g
R2 = 0.237 mL
R3 = 0.0119 mmol
3 3mL4.724E-5g/mL 3.15 g
R2 = 0.203 mL
R3 = 0.0102 mmol
4 1mL4.724E-5g/mL 1.04 g
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 %
29
Method
Method . . . . . . . . . . . . . . . . . . . . . 112 Method . . . . . . . . . . . . . . . . . . . . . 111

Title . . . . . . . . . . . . . . . . . . . . Br. Index Title . . . . . . . . . . . . . . . . . . . . Blank Br.Ind
Version . . . . . . . . . . . . . . . . . . . 20-11-2000 Version . . . . . . . . . . . . . . . . . . . 20-11-2000
15:37 15:32
Author . . . . . . . . . . . . . . . . . . . CDC Author . . . . . . . . . . . . . . . . . . . CDC
Sample parameters Sample parameters
ID . . . . . . . . . . . . . . . . . . . . . Request ID . . . . . . . . . . . . . . . . . . . . . Request
Type . . . . . . . . . . . . . . . . . . . . Mass Type . . . . . . . . . . . . . . . . . . . . Fixed volume
Minimum [g] . . . . . . . . . . . . . . . . . 8.0000 Density [g/mL] . . . . . . . . . . . . . . . 1.000
Maximum [g] . . . . . . . . . . . . . . . . . 30.0000 Volume [mL] . . . . . . . . . . . . . . . . . 55
Entry . . . . . . . . . . . . . . . . . . . . Before Speed [%] . . . . . . . . . . . . . . . . . . . 40
Speed [%] . . . . . . . . . . . . . . . . . . . 40 Mix time [s] . . . . . . . . . . . . . . . . . . 300
Mix time [s] . . . . . . . . . . . . . . . . . . 300 Titrant . . . . . . . . . . . . . . . . . . . . Br-/BrO3-
Titrant . . . . . . . . . . . . . . . . . . . . Br-/BrO3- Predisp.[mL] . . . . . . . . . . . . . . . . . . 0.0000
Predisp.[mL] . . . . . . . . . . . . . . . . . . 0.0000 Wait time [s] . . . . . . . . . . . . . . . . . 0
Wait time [s] . . . . . . . . . . . . . . . . . 0 Control parameters
Control parameters Current [uA] . . . . . . . . . . . . . . . . 1
Current [uA] . . . . . . . . . . . . . . . . 1 End point [mV] . . . . . . . . . . . . . . . 150
End point [mV] . . . . . . . . . . . . . . . 150 dVmin [uL] . . . . . . . . . . . . . . . . . 1.0
dVmin [uL] . . . . . . . . . . . . . . . . . 1.0 dVmax [uL] . . . . . . . . . . . . . . . . . 5.0
dVmax [uL] . . . . . . . . . . . . . . . . . 20.0 dVmax factor [%] . . . . . . . . . . . . . . 100
dVmax factor [%] . . . . . . . . . . . . . . 100 Start . . . . . . . . . . . . . . . . . . . . Cautious
Start . . . . . . . . . . . . . . . . . . . . Cautious Termination param.
Termination param. Max. time [s] . . . . . . . . . . . . . . . . 6000
Max. time [s] . . . . . . . . . . . . . . . . 6000 Delay [s] . . . . . . . . . . . . . . . . . . 30
Delay [s] . . . . . . . . . . . . . . . . . . 30 Vmax [mL] . . . . . . . . . . . . . . . . . . 5.000
Vmax [mL] . . . . . . . . . . . . . . . . . . 20.000 Blank [mmol] . . . . . . . . . . . . . . . . . . 0
Blank [mmol] . . . . . . . . . . . . . . . . . . Request Calculation 1
Calculation 1 R1 = . . . . . . . . . . . . . . . . . . . . x [mL]*f1
R1 = . . . . . . . . . . . . . . . . . . . . x [Br f1 = . . . . . . . . . . . . . . . . . . . . 0.0500
index]*f1 Unit . . . . . . . . . . . . . . . . . . . . mmol
f1 = . . . . . . . . . . . . . . . . . . . . 1.0000 Decimal places . . . . . . . . . . . . . . . 4
Unit Statistics . . . . . . . . . . . . . . . . . Yes
Decimal places . . . . . . . . . . . . . . . 2 Max. srel [%] . . . . . . . . . . . . . . . . 0.00
Statistics . . . . . . . . . . . . . . . . . Yes Calculation 2
Max. srel [%] . . . . . . . . . . . . . . . . 0.00 R2 = . . . . . . . . . . . . . . . . . . . . x [mL]*f2
Calculation 2 f2 = . . . . . . . . . . . . . . . . . . . . 1.0000
R2 = . . . . . . . . . . . . . . . . . . . . x [mL]*f2 Unit . . . . . . . . . . . . . . . . . . . . mL
f2 = . . . . . . . . . . . . . . . . . . . . 1.0000 Decimal places . . . . . . . . . . . . . . . 3
Unit . . . . . . . . . . . . . . . . . . . . mL Statistics . . . . . . . . . . . . . . . . . Yes
Decimal places . . . . . . . . . . . . . . . 3 Max. srel [%] . . . . . . . . . . . . . . . . 0.00
Statistics . . . . . . . . . . . . . . . . . No Calculation 3
Max. srel [%] . . . . . . . . . . . . . . . . 0.00 Report
Calculation 3 Output . . . . . . . . . . . . . . . . . . . Computer
R3 = . . . . . . . . . . . . . . . . . . . . x [mL]*f3
f3 = . . . . . . . . . . . . . . . . . . . . 0.0500
Unit . . . . . . . . . . . . . . . . . . . . mmol
Decimal places . . . . . . . . . . . . . . . 4
Statistics . . . . . . . . . . . . . . . . . Yes
Max. srel [%] . . . . . . . . . . . . . . . . 0.00
Report
Output . . . . . . . . . . . . . . . . . . . Computer
30
METTLER TOLEDO M090
Determination of Saponification Value

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

Sample preparation
1) The sample is dissolved in 50 mL toluene in a 100 mL
Erlenmeyer beaker.
Note: The Erlenmeyer beaker must be fit the reflux condenser.
Substance Saponifiable esterified acids
2) 20 mL 0.5 ml/L KOH are added to the sample solution.
3) Boil under reflux condition for 30 minutes.
4) Cool down the sample solution to room temperature before
Chemicals Toluene, 50 mL starting titration.
Ethanolic KOH, 20 mL c(KOH)=0.5 M
Boiling under reflux condiction:
1) The boiling time is crucial
2) Use organic solvents (or solvent mixtures) which do not
Titrant Hydrochloric acid in isopropanol undergo saponification and other side reactions: methanol,
c(HCl) = 0.5 mol/L ethanol, toluene, isopropanol, ethylene glycol. The
saponification temperature is determined by the solvent used.
3) If necessary: The reaction of the sample with carbon dioxide
is preventeed by flushing the titration vessel and reflux
Standard KHP for KOH, THAM for HCl condenser with nitrogen gas.
Instruments DL67/70ES/77, Titration:

The saponification value is determined by back-titration with HCl
DL50 Graphix, DL53/55/58
after saponification reaction. This is achieved by addition of a
known amount of KOH and subsequent reflux boiling. Unreacted
KOH is then determined by titration with HCl.
Accessories Reflux condenser, water bath
thermostat, 100 mL Erlenmeyer beaker,
AT261 Balance, printer, DL55/58,
DL70ES/77: addi. burettes
Remarks
Indication DG113-SC 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
Chemistry R1-CO-O-R2 + OH- = R1-COO- + saponification.
HO-R2
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.
Calculation Blank (Method 090B):
Two titration methods are used in this analysis: a blank and a
R1=Q ; mmol sample titration. The blank value is stored as auxiliary value
Stored as auxiliary value H12 H12 in the titrator.
Saponification value (Method 090A): Literature:

R1=(H12-Q)*(C1/m) 1. DIN 53401, 51559, 53404
C1=56.1 ; mg KOH/g 2. Schweizerisches Lebensmittelbuch, 5 th edition,
Results Eidgenössische Druck- und Materialzentrale, Bern, 1993
3. Application M618, Mettler-Toledo Application brochure 24,
Waste ME-51725054
Organic solvents (halogenated or not)
disposal
31
Results
DL67 (1) Market Support Laboratory
Method 090A Saponification Value 06-Apr-1994 11:42

User K.M.
RESULTS
1/1 Saponif. Resin 1 2.902 g Weight m

R1 = 157.266 mg KOH/g Saponif.value
STATISTICS
Mean value x = 158.144 mg KOH/g Saponif.value
Standard deviation s = 1.668318 mg KOH/g Saponif.value
32
Method
Method 090A Saponification Value Method 090B Saponification, Blank
Version 06-Apr-1994 11:42 Version 30-Mar-1994 13:46
Title Title
Title . . . . . . . . . . . . . . . Saponification Value Title . . . . . . . . . . . . . . . Saponification, Blank
Date/time . . . . . . . . . . . . . 06-Apr-1994 11:42 Date/time . . . . . . . . . . . . . 30-Mar-1994 13:46
Sample Sample
Upper limit [g] . . . . . . . . . 20.0 ID1 . . . . . . . . . . . . . . . . Saponif.
ID1 . . . . . . . . . . . . . . . . Saponif. Molar mass M . . . . . . . . . . . . 0
Equivalent number z . . . . . . . . 1 Temperatur sensor . . . . . . . . . Manual
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 60 Time [s] . . . . . . . . . . . . . . 10
Time [s] . . . . . . . . . . . . . . 10 Titration
Titration Titrant . . . . . . . . . . . . . . HCl
Titrant . . . . . . . . . . . . . . HCl Concentration [mol/L] . . . . . . . 0.5
Concentration [mol/L] . . . . . . . 0.5 Sensor . . . . . . . . . . . . . . . DG111-SC
Sensor . . . . . . . . . . . . . . . DG111-SC Unit of meas. . . . . . . . . . . . mV
Unit of meas. . . . . . . . . . . . mV Titration mode . . . . . . . . . . . EQP
Titration mode . . . . . . . . . . . EQP Predispensing 1 . . . . . . . . . mL
Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 12.0
Volume [mL] . . . . . . . . . 0.0 Titrant addition . . . . . . . . DYN
Titrant addition . . . . . . . . DYN dE(set) [mV] . . . . . . . . . 8.0
dE(set) [mV] . . . . . . . . . 8.0 Limits dV . . . . . . . . . . Absolute
Limits dV . . . . . . . . . . Absolute dV(min) [mL] . . . . . . . 0.02
dV(min) [mL] . . . . . . . 0.02 dV(max) [mL] . . . . . . . 0.2
dV(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU
Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 0.5
dE [mV] . . . . . . . . . . . 0.5 dt [s] . . . . . . . . . . . 1.0
dt [s] . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . 3.0
t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 30.0
t(max) [s] . . . . . . . . . . 30.0 Threshold . . . . . . . . . . . . 500.0
Threshold . . . . . . . . . . . . 250.0 EQP range . . . . . . . . . . . . Yes
EQP range . . . . . . . . . . . . Yes Limit A . . . . . . . . . . . -500
Limit A . . . . . . . . . . . -500 Limit B . . . . . . . . . . . +500
Limit B . . . . . . . . . . . +500 Maximum volume [mL] . . . . . . . 40.0
Maximum volume [mL] . . . . . . . 40.0 Termination after n EQPs . . . . Yes
Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1
n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard
Evaluation procedure . . . . . . Standard Calculation
Result name . . . . . . . . . . . . Saponif.value Formula . . . . . . . . . . . . . . R1=Q
Formula . . . . . . . . . . . . . . R1=(H12-Q1)*(C1/m) Constant . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . . C1=56.1 Result unit . . . . . . . . . . . . mmol
Result unit . . . . . . . . . . . . mg KOH/g Decimal places . . . . . . . . . . . 3
Results last sample . . . . . . . . Yes Table of values . . . . . . . . . . Yes
Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes
E - V curve . . . . . . . . . . . . Yes Statistics
Statistics Ri (i=index) . . . . . . . . . . . . R1
Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes
Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes
Rel. standard deviation srel . . . . Yes Outlier test . . . . . . . . . . . . Yes
Outlier test . . . . . . . . . . . . Yes Auxiliary value
Record ID text . . . . . . . . . . . . . . Saponification
Output unit . . . . . . . . . . . . Printer Formula . . . . . . . . . . . . . . H12=x
All results . . . . . . . . . . . . Yes Record
All results . . . . . . . . . . . . Yes
33
METTLER TOLEDO M091
Determination of Hydroxyl Value

Determination of hydroxyl value according to DIN 53240
Sample Trimethylolpropane Preparation and Procedures

(3-ethyl-2-(Hydroxymethyl)-1,3-propan The sample is dissolved in a mixture of 25 mL catalyst solution
ediol) and 3 mL acetylation mixture. The acetylation mixture can be
added either by pipette/dosing unit, or using a burette.
Substance Hydroxyl groups
Catalyst solution:
12 g 4-Dimethylaminopyridine in 1 L DMF
(DMF = N,N-Dimethylformamide),
Chemicals Catalyst solution: Acetylation mixture:
see preparation and procedures 250 mL acetic acid anhydride with 770 mL DMF
Acetylation mixture:
see preparation and procedures 1) The acetylation reaction is catalysed by 4-dimethyl amine
pyridine. This reaction takes place during the first stirring
Titrant Potassium hydroxide in methanol, function. The stirring time must be adapted to the speed of
c(KOH) = 0.5 mol/L acetylation reaction. The dosing precision of the acetylation
mixture also determines the overall accuracy of the analysis.
(A second burette is used for water)
Note: Water affects acetylation reaction.
Standard KHP 2) After completion of acetylation water is addded to the sample

mixture to hydrolize excess of acetic acid anhydride which is not
Instruments DL70ES/77, used for the acetylation. The reaction time is defined in the
second stirring function.
DL55+, DL58
3) As a result, acetic acid is formed which is then back-titrated
with methanolic KOH solution.
Accessories AT261 Balance, printer
DL55/58, DL70ES/77:
two additional burettes, ev. 1 DU200
Remarks
Indication DG113-SC The hydroxyl value is a reference number used to characterize
polyoles. It is expressed as the amount of KOH in mg to
neutralize the consumed equivalent amount of acetic acid used
Chemistry Acetylation: for the acetylation of 1 g of sample.
Two titration methods are used in this analysis: a blank and a

sample titration. The blank value is stored as auxiliary value
H13 in the titrator.
Calculation Blank (Method 091B):

Literature:
R1 = Q1 ; mmol 1. DIN 53240, ASTM 2849
Stored as auxiliary value H13 (without refluxing at elevated temperature of sample/mixture
solution).
Hydroxyl value (Method 091A):
R1 = (H13-Q)*(C1/m)
C1 = 56.1 ; mg KOH/g
Results
Waste Aromatic organic solvents

disposal
34
Results
DL67 (1) Market Support Laboratory
Method 091A Hydroxyl Number, Sample 20-Jul-1994 11:32

User K.M.
Measured 20-Jul-1994 17:41
RESULTS
1/1 Sample 3779 0.5006 g Weight m

R1 = 536.64 mg KOH/g Hydroxyl No.
STATISTICS
Mean value x = 631.01 mg KOH/gHydroxyl No.
Standard deviation s = 50.94823 mg KOH/gHydroxyl No.
Outlier test : sample No. 1/1, 1/6

Mean value x = 660.29 mg KOH/gHydroxyl No.
Standard deviation s = 6.502444 mg KOH/gHydroxyl No.
35
Method
Method 091A Hydroxyl Number, Sample Method 091B Hydroxyl number, Blank
Version 20-Jul-1994 11:32 Version 23-Jun-1994 8:35
Title Title
Title . . . . . . . . . . . . . . . Hydroxyl Number, Title . . . . . . . . . . . . . . . Hydroxyl number,
Sample Blank
Date/time . . . . . . . . . . . . . 20-Jul-1994 11:32 Date/time . . . . . . . . . . . . . 23-Jun-1994 8:35
Sample Sample
Upper limit [g] . . . . . . . . . 20.0 ID1 . . . . . . . . . . . . . . . . Blank
ID1 . . . . . . . . . . . . . . . . Sample Molar mass M . . . . . . . . . . . . 0.0
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 900
Time [s] . . . . . . . . . . . . . . 900 Dispense
Dispense Titrant . . . . . . . . . . . . . . Deionised water
Titrant . . . . . . . . . . . . . . Deionised water Concentration [mol/L] . . . . . . . 1.0
Concentration [mol/L] . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . . 10.0
Volume [mL] . . . . . . . . . . . . 10.0 Stir
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 300
Time [s] . . . . . . . . . . . . . . 300 Titration
Titration Titrant . . . . . . . . . . . . . . KOH (MeOH)
Titrant . . . . . . . . . . . . . . KOH (MeOH) Concentration [mol/L] . . . . . . . 0.5
Titrant addition . . . . . . . . DYN Volume [mL] . . . . . . . . . 20.0
dE(set) [mV] . . . . . . . . . 8.0 Titrant addition . . . . . . . . DYN
Limits dV . . . . . . . . . . Absolute dE(set) [mV] . . . . . . . . . 8.0
dV(min) [mL] . . . . . . . 0.02 Limits dV . . . . . . . . . . Absolute
dV(max) [mL] . . . . . . . 0.5 dV(min) [mL] . . . . . . . 0.02
Measure mode . . . . . . . . . . EQU dV(max) [mL] . . . . . . . 0.5
dE [mV] . . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . EQU
dt [s] . . . . . . . . . . . 1.0 dE [mV] . . . . . . . . . . . 0.5
t(min) [s] . . . . . . . . . . 3.0 dt [s] . . . . . . . . . . . 1.0
t(max) [s] . . . . . . . . . . 15.0 t(min) [s] . . . . . . . . . . 3.0
Threshold . . . . . . . . . . . . 250.0 t(max) [s] . . . . . . . . . . 15.0
EQP range . . . . . . . . . . . . Yes Threshold . . . . . . . . . . . . 500.0
Limit A . . . . . . . . . . . 0 EQP range . . . . . . . . . . . . Yes
Limit B . . . . . . . . . . . -600 Limit A . . . . . . . . . . . 0
Maximum volume [mL] . . . . . . . 50.0 Limit B . . . . . . . . . . . -600
Termination after n EQPs . . . . Yes Maximum volume [mL] . . . . . . . 50.0
n = . . . . . . . . . . . . . 1 Termination after n EQPs . . . . Yes
Evaluation procedure . . . . . . Standard n = . . . . . . . . . . . . . 1
Calculation Evaluation procedure . . . . . . Standard
Result name . . . . . . . . . . . . Hydroxyl No. Calculation
Formula . . . . . . . . . . . . . . R1=(H13-Q1)*(C1/m) Result name . . . . . . . . . . . . Blank
Constant . . . . . . . . . . . . . . C1=56.1 Formula . . . . . . . . . . . . . . R1=Q1
Result unit . . . . . . . . . . . . mg KOH/g Constant . . . . . . . . . . . . . .
Record Decimal places . . . . . . . . . . . 2
Results last sample . . . . . . . . Yes Output unit . . . . . . . . . . . . Printer
Table of values . . . . . . . . . . Yes Results last sample . . . . . . . . Yes
E - V curve . . . . . . . . . . . . Yes Table of values . . . . . . . . . . Yes
Statistics E - V curve . . . . . . . . . . . . Yes
Ri (i=index) . . . . . . . . . . . . R1 Statistics
Standard deviation s . . . . . . . . Yes Ri (i=index) . . . . . . . . . . . . R1
Rel. standard deviation srel . . . . Yes Standard deviation s . . . . . . . . Yes
Outlier test . . . . . . . . . . . . Yes Rel. standard deviation srel . . . . Yes
Record Outlier test . . . . . . . . . . . . Yes
Output unit . . . . . . . . . . . . Printer Auxiliary value
All results . . . . . . . . . . . . Yes ID text . . . . . . . . . . . . . . Blank (acetylation)
Formula . . . . . . . . . . . . . . H13=x
Record
All results . . . . . . . . . . . . Yes
36
METTLER TOLEDO M234
Hydroxyl Value of Polyols

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

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

DL70ES, DL77

Printer
Balance
Remarks
Indication DG113-SC Two titration methods are used:
1) Method BlOH allows the determination of the solvent blank

Chemistry value which is automatically stored as auxiliary value H14.
2) Method OH allows the determination of the hydroxide value

in polyols.
Calculation Blank determination (Method BlOH):

R1 = Q
Acid value det. (Method OH):

R1 = (Q1 - H14)*C1/m
C1 = 56.1
Results
Literature:
Waste ASTM D2474 (see www.astm.org)
Aromatic organic solvents
disposal
Author Ch. Walter, K. Racman
37
Results
*114* Market Support Laboratory
Method OH Hydr. Value Polyol Ester 31-Jul-1994 13:16

User
RESULTS
1/1 1.5022 g Weight m

R1 = 1.132 mg KOH/g Hydr. Value
1/2 1.8042 g Weight m
1/3 1.7529 g Weight m
STATISTICS
Mean value x = 1.143 mg KOH/gHydr. Value
Standard deviation s = 0.011567 mg KOH/gHydr. Value
38
Method
Method OH Hydr. Value Polyol Ester Method BlOH Blank Hydr. Value Polyol
Version 31-Jul-1994 13:16 Version 31-Jul-1994 12:27
Title Title
Method ID . . . . . . . . . . . . . OH Method ID . . . . . . . . . . . . . BlOH
Title . . . . . . . . . . . . . . . Hydr. Value Polyol Title . . . . . . . . . . . . . . . Blank Hydr. Value
Ester Polyol
Date/time . . . . . . . . . . . . . 31-Jul-1994 13:16 Date/time . . . . . . . . . . . . . 31-Jul-1994 12:27
Sample Sample
Upper limit [g] . . . . . . . . . 6.0 ID1 . . . . . . . . . . . . . . . .
ID1 . . . . . . . . . . . . . . . . Molar mass M . . . . . . . . . . . . 100.0
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 100 Time [s] . . . . . . . . . . . . . . 10
Time [s] . . . . . . . . . . . . . . 200 Titration
Titration Titrant . . . . . . . . . . . . . . KOH
Titrant . . . . . . . . . . . . . . KOH Concentration [mol/L] . . . . . . . 0.05
Titration mode . . . . . . . . . . . EQP Titrant addition . . . . . . . . INC
Predispensing 1 . . . . . . . . . mL ∆V [mL] . . . . . . . . . . . 0.01
Volume [mL] . . . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU
Titrant addition . . . . . . . . INC dE [mV] . . . . . . . . . . . 0.5
∆V [mL] . . . . . . . . . . . 0.025 dt [s] . . . . . . . . . . . 1.0
Measure mode . . . . . . . . . . EQU t(min) [s] . . . . . . . . . . 3.0
dE [mV] . . . . . . . . . . . 0.5 t(max) [s] . . . . . . . . . . 30.0
dt [s] . . . . . . . . . . . 1.0 Threshold . . . . . . . . . . . . 100
t(min) [s] . . . . . . . . . . 3.0 Maximum volume [mL] . . . . . . . 3.0
t(max) [s] . . . . . . . . . . 30.0 Termination after n EQPs . . . . Yes
Threshold . . . . . . . . . . . . 700 n = . . . . . . . . . . . . . 1
Maximum volume [mL] . . . . . . . 2.0 Evaluation procedure . . . . . . Standard
Result name . . . . . . . . . . . . Hydr. Value Formula . . . . . . . . . . . . . . R=Q
Constant . . . . . . . . . . . . . . C1=56.1 Result unit . . . . . . . . . . . . mmol
Result unit . . . . . . . . . . . . mg KOH/g Decimal places . . . . . . . . . . . 3
Record Ri (i=index) . . . . . . . . . . . . R1
Output unit . . . . . . . . . . . . Printer Standard deviation s . . . . . . . . Yes
Results last sample . . . . . . . . Yes Rel. standard deviation srel . . . . Yes
Table of values . . . . . . . . . . Yes Auxiliary value
E - V curve . . . . . . . . . . . . Yes ID text . . . . . . . . . . . . . . Blank
Statistics Formula . . . . . . . . . . . . . . H14=x
Ri (i=index) . . . . . . . . . . . . R1 Record
Standard deviation s . . . . . . . . Yes Output unit . . . . . . . . . . . . Printer
Rel. standard deviation srel . . . . Yes All results . . . . . . . . . . . . Yes
Outlier test . . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes
Record
All results . . . . . . . . . . . . Yes
39
METTLER TOLEDO M095
Determination of Isocyanate Content

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

1) Dissolve the sample in 25 mL monochlorobenzene and 20
mL methylethylketone.
2) Add manually 10 mL 2 mol/L diisobutylamine in

Substance Isocyanate groups, -NCO
chlorobenzene or by means of an additional burette or a DU200
Dispensing unit.
Chemicals 25 mL monochlorobenzene 3) Start back titration of excess diisobutylamine with

10 mL diisobutylamine in Cl-benzene hydrochloric acid.
20 mL methylethlyketone
Note:
Isocyanates are toxic compounds. Appropriate working
Titrant Hydrochloric acid, HCl, in methanol condictions are needed (fumehood, gloves, googles).
c(HCl) = 1 mol/L
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
Standard THAM sample. If this is not the case, the mixture can be heated using
a thermostatable beaker with a reflux condenser. The sample
Instruments DL50Graphix, DL53/55/58 solution should not be overheated since diisobutylamine might
decompose. If the sample solution becomes turbid, a more
DL70ES, DL77
diluted solution in a larger titraiton vessel must be used.
Auxiliary solvents (depending on the sample):

Accessories Glass titration beaker ME-101446 methylethylketone,methanol, ethanol, acetone
Printer, balance
Complete automation: additional burette
DV1010, or use a DU200 Dosing unit.
Remarks
Indication DG113-SC 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
Chemistry R-NCO + NH(iBu)2 = (iBu)2N-CO-NHR diisobutylamine is added to the non-aqueous sample solution.
Diisobutylamine reacts with isocyanate groups during the
stirring time of 300 s. Unreacted diisobutylamine is
NH(iBu)2 + HCl = (H2N(iBu)2)+ Cl-
subsequently titrated with hydrochloric acid.
Two titration methods are used:

1) Method 095B allows the determination of the solvent blank
Calculation value which is automatically stored as auxiliary value H15.
Blank determination (Method 095B):
2) Method 095A allows the determination of the isocyanate
R1 = Q content.
Hints:
Acid value det. (Method 095A): 1) Rinse accurately the electrode, the stirrer and the burette tip
R1 = (H15-Q1)*C1/m with e.g. acetone at the end of the titration series.
C1 = M/(10*z) 2) The DG113 electrode should be conditioned in pH buffer 7
Results over night to hydrate the pH glass membrane.
Waste Isocyanates solution: special waste Literature:

disposal Aromatic organic solvents DIN 53185, 16945 (see www.din.de)
See also ASTM D1638 (www.astm.org)
40
Results
DL67(1) Market Support Laboratory
Method 095A Isocyanate:Sample Titr. 17-Aug-1994 16:03

User
Measured 18-Aug-1994 13:53
RESULTS
1/1 NCO 4594 4.0 g Weight m

R1 = 9.881 % NCO Isocyanate
STATISTICS
Mean value x = 12.460 % NCO Isocyanate
Standard deviation s = 1.137420 % NCO Isocyanate

Mean value x = 12.890 % NCO Isocyanate
Standard deviation s = 0.010834 % NCO Isocyanate
41
Method
Method 095A Isocyanate:Sample Titr. Method 095B Isocyanate:Blank Determin.
Version 17-Aug-1994 16:03 Version 17-Aug-1994 16:03
Title Title
Title . . . . . . . . . . . . . . . Isocyanate:Sample Titr. Title . . . . . . . . . . . . . . . Isocyanate:Blank
Date/time . . . . . . . . . . . . . 17-Aug-1994 16:03 Determin.
Sample Date/time . . . . . . . . . . . . . 17-Aug-1994 16:03
Number samples . . . . . . . . . . . 7 Sample
Titration stand . . . . . . . . . . Stand 1 Number samples . . . . . . . . . . . 4
Entry type . . . . . . . . . . . . . Weight m Titration stand . . . . . . . . . . Stand 1
Lower limit [g] . . . . . . . . . 0.0 Entry type . . . . . . . . . . . . . Fixed volume U
Upper limit [g] . . . . . . . . . 10.0 Volume [mL] . . . . . . . . . . . 10.0
ID1 . . . . . . . . . . . . . . . . NCO ID1 . . . . . . . . . . . . . . . . Reagent
Temperature sensor . . . . . . . . . Manual Temperature sensor . . . . . . . . . Manual
Dispense Dispense
Titrant . . . . . . . . . . . . . . Dibutylamine Titrant . . . . . . . . . . . . . . Dibutylamine
Volume [mL] . . . . . . . . . . . . 10.0 Volume [mL] . . . . . . . . . . . . 10.0
Stir Stir
Speed [%] . . . . . . . . . . . . . 50 Speed [%] . . . . . . . . . . . . . 50
Time [s] . . . . . . . . . . . . . . 300 Time [s] . . . . . . . . . . . . . . 300
Titration Titration
Titrant . . . . . . . . . . . . . . HCl (MeOH) Titrant . . . . . . . . . . . . . . HCl (MeOH)
Predispensing 1 . . . . . . . . . mL Predispensing 1 . . . . . . . . . mL
Volume [mL] . . . . . . . . . 1.0 Volume [mL] . . . . . . . . . 17.5
Titrant addition . . . . . . . . DYN Titrant addition . . . . . . . . DYN
∆E(set) [mV] . . . . . . . . . 8.0 ∆E(set) [mV] . . . . . . . . . 8.0
Limits ∆V . . . . . . . . . . Absolute Limits ∆V . . . . . . . . . . Absolute
∆V(min) [mL] . . . . . . . 0.02 ∆V(min) [mL] . . . . . . . 0.02
∆V(max) [mL] . . . . . . . 0.2 ∆V(max) [mL] . . . . . . . 0.2
Measure mode . . . . . . . . . . EQU Measure mode . . . . . . . . . . EQU
dE [mV] . . . . . . . . . . . 0.5 dE [mV] . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . 1.0 dt [s] . . . . . . . . . . . 1.0
t(min) [s] . . . . . . . . . . 3.0 t(min) [s] . . . . . . . . . . 3.0
t(max) [s] . . . . . . . . . . 20.0 t(max) [s] . . . . . . . . . . 20.0
EQP range . . . . . . . . . . . . Yes EQP range . . . . . . . . . . . . Yes
Limit A . . . . . . . . . . . -500 Limit A . . . . . . . . . . . -500
Limit B . . . . . . . . . . . +500 Limit B . . . . . . . . . . . +500
Termination after n EQPs . . . . Yes Termination after n EQPs . . . . Yes
n = . . . . . . . . . . . . . 1 n = . . . . . . . . . . . . . 1
Evaluation procedure . . . . . . Standard Evaluation procedure . . . . . . Standard
Result name . . . . . . . . . . . . Isocyanate Result name . . . . . . . . . . . . Isocyan.Blank
Formula . . . . . . . . . . . . . . R1=(H15-Q)*C1/m Formula . . . . . . . . . . . . . . R=Q
Constant . . . . . . . . . . . . . . C1=M/(10*z) Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . % NCO Result unit . . . . . . . . . . . . mmol
Record Record
Output unit . . . . . . . . . . . . Printer Output unit . . . . . . . . . . . . Printer
Results last sample . . . . . . . . Yes Results last sample . . . . . . . . Yes
Table of values . . . . . . . . . . Yes Table of values . . . . . . . . . . Yes
E - V curve . . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes
Statistics Statistics
Ri (i=index) . . . . . . . . . . . . R1 Ri (i=index) . . . . . . . . . . . . R1
Standard deviation s . . . . . . . . Yes Standard deviation s . . . . . . . . Yes
Rel. standard deviation srel . . . . Yes Rel. standard deviation srel . . . . Yes
Outlier test . . . . . . . . . . . . Yes Outlier test . . . . . . . . . . . . Yes
Record Auxiliary value
Output unit . . . . . . . . . . . . Printer ID text . . . . . . . . . . . . . . Blank Isocyanate val
All results . . . . . . . . . . . . Yes Formula . . . . . . . . . . . . . . H15=x
Record
All results . . . . . . . . . . . . Yes
42
METTLER TOLEDO M235
NCO-Content of Isocyanates by Backtitration

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

0.5 g 1) Dissolve the sample in 20 mL methylethylketone.
2) Add manually 10 mL 2 mol/L diisobutylamine in isopro-

panol or by means of an additional burette or a DU200 unit.
Substance Isocyanate groups, -NCO
3) Add 50 mL isopropanol by means of an additional burette or
by using a peristaltic pump.
Chemicals 20 mL methylethlyketone
10 mL diisobutylamine in isopropanol 4) Start back titration of excess diisobutylamine with HCl.
50 mL isopropanol
Note:
Titrant Hydrochloric acid, HCl, in isopropanol condictions are needed (fumehood, gloves, googles).
c(HCl) = 1 mol/L
The stirring time must be long enough to ensure complete
dissolution and reaction of the sample before the back titration
starts.
Standard THAM
Acidic or basic compounds in the sample interfere.
Instead of diisobutylamine also di-n-butylamine can be used as
DL70ES, DL77
a reagent. Toluene can also serve as an alternative solvent for
the sample as well as for the titrant.
Accessories Glass titration beaker ME-101446 Use dried solvents and reagents.
Printer, balance
Complete automation: two add. burettes
DV1010, or use a DU200 Dosing unit.
Remarks
Indication DG113-SC 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
Chemistry R-NCO + NH(iBu)2 = (iBu)2N-CO-NHR diisobutylamine is added to the non-aqueous sample solution.
Diisobutylamine reacts with isocyanate groups during the
stirring time of 240 s. Unreacted diisobutylamine is
NH(iBu)2 + HCl = (H2N(iBu)2)+ Cl-
subsequently titrated with hydrochloric acid.

1) Method NCOB allows the determination of the solvent blank
Calculation value which is automatically stored as auxiliary value H16.
Blank determination (Method NCOB):
2) Method NCO allows the determination of the isocyanate
R1 = Q content.
Hints:
Acid value det. (Method NCO): 1) Rinse accurately the electrode, the stirrer and the burette tip
R1 = (H16-Q1)*C1/m with e.g. acetone at the end of the titration series.
C1 = M/(10*z) 2) The DG113 electrode should be conditioned in pH buffer 7
Results over night to hydrate the pH glass membrane.
Waste Isocyanates solution: special waste Literature:

disposal Aromatic organic solvents ASTM D1638 (www.astm.org)
DL40RC Application No. 163
43
Results
DL40RC:
*** 28-JAN-86 ***
INPUT:
WEIGHT .5203
IDENT. 12.51
METHOD 1631 2823

IDENT. 12.51
SAMPLE NO. 1
*R * % 32.718
STATISTICS:
N 6
MEAN 32.823
STAND.DEV.% 0.29
44
Method
Method NCO Isocyanate Method NCOB Isocyanate:Blank
Version 31-Jan-1994 14:30 Version 31-Jan-1994 14:32
Title Title
Method ID . . . . . . . . . . . . . NCO Method ID . . . . . . . . . . . . . NCOB
Title . . . . . . . . . . . . . . . Isocyanate Title . . . . . . . . . . . . . . . Isocyanate:Blank
Date/time . . . . . . . . . . . . . 31-Jan-1994 14:30 Date/time . . . . . . . . . . . . . 31-Jan-1994 14:32
Sample Sample
Upper limit [g] . . . . . . . . . 0.5 ID1 . . . . . . . . . . . . . . . . Reagent
ID1 . . . . . . . . . . . . . . . . NCO Molar mass M . . . . . . . . . . . . 129.25
Equivalent number z . . . . . . . . 1 Temperature sensor . . . . . . . . . Manual
Temperature sensor . . . . . . . . . Manual Dispense
Dispense Titrant . . . . . . . . . . . . . . Dibutylamine
Titrant . . . . . . . . . . . . . . Dibutylamine Concentration [mol/L] . . . . . . . 2.0
Volume [mL] . . . . . . . . . . . . 10.0 Stir
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 300
Time [s] . . . . . . . . . . . . . . 300 Dispense
Dispense Titrant . . . . . . . . . . . . . . Isopropanol
Titrant . . . . . . . . . . . . . . Isopropanol Concentration [mol/L] . . . . . . . 1.0
Volume [mL] . . . . . . . . . . . . 50.0 Stir
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10
Time [s] . . . . . . . . . . . . . . 10 Titration
Titration Titrant . . . . . . . . . . . . . . HCl (MeOH)
Titrant . . . . . . . . . . . . . . HCl (IPA) Concentration [mol/L] . . . . . . . 1.0
Predispensing 1 . . . . . . . . . mL Volume [mL] . . . . . . . . . 17.5
Volume [mL] . . . . . . . . . 1.0 Titrant addition . . . . . . . . DYN
Titrant addition . . . . . . . . DYN ∆E(set) [mV] . . . . . . . . . 8.0
∆E(set) [mV] . . . . . . . . . 8.0 Limits ∆V . . . . . . . . . . Absolute
Limits ∆V . . . . . . . . . . Absolute ∆V(min) [mL] . . . . . . . 0.02
∆V(min) [mL] . . . . . . . 0.02 ∆V(max) [mL] . . . . . . . 0.2
∆V(max) [mL] . . . . . . . 0.2 Measure mode . . . . . . . . . . EQU
Measure mode . . . . . . . . . . EQU dE [mV] . . . . . . . . . . . 1.0
dE [mV] . . . . . . . . . . . 1.0 dt [s] . . . . . . . . . . . 2.0
dt [s] . . . . . . . . . . . 2.0 t(min) [s] . . . . . . . . . . 3.0
t(min) [s] . . . . . . . . . . 3.0 t(max) [s] . . . . . . . . . . 20.0
t(max) [s] . . . . . . . . . . 20.0 Threshold . . . . . . . . . . . . 500
Threshold . . . . . . . . . . . . 500 EQP range . . . . . . . . . . . . Yes
EQP range . . . . . . . . . . . . Yes Limit A . . . . . . . . . . . -500
Limit A . . . . . . . . . . . -500 Limit B . . . . . . . . . . . +500
Limit B . . . . . . . . . . . +500 Maximum volume [mL] . . . . . . . 30.0
Maximum volume [mL] . . . . . . . 25.0 Termination after n EQPs . . . . Yes
Termination after n EQPs . . . . Yes n = . . . . . . . . . . . . . 1
n = . . . . . . . . . . . . . 1 Evaluation procedure . . . . . . Standard
Calculation Result name . . . . . . . . . . . . Isocyan.Blank
Result name . . . . . . . . . . . . Isocyanate Formula . . . . . . . . . . . . . . R=Q
Formula . . . . . . . . . . . . . . R1=(H16-Q)*C1/m Constant . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . . C1=M/(10*z) Result unit . . . . . . . . . . . . mmol
Result unit . . . . . . . . . . . . % NCO Decimal places . . . . . . . . . . . 3
Results last sample . . . . . . . . Yes Table of values . . . . . . . . . . Yes
Table of values . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes
Statistics Ri (i=index) . . . . . . . . . . . . R1
Ri (i=index) . . . . . . . . . . . . R1 Standard deviation s . . . . . . . . Yes
Standard deviation s . . . . . . . . Yes Rel. standard deviation srel . . . . Yes
Rel. standard deviation srel . . . . Yes Outlier test . . . . . . . . . . . . Yes
Outlier test . . . . . . . . . . . . Yes Auxiliary value
Record ID text . . . . . . . . . . . . . . Blank Isocyanate val
Output unit . . . . . . . . . . . . Printer Formula . . . . . . . . . . . . . . H16=x
All results . . . . . . . . . . . . Yes Record
All results . . . . . . . . . . . . Yes
45
METTLER TOLEDO M236
Determination of Free HCl and Isocyanates

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

1) Dissolve the sample in 40 mL methanol.
2) Start titration with sodium hydroxide.

Substance Free HCl and isocyanate groups, -NCO
Note:
Chemicals 40 mL methanol condictions are needed (fumehood, gloves, googles).
The titrant must be protected from CO2-intake from the air.
Titrant Sodium hydroxide, NaOH, in methanol

c(NaOH) = 0.1 mol/L
Standard KHP

DL70ES, DL77
Accessories Glass titration beaker ME-101446

Printer, balance
Remarks
Indication DG113-SC Hints:
1) The DG113 electrode should be conditioned in pH buffer 7
over night to hydrate the pH glass membrane.
Chemistry HCl + NaOH = H2O + NaCl
2) Clean the electrode and the stirrer after each sample titration
with eg. methanol.
R-NCO + NaOH = ??
Calculation Free HCl content:

R1 = Q1*C1/m ; %
C1 = 36.5/(10*z)
Isocyanate content:
R2 = Q2*C2/m ; %
C2 = M/(10*z)
Results
Waste Isocyanates solution: special waste

disposal Organic solvents
Author Roland Boehlen, MT-CH
46
Results
METTLER DL70 Titrator
7 Free HCl and Isocyanate measured 26-Oct-1992 12:38

26-Oct-1992 12:09 Titrator
SW Version 2.0 User BR****
SAMPLE
Nr. 1/1
Titration stand Stand 1
Identification R-N:C:O
Weight m = 0.5654 g
Correction factor f = 1.0
TITRATION
Titrant NaOH 0.1 mol/L t = 1.0
Concentration Drive 2 20 mL
Sensor DG113-SC
Consumption EQP 1 VEQ1 = 0.42703 mL

Q1 = 0.04270 mmol
EPOT1 = 423.4 mV
Consumption EQP 2 VEQ2 = 6.25668 mL
Q2 = 0.62567 mmol
EPOT2 = -318.8 mV
Excess VEX = 0.02829 mL
QEX = 0.00283 mmol
CALCULATION
Result R1 = 0.28 % Free HCl
CALCULATION
Result R2 = 28.94 % R-N:C:O
47
Method
Method 7 Free HCl and Isocyanate
Version 26-Oct-1992 12:09
Title
Method ID . . . . . . . . . . . . . 7
Title . . . . . . . . . . . . . . . Free HCl and Isocyanate
Date/time . . . . . . . . . . . . . 26-Oct-1992 12:09
Sample
Number samples . . . . . . . . . . . 1
Titration stand . . . . . . . . . . Stand 1
Entry type . . . . . . . . . . . . . Weight m
Lower limit [g] . . . . . . . . . 0.4
Upper limit [g] . . . . . . . . . 0.6
ID1 . . . . . . . . . . . . . . . . R-N:C:O
Molar mass M . . . . . . . . . . . . 261.5
Equivalent number z . . . . . . . . 1
Stir
Speed [%] . . . . . . . . . . . . . 50
Time [s] . . . . . . . . . . . . . . 100
Titration
Titrant . . . . . . . . . . . . . . NaOH
Concentration [mol/L] . . . . . . . 0.1
Sensor . . . . . . . . . . . . . . . DG113-SC
Unit of meas. . . . . . . . . . . . mV
Titration mode . . . . . . . . . . . EQP
Titrant addition . . . . . . . . DYN
∆E(set) [mV] . . . . . . . . . 8.0
Limits ∆V . . . . . . . . . . Absolute
∆V(min) [mL] . . . . . . . 0.02
∆V(max) [mL] . . . . . . . 0.5
Measure mode . . . . . . . . . . EQU
dE [mV] . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . 1.0
t(min) [s] . . . . . . . . . . 1.0
t(max) [s] . . . . . . . . . . 30.0
Threshold . . . . . . . . . . . . 500
Maximum volume [mL] . . . . . . . 25.0
Termination after n EQPs . . . . Yes
n = . . . . . . . . . . . . . 2
Evaluation procedure . . . . . . Standard
Calculation
Result name . . . . . . . . . . . . Free HCl
Formula . . . . . . . . . . . . . . R1=Q1*C1/m
Constant . . . . . . . . . . . . . . C1=36.5/(10*z)
Result unit . . . . . . . . . . . . %
Decimal places . . . . . . . . . . . 2
Calculation
Result name . . . . . . . . . . . . R-N:C:O
Formula . . . . . . . . . . . . . . R2=Q2*C2/m
Constant . . . . . . . . . . . . . . C2=M/(10*z)
Result unit . . . . . . . . . . . . %
Decimal places . . . . . . . . . . . 2
Record
Results last sample . . . . . . . . Yes
E - V curve . . . . . . . . . . . . Yes
Statistics
Ri (i=index) . . . . . . . . . . . . R1
Outlier test . . . . . . . . . . . . Yes
Record
All results . . . . . . . . . . . . Yes
48
METTLER TOLEDO M096
Iodine Value in Resins and Oils According to Wijs

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

1) The sample is dissolved in 10 mL solvent mixture consisting
of glacial acetic acid:cyclohexane 1:4 .
2) 15 mL Wijs solution are added automatically by a DV1020

Substance Carbon-carbon double bons, -CH=CH-
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.
Chemicals 10 mL Glacial acetic acid:Cyclohexane 1:4
15 mL, Wijs-sol.: with ICl, c(ICl) = 0.1 M 3) The function "Conditioning" is used to allow the sample
5 mL , Potassium iodide, KI, c(KI) = 1 mol/L solution to react completely during 1000 s. If the time is not
20 mL, deionized water enough, then the reaction time can be increased by repeatinmg
the function "Conditioning" (loop).
Titrant Sodium thiosulfate, Na2S2O3
4) 5 mL potassium iodide are added by a second burette, and
c(Na2S2O3)=0.1 mol/L
the second diaphragm pump adds 20 mL deionized water.
5) Excess iodine is back-titrated using sodium iodine. The

Standard Potassium iodate, KIO3 (see M526) electrode is rinsed with 10 mL ethanol.
Instruments DL70ES, DL77

Rondo 60 with two diaphragm pumps,
Printer, balance
two additional burettes DV1020
Remarks
Indication DM140-SC 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
Chemistry I2 + -CH=CH- = -CHI-IHC- bonds). It indicates the degree of unsaturation of the sample.

I2 + 2S2O32- = S4O62- + 2I-
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.
Calculation Blank determination (Method 096B):
Hints:
R1 = Q 1) The sample must be completely dissolved before addition of
R1 is stored as auxiliary value H17 Wijs redution. The stirring time must be selected accordingly. If
necessary, a ultrasonic bath can be used to dissolve sample.
Iodine value det. (Method 096A): 2) The composition of the solvent mixture must be adapted to
R1 = (H17-Q1)*C1/m the sample. In this case, the most appropriate solvent is a
C1 = M/(10*z) mixture fo glacial acetic acid and cyclohexane.
Results 3) The appropriate stirring speed for the back titration must be
chosen to get an homogeneous phase system.
Waste Organic solvents
disposal Literature:
DIN 53241 (www.din.de)
Application M051
49
Results
1/1 Dammar Resin 25.0 mL Fixed volume U

R1 = 1 LOOP
..........................................................
R1 = 1 LOOP
R1 = 1 LOOP
R1 = 1 LOOP
2/1 Dammar Resin 0.275 g Weight m
R2 = 79.81 g I2/100g Iodine number
STATISTICS
Mean value x = 1 LOOP
STATISTICS
Mean value x = 73.64 g I2/100g Iodine number
Standard deviation s = 2.852742 g I2/100g Iodine number
Mean value x = 72.62 g I2/100g Iodine number
Standard deviation s = 0.942869 g I2/100g Iodine number
Weitere Resultate:
Sample Mass (g) n x (g/100g) srel (%) Time (min)
Kolophonium 0.41 7 60.59 0.66 4

Dammharz 0.275 6 72.62 1.30 6
Lärchenöl 0.2326 7 101.62 0.85 4
Leinöl 0.1008 4 176.10 0.56 5
Blank value H17 5 2.9417 mmol 0.04 4
50
Method
Method 096A Wijs Iodine Number Titration
Version 10-May-1994 9:45 Titrant . . . . . . . . . . . . . . Na2S2O3
Title Sensor . . . . . . . . . . . . . . . DM140-SC
Method ID . . . . . . . . . . . . . 096A Unit of meas. . . . . . . . . . . . mV
Title . . . . . . . . . . . . . . . Wijs Iodine Value Titration mode . . . . . . . . . . . EQP
Date/time . . . . . . . . . . . . . 10-May-1994 9:45 Predispensing 1 . . . . . . . . . mL
Sample Volume [mL] . . . . . . . . . 1.0
Number samples . . . . . . . . . . . 7 Titrant addition . . . . . . . . DYN
Titration stand . . . . . . . . . . ST20 1 ∆E(set) [mV] . . . . . . . . . 8.0
Entry type . . . . . . . . . . . . . Weight m Limits ∆V . . . . . . . . . . Absolute
Lower limit [g] . . . . . . . . . 0.0
Upper limit [g] . . . . . . . . . 10.0 ∆V(min) [mL] . . . . . . . 0.02
ID1 . . . . . . . . . . . . . . . . Polymer ∆V(max) [mL] . . . . . . . 0.4
Molar mass M . . . . . . . . . . . . 254 Measure mode . . . . . . . . . . EQU
Equivalent number z . . . . . . . . 2 dE [mV] . . . . . . . . . . . 1.0
Temperature sensor . . . . . . . . . Manual dt [s] . . . . . . . . . . . 1.0
Dispense t(min) [s] . . . . . . . . . . 6.0
Titrant . . . . . . . . . . . . . . Wijs solution t(max) [s] . . . . . . . . . . 30.0
Concentration [mol/L] . . . . . . . 0.1 Threshold . . . . . . . . . . . . 300
Volume [mL] . . . . . . . . . . . . 15.0 EQP range . . . . . . . . . . . . Yes
Stir Limit A . . . . . . . . . . . 1000
Speed [%] . . . . . . . . . . . . . 50 Limit B . . . . . . . . . . . -1000
Time [s] . . . . . . . . . . . . . . 60 Maximum volume [mL] . . . . . . . 50.0
Calculation Termination after n EQPs . . . . Yes
Result name . . . . . . . . . . . . LOOP n = . . . . . . . . . . . . . 1
Formula . . . . . . . . . . . . . . R1=1 Evaluation procedure . . . . . . Standard
Constant . . . . . . . . . . . . . . Calculation
Result unit . . . . . . . . . . . . Result name . . . . . . . . . . . . Iodine Number
Decimal places . . . . . . . . . . . 0 Formula . . . . . . . . . . . . . . R1=(H17-Q)*C1/m
Rinse Constant . . . . . . . . . . . . . . C1=M/(10*z)
Auxiliary reagent . . . . . . . . . Ethanol Result unit . . . . . . . . . . . . % NCO
Volume [mL] . . . . . . . . . . . . 10.0 Decimal places . . . . . . . . . . . 2
Statistics Condition . . . . . . . . . . . . . Yes
Ri (i=index) . . . . . . . . . . . . R1 Condition . . . . . . . . . . . . VEQ>0
Dispense Record
Titrant . . . . . . . . . . . . . . Isopropanol Output unit . . . . . . . . . . . . Printer
Concentration [mol/L] . . . . . . . 1.0 Results last sample . . . . . . . . Yes
Volume [mL] . . . . . . . . . . . . 50.0 Table of values . . . . . . . . . . Yes
Stir E - V curve . . . . . . . . . . . . Yes
Speed [%] . . . . . . . . . . . . . 0 Condition . . . . . . . . . . . . . Yes
Time [s] . . . . . . . . . . . . . . 0 Condition . . . . . . . . . . . . VEQ>0
Conditioning Record
Interval . . . . . . . . . . . . . . 1 Output unit . . . . . . . . . . . . Printer
Time [s] . . . . . . . . . . . . . . 1000 Results last sample . . . . . . . . Yes
Sample Table of values . . . . . . . . . . Yes
Number samples . . . . . . . . . . . 7 E - V curve . . . . . . . . . . . . Yes
Titration stand . . . . . . . . . . ST20 1 Condition . . . . . . . . . . . . . Yes
Entry type . . . . . . . . . . . . . Weight m Condition . . . . . . . . . . . . VEQ<=0
Lower limit [g] . . . . . . . . . 0.0 Rinse
Upper limit [g] . . . . . . . . . 10.0 Auxiliary reagent . . . . . . . . . Ethanol
ID1 . . . . . . . . . . . . . . . . Polymer Volume [mL] . . . . . . . . . . . . 10.0
Molar mass M . . . . . . . . . . . . 254 Statistics
Equivalent number z . . . . . . . . 2 Ri (i=index) . . . . . . . . . . . . R2
Temperature sensor . . . . . . . . . Manual Standard deviation s . . . . . . . . Yes
Dispense Rel. standard deviation srel . . . . Yes
Titrant . . . . . . . . . . . . . . KI (1) Outlier test . . . . . . . . . . . . Yes
Concentration [mol/L] . . . . . . . 1.0 Record
Volume [mL] . . . . . . . . . . . . 5.0 Output unit . . . . . . . . . . . . Printer
Pump All results . . . . . . . . . . . . Yes
Auxiliary reagent . . . . . . . . . H2O Conditioning
Volume [mL] . . . . . . . . . . . . 20.0 Interval . . . . . . . . . . . . . . 1
Stir Time [s] . . . . . . . . . . . . . . 60
Speed [%] . . . . . . . . . . . . . 70 Rinse . . . . . . . . . . . . . . . Yes
Time [s] . . . . . . . . . . . . . . 60 Auxiliary reagent . . . . . . . . H2O
Volume [mL] . . . . . . . . . . . 10.0
Blank Determination:
Method 096B is used for the blank determination and is similar
to method 096A. The blank value is stored as auxiliary value
H17 (function "Auxiliary value")
51
METTLER TOLEDO M051
Iodine Value of Edible Oils and Fats According to Wijs (AOAC Method
Method for the determination of iodine value (g I2/100g) of edible oils and fats according to Wijs as
indicated by AOAC Official Methods of Analysis (1984), Chapter 28.023
Sample Fats and oils, approx. 25 g / expected Preparation and Procedures

Iodine value 1) Dissolve the sample in CCl4, add 25 mL Wijs solution and
keep in the dark for approx. 1 hour to complete the reaction.
Substance C-C double bonds, -CH=CH- 2) Add deionized water and titrate excess iodine with sodium
thiosulphate.
Chemicals 15 mL carbon tetrachloride, CCl4 ; Wijs solution:

25 mL Wijs solution; 100mL water; Dissolve 16.2 g iodine monochloride (ICl) in a 1 L volumetric
15 mL 10% potassium iodide, KI flask with glacial acetic acid. Store the Wijs solution in amber
bottle sealed with paraffin until it is used.
Titrant Sodium thiosulphate, Na2S2O3 Wijs solution is sensitive to temperature, moisture and light.
c(Na2S2O3)=0.1 mol/L; Slight variations of the temperature considerably affect titer of the
Wijs solution. Therefore it is essential that blanks and samples
are titrated at same time.
Standard Potassium iodate, KIO3 The mean value of the blank determination (method 051b) is
automatically stored as auxiliary value H3.
Instruments DL70, AT250, Matrix printer EPSON Typical results:
FX800 with serial interface Blank = 4.94 mmol, srel = 0.04%, n = 5
Accessories 250 mL Titration beakers ME-23829,

Additional burette drive DV90
Remarks
Indication DM140-SC at Sensor 2 The iodine value is defined as the weight of iodine absorbed by
100 g of an oil or fat.
Chemistry ICl3 + I2 = 3 ICl 1) The excess of Wijs solution should be 50-60% of the
amount added, ie. 100-150% of amount reacted with the
sample.
ICl + KI = I2 + KCl
2) If the result will be assumed (e.g. in routinr quality control)
2(SO3S)2- + I2 = 2 I- + (S2O6S2)2- the predispensing can be adjusted accordingly in volume or
changed to % nominal content . This also shortens the titration
Calculation time.
Blank determination (Method 096B):
R1 = Q 3) The addition of 10 mL 2.5% mercury (II) acetate in glacial
R1 is stored as auxiliary value H3 acetic acid (after Wijs solution is added) shortens the reaction
time to 5 minutes
Iodine value det. (Method 096A):
R1 = (H3-Q1)*C1/m
C1 = M/(10*z)
Results Literature:
AOAC Official Method of Analysis, 1984, Chapter 28.023
Waste Halogenated organic solvent
disposal
Author Ruth von Rotz
52
Results
METTLER DL70 Titrator
051a I2-value of oils and fats
Measured 25-June-1991 3:37 pm

User rvr
Titrator PT 2
Version SW 2.0
RESULTS
No ID1 Weight Results
1/1 cocofat 2.0267 g 11.85 g I2/100 gI2-value
STATISTICS
Mean value x = 11.85 g I2/100 gI2-value
Standard deviation s = 0.013 g I2/100 gI2-value
Various Samples
Sample Weight n Iodine value RSD t

(g) (gI2/100g) (%) (min)
Coconut fat 2.00-2.10 5 11.8 0.11 5
Margarine
"light" 0.40-0.45 3 37.3 0.26 5
Lard 0.40-0.45 5 57.6 0.13 5
Olive oil 0.20-0.25 5 82.5 0.16 6
Margarine 0.50-0.55 3 86.1 0.21 3
Rape oil 0.20-0.25 4 113.4 0.15 5
Sunflower oil 0.20-0.25 3 132.7 0.06 4
53
Method
Method 051a I2 - value of oils and fats Method 051b Blank I2 - value
Version 19-June-1991 16:21 Version 19-June-1991 16:15
Title Title
Method ID . . . . . . . . . . . . . 051a Method ID . . . . . . . . . . . . . 051b
Title . . . . . . . . . . . . . . . I2 - value of oils and Title . . . . . . . . . . . . . . . Blank I2 - value
fats Date/time . . . . . . . . . . . . . 19-June-1991 16:15
Date/time . . . . . . . . . . . . . 19-June-1991 16:21 Sample
Sample Number samples . . . . . . . . . . . 3
Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1
Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U
Entry type . . . . . . . . . . . . . Weight m Volume [mL] . . . . . . . . . 25.0
Lower limit [g] . . . . . . . . . 0.02 ID1 . . . . . . . . . . . . . . . . Blank
ID1 . . . . . . . . . . . . . . . . Equivalent number z . . . . . . . . 1
Molar mass M . . . . . . . . . . . . 254 Dispense
Equivalent number z . . . . . . . . 2 Titrant . . . . . . . . . . . . . . KI 10%
Dispense Concentration [mol/L] . . . . . . . 10.0
Titrant . . . . . . . . . . . . . . KI 10% Volume [mL] . . . . . . . . . . . . 15.0
Concentration [mol/L] . . . . . . . 10.0 Stir
Volume [mL] . . . . . . . . . . . . 15.0 Speed [%] . . . . . . . . . . . . . 50
Stir Time [s] . . . . . . . . . . . . . . 45
Speed [%] . . . . . . . . . . . . . 50 Titration
Time [s] . . . . . . . . . . . . . . 45 Titrant . . . . . . . . . . . . . . Na2S2O3H2O
Titrant . . . . . . . . . . . . . . Na2S2O3H2O Sensor . . . . . . . . . . . . . . . DM140-SC
Sensor . . . . . . . . . . . . . . . DM140-SC Titration mode . . . . . . . . . . . EQP
Unit of meas. . . . . . . . . . . . mV Predispensing 1 . . . . . . . . . mL
Titration mode . . . . . . . . . . . EQP Volume [mL] . . . . . . 40.0
Predispensing 1 . . . . . . . . . mL Predispensing 2 . . . . . . . . . To slope
Volume [mL] . . . . . . 20.0 slope [mV,pH, .../mL] . . . . 4.0
Predispensing 2 . . . . . . . . . To slope Titrant addition . . . . . . . . DYN
slope [mV,pH, .../mL] . . . . 4.0 dE (set)[mV] . . . . . . . . . 4.0
Titrant addition . . . . . . . . DYN Limits dV . . . . . . . . . . Absolute
dE (set)[mV] . . . . . . . . . 0.02 dV(min) [mL] . . . . . . . 0.02
Limits dV . . . . . . . . . . Absolute dV(max) [mL] . . . . . . . 0.5
dV(min) [mL] . . . . . . . 0.02 Measure mode . . . . . . . . . . EQU
dV(max) [mL] . . . . . . . 0.5 dE [mV] . . . . . . . . . . . 1.0
dE [mV] . . . . . . . . . . . 1.0 t (min) [s] . . . . . . . . 6.0
dt [s] . . . . . . . . . . . . 1.0 t (max) [s] . . . . . . . . 30.0
t (min) [s] . . . . . . . . 6.0 Threshold . . . . . . . . . . . . 50.0
t (max) [s] . . . . . . . . 30.0 Maximum volume [mL] . . . . . . . 60.0
Threshold . . . . . . . . . . . . 50.0 Termination after n EQPs . . . . Yes
Termination after n EQPs . . . . Yes Evaluation procedure . . . . . . Standard
n = . . . . . . 1 Calculation
Evaluation procedure . . . . . . Standard Result name . . . . . . . . . . . . Blank I2 - value
Calculation Formula . . . . . . . . . . . . . . R1=Q[1]
Result name . . . . . . . . . . . . I2 - value Constant . . . . . . . . . . . . . .
Formula . . . . . . . . . . . . . . R=(H3-Q)*C/m Result unit . . . . . . . . . . . . mmol
Constant . . . . . . . . . . . . . . C=M/(10*z) Decimal places . . . . . . . . . . . 4
Result unit . . . . . . . . . . . . g I2/100g Record
Record Raw results last sample . . . . . . Yes
Raw results last sample . . . . . . Yes Table of measured values . . . . . . Yes
Table of measured values . . . . . . Yes Ri (i=index) . . . . . . . . . . . . R1
Statistics Standard deviation s . . . . . . . . Yes
Ri (i=index) . . . . . . . . . . . . R1 Rel. standard deviation srel . . . . Yes
Standard deviation s . . . . . . . . Yes Outlier test . . . . . . . . . . . . Yes
Rel. standard deviation srel . . . . Yes Auxiliary value
Outlier test . . . . . . . . . . . . Yes ID text . . . . . . . . . . . . . . Blank I2 - value
All results . . . . . . . . . . . . Yes Output unit . . . . . . . . . . . . Printer
All results . . . . . . . . . . . . Yes
54
METTLER TOLEDO M211
Iodine Value of Cosmetic Fats According to Wijs

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

according to the expected iodine value 1) Dissolve the sample in 10 mL carbon tetrachloride. The Wijs
solution, mercuric acetate and potassium iodide solution are
added automatically by the DL70 titrator.
Substance C-C double bonds, -CH=CH-
2) The mercuric acetate in glacial acetic acid, which is only
added after the Wijs reagent, is used to speed up the reaction.
Chemicals 10 mL CCl4 ; 10 mL Wijs solution; 3) It is important to determine the blank 3 times before the
20 mL 2.5 % mercury (II) acetate; iodine value determination. The mean value of the three blank
20 mL 20% potassium iodide, KI determinations is stored as auxiliary value (H3).
Titrant Sodium thiosulphate,

c(Na2S2O3)=0.1 mol/L;
Note:
Standard Potassium iodate, KIO3 1. Wijs solution, c(ICl) = 0.2 mol/L
Instruments DL70, ST20A Sample changer, AT250 2. The 2.5% solution is prepared by dissolving mercury (II)
acteta in glacial acetic acid.
Balance, Matrix printer EPSON FX800
with serial interface
Accessories Titration beaker ME-101974,

3 Peristaltic pumps ME-65241,
1 Additional burette drive DV90
Remarks
Indication DM140-SC at Sensor 2 The iodine value is defined as the amount of iodine which reacts
with 100 g of an oil or fat.
Chemistry ICl3 + I2 = 3 ICl
ICl + KI = I2 + KCl
2(SO3S)2- + I2 = 2 I- + (S2O6S2)2-
Literature:
Calculation See Application No. M051, M096 and M617
Blank value:
R1 = Q1[1] ; in mmol
Iodine value:
R2 = (H3-Q1[2])/m ; mmol/g
Results
Waste Halogenated organic solvents

disposal containing mercury ions.
Author Angelo Bonetti
55
Results
METTLER DL70 Laboratorio controllo M.P.
Automatic: Indice di Iodio
Measured 01-Dec-1989 11:23

User RGF
Titration 01-Dec-1989 09:46
Version SW 1.2
RESULTS
No ID1 Volume Results
1/1 Bianco J 10.0 mL 1.7659 mmol Bianco J
1/2 Bianco J 10.0 mL 1.7682 mmol Bianco J
1/3 Bianco J 10.0 ml 1.7688 mmol Bianco J
2/1 No. Iodio 0.151 g 87.74 gI 2/100g Indice Iodio
STATISTICS
Number results n = 3
Mean value x = 1.7676 mmol Bianco J
Standard deviation s = 0.00152 mmol Bianco J
STATISTICS
Mean value x = 87.80 gI 2/100g Indice Iodio
Standard deviation s = 0.056 gI 2/100g Indice Iodio
AUXILIARY VALUE
Nouvelle value H3 = 1.767644 Bianco del Wijs
56
Method
Method 211 Automatiz. Indice di Iodio Dispense
Version 30-Nov-1989 11.27 Titrant . . . . . . . . . . . . . . Reatt.di Wijs
Concentration . . . . . . . . . . . 0.2
Title Volume [mL] . . . . . . . . . . . . 10.0
Method ID . . . . . . . . . . . . . 211 Dispense
Title . . . . . . . . . . . . . . . Automatiz.Indice di Titrant . . . . . . . . . . . . . . (CH3COO)2Hg
Iodio Concentration . . . . . . . . . . . 0.0
Date/time . . . . . . . . . . . . . 30-Nov-1989 11.27 Volume [mL] . . . . . . . . . . . . 10.0
Sample Stir
Number samples . . . . . . . . . . . 3 Speed [%] . . . . . . . . . . . . . 65
Titration stand . . . . . . . . . . ST20 Time [s] . . . . . . . . . . . . . . 300
Entry type . . . . . . . . . . . . . Fixed volume U Auxilliary instrument
Volume [mL] . . . . . . . . . 10.0 Name . . . . . . . . . . . . . . . . Pompa KI
ID1 . . . . . . . . . . . . . . . . Bianco J Time (s) . . . . . . . . . . . . . . 3.0
Molar mass M . . . . . . . . . . . . 1.0 Stir
Equivalent number z . . . . . . . . 1 Speed [%] . . . . . . . . . . . . . 100
Dispense Time [s] . . . . . . . . . . . . . . 10
Titrant . . . . . . . . . . . . . . Reatt.di Wijs Titration
Concentration . . . . . . . . . . . 0.2 Titrant . . . . . . . . . . . . . . Na2S2O3
Volume [mL] . . . . . . . . . . . . 10.0 Concentration [mol/L] . . . . . . . 0.1
Dispense Sensor . . . . . . . . . . . . . . . DM-140-SC
Titrant . . . . . . . . . . . . . . (CH3COO)2Hg Unit of meas. . . . . . . . . . . . mV
Concentration . . . . . . . . . . . 0.0 Titration mode . . . . . . . . . . . EQP
Volume [mL] . . . . . . . . . . . . 10.0 Predespensing 1 . . . . . . . . . mL
Stir Volume [mL] . . . . . . . . . 16.0
Speed [%] . . . . . . . . . . . . . 60 Titrant addition . . . . . . . . DYN
Time [s] . . . . . . . . . . . . . . 120 dV (set) [mL] . . . . . . . . 5.0
Auxilliary instrument Limits dV . . . . . . . . . . Absolute
Name . . . . . . . . . . . . . . . . Pompa KI dV (min) [mL] . . . . . . . . 0.03
Time [s] . . . . . . . . . . . . . . 3.0 dV (max) [mL] . . . . . . . . 0.5
Stir Measure mode . . . . . . . . . . EQU
Speed [%] . . . . . . . . . . . . . 100 dE [mV] . . . . . . . . . . . 0.5
Time [s] . . . . . . . . . . . . . . 30 dt [s] . . . . . . . . . . . . 1.0
Titration t(min) [s] . . . . . . . . . . 2.0
Titrant . . . . . . . . . . . . . . Na2S2O3 t(max) [s] . . . . . . . . . . 10.0
Concentration [mol/L] . . . . . . . 0.1 Threshold . . . . . . . . . . . . 200.0
Sensor . . . . . . . . . . . . . . . DM-140-SC Maximum volume [mL] . . . . . . . 25.0
Unit of meas. . . . . . . . . . . . mV Termination after n EQPs . . . . Yes
Titration mode . . . . . . . . . . . EQP n = . . . . . . . . . . . . . 1
Predespensing 1 . . . . . . . . . mL Evaluation procedure . . . . . . Asymmetric
Volume [mL] . . . . . . . . . 16.0 Rinse
Predespensing 2 . . . . . . . . . f (potential) Solution aux. . . . . . . . . . . . H2O
Potential (mV,pH...) . . . . . 230.0 Volume [mL] . . . . . . . . . . . . 10.0
Titrant addition . . . . . . . . INC Calculation
dV [mL] . . . . . . . . . . 0.05 Result name . . . . . . . . . . . . Indice Iodio
Measure mode . . . . . . . . . . EQU Formula . . . . . . . . . . . . . . R2=(H3-Q[2])*C2/m
dE [mV] . . . . . . . . . . . 0.5 Constant . . . . . . . . . . . . . . C2=M/(10*z)
dt [s] . . . . . . . . . . . . 1.0 Result unit . . . . . . . . . . . . gI2/100g
t(min) [s] . . . . . . . . . . 2.0 Decimal places . . . . . . . . . . . 2
t(max) [s] . . . . . . . . . . 10.0 Statistics
Threshold . . . . . . . . . . . . 350.0 Ri (i=index) . . . . . . . . . . . . R2
Maximum volume [mL] . . . . . . . 25.0 Standard deviation s . . . . . . . . Yes
Termination after n EQPs . . . . Yes Rel. standard deviation srel . . . . Yes
n = . . . . . . . . . . . . . 1 Record
Evaluation procedure . . . . . . Asymmetric All results . . . . . . . . . . . . Yes
Rinse Table of values . . . . . . . . . . Yes
Solution aux. . . . . . . . . . . . H2O
Volume [mL] . . . . . . . . . . . . 10.0
Calculation
Result name . . . . . . . . . . . . Bianco J
Formula . . . . . . . . . . . . . . R1=Q1[1]
Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . mmol
Decimal places . . . . . . . . . . . 4
Statistics
Ri (i=index) . . . . . . . . . . . . R1
Auxiliary value
ID text . . . . . . . . . . . . . . Bianco del Wijs
Formula . . . . . . . . . . . . . . H3=x
Record
All results . . . . . . . . . . . . Yes
Sample
Number samples . . . . . . . . . . . 1
Titration stand . . . . . . . . . . ST20
Entry type . . . . . . . . . . . . . Poids m
Lower limit [g] . . . . . . . . . 0.05
Upper limit [g] . . . . . . . . . 2.0
ID1 . . . . . . . . . . . . . . . . No. Iodio
Molar mass M . . . . . . . . . . . . 254
57
METTLER TOLEDO M206
Determination of Carboxyl Groups in PET

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

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

Adapter cable DIN-Lemo ME-89600
Remarks
Indication DP550 Phototrode, colour indicator: 1) The titer determination is performed using potassium
0.1% Bromphenol blue in ethanol hydrogen phtalate, KHP, as a primary standard:
KHP is dissolved in 10 mL deionized water and diluted to 100
Chemistry mL with benzyl alcohol. 2 mL of this solution was added to 50
mL benzyl alcohol and titrated with KOH.
Phenolphtalein in ethanol is used as colour indicator.
2) The DP550 phototrode has to be adjusted to approximately

1000 mV by dipping it in deionized water and turning the knob
on the top of the housing.
Calculation R=Q*C/m
3) The sensor and the stirrer have to be cleaned thoroughly with
C=1000 , in eq/ton water and benzyl alcohol afte reach sample deteremination.
Literature:
See Application No. M051, M096 and M617
Results

disposal
Author Viola Schindler
58
Results
METTLER DL77 Titrator V3.1 Mettler - Toledo AG
23 Market Support Laboratory
Method 206A COOH in PET determination 08-Jan-1997 12:44

User V. Schindler
Measured 08-Jan-1997 17:44
RESULTS
1/1 COOH 1.0008 g Weight m

R1 = 21.39511 eq/ton COOH content
R2 = 1.3474 mL mL consump
STATISTICS
Mean value x = 21.35287 eq/ton COOH content
Standard deviation s = 0.189344 eq/ton COOH content
59
Method
Method 206A COOH in PET determination Method 206B Blank: COOH in PET
Version 08-Jan-1994 12:44 Version 08-Jan-1994 12:47
Title Title
Title . . . . . . . . . . . . . . . COOH in PET Title . . . . . . . . . . . . . . . Blank: COOH in PET
determination Date/time . . . . . . . . . . . . . 08-Jan-1994 12:47
Date/time . . . . . . . . . . . . . 08-Jan-1994 12:44 Sample
Sample Number samples . . . . . . . . . . . 3
Number samples . . . . . . . . . . . 3 Titration stand . . . . . . . . . . Stand 1
Titration stand . . . . . . . . . . Stand 1 Entry type . . . . . . . . . . . . . Fixed volume U
Entry type . . . . . . . . . . . . . Weight m Volume [mL] . . . . . . . . . 50.0
Lower limit [g] . . . . . . . . . 0.0 ID1 . . . . . . . . . . . . . . . . COOH
ID1 . . . . . . . . . . . . . . . . COOH Equivalent number z . . . . . . . . 1
Molar mass M . . . . . . . . . . . . 54.02 Temeprature sensor . . . . . . . . . Manual
Equivalent number z . . . . . . . . 1 Instruction
Temeprature sensor . . . . . . . . . Manual Add bromphenol Blue
Instruction Stir
Add bromphenol Blue Speed [%] . . . . . . . . . . . . . 80
Stir Time [s] . . . . . . . . . . . . . . 40
Speed [%] . . . . . . . . . . . . . 80 Stir
Time [s] . . . . . . . . . . . . . . 40 Speed [%] . . . . . . . . . . . . . 50
Stir Time [s] . . . . . . . . . . . . . . 2
Speed [%] . . . . . . . . . . . . . 50 Titration
Time [s] . . . . . . . . . . . . . . 2 Titrant . . . . . . . . . . . . . . KOH
Titrant . . . . . . . . . . . . . . KOH Sensor . . . . . . . . . . . . . . . DP550
Sensor . . . . . . . . . . . . . . . DP550 Titration mode . . . . . . . . . . . EQP
Unit of meas. . . . . . . . . . . . mV Titrant addition . . . . . . . . INC
Titration mode . . . . . . . . . . . EQP dV [mL] . . . . . . . . . . 0.02
Titrant addition . . . . . . . . INC Measure mode . . . . . . . . . . EQU
dV [mL] . . . . . . . . . . 0.1 dE [mV] . . . . . . . . . . . 0.5
dE [mV] . . . . . . . . . . . 0.5 t(min) [s] . . . . . . . . . . 5.0
dt [s] . . . . . . . . . . . . 1.0 t(max) [s] . . . . . . . . . . 40.0
t(min) [s] . . . . . . . . . . 5.0 Threshold . . . . . . . . . . . . 250.0
t(max) [s] . . . . . . . . . . 40.0 Maximum volume [mL] . . . . . . . 3.0
Threshold . . . . . . . . . . . . 250.0 Termination after n EQPs . . . . Yes
Termination after n EQPs . . . . Yes Evaluation procedure . . . . . . Standard
n = . . . . . . . . . . . . . 1 Calculation
Evaluation procedure . . . . . . Standard Result name . . . . . . . . . . . . Blank
Calculation Formula . . . . . . . . . . . . . . R=Q
Result name . . . . . . . . . . . . COOH content Constant . . . . . . . . . . . . . .
Formula . . . . . . . . . . . . . . R=(Q-H18)*C/m Result unit . . . . . . . . . . . . mmol
Constant . . . . . . . . . . . . . . C=1000 Decimal places . . . . . . . . . . . 5
Result unit . . . . . . . . . . . . eq/ton Record
Calculation Sample data . . . . . . . . . . . . Yes
Result name . . . . . . . . . . . . mL consump All results . . . . . . . . . . . . Yes
Formula . . . . . . . . . . . . . . R2=VEQ Table of values . . . . . . . . . . Yes
Constant . . . . . . . . . . . . . . dE/dV - V curve . . . . . . . . . . Yes
Result unit . . . . . . . . . . . . mL Statistics
Decimal places . . . . . . . . . . . 4 Ri (i=index) . . . . . . . . . . . . R1
Record Standard deviation s . . . . . . . . Yes
Output unit . . . . . . . . . . . . Printer Rel. standard deviation srel . . . . Yes
Sample data . . . . . . . . . . . . Yes Outlier test . . . . . . . . . . . . Yes
All results . . . . . . . . . . . . Yes Auxiliary value
Table of values . . . . . . . . . . Yes ID text . . . . . . . . . . . . . . Blank
dE/dV - V curve . . . . . . . . . . Yes Formula . . . . . . . . . . . . . . H18=x
Statistics Record
Ri (i=index) . . . . . . . . . . . . R1 Output unit . . . . . . . . . . . . Printer
Standard deviation s . . . . . . . . Yes All results . . . . . . . . . . . . Yes
Outlier test . . . . . . . . . . . . Yes
Record
All results . . . . . . . . . . . . Yes
60
METTLER TOLEDO M237
Peroxide Value of Lecithin

Determination of the peroxide value of lecithin
Sample Lecithin, 5 g Preparation and Procedures

1) Lecithin is dissolved in a solvent mixture consisting of 12 mL
chloroform and 18 mL glacial acetic acid.
2) After manually adding 0.5 mL saturated potassium iodide

Substance Peroxide, ROOR
solution, the sample is stirred 60 s using the auxiliary function
Stir of the titrator. Iodine is generated.
Chemicals 12 mL Chloroform, CHCl3 , 18 mL 3) 30 mL deionised water are added to the sample together with
glacial acetic acid, 0.5 mL saturated starch.
KI solution, 30 mL deion. water, starch
4) The sample is titrated using sodium thiosulphate.

c(Na2S2O3)= 0.01mol/L;
Note:
Starch is added in order to select the most appropriate titarnt
Standard Potassium iodate, KIO3 increment size for the titration depending on the colour obtained:
Instruments DL50 Graphix Faint blue: increment size 0.05 mL

Dark blue: increment size 0.5 mL

Printer
Balance
Remarks
Indication DM140-SC A blank value is determined previous sample titration.
Chemistry 2R-OOH + 2KI = 2R-OH + 2KOH + I2 This application was perforemd with theDL40RC titrator and the
method was adapted tot he DL50 Graphix.
The method can be completely automated using a DL58 or a
I2 + 2Na2S2O3 = 2NaI + Na2S4O6
DL7x titrator using the flexible method concept.
Calculation Literature:
Peroxide value det. (Method 40014)
Application DL40RC No. 311.
R = (Q-H2)*C/m
C=1000 , meq O2/kg
Blank determination (Method 40015)

R = Q ; mmol
R is stored as auxiliary value H2
Results

disposal
Author R. Günter, MT-D
61
Results
DL40RC:
*** 20-NOV-81 ***
METHOD 2 9147
IDENT. 1.2
SAMPLE NO. 1
*R * .10000
STATISTICS:
N 5
MEAN 3.5
STAND.DEV.% 3.1
62
Method
Method 40014 Peroxide value Method 40015 Blank
Version 7-Feb-2002 11:00 Version 7-Feb-2002 11:05
Title Title
Method ID . . . . . . . . . . . . . 40014 Method ID . . . . . . . . . . . . . 40015
Title . . . . . . . . . . . . . . . Peroxide value Title . . . . . . . . . . . . . . . Blank
Date/time . . . . . . . . . . . . . 7-Feb-2002 11:00 Date/time . . . . . . . . . . . . . 11-Dec-2001 11:05
Sample Sample
Sample ID . . . . . . . . . . . . . Lecithin Sample ID . . . . . . . . . . . . . Blank peroxide
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10
EQP Titration Titrant . . . . . . . . . . . . . . Na2S2O3
Titrant . . . . . . . . . . . . . . Na2S2O3 Concentration [mol/L] . . . . . . . 0.01
Concentration [mol/L] . . . . . . . 0.01 Sensor . . . . . . . . . . . . . . . DM140
Sensor . . . . . . . . . . . . . . . DM140 Unit of meas. . . . . . . . . . . . mV
Predispensing . . . . . . . . . . . No Titrant addition . . . . . . . . . . Incremental
Titrant addition . . . . . . . . . . Incremental dV[mL] . . . . . . . . . . . . . 0.02
dV[mL] . . . . . . . . . . . . . 0.05 Measure mode . . . . . . . . . . . . Equilibrium
controlled dE [mV] . . . . . . . . . . . . . 0.2
dE [mV] . . . . . . . . . . . . . 0.2 dt [s] . . . . . . . . . . . . . 1.0
dt [s] . . . . . . . . . . . . . 1.0 t(min) [s] . . . . . . . . . . . 5.0
t(min) [s] . . . . . . . . . . . 5.0 t(max) [s] . . . . . . . . . . . 30.0
Potential 2 . . . . . . . . . . . No Stop for reevaluation . . . . . . Yes
Stop for reevaluation . . . . . . Yes Condition . . . . . . . . . . neq=0
Condition . . . . . . . . . . neq=0 Calculation
Constant . . . . . . . . . . . . . . C1=1000 Decimal places . . . . . . . . . . . 5
Result unit . . . . . . . . . . . . meq O2/kg Result name . . . . . . . . . . . .
Result name . . . . . . . . . . . . Peroxide value Statistics . . . . . . . . . . . . . Yes
Statistics . . . . . . . . . . . . . Yes Calculation
Formula . . . . . . . . . . . . . . R2=Q Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . mmol Result name . . . . . . . . . . . .
Result name . . . . . . . . . . . . Statistics . . . . . . . . . . . . .
Calculation ID text . . . . . . . . . . . . . . Blank peroxide
Constant . . . . . . . . . . . . . . Report
d2E/dV2 - V curve . . . . . . . . . No
E - t curve . . . . . . . . . . . . No
V - t curve . . . . . . . . . . . . No
dV/dt - t curve . . . . . . . . . . No
63
METTLER TOLEDO M624
Peroxide Value of Edible oils and Fats

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

1) Beakers have to be cleaned very well. Invisible fat residues or
metal traces can affect the result strongly.
2) About 3 g of sample were dissolved in 20 mL of acetic

Substance Peroxide, ROOR
acid/chloroform (3:2) The acetic acid/chloroform mixture was
added by the function DISPENSE.
Chemicals 20 mL acetic acid/chloroform 3) 1 mL of saturated potassium iodide solution is added

1 mL saturated KI solution manually. Thereaction takes place and iodine is formed.
50 mL deion. water
4) 50 mL deionized water are added manually to the sample
solution. Iodine is titrated with sodium thiosulphate.
c(Na2S2O3)= 0.01mol/L;
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.
Standard Potassium iodate, KIO3
Optimum stir time
Instruments DL58; DL70ES/DL77 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
Accessories Titration beakers ME-101974 between the liberated iodine and the oil.
Balance, Printer
Remarks
Indication DM140-SC Blank value determination
Impurities of the solvent are taken into account by a blank value
determination. The blank value determination is done under the
Chemistry 2R-OOH + 2KI = 2R-OH + 2KOH + I2 same conditions as the peroxide value determination itself. The
blank value is automatically stored as auxiliary value H1 with the
function AUXILIARY VALUE (see method 91015)
I2 + 2Na2S2O3 = 2NaI + Na2S4O6
Definitions
Fats and oils undergo changes during storage due to oxidation
with air (oxidative rancidity). The compounds formed react as
Calculation peroxides. Their content is commonly expressed as the "peroxide
Peroxide value det. (Method 91016) value" in milliequivalents peroxidic oxygen per kg of sample.
R = (Q-H1)*C/m Peroxide values higher than 10 to 20 meq O2/kg are commonly
C=1000 , meq O2/kg interpreted as rancidity. Unrefined oils have higher peroxide
values. They are usually in the range between 5 to 20 meq
Blank determination (Method 91015) O2/kg.
R=Q
Q is stored as auxiliary value H1 Influence stir time
Results
Stir time [s] Result [meq/kg]
Waste 60 3.201
The waste contains organic solvents 180 4.947
disposal and is disposed accordingly. 300 6.817
600 6.491
Author K. Wydler
64
Results
Peroxide value of olive oil
ALL RESULTS
No. ID Sample size and results
1 ROOR 3.2691 g
R1 = 16.104 meq/kg Peroxide Val.
2 ROOR 3.1461 g
3 ROOR 3.1838 g
4 ROOR 3.2309 g
5 ROOR 3.0293 g
Etc.
STATISTICS
Number of results R1 n = 5
Mean value x = 16.545 meq/kg Peroxide Val.
Standard deviation s = 0.26372 meq/Kg Peroxide Val.
Peroxide value: comparison of different oils and fats
Oil Sample mass n Mean value Stand. Deviation srel

[g] [% water] [% water] [%]
Thistle oil 3.0435 - 4.2328 5 18.310 0.35621 1.945

Sunflower oil 2.3521 - 4.5656 5 13.880 0.75799 5.461
Peanut oil 1.9836 - 3.0248 5 13.179 0.58047 4.405
Olive oil 3.0293 - 3.2691 5 16.545 0.26372 1.594
Palm oil 2.3217 - 3.8720 5 11.680 0.62599 5.359
Margarine 3.9440 - 2.7137 5 8.312 0.45597 5.486
Coconut fat 2.0889 - 2.6050 5 5.542 0.23404 4.224
65
Method
Method 91016 Peroxide Value Method 91015 Blank Peroxide Value
Version 30-Jul-1999 13:14 Version 30-Jul-1999 12:18
Title Title
Method ID . . . . . . . . . . . 91016 Method ID . . . . . . . . . . . 91015
Title . . . . . . . . . . . . . Peroxide Value Title . . . . . . . . . . . . . Blank Peroxide Value
Date/time . . . . . . . . . . . 30-Jul-1999 13:14 Date/time . . . . . . . . . . . 30-Jul-1999 13:14
Sample Sample
Sample ID . . . . . . . . . . . O2 Sample ID . . . . . . . . . . . O2
Entry type . . . . . . . . . . . Weight Entry type . . . . . . . . . . . Weight
Lower limit [g] . . . . . . . 0.0 Lower limit [g] . . . . . . . 0.0
Upper limit [g] . . . . . . . 5.0 Upper limit [g] . . . . . . . 5.0
Molar mass M . . . . . . . . . . 32.0 Molar mass M . . . . . . . . . . 32.0
Equivalent number z . . . . . . 1 Equivalent number z . . . . . . 1
Titration stand . . . . . . . . Stand 1 Titration stand . . . . . . . . Stand 1
Temperature sensor . . . . . . . Manual Temperature sensor . . . . . . . Manual
Dispense Dispense
Titrant . . . . . . . . . . . . Chloroform/AA Titrant . . . . . . . . . . . . Chloroform/AA
Concentration [mol/L] . . . . . 0.1 Concentration [mol/L] . . . . . 0.1
Volume [mL] . . . . . . . . . . 20 Volume [mL] . . . . . . . . . . 20
Instruction Instruction
Text . . . . . . . . . . . . . . Add 1 mL KI solution Text . . . . . . . . . . . . . . Add 1 mL KI solution
Stir Stir
Speed [%] . . . . . . . . . . . 50 Speed [%] . . . . . . . . . . . 50
Time [s] . . . . . . . . . . . . 300 Time [s] . . . . . . . . . . . . 300
Instruction Instruction
Text . . . . . . . . . . . . . . Add 50 mL destilled water Text . . . . . . . . . . . . . . Add 50 mL destilled water
EQP titration EQP titration
Titrant/Sensor Titrant/Sensor
Titrant . . . . . . . . . . . Na2S2O3 Titrant . . . . . . . . . . . Na2S2O3
Concentration [mol/L] . . . . 0.01 Concentration [mol/L] . . . . 0.01
Sensor . . . . . . . . . . . DM140 Sensor . . . . . . . . . . . DM140
Unit of meas . . . . . . . . mV Unit of meas . . . . . . . . mV
Predispensing . . . . . . . . . No Predispensing . . . . . . . . . No
Titrant addition . . . . . . . . Dynamic Titrant addition . . . . . . . . Dynamic
dE(set) [mV] . . . . . . . . 8.0 dE(set) [mV] . . . . . . . . 8.0
dV(min) [mL] . . . . . . . . 0.02 dV(min) [mL] . . . . . . . . 0.02
dV(max) [mL] . . . . . . . . 0.2 dV(max) [mL] . . . . . . . . 0.2
Measure mode . . . . . . . . . Equilibrium controlled Measure mode . . . . . . . . . Equilibrium controlled
dE [mV] . . . . . . . . . . . 0.5 dE [mV] . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . 1.0 dt [s] . . . . . . . . . . . 1.0
t(min) [s] . . . . . . . . . 3.0 t(min) [s] . . . . . . . . . 3.0
t(max) [s] . . . . . . . . . 30.0 t(max) [s] . . . . . . . . . 30.0
Threshold . . . . . . . . . . 200.0 Threshold . . . . . . . . . . 200.0
Steepest jump only . . . . . No Steepest jump only . . . . . No
Range . . . . . . . . . . . . No Range . . . . . . . . . . . . No
Tendency . . . . . . . . . . Negative Tendency . . . . . . . . . . Negative
at maximum volume [mL] . . . 20.0 at maximum volume [mL] . . . 20.0
at potential . . . . . . . . No at potential . . . . . . . . No
at slope . . . . . . . . . . No at slope . . . . . . . . . . No
afternumber EQPs . . . . . . Yes afternumber EQPs . . . . . . Yes
n = . . . . . . . . . . . 1 n = . . . . . . . . . . . 1
comb. term. conditions . . . No comb. term. conditions . . . No
Procedure . . . . . . . . . . Standard Procedure . . . . . . . . . . Standard
Potential 1 . . . . . . . . . No Potential 1 . . . . . . . . . No
Stop for reevaluation . . . . No Stop for reevaluation . . . . No
Formula . . . . . . . . . . . . R=(Q-H1)*C/m Formula . . . . . . . . . . . . R=VEQ
Constant . . . . . . . . . . . . C=1000 Constant . . . . . . . . . . . .
Decimal places . . . . . . . . . 3 Decimal places . . . . . . . . . 3
Result unit . . . . . . . . . . meq/kg Result unit . . . . . . . . . . mL
Result name . . . . . . . . . . Peroxide Val. Result name . . . . . . . . . . Blank
Statistics . . . . . . . . . . . Yes Statistics . . . . . . . . . . . Yes
Report Auxiliary value
Output . . . . . . . . . . . . Printer ID . . . . . . . . . . . . . . . Blank Peroxide Value
Results . . . . . . . . . . . . No Formula . . . . . . . . . . . . H1=x
All results . . . . . . . . . . Yes Report
Raw results . . . . . . . . . . Yes Output . . . . . . . . . . . . Printer
Table of measured values . . . . Yes Results . . . . . . . . . . . . No
Sample data . . . . . . . . . . Yes All results . . . . . . . . . . Yes
E - V curve . . . . . . . . . . Yes Raw results . . . . . . . . . . Yes
dE/dV - V curve . . . . . . . . Yes Table of measured values . . . . Yes
Sample data . . . . . . . . . . Yes
E - V curve . . . . . . . . . . Yes
dE/dV - V curve . . . . . . . . Yes
66
METTLER TOLEDO M238
Determination of Permanganate Index in Waste Water

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

1) The sample is heated for at least 10 minutes at more than
85°C.
2) The solution is acidified by adding manually (or with a

Substance Oxidazable substances
burette) 5 mL 20 % sulphuric acid.
3) 2 mL 0.1 KMnO4 are dispensed with a burette. After waiting

Chemicals 5 mL 20% sulphuric acid, H2SO4 150 s, an EP titration is started. The time delay is set to 60 s
according to the application.
Titrant Potassium permanganate KMnO4, Note:

c(KMnO4) = 0.1 mol/L 1) The titer determination is performed using sodium oxalate.
ca. 25-40 mg are dissolved in 50 mL 5% sulfuric acid and
wormed to 80°C, since the titration runs slowly at room T.
(See application no. M527).
Standard Sodium oxalate, Na2C2O4 (see M527)
2) Do not dip the tip of the burettes into the sample solution to
Instruments DL55+, DL58, DL70ES/DL7 avoid diffusion into sample solution.
DH100 Heating System,
Balance, printer

2 (1) Additional burette
Cable DH100-Titrator
(DL5x: 51 07424, DL7x: 51 108404)
Remarks
Indication DM140-SC 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
Chemistry MnO4- + 5e- + 8H2O = Mn2- + 12H2O 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

Calculation th COD determination. Since the oxidative power is lower
R= (QDISP+Q)*C/m
compared to COD, not all substances are oxidazed.
C= 1000 , mmol/L
DL7x: U ; instead of m
Literature:
DIN 38409-H5, ISO 8467
Results
Waste Aqueous acid solutions containing

disposal metal ions.
Author Ch. Walter, A. Aichert
67
Results
IC113 Market Support Laboratory
Method 238 KMnO 4 Number 12-Jan-1994 11:38

User
Measured 12-Jan-1994 12:06
RESULTS
1/1 COOH 50.0 mL Fixed volume U

R1 = 7.900 mmol/L KMnO 4 Number
STATISTICS
Mean value x = 7.800 mmol/L KMnO 4 Number
Standard deviation s = 0.100000 mmol/L KMnO 4 Number
68
Method
Method 238 KMnO4 Number
Version 12-Jan-1994 11:38
Title
Method ID . . . . . . . . . . . . . 238
Title . . . . . . . . . . . . . . . KMnO4 Number
Date/time . . . . . . . . . . . . . 12-Jan-1994 11:38
Sample
Number samples . . . . . . . . . . . 3
Entry type . . . . . . . . . . . . . Fixed volume U
Volume [mL] . . . . . . . . . . . 50.0
ID1 . . . . . . . . . . . . . . . .
Molar mass M . . . . . . . . . . . . 100.0
Temperature sensor . . . . . . . . . TEMP A
Temperature
Sensor . . . . . . . . . . . . . . . TEMP A
Unit of meas. . . . . . . . . . . . °C
dT [°C,°F, K] . . . . . . . . . . . 1.0
dt [s] . . . . . . . . . . . . . . . 2.0
t(min) mode . . . . . . . . . . . . T larger Set
Set value [°C,°F, K] . . . . . . 85.0
t(max) [s] . . . . . . . . . . . . . 600.0
Dispense
Titrant . . . . . . . . . . . . . . KMnO4
Volume [mL] . . . . . . . . . . . . 2
Measure
Sensor . . . . . . . . . . . . . . . DM140-SC
Unit of meas. . . . . . . . . . . . mV
dE [mV] . . . . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . . . . . 1.0
t(min) mode . . . . . . . . . . . . Fix
Set value [°C,°F, K] . . . . . . 150.0
t(max) [s] . . . . . . . . . . . . . 150.0
Titration
Titrant . . . . . . . . . . . . . . KMnO4
Sensor . . . . . . . . . . . . . . . DM140-SC
Unit of meas. . . . . . . . . . . . mV
Titration mode . . . . . . . . . . . EP
Predispensing . . . . . . . . . . mL
Volume [mL] . . . . . . . . . 0
Titrant addition . . . . . . . . Continuous
Control band [mV, pH, ...] . . 100.0
Time delay [s] . . . . . . . . 60.0
dV [mL] . . . . . . . . . . . 0.05
End point mode . . . . . . . . . EPA
Potential [mV, pH, ...] . . . 1150.0
Tendency . . . . . . . . . . . . Positive
Calculation
Result name . . . . . . . . . . . . KMnO4 Number
Formula . . . . . . . . . . . . . . R=(QDISP+Q)*C/U
Constant . . . . . . . . . . . . . . C=1000
Result unit . . . . . . . . . . . . mmol/L
Decimal places . . . . . . . . . . . 3
Record
All results . . . . . . . . . . . . Yes
E - V curve . . . . . . . . . . . . Yes
Statistics
Ri (i=index) . . . . . . . . . . . . R1
Outlier test . . . . . . . . . . . . Yes
Record
All results . . . . . . . . . . . . Yes
69
METTLER TOLEDO M239
Chemical Oxygen Demand (COD) of Waste Water

Determination of the COD value in waste water according to DIN 38409 part 4, H4
Sample Waste water, 20 mL Preparation and Procedures

(Or: KHP solution as standard) 1) The sample preparation is performed automatically on the
Rondo 60 sample changer using method 4001:
1.1 Add magnetic stirrer into the COD glass tube (boiling add).
1.2 20 mL waste water are added
Substance Oxidazable organic substances
1.3 Add 10 mL 0.12 molL 1/6 K2Cr2O7 containing Hg2SO4 to
mask chloride (conc.: 0.4g/20 mL, commercially available).
1.4 30 mL Ag2SO4/H2SO4 are slowly added by a burette.
Chemicals 10 mL potassium dichromate, K2Cr2O7 Be careful: Heat is developed !
c(1/6 K2Cr2O7) = 0.12 mol/L 2) The COD glass tubes are brought to the digestor for heating.
The sample solutions are boiled at 148 +/- 3°C for 2 hours.
30 mL 0.1 mol/L Ag2SO4/H2SO4
Afterwards, the COD tubes are let to cool down to at least 60°C.
3) The condenser is rinsed with distilled water, and the tubes
Titrant FAS, (NH4)2Fe(II)(SO4)2 are filled with distilled water up to 100 mL. The tubes are cooled
down to room temperature and placed on the sample changer
c(FAS)= 0.12 mol/L;
rack. Excess dichromate solution is titrated with FAS and the
results expressed as mg O2/L.
The whole COD procedure is tested with 20 mL potassium
Standard K2Cr2O7 (see application M548) hydrogen phtalate KHP solution (COD = 200 +/- 8 mg O2/L).
Preparation: KHP is dried at 105°C for 2 hours. 0.17 g KHP are
Instruments DL50Graphix, DL5x, DL70ES/DL77 dissolved in some water in a 1 L volumetric flask. Add 5 mL
concentrated H2SO4, and fill up to 1000 mL. The solution
Rondo 60, Rondo COD Set, magnetic
remains stable for 1 week when kept cool.
stirrer for Rondo 60.
Accessories Heater with reflux condenser (third

party), 1 additional burette DV1010
(DL7x: two additional burettes),
Balance, Printer
Remarks
Indication DM144-SC 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
Chemistry Cr2O72- + 6Fe2+ + 14H+ = 2Cr3+ + 6Fe3+ + 7H2O organic matter -expressed as the equivalent amount of oxygen-
2 Cr3+ = 2 Cr3+ + 6 e- is determined by oxidation with potassium dichromate. First the
1.5 mol O2 = 6 mol 1/6Cr2O72- = 6mol FAS amount of dichromate (without sample) is determined using
1 mol O2 = 4 mol 1/6Cr2O72- = 4 mol FAS method 4002 and stored as auxiliary value. After oxidation the
Therefore: z = 4 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
Calculation matter. Therefore all inorganic components that could be
COD determination (Method 4003)
oxidized too have to be masked during or removed before
R = (H18-Q)*C/m oxidation step (masking agent: mercury(II) sulfate).
C = M*1000/z , mg O2/L 3) The same special flask of the Rondo 60 COD set is used for
the sample preparation (oxidation step) and titration.
Back value determination (4002) 4) The titer of FAS must be checked daily.
R=Q 5) For accurate results, it is recommended to use distilled water
Q is stored as auxiliary value H18 instead of deionized water.
Results
Literature:
Waste DIN 38409 part 4, H4
The waste contains organic solvents
disposal and is disposed accordingly.
Author Peter Burri
70
Results
METTLER TOLEDO DL58 Titrator V2.3 Titration Basic Course
DL Basic Course Market Support Analytical
Method 4003 COD Determination 10-May-2000 16:36

Measured 10-May-2000 16:46
User PB
ALL RESULTS
1 8.0mL FAS 20.0 mL

R1 = 427.828 mg O2/L COD
R2 = 1.532 mL FAS consumed
2 8.0mL FAS 20.0 mL
R1 = 427.682 mg O2/L COD
3 8.0mL FAS 20.0 mL
R1 = 428.336 mg O2/L COD
STATISTICS
Mean value x = 427.948 mg O2/L COD
Standard deviation s = 0.3432 mg O2/L COD
Mean value x = 1.530 mL
Standard deviation s = 0.00626 mL
71
Method
Method 4003 COD Determination Method 4003:
Version 10-May-2000 16:36 similar to 4002, an additional auxiliary function is used to
store the result in mmol (Q) as auxiliary value H18
Title
Method ID . . . . . . . . . . . 4002
Title . . . . . . . . . . . . . COD Determination Method 4001 COD Preparation
Date/time . . . . . . . . . . . 10-May-2000 16:36 Version 08-May-2000 17:12
Sample
Sample ID . . . . . . . . . . . Effluent Title
Entry type . . . . . . . . . . . Fixed volume Method ID . . . . . . . . . . . 4001
Volume [mL] . . . . . . . . . 20.0 Title . . . . . . . . . . . . . COD Preparation
Molar mass M . . . . . . . . . . 32.0 Date/time . . . . . . . . . . . 08-May-2000 17:12
Equivalent number z . . . . . . 4 Sample
Titration stand . . . . . . . . ST20A Sample ID . . . . . . . . . . . Chemicals
Pump . . . . . . . . . . . . No Entry type . . . . . . . . . . . Fixed volume
Pump . . . . . . . . . . . . No Volume [mL] . . . . . . . . . 20.0
Rinse . . . . . . . . . . . . Yes Molar mass M . . . . . . . . . . 58.43
Solvent . . . . . . . . . H2SO4 5% Equivalent number z . . . . . . 1
Volume [mL] . . . . . . . 20.0 Titration stand . . . . . . . . ST20A
Conditioning . . . . . . . . No Pump . . . . . . . . . . . . No
Temperature sensor . . . . . . . Manual Pump . . . . . . . . . . . . No
Stir Rinse . . . . . . . . . . . . Yes
Speed [%] . . . . . . . . . . . 22 Solvent . . . . . . . . . H2SO4 5%
Time [s] . . . . . . . . . . . . 25 Volume [mL] . . . . . . . 2.0
EQP titration Conditioning . . . . . . . . No
Titrant/Sensor Temperature sensor . . . . . . . Manual
Titrant . . . . . . . . . . . (NH4)2Fe(II)(SO4)2 Dispense
Concentration [mol/L] . . . . 0.12 Titrant . . . . . . . . . . . . 1/6 K2Cr2O7
Sensor . . . . . . . . . . . DM144 Concentration [mol/L] . . . . . 0.12
Unit of meas . . . . . . . . mV Volume [mL] . . . . . . . . . . 10.0
Predispensing . . . . . . . . . to volume Stir
Volume [mV] . . . . . . . . . 0.5 Speed [%] . . . . . . . . . . . 25
Wait time [s] . . . . . . . . 10 Time [s] . . . . . . . . . . . . 20
Titrant addition . . . . . . . . Dynamic EQP titration
dE(set) [mV] . . . . . . . . 6.0 Titrant/Sensor
dV(min) [mL] . . . . . . . . 0.05 Titrant . . . . . . . . . . . H2SO4/Ag2SO4
dV(max) [mL] . . . . . . . . 0.5 Concentration [mol/L] . . . . 0.1
Measure mode . . . . . . . . . Equilibrium controlled Sensor . . . . . . . . . . . DM144
dE [mV] . . . . . . . . . . . 0.5 Unit of meas . . . . . . . . mV
dt [s] . . . . . . . . . . . 1.0 Predispensing . . . . . . . . . No
t(min) [s] . . . . . . . . . 5.0 Titrant addition . . . . . . . . Incremental
t(max) [s] . . . . . . . . . 30.0 dV [mL] . . . . . . . . . . . 0.5
Recognition Measure mode . . . . . . . . . Timed increment
Threshold . . . . . . . . . . 200.0 dt [s] . . . . . . . . . . . 10.0
Steepest jump only . . . . . No Recognition
Range . . . . . . . . . . . . No Threshold . . . . . . . . . . 400.0
Tendency . . . . . . . . . . Negative Steepest jump only . . . . . No
Termination Range . . . . . . . . . . . . No
at maximum volume [mL] . . . 15.0 Tendency . . . . . . . . . . None
at potential . . . . . . . . No Termination
at slope . . . . . . . . . . No at maximum volume [mL] . . . 30.0
after number EQPs . . . . . . Yes at potential . . . . . . . . No
n = . . . . . . . . . . . 1 at slope . . . . . . . . . . No
comb. term. conditions . . . No after number EQPs . . . . . . No
Procedure . . . . . . . . . . Standard Procedure . . . . . . . . . . Standard
Stop for reevaluation . . . . Yes Stop for reevaluation . . . . No
Condition . . . . . . . . neq=0 Calculation
Calculation Formula . . . . . . . . . . . . R=VEND
Formula . . . . . . . . . . . . R=(H18-Q)*C/m Constant . . . . . . . . . . . .
Constant . . . . . . . . . . . . C=M*1000/z Decimal places . . . . . . . . . 3
Decimal places . . . . . . . . . 3 Result unit . . . . . . . . . . mL
Result unit . . . . . . . . . . mg O2/L Result name . . . . . . . . . . H2SO4
Result name . . . . . . . . . . COD Statistics . . . . . . . . . . . No
Statistics . . . . . . . . . . . Yes Report
Calculation Output . . . . . . . . . . . . Printer
Formula . . . . . . . . . . . . R2=VEQ Results . . . . . . . . . . . . No
Constant . . . . . . . . . . . . All results . . . . . . . . . . Yes
Decimal places . . . . . . . . . 3 Raw results . . . . . . . . . . No
Result unit . . . . . . . . . . mL Table of measured values . . . . No
Result name . . . . . . . . . . FAS consumed Sample data . . . . . . . . . . No
Statistics . . . . . . . . . . . Yes E - V curve . . . . . . . . . . No
Report dE/dV - V curve . . . . . . . . No
Output . . . . . . . . . . . . Printer d2E/dV2 - V curve . . . . . . . No
Results . . . . . . . . . . . . No log dE/dV - v curve . . . . . . No
All results . . . . . . . . . . Yes E - t curve . . . . . . . . . . No
Raw results . . . . . . . . . . No V - t curve . . . . . . . . . . No
Table of measured values . . . . Yes dV/dt - t curve . . . . . . . . No
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
72
METTLER TOLEDO M517
Blank determination according to ASTM D664-89

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

1) The blank determination of solvent 664 used for AN-Analysis
(toluene/2-propanol/water 500:495:5) is done automatically
with the sample changer.
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.
Chemicals Toluene/2-propanol/water 500:495:5
Titrant Potassium hydroxide in 2-propanol

c(KOH) = 0.1 mol/L;
Instruments DL50Graphix, DL53/55/58,

DL70ES/77
Sample changer, Printer

Pump ME-65241
Remarks
Indication DG113 1) The analysis is performed by placing the following
succession of beakers on the sample turntable:
1.1 An empty beaker followed by a beaker with 60 mL deion.
Chemistry water for conditioning (indicated with a yellow clip).
1.2 Before starting the method the alkaline buffer potential
(buffer B) must be entered as endpoint in the function
TITRATION.
1.3 The result of this blank determination is stored as auxiliary
value H10. It is used for calculation in the acid number
determination (method 90019).
Calculation R = Q ; mmol
R is stored as auxiliary value H10.
Literature:
ASTM D664-89 (see www.astm.org)
Application brochrue 3, "TAN and TBN", ME-724559
Results
Waste Aromatic organic waste

disposal
Author A. Aichert, A. Logean
73
Results
METTLER TOLEDO DL53 Titrator V1.0 Mettler-Toledo AG
Method 90017 Blindwert AN ASTM D664 01-Jul-1995 12:00

User
RESULTS
1 60.0 mL
R1 = 0.0044 mmol Blank
2 60.0 mL
3 60.0 mL
STATISTICS
Mean value x = 0.0043 mmol Blank
Standard deviation s = 0.00015 mmol Blank
AUXILIARY VALUE
New value H10 = 0.00429 Blank AN ASTM D
74
Method
Method 90017 Blank AN ASTM D664 Report
Version 01-Jul-1995 12:00 Output unit . . . . . . . . . . . . Printer
Results . . . . . . . . . . . . . . No
Title All results . . . . . . . . . . . . Yes
Method ID . . . . . . . . . . . . . 00017 Raw results . . . . . . . . . . . . No
Title . . . . . . . . . . . . . . . Blank AN ASTM D664 Table of measured values . . . . . . Yes
Date/time . . . . . . . . . . . . . 01-Jul-1995 12:00 Sample data . . . . . . . . . . . . No
Sample E - V curve . . . . . . . . . . . . No
Sample ID . . . . . . . . . . . . . dE/dV - V curve . . . . . . . . . . No
Entry type . . . . . . . . . . . . . Fixed volume d2E/dV2 - V curve . . . . . . . . . No
Volume [mL] . . . . . . . . . . . 60.0 log dE/dV - V curve . . . . . . . . No
Molar mass M . . . . . . . . . . . . 100.0 E - t curve . . . . . . . . . . . . No
Equivalent number z . . . . . . . . 1 V - t curve . . . . . . . . . . . . No
Titration stand . . . . . . . . . . ST20A dV/dt - t curve . . . . . . . . . .
Pump . . . . . . . . . . . . . . Yes
Solvent . . . . . . . . . . . Solvent 664
Volume [mL] . . . . . . . . . 60.0
Rinse . . . . . . . . . . . . . . Yes
Solvent . . . . . . . . . . . Solvent 664
Volume [mL] . . . . . . . . . 20.0
Conditioning . . . . . . . . . . Yes
Time [s] . . . . . . . . . . . 300
Rinse . . . . . . . . . . . . Yes
Solvent . . . . . . . . . . Solvent 664
Volume [mL] . . . . . . . . 20.0
Temperature sensor . . . . . . . . . Manual
Stir
Speed [%] . . . . . . . . . . . . . 50
Time [s] . . . . . . . . . . . . . . 10
EP titration
Titrant/Sensor
Titrant . . . . . . . . . . . . . KOH (i-PrOH)
Concentration [mol/L] . . . . . . 0.1
Sensor . . . . . . . . . . . . . DG113
Unit of meas. . . . . . . . . . . mV
Predispensing . . . . . . . . . . . No
Titrant addition . . . . . . . . . . Dynamic
dE(set) [mV] . . . . . . . . . . 4.0
dV(min) [mL] . . . . . . . . . . 0.02
dV(max) [mL] . . . . . . . . . . 0.05
dE [mV] . . . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . . . 6.0
t(min) [s] . . . . . . . . . . . 6.0
t(max) [s] . . . . . . . . . . . 30.0
End point . . . . . . . . . . . . . EP absolute
Potential [mV,pH,..] . . . . . . -143
Tendency
Tendency . . . . . . . . . . . . Negative
Termination
Delay [s] . . . . . . . . . . . . 0
Calculation
Formula . . . . . . . . . . . . . . R=Q
Constant . . . . . . . . . . . . . .
Decimal places . . . . . . . . . . . 4
Result unit . . . . . . . . . . . . mmol
Result name . . . . . . . . . . . . Blank
Statistics . . . . . . . . . . . . . Yes
Calculation
Formula . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . .
Decimal places . . . . . . . . . . . 0
Result unit . . . . . . . . . . . .
Result name . . . . . . . . . . . .
Statistics . . . . . . . . . . . . . No
Auxiliary value
ID . . . . . . . . . . . . . . . . . Blank AN ASTM D664
Formula . . . . . . . . . . . . . . H10=x
75
METTLER TOLEDO M518
Blank determination according to ASTM D4739-92

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

1) The blank determination of solvent 4739
(toluene/2-propanol/chloroform/water 100:100:100:3) is done
automatically with the sample changer.
Substance Alkaline components
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.
Chemicals toluene/2-propanol/chloroform/water
100:100:100:3
Titrant Hydrochloric acid in 2-propanol c(HCl)

= 0.1 mol/L
Standard KOH 0.1 mol/L
Instruments DL50Graphix, DL53/55/58,

DL70ES/77
Rondo 60
Accessories Titration beaker ME-101974,

Printer
Remarks
Indication DG113 1) The analysis is performed by placing the following
succession of beakers on the sample turntable:
1.1 An empty beaker followed by a beaker with 60 mL deion.
Chemistry water for conditioning (indicated with a yellow clip).
1.2 Before starting the method, the acidic buffer potential (buffer
A) must entered as endpoint in the function TITRATION.
2) The result of this blank determination is stored as auxiliary

value H11. It is used for calculation in the base number
determination (method 90020).
Calculation R = Q ; mmol
R is stored as auxiliary value H11
Results Literature:
ASTM D4789-92 (www.astm.org)
Waste Application brochure 3, "TAN and TBN", ME-724559
The conditioning beakers contain a
disposal mixture of water/aromatic organic
solvents. For waste disposal, separate
water and solvent.
76
Results
Method 90018 Blank BN ASTM D4739 01-Jul-1995 12:00

User
RESULTS
1 60.0 mL
R1 = 0.0011 mmol Blank value
2 60.0 mL
3 60.0 mL
STATISTICS
Mean value x = 0.0011 mmol Blank value
Standard deviation s = 0.00004 mmol Blank value
AUXILIARY VALUE
New value H11 = 0.00108 Blank value BN
77
Method
Method 90018 Blank BN ASTM D4739
Version 01-Jul-1995 12:00
Title
Method ID . . . . . . . . . . . . . 90018
Title . . . . . . . . . . . . . . . Blank BN ASTM D4739
Date/time . . . . . . . . . . . . . 01-Jul-1995 12:00
Sample
Sample ID . . . . . . . . . . . . .
Entry type . . . . . . . . . . . . . Fixed volume
Volume [mL] . . . . . . . . . . . 60.0
Molar mass M . . . . . . . . . . . . 100.0
Titration stand . . . . . . . . . . ST20A
Pump . . . . . . . . . . . . . . Yes
Solvent . . . . . . . . . . . Solvent 4739
Volume [mL] . . . . . . . . . 60.0
Rinse . . . . . . . . . . . . . . Yes
Solvent . . . . . . . . . . . Solvent 4739
Volume [mL] . . . . . . . . . 20.0
Conditioning . . . . . . . . . . Yes
Time [s] . . . . . . . . . . . 300
Rinse . . . . . . . . . . . . Yes
Solvent . . . . . . . . . . Solvent 4739
Volume [mL] . . . . . . . . 20.0
Stir
Speed [%] . . . . . . . . . . . . . 50
Time [s] . . . . . . . . . . . . . . 10
EP titration
Titrant/Sensor
Titrant . . . . . . . . . . . . . HCl (i-PrOH)
Concentration [mol/L] . . . . . . 0.1
Sensor . . . . . . . . . . . . . DG113
Unit of meas. . . . . . . . . . . mV
Predispensing . . . . . . . . . . . No
dE(set) [mV] . . . . . . . . . . 4.0
dV(min) [mL] . . . . . . . . . . 0.02
dV(max) [mL] . . . . . . . . . . 0.05
dE [mV] . . . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . . . 6.0
t(min) [s] . . . . . . . . . . . 30.0
t(max) [s] . . . . . . . . . . . 90.0
End point . . . . . . . . . . . . . EP absolute
Potential [mV,pH,..] . . . . . . 154
Tendency
Termination
Delay [s] . . . . . . . . . . . . 0
Calculation
Formula . . . . . . . . . . . . . . R=Q
Constant . . . . . . . . . . . . . .
Decimal places . . . . . . . . . . . 4
Result unit . . . . . . . . . . . . mmol
Result name . . . . . . . . . . . . Blank value
Statistics . . . . . . . . . . . . . Yes
Calculation
Formula . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . .
Decimal places . . . . . . . . . . . 0
Result unit . . . . . . . . . . . .
Result name . . . . . . . . . . . .
Statistics . . . . . . . . . . . . . No
Auxiliary value
ID . . . . . . . . . . . . . . . . . Blank value BN D4739
Formula . . . . . . . . . . . . . . H11=x
Report
Results . . . . . . . . . . . . . . No
All results . . . . . . . . . . . . Yes
Raw results . . . . . . . . . . . . No
Table of measured values . . . . . . Yes
Sample data . . . . . . . . . . . . No
E - V curve . . . . . . . . . . . . No
dE/dV - V curve . . . . . . . . . . No
d2E/dV2 - V curve . . . . . . . . . No
E - t curve . . . . . . . . . . . . No
V - t curve . . . . . . . . . . . . No
78
METTLER TOLEDO M519
AN (acid number) according to ASTM D664-89

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

1) Weigh in a well homogenised oil sample in the titration
beaker and place it on the sample changer.
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.
Chemicals ASTM 664 solvent

Toluene/2-propanol/water 500:495:5
To proceed with this determination, the following steps are
needed:
Titrant Potassium hydroxide in 2-propanol 1. Determination of the alkaline buffer value (buffer B).
c(KOH) = 0.1 mol/L; 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").
Standard Potassium hydrogen phthalate, KHP
Instruments DL50Graphix, DL53/55/58, DL7x General procedure:

1. Titer det. of 0.1 mol/L KOH 0.1 with KHP
Rondo 60,
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)
balance, printer
Remarks
Indication DG113-SC Acid number according to ASTM D664-89:
Consumption of mg KOH/g oil to buffer value B or to the EQP
nearest to the buffer value B.
Chemistry
Titration parameters:
The titration parameters correspond exactly to the standard ASTM
D664-89:
1. Titrant addition: max. speed 0.2 mL/min

2. dE< 30 mV/0.1 mL —> Increment = 0.1 mL
Calculation 3. dE> 30 mV/0.1 mL —> Increment = 0.05 mL
R1 = consumption of mg KOH/g oil to the
4. The titration will be terminated if the potential is below buffer
buffer value B
value B and the change is smaller than 50 mV/mL KOH.
R2 = consumption of mg KOH/g oil to EQP
nearest to the buffer value B Conditioning
After every titration the electrode is conditioned in water for 5
If there is no EQP, the result is negative. minutes and then rinsed with solvent 664. With this method the
(Blank value of the solvent) conditioning proceeds automatically, if the sample changer
Results holds a conditioning beaker with 60 mL deion. water after every
sample.
Waste Aromatic organic waste. The Literature:
disposal conditioning beakers contain a mixture ASTM D664-89 (see www,astm.org)
of water and organic solvents. Application brochure 3, "TAN and TBN", ME-724559
79
Results
Method 90019 AN ASTM D664 01-Jul-1995 12:00

User
RESULTS
1 Oil 7.275 g
R1 = 1.83 mg KOH/g AN (Buffer B)
R2 = -0.03 mg KOH/g AN (EQP)
2 Oil 6.768 g
3 Oil 6.975 g
4 Oil 6.706 g
5 Oil 7.227 g
STATISTICS
Mean value x = 1.79 mg KOH/gAN (Buffer B)
Standard deviation s = 0.03513 mg KOH/gAN (Buffer B)
80
Method
Method 90019 AN ASTM D664 Calculation
Version 01-Jul-1995 12:00 Formula . . . . . . . . . . . . . . R1=(QP1-H10)*M/m
Constant . . . . . . . . . . . . . .
Title Decimal places . . . . . . . . . . . 2
Method ID . . . . . . . . . . . . . 90019 Result unit . . . . . . . . . . . . mg KOH/g
Title . . . . . . . . . . . . . . . AN ASTM D664 Result name . . . . . . . . . . . . AN (Buffer B)
Date/time . . . . . . . . . . . . . 01-Jul-1995 12:00 Statistics . . . . . . . . . . . . . Yes
Sample Calculation
Sample ID . . . . . . . . . . . . . Oil Formula . . . . . . . . . . . . . . R2=(Q(EPOT~P1)-H10)*C2
Entry type . . . . . . . . . . . . . Weight Constant . . . . . . . . . . . . . . C2=M/m
Lower limit [g] . . . . . . . . . 0.1 Decimal places . . . . . . . . . . . 2
Upper limit [g] . . . . . . . . . 20.0 Result unit . . . . . . . . . . . . mg KOH/g
Molar mass M . . . . . . . . . . . . 56.1 Result name . . . . . . . . . . . . AN (EQP)
Equivalent number z . . . . . . . . 1 Statistics . . . . . . . . . . . . . Yes
Titration stand . . . . . . . . . . ST20A Calculation
Pump . . . . . . . . . . . . . . Yes Formula . . . . . . . . . . . . . .
Solvent . . . . . . . . . . . Solvent 664 Constant . . . . . . . . . . . . . .
Volume [mL] . . . . . . . . . 60.0 Decimal places . . . . . . . . . . . 0
Rinse . . . . . . . . . . . . . . Yes Result unit . . . . . . . . . . . .
Solvent . . . . . . . . . . . Solvent 664 Result name . . . . . . . . . . . .
Volume [mL] . . . . . . . . . 20.0 Statistics . . . . . . . . . . . . . No
Conditioning . . . . . . . . . . Yes Report
Time [s] . . . . . . . . . . . 300 Output unit . . . . . . . . . . . . Printer
Rinse . . . . . . . . . . . . Yes Results . . . . . . . . . . . . . . No
Solvent . . . . . . . . . . Solvent 664 All results . . . . . . . . . . . . Yes
Volume [mL] . . . . . . . . 20.0 Raw results . . . . . . . . . . . . Yes
Temperature sensor . . . . . . . . . Manual Table of measured values . . . . . . Yes
Stir Sample data . . . . . . . . . . . . No
Speed [%] . . . . . . . . . . . . . 60 E - V curve . . . . . . . . . . . . Yes
Time [s] . . . . . . . . . . . . . . 60 dE/dV - V curve . . . . . . . . . . No
EQP titration d2E/dV2 - V curve . . . . . . . . . No
Titrant/Sensor log dE/dV - V curve . . . . . . . . No
Titrant . . . . . . . . . . . . . KOH (i-PrOH) E - t curve . . . . . . . . . . . . No
Concentration [mol/L] . . . . . . 0.1 V - t curve . . . . . . . . . . . . No
Sensor . . . . . . . . . . . . . DG113 dV/dt - t curve . . . . . . . . . . No
Unit of meas. . . . . . . . . . . mV
Predispensing . . . . . . . . . . . to volume
Volume [mL] . . . . . . . . . . . 0.2
dE(set) [mV] . . . . . . . . . . 30.0
dV(min) [mL] . . . . . . . . . . 0.05
dV(max) [mL] . . . . . . . . . . 0.2
dE [mV] . . . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . . . 6.0
t(min) [s] . . . . . . . . . . . 30.0
t(max) [s] . . . . . . . . . . . 90.0
Recognition
Threshold . . . . . . . . . . . . 250.0
Steepest jump only . . . . . . . No
Range . . . . . . . . . . . . . . Yes
Limit A [mV,pH,...] . . . . . -20
Limit B [mV,pH,...] . . . . . -300
Tendency . . . . . . . . . . . . Negative
Termination
at maximum volume [mL] . . . . . 10.0
at potential . . . . . . . . . . Yes
Potential [mV,pH,..] . . . . . -150
at slope . . . . . . . . . . . . Yes
Slope [mV,pH,.../mL] . . . . . 50.0
after number EQPs . . . . . . . . No
comb. termination conditions . . Yes
Evaluation
Procedure . . . . . . . . . . . . Standard
Potential 1 . . . . . . . . . . . Yes
Pot. 1 [mV,pH,...] . . . . . . -150
Potential 2 . . . . . . . . . . . No
Stop for reevaluation . . . . . . No
81
METTLER TOLEDO M520
BN (base number) ASTM D4739-92

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

1) Weigh in a well homogenized oil sample in the titration
beaker and place it on the sample changer.
2) The 60 mL solvent 4739 needed to dissolve the sample are

Substance Basic components
added automatically with the pump. The pump also rinses with
solvent 4739 after titration and conditioning are done.
Chemicals ASTM 4739 solvent

Toluene/2-propanol/chloroform/water To proceed with this determination, the following steps are
100:100:100:3 needed:
1. Determination of the acid buffer value (buffer A)
2. Blank of solvent 4739 (method 90018)
Titrant Hydrochloric acid in 2-propanol c(HCl) 3. Enter the buffer A value in the function TITRATION of method
= 0.1 mol/L; 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").
Standard
General procedure:
Instruments DL50Graphix, DL53/55/58, 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)
Rondo 60 Sample changer
3. Blank determ. of Solvent 4739 (M518, Method 90018)
4. Determ. of the base number (BN) (M520, Method 90020)
Balance, printer
Remarks
Indication DG113-SC Base number according to ASTM D4739-92
Consumption of mg KOH/g oil to buffer value A or to the EQP in
the range "buffer value A + 100 mV"
Chemistry
Titration parameters
The titration parameters correspond exactly to the standard ASTM
D4739:
1. Titrant addition 0.1 mL every 90 seconds.
2. The titration will be terminated when the potential is 120 mV
above buffer value A.
Calculation R1 = consumption of mg KOH/g oil to the
buffer value A
Conditioning
R2 = consumption of mg KOH/g oil to EQP After every titration the electrode is conditioned in water for 5
nearest to the buffer value A minutes and then rinsed with solvent 4739. With this method
the conditioning is automatically proceeded, if on the sample
If there is no EQP, the result is negative. changer after every sample a conditioning beaker with 60 mL
deion. water is placed.
(Blank value of the solvent).
Results
Waste Separate water and halogenated Literature:

disposal organic solvent before disposing. ASTM D4739-92 (www.astm.org)
Application brochure 3, "TAN and TBN", ME-724559
82
Results
Method 90020 BN ASTM D4739 01-Jul-1995 12:00

User
RESULTS
1 Oil 1.7955 g
R1 = 9.90 mg KOH/g BN (buffer A)
R2 = 10.88 mg KOH/g BN (EQP)
2 Oil 2.1974 g
3 Oil 1.9269 g
4 Oil 2.1927 g
5 Oil 1.8911 g
STATISTICS
Mean value x = 9.74 mg KOH/gBN (buffer A)
Standard deviation s = 0.10709 mg KOH/gBN (buffer A)
STATISTICS
Mean value x = 10.86 mg KOH/gBN (EQP)
Standard deviation s = 0.04364 mg KOH/gBN (EQP)
83
Method
Method 90020 BN ASTM D4739 Calculation
Version 01-Jul-1995 12:00 Formula . . . . . . . . . . . . . . R1=(QP1-H11)*M/m
Constant . . . . . . . . . . . . . .
Title Decimal places . . . . . . . . . . . 2
Method ID . . . . . . . . . . . . . 90020 Result unit . . . . . . . . . . . . mg KOH/g
Title . . . . . . . . . . . . . . . BN ASTM D4739 Result name . . . . . . . . . . . . BN (buffer A)
Date/time . . . . . . . . . . . . . 01-Jul-1995 12:00 Statistics . . . . . . . . . . . . . Yes
Sample Calculation
Sample ID . . . . . . . . . . . . . Oil Formula . . . . . . . . . . . . . . R2=(Q(EPOT~P1)-H11)*C2
Entry type . . . . . . . . . . . . . Weight Constant . . . . . . . . . . . . . . C2=M/m
Lower limit [g] . . . . . . . . . 0.1 Decimal places . . . . . . . . . . . 2
Upper limit [g] . . . . . . . . . 20.0 Result unit . . . . . . . . . . . . mg KOH/g
Molar mass M . . . . . . . . . . . . 56.1 Result name . . . . . . . . . . . . BN (EQP)
Equivalent number z . . . . . . . . 1 Statistics . . . . . . . . . . . . . Yes
Titration stand . . . . . . . . . . ST20A Calculation
Pump . . . . . . . . . . . . . . Yes Formula . . . . . . . . . . . . . .
Solvent . . . . . . . . . . . Solvent 4739 Constant . . . . . . . . . . . . . .
Volume [mL] . . . . . . . . . 60.0 Decimal places . . . . . . . . . . . 0
Rinse . . . . . . . . . . . . . . Yes Result unit . . . . . . . . . . . .
Solvent . . . . . . . . . . . Solvent 4739 Result name . . . . . . . . . . . .
Volume [mL] . . . . . . . . . 20.0 Statistics . . . . . . . . . . . . . No
Conditioning . . . . . . . . . . Yes Report
Time [s] . . . . . . . . . . . 300 Output unit . . . . . . . . . . . . Printer
Rinse . . . . . . . . . . . . Yes Results . . . . . . . . . . . . . . No
Solvent . . . . . . . . . . Solvent 4739 All results . . . . . . . . . . . . Yes
Volume [mL] . . . . . . . . 20.0 Raw results . . . . . . . . . . . . Yes
Temperature sensor . . . . . . . . . Manual Table of measured values . . . . . . Yes
Stir Sample data . . . . . . . . . . . . No
Speed [%] . . . . . . . . . . . . . 60 E - V curve . . . . . . . . . . . . Yes
Time [s] . . . . . . . . . . . . . . 60 dE/dV - V curve . . . . . . . . . . No
EQP titration d2E/dV2 - V curve . . . . . . . . . No
Titrant/Sensor log dE/dV - V curve . . . . . . . . No
Titrant . . . . . . . . . . . . . HCl (i-PrOH) E - t curve . . . . . . . . . . . . No
Concentration [mol/L] . . . . . . 0.1 V - t curve . . . . . . . . . . . . No
Sensor . . . . . . . . . . . . . DG113 dV/dt - t curve . . . . . . . . . . No
Unit of meas. . . . . . . . . . . mV
Predispensing . . . . . . . . . . . to volume
Volume [mL] . . . . . . . . . . . 0.2
Titrant addition . . . . . . . . . . Incremental
dV [mL] . . . . . . . . . . . . . 0.1
Measure mode . . . . . . . . . . . . Time incremental
dt [s] . . . . . . . . . . . . . 90.0
Recognition
Threshold . . . . . . . . . . . . 200.0
Steepest jump only . . . . . . . No
Range . . . . . . . . . . . . . . Yes
Limit A [mV,pH,...] . . . . . 154
Limit B [mV,pH,...] . . . . . 254
Termination
at potential . . . . . . . . . . Yes
Potential [mV,pH,..] . . . . . 300
at slope . . . . . . . . . . . . No
after number EQPs . . . . . . . . No
comb. termination conditions . . No
Evaluation
Procedure . . . . . . . . . . . . Standard
Potential 1 . . . . . . . . . . . Yes
Pot. 1 [mV,pH,...] . . . . . . 154
Potential 2 . . . . . . . . . . . No
Stop for reevaluation . . . . . . No
84
METTLER TOLEDO M057
TBN According to ASTM D 2896-85

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

1) The sample is weighed in a titration beaker and placed on
the sample changer rack.
2) The solvent 2896 is automatically added by the pump
(Function PUMP).
General procedure for direct titration :
1. Blank determination of solvent 2896 (method 096B). The
Chemicals 50 mL Solvent mixture blank is stored as auxiliary value H10 (mL)
(Acetic acid:chlorobenzene, 1:2) 2. Titer determination of perchloric acid using KHP in solvent
2896. The solvent blank H10 in mL has to be taken into
account for the titer determination (method 096C).
3. The solvent blank value H10 (mL) is expressed in mmol
Titrant 0.1 mol/L HClO4 in glacial acetic acid, using the titer. The result is stored as auxiliary value H11.
4. TBN determination (method 096A)
Sodium acetate in glacial acetic acid
c(CH3COONa)= 0.1 mol/L Note:
If the direct titration cannot find an equivalence point, a back
Standard KHP; HClO4 in glacial acetic acid titration has to be performed: a known amount HClO4 is added
to the sample, and the excess is titrated with sodium acetate.
Instruments DL70ES, DL77; General procedure (back titration):
Rondo 60 Sample changer 1. Titer determination of sodium acetate with standardized
perchloric acid. Blank H11 must be taken into account in the
calculation for the titer: R=(QDISP-H11)/(VEQ*c)
2. TBN determination by back titration. Blank H11 must be
Accessories 100 mL beaker ME-101974, taken into account for the base number:
1 additional burette DV1010, R=(QDISP-H11-Q)*C/m
10 mL syringe ME-71482
Remarks
Indication DG113-SC at Sensor 1 TBN:
Consumption of perchloric acid until the inflection point. It is
expressed as the equivalent quantity t of mg KOH/g sample.
Chemistry
1) The blank of the solvent has to be determined regularly, at
least after preparing a new stock of solvent mixture.
2) After each titration the electrode is conditioned in water.
3) It is recommended to condition a spare electrode in water.

Calculation This allows an alternating use of the electrodes or a quick
Base no. determination (096A):
replacement.
R = (Q-H11)*C/m
C = M/z , where M = 56.1, z = 1 4) ASTM D2896 specifies saturated sodium perchlorate in acetic
mg KOH/g acid as electrolyte. The replacement is straighforward.
5) The sample size is calculated according to the standard will

give a titrant consumption of about 5 mL.
Results
6) Using the methods of this application note the titrations will
Waste take about 10 to 15 minutes only.
Halogenated organic waste. Separate
disposal the aquoeus pahse (upper) from the 7) KHP is dissolved externally in 50 mL solvent at 50°C using
organic phase (lower). an ultra sonic bath.
Literature: ASTM 2896-85 (www.astm.org)

Author Urs Büchi
85
Results
METTLER DL70 Titrator Mettler-Toledo AG
Application Laboratory
96d ASTM D 2896-85 (direct) measured 11-11-1991 10:08

08-11-1991 13:40 Titrator PT 7
SW Version 2.0 User ub
RESULTS
No IDentification Weight Results
1/1 Oil 85/06 1.9882 g 12.78 mg KOH/g base number
STATISTICS
Mean value x = 12.74 mg KOH/g base number
Standard deviation s = 0.039 mg KOH/g base number
Note:
The same oil was titrated directly and by back titration.
The results differ less than 1%.
86
Method
Method 096A ASTM D 2896-85 (direct) Title
Version 08-Nov-1991 13:40 Method ID . . . . . . . . . . . . . 096B
Title . . . . . . . . . . . . . . . Blank ASTM D2896-85
Title Date/time . . . . . . . . . . . . . 07-11-1991 11:26
Method ID . . . . . . . . . . . . . 096A Sample
Title . . . . . . . . . . . . . . . ASTM D 2896-85 (direct) Number samples . . . . . . . . . . . 3
Date/time . . . . . . . . . . . . . 08-Nov-1991 13:40 Titration stand . . . . . . . . . . ST20
Sample Entry type . . . . . . . . . . . . . Fixed volume U
Number samples . . . . . . . . . . . 3 Volume[mL] . . . . . . . . . . . 50.0
Titration stand . . . . . . . . . . ST20 ID1 . . . . . . . . . . . . . . . . Blank
Entry type . . . . . . . . . . . . . Weight m Molar mass M . . . . . . . . . . . . 0.0
Lower limits[g] . . . . . . . . . 0.1 Equivalent number z . . . . . . . . 1
Upper limits[g] . . . . . . . . . 20.0 Pump
ID1 . . . . . . . . . . . . . . . . Oil Auxiliary reagent . . . . . . . . . AcOH-C6H5Cl 1:2
Molar mass M . . . . . . . . . . . . 56.1 Volume [mL] . . . . . . . . . . . . 50.0
Equivalent number z . . . . . . . . 1 Stir
Pump Speed [%] . . . . . . . . . . . . . 60
Auxiliary reagent . . . . . . . . . AcOH-C6H5Cl 1:2 Time [s] . . . . . . . . . . . . . . 30
Volume [mL] . . . . . . . . . . . . 50.0 Titration
Stir Titrant . . . . . . . . . . . . . . HClO4
Speed [%] . . . . . . . . . . . . . 60 Concentration [mol/L] . . . . . . . 0.1
Time [s] . . . . . . . . . . . . . . 60 Sensor . . . . . . . . . . . . . . . DG113-SC
Titration Unit of meas. . . . . . . . . . . . mV
Titrant . . . . . . . . . . . . . . HClO4 Titration mode . . . . . . . . . . . EQP
Concentration [mol/L] . . . . . . . 0.1 Titrant addition . . . . . . . . INC
Sensor . . . . . . . . . . . . . . . DG113-SC dV(min) [mL] . . . . . . . . . 0.01
Unit of meas. . . . . . . . . . . . mV Measure mode . . . . . . . . . . EQU
Titration mode . . . . . . . . . . . EQP dE [mV] . . . . . . . . . . . 0.5
Predispensing 1 . . . . . . . . . mL dt [s] . . . . . . . . . . . 6.0
Volume [mL] . . . . . . . . 2.0 t(min) [s] . . . . . . . . . . 6.0
Titrant addition . . . . . . . . DYN t(max) [s] . . . . . . . . . . 60.0
dE(set) [mV] . . . . . . . . 30.0 Threshold . . . . . . . . . . . 500.0
Limits dV . . . . . . . . . . Absolute Maximum volume [mL] . . . . . . . 0.5
dV(min) [mL] . . . . . . . 0.05 Termination after n EQPs . . . . Yes
dV(max) [mL] . . . . . . . 0.1 n = . . . . . . . . . . . . . 1
Measure mode . . . . . . . . . . EQU Evaluation procedure . . . . . . Standard
dE [mV] . . . . . . . . . . . 0.5 Calculation
dt [s] . . . . . . . . . . . 6.0 Result name . . . . . . . . . . . . Blank volume
t(min) [s] . . . . . . . . . . 6.0 Formula . . . . . . . . . . . . . . R=VEQ
t(max) [s] . . . . . . . . . . 60.0 Result unit . . . . . . . . . . . . mL
Threshold . . . . . . . . . . . 75.0 Decimal places . . . . . . . . . . 4
Maximum volume [mL] . . . . . . . 10.0 Record
Termination after n EQPs . . . . Yes Output unit . . . . . . . . . . . . Printer
n = . . . . . . . . . . . . . 1 Raw results last sample . . . . . . Yes
Evaluation procedure . . . . . . Standard Rinse
Calculation Auxiliary reagent . . . . . . . . . AcOH-C6H5Cl 1:2
Result name . . . . . . . . . . . . base number Volume [mL] . . . . . . . . . . . . 15.0
Formula . . . . . . . . . . . . . . R=(Q-H11)*C/m Conditioning
Constant . . . . . . . . . . . . . C=M/z Interval . . . . . . . . . . . . . 1
Result unit . . . . . . . . . . . . mg KOH/g Time [s] . . . . . . . . . . . . . 30
Decimal places . . . . . . . . . . 2 Rinse . . . . . . . . . . . . . . . Yes
Condition . . . . . . . . . . . . . Yes Auxiliary reagent . . . . . . . . AcOH-C6H5Cl 1:2
Condition . . . . . . . . . . . Q>0 Volume [mL] . . . . . . . . . . . 15.0
Record Statistics
Output unit . . . . . . . . . . . . Printer Ri (i=index) . . . . . . . . . . . . R1
Raw results last sample . . . . . . Yes Auxiliary value
Table of measured values . . . . . . Yes ID text . . . . . . . . . . . . . . Blank volume
E - V curve . . . . . . . . . . . . Yes Formula . . . . . . . . . . . . . . H10=x
Rinse Record
Auxiliary reagent . . . . . . . . . AcOH-C6H5Cl 1:2 Output unit . . . . . . . . . . . . Printer
Volume [mL] . . . . . . . . . . . . 15.0 All results . . . . . . . . . . . . Yes
Conditioning Conditioning
Interval . . . . . . . . . . . . . 1 Interval . . . . . . . . . . . . . 1
Time [s] . . . . . . . . . . . . . 180 Time [s] . . . . . . . . . . . . . 1
Rinse . . . . . . . . . . . . . . . Yes
Auxiliary reagent . . . . . . . . AcOH-C6H5Cl 1:2
Volume [mL] . . . . . . . . . . . 15.0 Method 096C Titer of HClOO4 (0.1mol/L)
Statistics
Ri (i=index) . . . . . . . . . . . . R1 Calculation
Standard deviation s . . . . . . . . Yes Result name . . . . . . . . . . . . Titer HClO4
Rel. standard deviation srel . . . . Yes Formula . . . . . . . . . . . . . . R=m/((VEQ-H10)*c*C)
Outlier test . . . . . . . . . . . Yes Result unit . . . . . . . . . . . . mL
Record Calculation
Output unit . . . . . . . . . . . . Printer Result name . . . . . . . . . . . . Blank
All results . . . . . . . . . . . . Yes Formula . . . . . . . . . . . . . . R2=H10*0.1*x
Conditioning Result unit . . . . . . . . . . . . mmoL
Interval . . . . . . . . . . . . . 1 Auxiliary value
Time [s] . . . . . . . . . . . . . 1 ID text . . . . . . . . . . . . . . Blank
Formula . . . . . . . . . . . . . . H11=R2
87
METTLER TOLEDO M058
TBN According to ASTM D4739-87

Method for the determination of TBN according to ASTM D 4739-87 in motor oil.
Sample Various oil, 0.1-20 g Preparation and Procedures

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

Method for the determination of TAN According to ASTM D 664-89, in various oils.
Sample Various oils 0.1 - 20 g Preparation and Procedures

1) The sample is weighed in a titration beaker and placed onthe
sample changer rack.
2) The solvent 664 is automatically added by the pump.
(Function PUMP).
General procedure:
1. Titer determination of KOH in isopropanol by dissolving
Chemicals 50 mL Solvent mixture 664, 70-100 mg in 50 mL water (example: M002, M027, M534).
Toluene:water:isopropanol 2. Titer determination of HCl in isopropanol using 5 mL of
500:5:495 standardized KOH titrant soltuion (Method 059C).
3. Measurement of the buffer potential A and B (059B).
4. Blank determination for Acid Number AN (with KOH, method
Titrant KOH in iopropanol (i-PrOH) 059D) and Strong Acid Number SAN (with HCl, method 059E).
HCl in i-PrOH c(HCl) = 0.1 mol/L 5. Titration of samples (method 059A).
Note:
1. The sample has to be well homogenized before weighing.
Standard 1) KHP, 2) standard. KOH in i-PrOH Used oils may be heated to 50 - 60 °C and filtered if sediments
are present.
Instruments DL70ES/DL77; 2. The values for buffer potentials from method 059B have to be
entered manually into method 059A.
Rondo 60 sample changer,
3. The difference between the two potential values must be at
Balance, printer 300 mV, otherwise the electrode must be checked.
Accessories Glass beaker ME101446,
1 add. burette drive DV90, 1 add. glas
burette Dv1010
Remarks
Indication DG113-SC at Sensor 1 1) Standard ASTM 664-89 requires the evaluation of the KOH
consumption at acid buffer potential (SAN) or the consumption
up to the EQP nearest to buffer B (AN).
Chemistry If no EQP can be found, then the consumption at buffer B (i.e.
buffer potential 2) is evaluated (AN). Therefore, an evaluation
window "EQP range" is activated. Within this range, the most
significant EQP only is evaluated ("steepest jump only yes").
2) The limits of the EQP range in method 059A are set to ± 100
mV of the buffer B (manual entry). The window can be modified
as required by the user. The limits are entered manually.
Calculation 3) Calculations in method 059A:
Method 059A (Sample determination):
R1: Calculation of the SAN if there is a titrant consumption up to
R1=(QP1+H15)*C/m , C=56.1 the acidic buffer A (Condition: "VP1>0).
SAN (Strong acid number), mg KOH/g R2: Calculation of the BN based on the titrant consumption up to
R2=(QP2-H14)*C2/m , C2=56.1 basic baffer B , if no EQP was found (Condition: "VEQ=0").
AN (Acid number), mg KOH/g R3: BN based on a found EQP (Condition: "VEQ>0").
R3=(Q-H14)*C/m, C3=56.1 4) A conditioning beaker with 60 mL deion. water is placed after
AN (acid number), mg KOH/g each sample on the sample tray ("conditioning interval = 1").
Results 5) The electrode, stirrer and burette tip are rinsed with 20 mL
solvent 664 before next sample. At the end of a series two
Waste conditioning beakers are placed to store the electrode in water.
Separate organic phase from water.
disposal Disposal as aromatic organic solvent. Literature:
ASTM D664-89 (www.atm.org)
Application brochure 20, ME51725020
Applications M576, M577, M578, M579, M580, M581, M582
Author Urs Büchi
91
Results
Sample Weight n Strong Acid Number (SAN) Acid Number (AN) Time
[g] mg KOH/g sabs RSD[%] mg KOH/g sabs RSD[%] [min]
Motor
Oil new ~5 3 no SAN - - 1.33 1) 0.036 2.71 31
Motor Oil
I used ~1 3 1.06 0.023 2.15 8.73 1) 0.032 0.36 27
Motor Oil
II used ~5 3 no SAN - - 2.93 1) 0.054 1.86 35
Arabian
light 15-20 3 no SAN - - 0.09 2) 0.005 5.12 25
Hydraulic
Oil I 15-20 3 0.11 0.002 1.97 0.25 1) 0.004 1.56 15
Hydraulic
Oil II 15-20 3 no SAN - - 0.06 2) 0.005 7.92 13
Hydraulic
Oil III 15-20 3 no SAN - - 0.12 1) 0.001 0.85 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( γ-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.
92
Method
Method 059A ASTM D 664-89 Record
Version 07-May-1992 09:32 Output unit . . . . . . . . . . . . Printer
Raw results last sample . . . . . . Yes
Title E - V curve . . . . . . . . . . . . Yes
Method ID . . . . . . . . . . . . . 059A Table of measured samples . . . . . Yes
Title . . . . . . . . . . . . . . . ASTM D 664-89 dE/dV - V curve . . . . . . . . . . Yes
Date/time . . . . . . . . . . . . . 07-May-1992 09:32 Conditioning
Sample Interval . . . . . . . . . . . . . 1
Number samples . . . . . . . . . . . 3 Time [s] . . . . . . . . . . . . . 300
Titration stand . . . . . . . . . . ST20 Rinse . . . . . . . . . . . . . Yes
Entry type . . . . . . . . . . . . . Weight m Auxiliary reagent . . . . . . . . Solvent 664
Lower limits[g] . . . . . . . . . 0.1 Volume [mL] . . . . . . . . . . . 20.0
Upper limits[g] . . . . . . . . . 20.0 Statistics
ID1 . . . . . . . . . . . . . . . . Oil Ri (i=index) . . . . . . . . . . . . R1
Molar mass M . . . . . . . . . . . . 56.1 Standard deviation s . . . . . . . . Yes
Equivalent number z . . . . . . . . 1 Rel. standard deviation srel . . . . Yes
Pump Outlier test . . . . . . . . . . . Yes
Auxiliary reagent . . . . . . . . . solvent 664 Statistics
Volume [mL] . . . . . . . . . . . . 50.0 Ri (i=index) . . . . . . . . . . . . R2
Stir Standard deviation s . . . . . . . . Yes
Speed [%] . . . . . . . . . . . . . 60 Rel. standard deviation srel . . . . Yes
Time [s] . . . . . . . . . . . . . . 60 Outlier test . . . . . . . . . . . Yes
Titration Statistics
Titrant . . . . . . . . . . . . . . KOH in i-PrOH Ri (i=index) . . . . . . . . . . . . R3
Concentration [mol/L] . . . . . . . 0.1 Standard deviation s . . . . . . . . Yes
Sensor . . . . . . . . . . . . . . . DG113-SC Rel. standard deviation srel . . . . Yes
Unit of meas. . . . . . . . . . . . mV Outlier test . . . . . . . . . . . Yes
Titration mode . . . . . . . . . . . EQP Record
Predispensing 1 . . . . . . . . . mL Output unit . . . . . . . . . . . . Printer
Volume [mL] . . . . . . . . 0.2 All results . . . . . . . . . . . . Yes
Titrant addition . . . . . . . . DYN Conditioning
dE(set) [mV] . . . . . . . . 30.0 Interval . . . . . . . . . . . . . 1
Limits dV . . . . . . . . . . Absolute Time [s] . . . . . . . . . . . . . 10
dV(min) [mL] . . . . . . . . . 0.05
dV(max) [mL] . . . . . . . . . 0.2
Measure mode . . . . . . . . . . EQU
dE [mV] . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . . 6.0
t (min) [s] . . . . . . . . 30.0 Buffer determination ASTM D 664-89:
t (max) [s] . . . . . . . . 90.0
Threshold . . . . . . . . . . . . 300 Both buffers can be determined automatically with the sample
EQP range . . . . . . . . . . . . yes changer. First buffer A is measured, then buffer B. The
Limit A [mV,pH..] . . . . . -44.7 electrode is conditioned before measuring the next buffer.
Limit B [mV,pH..] . . . . . -244.7
Maximum volume [mL] . . . . . . . 10.0 Buffer A -> R1 = E[1] = 166.4147 mV -> stored as aux. value
Termination at slope . . . . . . Yes H12
Slope [mV,pH../mL] . . . . . 50.0 Buffer B -> R2 = E[2] = -144.7011 mV -> stored as aux. value
Evaluation prodedure . . . . . . Standard H13
Steepest jump only . . . . . . . Yes
Buffer potential 1 . . . . . . . Yes
Buffer potential 1 . . . . . 166.4
Buffer potential 2 . . . . . . . Yes Blank determination for AN Method 059D:
Buffer potential 2 . . . . . -144.7 Solvent 664-89 is dispensed automatically by a pump.
Calculation Titrant:
Result name . . . . . . . . . . . . SAN KOH in isopropanol, R = Q , stored as aux. value H14
Formula . . . . . . . . . . . . . . R=(QP1+H15)*C/m
Constant . . . . . . . . . . . . . . C=56.1
Result unit . . . . . . . . . . . . mg KOH/g Blank determination for SAN Method 059E:
Decimal places . . . . . . . . . . . 2 Solvent 664-89 is dispensed automatically by a pump.
Condition . . . . . . . . . . . . . Yes Titrant:
Condition . . . . . . . . . . . VP1>0 HCl in isopropanol, R = Q , stored as aux. value H15
Calculation
Result name . . . . . . . . . . . . Acid number
Formula . . . . . . . . . . . . . . R2=(QP2+H14)*C2/m
Constant . . . . . . . . . . . . . . C2=56.1
Decimal places . . . . . . . . . . . 2
Condition . . . . . . . . . . . . . Yes
Condition . . . . . . . . . . . VEQ=0
Calculation
Result name . . . . . . . . . . . . Acid number
Formula . . . . . . . . . . . . . . R3=(Q+H14)*C/m
Constant . . . . . . . . . . . . . . C3=56.1
Decimal places . . . . . . . . . . . 2
Condition . . . . . . . . . . . . . Yes
Condition . . . . . . . . . . . VEQ]0
Rinse
Auxiliary reagent . . . . . . . . . Solvent 664
Volume [mL] . . . . . . . . . . . . 20.0
93
METTLER TOLEDO M099
Conductometric Base Number Titration of Motor Oil

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

1) Titrant preparation:
The titrant can be prepared manually by adding 9 mL 37% v/v
HCl and filling up to 1 L with isopropanol (2-propanol).
Substance Basic components, expressed as KOH
2) The titrant is standardized with a solution of potassium
hydrogen phtalate of known concentration (see application
M100).
Toluene:isopropanol:distilled water 3) MCP227 calibration:
(50% (v/v):49.5%(v/v):0.5%(v/v) ) 3.1 The conductivity meter is calibrated before titration using air
(0 µS/cm) and 1413 µS/cm.
3.2 The linear output range of the MPC227 conductivity meter
Titrant HCl in isopropanol: has to be appropriate to the measuring range during the
c(HCl) = 0.1 mol/L 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.
Standard Potassium hydrogen phthalate c. Keep pressing "Mode" until P5 is reached.
d. Select the lowest millivolt output range /midpoint: 20 µS/cm.
Instruments DL50Graphix, DL53/55/58 e. Confirm it by pressing "Mode".
DL70ES, DL77 e. Return to normal measuring by pressing "Read".
f. Check whether you have turned the automatic endpoint off.
MPC227 conductivity meter
4) If the sample contains insoluble material it must be shaken
Accessories 100 mL titration beaker ME-101974 thoroughly in the original container before it is taken.
Connection cable 51302258
1 additional burette drive DV90, 1
additional DV1010, Printer, balance
Remarks
Indication InLab717 conductivity probe 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:
Chemistry 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.
Calculation Afterwards, the probe is rinsed again with solvent mixture to
Base number determination (BN 1):
remove the last impurities. Therefore, an automatic procedure
R1 = Q*C/m ; mg KOH/g using a sample changer is not recommended.
C1 = M/z
3) If you want to monitor the conductivity values at the titrator,
M = 56.1, z =1 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 µS/cm the slope is 9.00 µS/cm,
Results and the unit is µS/cm (Check MPC227 op. instructions p. 17).
Waste Literature: IP 400/94, "Determination of Base Number of

Organic solvent waste
Petroleum Products - Conductimetric titration method"
disposal The Institute of Petroleum, London, 1994
Author K. Saegesser
94
Results
METTLER TOLEDO DL77 Titrator V3.1 Mettler-Toledo GmbH
Method BN 1 BN conductometric 23-Apr-1998 9:50

User K Sägesser
RESULTS
1/1 Oil 1.009 g Weight m

R1 = 10.338 mg KOH/g base number
STATISTICS
Outlier test: sample No. 1/2
Statistics without sample No. 1/2

95
Method
Method BN 1 BN conductometric
Version 23-Apr-1998 9:50
Title
Method ID . . . . . . . . . . . . . BN 1
Title . . . . . . . . . . . . . . . BN conductometric
Date/time . . . . . . . . . . . . . 23-Apr-1998 9:50
Sample
Number samples . . . . . . . . . . . 6
Lower limit [g] . . . . . . . . . 0.5
Upper limit [g] . . . . . . . . . 2.0
ID1 . . . . . . . . . . . . . . . . Oil
Molar mass M . . . . . . . . . . . . 56.1
Dispense
Titrant . . . . . . . . . . . . . . BN solvent
Volume [mL] . . . . . . . . . . . . 50
Stir
Speed [m%] . . . . . . . . . . . . . 45
Time [s] . . . . . . . . . . . . . . 120
Titration
Titrant . . . . . . . . . . . . . . HCl (2-prop)
Sensor . . . . . . . . . . . . . . . Cond
Unit of meas. . . . . . . . . . . . mV
Volume [mL] . . . . . . . . . 0.6
Titrant addition . . . . . . . . INC
dV [mL] . . . . . . . . . . . 0.1
Measure mode . . . . . . . . . . TFIX
dt [s] . . . . . . . . . . . . 5.0
Threshold . . . . . . . . . . . . 50.0
n = . . . . . . . . . . . . . 1
Evaluation procedure . . . . . . Segmented
Calculation
Result name . . . . . . . . . . . . base number
Formula . . . . . . . . . . . . . . R=Q*C/m
Constant . . . . . . . . . . . . . . C=M/z
Decimal places . . . . . . . . . . . 3
Record
All results . . . . . . . . . . . . Yes
E - V curve . . . . . . . . . . . . Yes
dE/dV - V curve . . . . . . . . . . Yes
d2E/dV2 - V curve . . . . . . . . . Yes
Statistics
Ri (i=index) . . . . . . . . . . . . R1
Outlier test . . . . . . . . . . . . Yes
Record
Sample data . . . . . . . . . . . . Yes
All results . . . . . . . . . . . . Yes
96
METTLER TOLEDO M100
Standardization of HCl in Isopropanol by Conductometric Titration

Standardization of alcoholic HCl by conductometric titration.
Sample 5 mL 0.1 mol/L potassium hydrogen Preparation and Procedures

phtalate solution (KHP) 1) Titrant preparation:
The titrant can be prepared manually by adding 9 mL 37% v/v
HCl and filling up to 1 L with isopropanol (2-propanol).
Substance KHP
2) 0.1 mol/L KHP solution:
Dissolve KHP in 200 mL water by means of an ultrasonic bath
and fill up to 1 L with isopropanol.
Toluene:isopropanol:distilled water 3) MCP227 calibration:
(50% (v/v):49.5%(v/v):0.5%(v/v) ) 3.1 The conductivity meter is calibrated before titration using air
(0 µS/cm) and 1413 µS/cm.
3.2 The linear output range of the MPC227 conductivity meter
Titrant HCl in isopropanol: has to be appropriate to the measuring range during the
c(HCl) = 0.1 mol/L 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.
Standard c. Keep pressing "Mode" until P5 is reached.
d. Select the lowest millivolt output range /midpoint: 20 µS/cm.
Instruments DL50Graphix, DL53/55/58 e. Confirm it by pressing "Mode".
DL70ES, DL77 e. Return to normal measuring by pressing "Read".
f. Check whether you have turned the automatic endpoint off.
MPC227 conductivity meter

Connection cable 51302258
1 additional burette drive DV90, 1
additional DV1010, Printer, balance
Remarks
Indication InLab717 conductivity probe 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
Chemistry range with a midpoint of 20 µS/cm the slope is 9.00 µS/cm,
and the unit is µS/cm (Check MPC227 op. instructions p. 17).
2) MPC227 Linear ranges:
Range 1: 2-200 µS/cm

Midpoint: 20 µS/cm; Slope: 9.00 mV/(µS/cm); Unit: µS/cm
Calculation Titer determination (BN 2):
Range 2: 20-2000 µS/cm
R1 = U/(VEQ*c*C)
Midpoint: 200 µS/cm Slope: 0.90 mV/(µS/cm), Unit: µS/cm
C1 = 1/(0.1*z)
Range 3: 0.2-20 mS/cm
Midpoint: 2.0 mS/cm; Slope: 90.00 mV/(µS/cm); Unit: mS/cm
Range 4: 2-200 mS/cm

Results Midpoint: 20 mS/cm Slope: 9.00 mV/(µS/cm), Unit: mS/cm
Waste Organic solvent waste Range 5: 20-2000 mS/cm

Midpoint: 200 mS/cm Slope: 0.90 mV/(µS/cm), Unit: mS/cm
disposal
Author K. Saegesser
97
Results
Method BN 1 BN conductometric 23-Apr-1998 9:50

User K Sägesser
RESULTS

STATISTICS
Outlier test: sample No. 1/2
98
Method
Method BN 1 BN conductometric
Version 23-Apr-1998 9:50
Title
Method ID . . . . . . . . . . . . . BN 1
Title . . . . . . . . . . . . . . . BN conductometric
Date/time . . . . . . . . . . . . . 23-Apr-1998 9:50
Sample
Number samples . . . . . . . . . . . 6
Lower limit [g] . . . . . . . . . 0.5
Upper limit [g] . . . . . . . . . 2.0
ID1 . . . . . . . . . . . . . . . . Oil
Molar mass M . . . . . . . . . . . . 56.1
Dispense
Titrant . . . . . . . . . . . . . . BN solvent
Volume [mL] . . . . . . . . . . . . 50
Stir
Speed [m%] . . . . . . . . . . . . . 45
Time [s] . . . . . . . . . . . . . . 120
Titration
Titrant . . . . . . . . . . . . . . HCl (2-prop)
Sensor . . . . . . . . . . . . . . . Cond
Unit of meas. . . . . . . . . . . . mV
Volume [mL] . . . . . . . . . 0.6
dV [mL] . . . . . . . . . . . 0.1
Measure mode . . . . . . . . . . TFIX
dt [s] . . . . . . . . . . . . 5.0
Threshold . . . . . . . . . . . . 50.0
n = . . . . . . . . . . . . . 1
Evaluation procedure . . . . . . Segmented
Calculation
Result name . . . . . . . . . . . . base number
Formula . . . . . . . . . . . . . . R=Q*C/m
Constant . . . . . . . . . . . . . . C=M/z
Decimal places . . . . . . . . . . . 3
Record
All results . . . . . . . . . . . . Yes
E - V curve . . . . . . . . . . . . Yes
dE/dV - V curve . . . . . . . . . . Yes
d2E/dV2 - V curve . . . . . . . . . Yes
Statistics
Ri (i=index) . . . . . . . . . . . . R1
Outlier test . . . . . . . . . . . . Yes
Record
Sample data . . . . . . . . . . . . Yes
All results . . . . . . . . . . . . Yes
99
METTLER TOLEDO M061
pH, Acidity, Lactone and Formol Value of Honey

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

1) The sample is weighed in the titration beaker and mounted at
the titration head.
2) Deionized water is automatically added by the peristaltic

Substance Organic acids, lactone, free amino
pump.
acids
3) First the pH value and the acidity content are determined.
Chemicals 40 mL deionized water
4) Then the lactone value is determined by means of two
titration.
5) Finally, the formol value is determined after addition of formol

Titrant 0.1mol/L HCl; 0.1 mol/L NaOH; 36.5% solution which is neutralized to pH 8.
Formol to pH 8.0 with NaOH
Note:
Standard 1) THAM (NaOH), 2) KHP (HCl) A blank value determination is performed before sample
analysis. This is used in calculation R3 (Lactone content). The
Instruments DL70ES/DL77, balance 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
Remarks
Indication DG111-SC at Sensor 1 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.
Chemistry Free amino acids (formol no.):
R-COOH-NH2 + HCHO = H2O + R-COOH-N=CH2 1) pH and acidity:
R-COOH-N=CH2 + OH- = R-COO--N=CH2 + H2O 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
Calculation may further contain butyric, acetic, formic and lactic acid.
pH (R1) & Acidity (R2):
R1=E ; R2=Q[1]*C2/m, C2=1000; 2) Formol value:
Lactone content: The formol value is a measure of the free amino acids. Its usual
R3=(Q[2]+Q[3]-H11)*C3, level is between 4.5 and 15.5 mmol/kg. A low formol value
C3=1000/m indicates adulteration with artificial honey or additional feeding
Formol value: of the bees with sugar. The formol value is determined by
R4=Q[5]*C4/m, C4=1000 adding a formol solution which must be neutralized prior
Results determination.
Waste 3) Lactone value:

Aqueous solutions The lactone content varies between 2-20 mmol/kg.
disposal
Literature:
Schweizerisches Lebensmittelbuch, Band II, Chap. 23
AOAC Official Methods of Analysis, 1984, pages 595-596
Author Ruth von Rotz
100
Results
RESULTS
1/1 Ex.honey 10.3302 g 3.819 pH
21.869 mmol/kg Acidity
15.010 mmol/kg Lactone cont.
8.539 mmol/kg Formol value
1/2 Ex.honey 10.287 g 3.782 pH
1/3 Ex.honey 10.3434 g 3.768 pH
1/4 Ex.honey 10.3955 g 3.766 pH
1/5 Ex.honey 10.3756 g 3.764 pH
STATISTICS
Mean value x = 21.642 mmol/kg Acidity
Standard deviation s = 0.1413 mmol/kg Acidity
STATISTICS
Mean value x = 14.853 mmol/kg Lactone cont.
Standard deviation s = 0.1504 mmol/kg Lactone cont.
STATISTICS
Mean value x = 21.642 mmol/kg Formol value
Standard deviation s = 0.1413 mmol/kg Formol value
Outlier test: Sample No. 1/1
Statistics without sample No 1/1

Mean value x = 9.026 mmol/kg Formol value
Standard deviation s = 0.0723 mmol/kg Formol value
pH Acidity Lactone Formol value

Sample Result RSD Result RSD Result RSD Result RSD
(%) (mmol/kg) (%) (mmol/kg) (%) mmol/kg) (%)
Mountain honey 3.78 0.61 21.64 0.65 14.85 1.01 8.93 2.54
French honey 4.01 0.33 17.11 0.70 10.16 1.65 4.27 1.95
Swiss honey 1 4.37 0.33 11.59 0.75 6.39 2.57 2.36 3.56
Swiss honey 2 3.98 0.69 8.51 0.81 3.95 4.85 2.77 0.30
101
Method
Method R1 pH,ac.,lact.,form. No Honey Dispense
Version 11-July-1991 1:23 pm Titrant . . . . . . . . . . . . . . Formol 36.5%
Volume [mL] . . . . . . . . . . . . 15.0
Title Stir
Method ID . . . . . . . . . . . . . R1 Speed [%] . . . . . . . . . . . . . 50
Title . . . . . . . . . . . . . . . pH,ac.,lact.,form. No Honey Time [s] . . . . . . . . . . . . . . 60
Date/time . . . . . . . . . . . . . 11-July-1991 1:23 pm Titration
Sample Titrant . . . . . . . . . . . . . . NaOH
Number samples . . . . . . . . . . . 3 Concentration [mol/L] . . . . . . . 0.1
Titration stand . . . . . . . . . . Stand 1 Sensor . . . . . . . . . . . . . . . DG111-SC
Entry type . . . . . . . . . . . . . Weight m Unit of meas. . . . . . . . . . . . As installed
Lower limit [g] . . . . . . . . . 9.0 Titration mode . . . . . . . . . . . EP
Upper limit [g] . . . . . . . . . 11.0 Titrant addition . . . . . . . . Continuous
ID1 . . . . . . . . . . . . . . . . CH honey Control band[mV,pH..] . . . . 3.0
Molar mass M . . . . . . . . . . . . 0.0 Delay [s] . . . . . . . . . . 10
Equivalent number z . . . . . . . . 1 End point mode . . . . . . . . . EPA
Pump Potential [mV,pH..] . . . . 8.0
Auxiliary reagent . . . . . . . . . H2O Tendency . . . . . . . . . . . . Positive
Volume [mL] . . . . . . . . . . . . 40.0 Maximum volume [mL] . . . . . . . 10.0
Stir Calculation
Speed [%] . . . . . . . . . . . . . 90 Result name . . . . . . . . . . . . pH
Time [s] . . . . . . . . . . . . . . 150 Formula . . . . . . . . . . . . . . R=E
Stir Constant . . . . . . . . . . . . . .
Speed [%] . . . . . . . . . . . . . 50 Result unit . . . . . . . . . . . .
Time [s] . . . . . . . . . . . . . . 30 Decimal places . . . . . . . . . . . 3
Measure Calculation
Sensor . . . . . . . . . . . . . . . DG111-SC Result name . . . . . . . . . . . . Acidity
Unit of meas. . . . . . . . . . . . As installed Formula . . . . . . . . . . . . . . R2=Q[1]*C2/m
dE [mV] . . . . . . . . . . . 0.5 Constant . . . . . . . . . . . . . . C2=1000
dt [s] . . . . . . . . . . . . 1.5 Result unit . . . . . . . . . . . . mmol/kg
t(min) mode . . . . . . . . . Fix Decimal places . . . . . . . . . . . 3
t (min) [s] . . . . . . . . 10.0 Calculation
t (max) [s] . . . . . . . . 30.0 Result name . . . . . . . . . . . . Lactone cont.
Titration Formula . . . . . . . . . . . . . . R3=(Q[2]+Q[3]-H11)*C3
Titrant . . . . . . . . . . . . . . NaOH Constant . . . . . . . . . . . . . . C3=1000/m
Concentration [mol/L] . . . . . . . 0.1 Result unit . . . . . . . . . . . . mmol/kg
Sensor . . . . . . . . . . . . . . . DG111-SC Decimal places . . . . . . . . . . . 3
Unit of meas. . . . . . . . . . . . As installed Calculation
Titration mode . . . . . . . . . . . EP Result name . . . . . . . . . . . . Formol value
Predispensing 1 . . . . . . . . . mL Formula . . . . . . . . . . . . . . R4=Q[5]*C4/m
Volume [mL] . . . . . . 0.7 Constant . . . . . . . . . . . . . . C4=1000
Titrant addition . . . . . . . . Dynamic Result unit . . . . . . . . . . . . mmol/kg
dV (set)[mV] . . . . . . . 8.0 Decimal places . . . . . . . . . . . 3
dV(min) [mL] . . . . . . . 0.02 Record
dV(max) [mL] . . . . . . . 0.1 Output unit . . . . . . . . . . . . Printer
dE [mV] . . . . . . . . . . . 0.5 Raw results last sample . . . . . . Yes
dt [s] . . . . . . . . . . . . 0.5 Results last sample . . . . . . . . Yes
t (min) [s] . . . . . . . . 2.0 Table of measured values . . . . . . Yes
t (max) [s] . . . . . . . . 20.0 Statistics
End point mode . . . . . . . . . EPA Ri (i=index) . . . . . . . . . . . . R2
Potential [mV,pH..] . . . . 7.0 Standard deviation s . . . . . . . . Yes
Tendency . . . . . . . . . . . . Positive Rel. standard deviation srel . . . . Yes
Maximum volume [mL] . . . . . . . 10.0 Outlier test . . . . . . . . . . . . Yes
Record Statistics
Output unit . . . . . . . . . . . . Printer Ri (i=index) . . . . . . . . . . . . R3
Table of measured values . . . . . . Yes Standard deviation s . . . . . . . . Yes
Titration Rel. standard deviation srel . . . . Yes
Titrant . . . . . . . . . . . . . . NaOH Outlier test . . . . . . . . . . . . Yes
Concentration [mol/L] . . . . . . . 0.1 Statistics
Sensor . . . . . . . . . . . . . . . DG111-SC Ri (i=index) . . . . . . . . . . . . R4
Unit of meas. . . . . . . . . . . . As installed Standard deviation s . . . . . . . . Yes
Titration mode . . . . . . . . . . . EP Rel. standard deviation srel . . . . Yes
Predispensing 1 . . . . . . . . . mL Outlier test . . . . . . . . . . . . Yes
Volume [mL] . . . . . . 3.0 Record
Titrant addition . . . . . . . . Dynamic Output unit . . . . . . . . . . . . Printer
dV (set)[mV] . . . . . . . 8.0 All results . . . . . . . . . . . . Yes
dV(min) [mL] . . . . . . . 0.02
dV(max) [mL] . . . . . . . 0.3
dE [mV] . . . . . . . . . . . 0.5 Method R1a Blank for Honey
dt [s] . . . . . . . . . . . . 0.5 Version 11-07-1991 11:25 am
t (min) [s] . . . . . . . . 2.0
t (max) [s] . . . . . . . . 20.0 Title
End point mode . . . . . . . . . EPA Method ID . . . . . . . . . . . . . R1a
Potential [mV,pH..] . . . . 9.8 Title . . . . . . . . . . . . . . . Blank for Honey
Tendency . . . . . . . . . . . . Positive Date/time . . . . . . . . . . . . . 11-07-1991 11:25 am
Maximum volume [mL] . . . . . . . 10.0 Sample
Stir Number samples . . . . . . . . . . . 3
Speed [%] . . . . . . . . . . . . . 50 Titration stand . . . . . . . . . . Stand 1
Time [s] . . . . . . . . . . . . . . 60 Entry type . . . . . . . . . . . . . Fixed volume U
Dispense Volume [mL] . . . . . . . . . . . 5.0
Titrant . . . . . . . . . . . . . . HC1 ID1 . . . . . . . . . . . . . . . . Blank
Concentration [mol/L] . . . . . . . 0.1 Molar mass M . . . . . . . . . . . . 0.0
Volume [mL] . . . . . . . . . . . . 5.0 Equivalent number z . . . . . . . . 1
Titration Stir
Titrant . . . . . . . . . . . . . . NaOH Speed [%] . . . . . . . . . . . . . 50
Concentration [mol/L] . . . . . . . 0.1 Time [s] . . . . . . . . . . . . . . 30
Sensor . . . . . . . . . . . . . . . DG111-SC Titration
Unit of meas. . . . . . . . . . . . As installed Titrant . . . . . . . . . . . . . . NaOH
Titration mode . . . . . . . . . . . EP Concentration [mol/L] . . . . . . . 0.1
Titrant addition . . . . . . . . Continuous Sensor . . . . . . . . . . . . . . . DG111-SC
Control band[mV,pH..] . . . . 3.0 Unit of meas. . . . . . . . . . . . As installed
Delay [s] . . . . . . . . . . 10 Titration mode . . . . . . . . . . . EP
End point mode . . . . . . . . . EPA Predispensing 1 . . . . . . . . . mL
Potential [mV,pH..] . . . . 7.0 Volume [mL] . . . . . . 3.0
Tendency . . . . . . . . . . . . Positive Titrant addition . . . . . . . . Dynamic
Maximum volume [mL] . . . . . . . 10.0 dV (set)[mV] . . . . . . . 8.0
Record dV(min) [mL] . . . . . . . 0.02
Output unit . . . . . . . . . . . . Printer dV(max) [mL] . . . . . . . 0.2
Table of measured values . . . . . . Yes dE [mV] . . . . . . . . . . . 0.5
Titration dt [s] . . . . . . . . . . . . 0.5
Titrant . . . . . . . . . . . . . . NaOH t (min) [s] . . . . . . . . 2.0
Concentration [mol/L] . . . . . . . 0.1 t (max) [s] . . . . . . . . 20.0
Sensor . . . . . . . . . . . . . . . DG111-SC End point mode . . . . . . . . . EPA
Unit of meas. . . . . . . . . . . . As installed Potential [mV,pH..] . . . . 7.0
Titration mode . . . . . . . . . . . EP Tendency . . . . . . . . . . . . Positive
Titrant addition . . . . . . . . Continuous Maximum volume [mL] . . . . . . . 10.0
Control band[mV,pH..] . . . . 2.0 Calculation
Delay [s] . . . . . . . . . . 10 Result name . . . . . . . . . . . .
End point mode . . . . . . . . . EPA Formula . . . . . . . . . . . . . . R=Q[1]
Potential [mV,pH..] . . . . 8.0 Constant . . . . . . . . . . . . . .
Tendency . . . . . . . . . . . . Positive Result unit . . . . . . . . . . . . mmol
Maximum volume [mL] . . . . . . . 10.0 Decimal places . . . . . . . . . . . 3
Record
Table of measured values . . . . . . Yes
Statistics
Ri (i=index) . . . . . . . . . . . . R1
Outlier test . . . . . . . . . . . . Yes
Auxiliary value
ID t t Bl k l t
102
METTLER TOLEDO M240
Formol Number, Acidity and True Brix Value of Orange Juice

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

1) The DG111 electrode must be calibrated with pH buffers.
2) The sample is weighed in the titration beaker and mounted at

the titration head. If drinkable orange juice is used, then weigh
Substance Organic acids, free amino acids
in approximately 20 g. The sample is diluted using the second
pump of the sample changer (DOSE).
Chemicals 50 mL deionized water 3) First the acidity content is determined by performing an EP

titration to pH 8.2 with NaOH. This is given as citric acid
content.
4) Formol is dispensed by the second burette. After 1 minute

Titrant NaOH, c(NaOH) = 0.5 mol/L reaction time, an EP titration to pH 8.2 with NaOH is started.
Formol , c(Formol) = 36.5%
5) The formol number is defined in calculation R4 as mmol
Adjusted to pH 8.2 with NaOH
NaOH/10g sample, normalized to 65 True Brix:
FN = (mmol NaOH*10*10*65)/(m*True Brix).
Standard THAM (NaOH)
6) A blank is run and stored as auxiliary value H2.
Instruments DL70ES/DL77
Note:
Rondo 60 sample changer
1. The molar mass M is set to 1.0 and is not used.
Balance, printer 2. Prior titration the Brix value of the sample is measured with a
refractometer. The value is stored as auxiliary value H1and usd
Accessories Beakers ME-101974; in calculation R3 (correction for true brix).
1 additional burette drive DV90;
1 burette DV1010;
1 additional diaphragma pump (DOSE)
Remarks
Indication DG111-SC at Sensor 1 1) Formol value:
The formol value is a measure of the free amino acids and
allows an estimation of of the protein content.
Chemistry Free amino acids (formol no.): Amino acids can not be titrated directly with a base since the
R-COOH-NH2 + HCHO = H2O + R-COOH-N=CH2 dissociation constant of the -COOH group is too weak. By
R-COOH-N=CH2 + OH- = R-COO--N=CH2 + H2O 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.
Calculation Citric acid (R1):
R1 = Q[1]*C1/m, C1= 192/(10*3); 2) The formol value is generally given as the titrant
consumption of 0.1 mol/L NaOH needed for 10 g or sample.
True Brix correction (R2):
R2 = R1*R1*(-0.000035)+C2, 3) True Brix: correction of the measured refrative index for the
C2 = (R1*0.191)+0.024 citric acid concentration (given in R1):
True Brix (R3): R3 = H1+R2 Corrected value = (-0.00035)*R12 + 0.191*R1 + 0.024
Formol No. R4 = 6500*C4/(m*R3), (According to Stevens and Baier, 1959)
Results C4=Q[2]-H2+QEX[1]
Literature:
Waste Aqueous solution NEN 2843, NEN 2861
J. Stevens, W.Baier, Die Fruchtsaftindustrie, 4 (1959), p. 28.
disposal
(See also: C.W. Lindsay, J. of AOAC International,
Vol. 76, NO.2, 1993, page 424).
AOAC Official Methods of Analysis, 1984.
Author Ko Schaap, MT-NL
103
Results
METTLER DL70 Titrator Quest Naarden
Analytical Laboratory
4 F.N./Acid./True Brix measured 30-Oct-1991 11:13

11-Oct-1991 9:00 Titrator
SW Version 2.0 User jan
RESULTS
No Identification Weight Results
1/1 11570 03500 1.5503 g 31.3 % Citric acid

5.66 True Bx corr.
57.76 True brix
18.35 mmol NaOH/10g(65wBx)
1/2 11570 03500 1.5503 g 31.4 % Citric acid
5.67 True Bx corr.
57.77 True brix
18.35 mmol NaOH/10g(65wBx)
STATISTICS
Mean value x = 31.3 % Citric acid
Standard deviation s = 0.04 % Citric acid
STATISTICS
Mean value x = 5.67 True Bx. corr.
Standard deviation s = 0.1504 True Bx. corr.
STATISTICS
Mean value x = 57.77 True brix
Standard deviation s = 0.007 True brix
STATISTICS
Mean value x = 18.66 mmol NaOH/10g(65wBx)
Standard deviation s = 0.443 mmol NaOH/10g(65wBx)
104
Method
Method 4 F.N./Acid./True Brix Calculation
Version 11-Oct-1991 9:00 Result name . . . . . . . . . . . . True brix
Formula . . . . . . . . . . . . . . R3=H1+R2
Constant . . . . . . . . . . . . . .
Title Result unit . . . . . . . . . . . .
Method ID . . . . . . . . . . . . . R1 Decimal places . . . . . . . . . . . 2
Title . . . . . . . . . . . . . . . F.N./Acid./True Brix Calculation
Date/time . . . . . . . . . . . . . 11-Oct-1991 9:00 Result name . . . . . . . . . . . . mmol NaOH/10g(65wBx)
Conditioning Formula . . . . . . . . . . . . . . R4=6500*C4/(m*R3)
Interval . . . . . . . . . . . . . . 1 Constant . . . . . . . . . . . . . . C4=Q[2]-H2+QEX[1]
Time [s] . . . . . . . . . . . . . . 10 Result unit . . . . . . . . . . . .
Sample Decimal places . . . . . . . . . . . 2
Number samples . . . . . . . . . . . 2 Statistics
Titration stand . . . . . . . . . . ST20 Ri (i=index) . . . . . . . . . . . . R1
Entry type . . . . . . . . . . . . . Weight m Standard deviation s . . . . . . . . Yes
Lower limit [g] . . . . . . . . . 1.0 Rel. standard deviation srel . . . . Yes
Upper limit [g] . . . . . . . . . 4.0 Statistics
ID1 . . . . . . . . . . . . . . . . Ri (i=index) . . . . . . . . . . . . R2
Molar mass M . . . . . . . . . . . . 1.0 Standard deviation s . . . . . . . . Yes
Equivalent number z . . . . . . . . 1 Rel. standard deviation srel . . . . Yes
Stir Statistics
Speed [%] . . . . . . . . . . . . . 70 Ri (i=index) . . . . . . . . . . . . R3
Time [s] . . . . . . . . . . . . . . 15 Standard deviation s . . . . . . . . Yes
Auxiliary instrument Rel. standard deviation srel . . . . Yes
Name . . . . . . . . . . . . . . . . DOSE Statistics
Time [s] . . . . . . . . . . . . . . 5.0 Ri (i=index) . . . . . . . . . . . . R4
Titration Standard deviation s . . . . . . . . Yes
Titrant . . . . . . . . . . . . . . NaOH Rel. standard deviation srel . . . . Yes
Concentration [mol/L] . . . . . . . 0.5 Record
Sensor . . . . . . . . . . . . . . . DG111-SC Output unit . . . . . . . . . . . . Printer
Unit of meas. . . . . . . . . . . . As installed All results . . . . . . . . . . . . Yes
Titrant addition . . . . . . . . Dynamic
dE(set)[mV] . . . . . . . . . 4.0
dV(min) [mL] . . . . . . . . . 0.005
dV(max) [mL] . . . . . . . . . 0.5
dE [mV] . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . . 0.5
t(min) [s] . . . . . . . . . . 2.0
t(max) [s] . . . . . . . . . . 20.0
Potential [mV,pH..] . . . . 8.2
Dispense
Titrant . . . . . . . . . . . . . . Formol
Concentration [mol/L] . . . . . . . 36.5%
Volume . . . . . . . . . . . . . . 10 mL
Stir
Speed [%] . . . . . . . . . . . . . 70
Time [s] . . . . . . . . . . . . . . 60
Titration
Titrant . . . . . . . . . . . . . . NaOH
Sensor . . . . . . . . . . . . . . . DG111-SC
Unit of meas. . . . . . . . . . . . As installed
Titrant addition . . . . . . . . Continuous
Control band [mV,pH,...] . . 3.0
Delay [s] . . . . . . . . . . 10
Potential [mV,pH..] . . . . 8.2
Rinse
Auxiliary reagent . . . . . . . . . H2O
Volume [mL] . . . . . . . . . . . . 10.0
Conditioning
Interval . . . . . . . . . . . . . . 1
Time [s] . . . . . . . . . . . . . . 10
Calculation
Result name . . . . . . . . . . . . Citric acid
Formula . . . . . . . . . . . . . . R1=Q[1]*C1/m
Constant . . . . . . . . . . . . . . C1=192/(m*3)
Result unit . . . . . . . . . . . . %
Decimal places . . . . . . . . . . . 1
Calculation
Result name . . . . . . . . . . . . True Bx corr.
Formula . . . . . . . . . . . . . . R2=R1*R1*(-0.00035)+C2
Constant . . . . . . . . . . . . . . C2=(R1*0.191)+0.024
Result unit . . . . . . . . . . . .
Decimal places . . . . . . . . . . . 2
105
METTLER TOLEDO M241 / 1
Carbon Black Surface Area (ASTM D3765-99): Standardization

Titration of unadsorbed CTAB (cetyltrimethylammonium bromide) on the ITRB standards for the carbon
black surface area determination according to ASTM D3765-99 (see also 241 / 2, and 241 / 3).
Sample 5 Standard samples with ITRB Preparation and Procedures

5 samples (0.2-0.6 g, with 0.1 g diff.) The sample must be prepared according to ASTM D3765-99.
ITRB (Industry Tint Reference Black) After filtration, the standard samples are ready for titration:
1) Add 45 mL deionized water

Substance ITRB, accessible surface area:
2) Mount the beaker on the titration stand, start method ALG1.
83.0 x103 m2/kg 3) 5 mL 0.15% Triton X-100 solution are added by a burette,
4) 10 mL 0.01 CTAB solution are added by a second burette.
Chemicals 45 mL deionized water
5 mL 0.15% Triton X-100
10 mL 0.01 mol/L CTAB CTAB Standard solution (0.01 mol/L):
(Cetyltrimethylammonium bromide) Dissolve 3.64 g of reagent-grade CTAB (Cetyltrimethylammonim
bromide, available from e.g. J.T. Baker, Cat. No. 7N121) in
Titrant Dioctyl sodium sulfosuccinate 900 mL distilled or deionized water. Add 100 mL of the pH 7.0
(Aerosol OT) 0.05 mol/L buffer solution. Warm the solution to a temperature
of 27-37°C to facilitate the dissolution. Cool to a temperature
c(Aerosol OT) = 0.1 mol/L
between 22 and 25°C before using.
Standard --- Aerosol OT (Dioctyl sodium sulfosuccinate):

Dissolve 1g/L of Aerosol OT solution in distilled or deionized
Instruments DL70ES, DL77 water containing 2.5 mL/L of 37% formaldehyde, by swirling
vogourously with a magnetic stirrer for 48 h. Allow to stand an
additional twelve days before standardization and use. The
AT261 Balance, printer solution should be capped tightly and stored in a cool place
(once opened, the solution should be store in a dessiccator).
Accessories 2 additional burette drive DV90,
DT120 Temperature sensor
Remarks
Indication DP550 with adapter cable ME-89600 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
Chemistry 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,
Calculation the CTAB surface area reflects only the surface f the carbon black
See method below
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.
Results All results are scaled by using the Industry Tint reference Black
(ITRB) as a primary standard and taking its accessible surface
Waste area to be exactly 83.0 x 103 m2/kg.
Aqueous waste
disposal
Literature:
ASTM D3765 (www.astm.org)
Author K. Mooibroek/C. Gordon/Ch. Walter
106
Results
107
Method
Method ALG1 ASTM3765: Standards Auxiliary value
Version 22-Feb-2002 10:30 ID text . . . . . . . . . . . . . . H17 4. standard
Formula . . . . . . . . . . . . . . H17=m
Title Auxiliary value
Method ID . . . . . . . . . . . . . ALG1 ID text . . . . . . . . . . . . . . ITBR(4)
Title . . . . . . . . . . . . . . . ASTM3765: Standards Formula . . . . . . . . . . . . . . H4=R1
Date/time . . . . . . . . . . . . . 22-Feb-2002 10:30 Condition . . . . . . . . . . . . . Yes
Sample Condition . . . . . . . . . . . . f=4
Number samples . . . . . . . . . . . 5 Auxiliary value
Titration stand . . . . . . . . . . ST20 1 ID text . . . . . . . . . . . . . . H16 5. standard
Entry type . . . . . . . . . . . . . Weight m Formula . . . . . . . . . . . . . . H16=m
Lower limit [g] . . . . . . . . . 0.2 Auxiliary value
Upper limit [g] . . . . . . . . . 0.6 ID text . . . . . . . . . . . . . . ITBR(5)
ID1 . . . . . . . . . . . . . . . . ITRB Formula . . . . . . . . . . . . . . H5=R1
Molar mass M . . . . . . . . . . . . 0.0 Condition . . . . . . . . . . . . . Yes
Equivalent number z . . . . . . . . 1 Condition . . . . . . . . . . . . f=5
Temperatur sensor . . . . . . . . . TEMP A Statistics
Dispense Ri (i=index) . . . . . . . . . . . . R1
Titrant . . . . . . . . . . . . . . Triton X-100 Standard deviation s . . . . . . . . Yes
Concentration [mol/L] . . . . . . . 0.15 Rel. standard deviation srel . . . . Yes
Volume [mL] . . . . . . . . . . . . 5.0 Record
Dispense Output unit . . . . . . . . . . . . Printer
Titrant . . . . . . . . . . . . . . CTAB All results . . . . . . . . . . . . Yes
Volume [mL] . . . . . . . . . . . . 10.0
Stir
Speed [%] . . . . . . . . . . . . . 50
Time [s] . . . . . . . . . . . . . . 30
Titration
Titrant . . . . . . . . . . . . . . Aerosol OT
Sensor . . . . . . . . . . . . . . . DP550
Unit of meas. . . . . . . . . . . . mV
dV[mL] . . . . . . . . . . . 0.1
Measure mode . . . . . . . . . . EQU
dE [mV] . . . . . . . . . . . 1.0
dt [s] . . . . . . . . . . . . 2.0
t(min) [s] . . . . . . . . . . 3.0
t(max) [s] . . . . . . . . . . 30.0
Threshold . . . . . . . . . . . . 500
n = . . . . . . . . . . . . . 1
Evaluation procedure. . . . . . . Minimum
Calculation
Result name . . . . . . . . . . . . Volume/gram
Formula . . . . . . . . . . . . . . R1=VEQ/m
Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . cm3/g
Decimal places . . . . . . . . . . . 4
Auxiliary value
ID text . . . . . . . . . . . . . . H20 1. standard
Formula . . . . . . . . . . . . . . H20=m
Auxiliary value
ID text . . . . . . . . . . . . . . ITBR(1)
Formula . . . . . . . . . . . . . . H1=R1
Condition . . . . . . . . . . . . . Yes
Condition . . . . . . . . . . . . f=1
Auxiliary value
Formula . . . . . . . . . . . . . . H19=m
Auxiliary value
ID text . . . . . . . . . . . . . . ITBR(2)
Formula . . . . . . . . . . . . . . H2=R1
Condition . . . . . . . . . . . . . Yes
Condition . . . . . . . . . . . . f=2
Auxiliary value
Formula . . . . . . . . . . . . . . H18=m
Auxiliary value
ID text . . . . . . . . . . . . . . ITBR(3)
Formula . . . . . . . . . . . . . . H3=R1
Condition . . . . . . . . . . . . . Yes
Condition . . . . . . . . . . . . f=3
108
Carbon Black Surface Area (ASTM D3765-99): Linear regression

Linear regression for calibration line of Carbon Black Area Determination according to ASTM D3765-99.
Five ITRB standards have been determined in Application 241/1, while sample titration is described in 241/3
.
5 samples (0.2-0.6 g, with 0.1 g diff.) For the calculation of the calibration line starts method ALG2.
ITRB (Industry Tint Reference Black)

83.0 x103 m2/kg
CTAB Standard solution (0.01 mol/L):
Chemicals 45 mL deionized water Dissolve 3.64 g of reagent-grade CTAB (Cetyltrimethylammonim
5 mL 0.15% Triton X-100 bromide, available from e.g. J.T. Baker, Cat. No. 7N121) in
10 mL 0.01 mol/L CTAB 900 mL distilled or deionized water. Add 100 mL of the pH 7.0
(Cetyltrimethylammonium bromide) 0.05 mol/L buffer solution. Warm the solution to a temperature
Titrant Dioctyl sodium sulfosuccinate between 22 and 25°C before using.
(Aerosol OT)
Aerosol OT (Dioctyl sodium sulfosuccinate):
water containing 2.5 mL/L of 37% formaldehyde, by swirling
Standard --- vogourously with a magnetic stirrer for 48 h. Allow to stand an
Instruments DL70ES, DL77 solution should be capped tightly and stored in a cool place
(once opened, the solution should be store in a dessiccator).
AT261 Balance, printer
Accessories 2 additional burette drive DV90,

Remarks
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
Calculation roughness. Thus, the CTAB surface area reflects only the surface
Calculation of linear regression:
f the carbon black that is available for interaction with rubber
see below molecules.
Titration with Aerosol OT soltuion to a turbidity maximum

ultrafiltration.
Results
All results are scaled by using the Industry Tint reference Black
Waste (ITRB) as a primary standard and taking its accessible surface
Aqueous waste area to be exactly 83.0 x 103 m2/kg.
disposal
Literature:
109
Results
110
Method
Method ALG2 ASTM3765: Lin. regr. Calculation
Version 22-Feb-2002 11:30 Result name . . . . . . . . . . . . Bottom line calc. (1)
Formula . . . . . . . . . . . . . . R4=-sq(H7)
Title Constant . . . . . . . . . . . . . .
Method ID . . . . . . . . . . . . . ALG2 Result unit . . . . . . . . . . . .
Title . . . . . . . . . . . . . . . ASTM3765: Lin. regr. Decimal places . . . . . . . . . . . 4
Date/time . . . . . . . . . . . . . 22-Feb-2002 11:30 Calculation
Sample Result name . . . . . . . . . . . . Bottom line calc. (2)
Number samples . . . . . . . . . . . 1 Formula . . . . . . . . . . . . . . R5=4*H15
Titration stand . . . . . . . . . . Stand 1 Constant . . . . . . . . . . . . . .
Entry type . . . . . . . . . . . . . Fixed volume U Result unit . . . . . . . . . . . .
Volume [mol/L] . . . . . . . . . 1.0 Decimal places . . . . . . . . . . . 4
ID1 . . . . . . . . . . . . . . . . ITRB Calculation
Molar mass M . . . . . . . . . . . . 0.0 Result name . . . . . . . . . . . . Bottom line calc. (3)
Equivalent number z . . . . . . . . 1 Formula . . . . . . . . . . . . . . R6=R4+R5
Temperatur sensor . . . . . . . . . TEMP A Constant . . . . . . . . . . . . . .
Auxiliary value Result unit . . . . . . . . . . . .
ID text . . . . . . . . . . . . . . Sum of masses (1) Decimal places . . . . . . . . . . . 4
Formula . . . . . . . . . . . . . . H6=H20+H19+H18 Calculation
Auxiliary value Result name . . . . . . . . . . . . Slope b
ID text . . . . . . . . . . . . . . Sum of masses (2) Formula . . . . . . . . . . . . . . R7=R3/R6
Formula . . . . . . . . . . . . . . H7=H6+H17+H16 Constant . . . . . . . . . . . . . .
Auxiliary value Result unit . . . . . . . . . . . . cm3/g
ID text . . . . . . . . . . . . . . Sum of volumes Decimal places . . . . . . . . . . . 4
Formula . . . . . . . . . . . . . . H8=H1+H2+H3+H4+H5 Calculation
Auxiliary value Result name . . . . . . . . . . . . Intercept, V0 (1)
ID text . . . . . . . . . . . . . . Products (1) Formula . . . . . . . . . . . . . . R8=H8/4
Formula . . . . . . . . . . . . . . H9=H20*H1+H19*H2 Constant . . . . . . . . . . . . . .
Auxiliary value Result unit . . . . . . . . . . . . cm3
ID text . . . . . . . . . . . . . . Products (2) Decimal places . . . . . . . . . . . 4
Formula . . . . . . . . . . . . . . H10=H18*H3+H17*H4 Calculation
Auxiliary value Result name . . . . . . . . . . . . Intercept, V0(2)
ID text . . . . . . . . . . . . . . Products (3) Formula . . . . . . . . . . . . . . R9=(R7*H7)/4
Formula . . . . . . . . . . . . . . H11=H16*H5 Constant . . . . . . . . . . . . . .
ID text . . . . . . . . . . . . . . Sum of products Decimal places . . . . . . . . . . . 4
Formula . . . . . . . . . . . . . . H12=H9+H10+H11 Calculation
Auxiliary value Result name . . . . . . . . . . . . Intercept, V0 (3)
ID text . . . . . . . . . . . . . . Sum of squares (1) Formula . . . . . . . . . . . . . . R10=R8-R9
Formula . . . . . . . . . . . . . . H13=sq(H20)+sq(H19) Constant . . . . . . . . . . . . . .
ID text . . . . . . . . . . . . . . Sum of squares (2) Decimal places . . . . . . . . . . . 4
Formula . . . . . . . . . . . . . . H14=sq(H18)+sq(H17) Record
Auxiliary value Output unit . . . . . . . . . . . . Printer
ID text . . . . . . . . . . . . . . Sum of squares (3) All results . . . . . . . . . . . . Yes
Formula . . . . . . . . . . . . . . H15=H13+H14+sq(H16)
Calculation
Result name . . . . . . . . . . . . Top line calc. (1)
Formula . . . . . . . . . . . . . . R1=4*H12
Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . .
Decimal places . . . . . . . . . . . 4
Calculation
Formula . . . . . . . . . . . . . . R2=-H7*H8
Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . .
Decimal places . . . . . . . . . . . 4
Calculation
Formula . . . . . . . . . . . . . . R3=R1+R2
Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . .
Decimal places . . . . . . . . . . . 4
111
Carbon Black Surface Area (ASTM D3765-99): Sample Titration

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

5 samples (0.2-0.6 g, with 0.1 g diff.) The sample must be prepared according to ASTM D3765-99.
ITRB (Industry Tint Reference Black) 1) Dry an adequate sample of carbon black at 125°C for 1 hour
and cool in dessiccator.
2) Weigh to 0.1 mg a suitable sample into a glass vial, and
proceed according to ASTM D3765-99, chap. 9.
83.0 x103 m2/kg After filtration, the samples are ready for titration:
1) Add 45 mL deionized water
Chemicals 45 mL deionized water 2) Mount the beaker on the titration stand, start method ALG3.
5 mL 0.15% Triton X-100 3) 5 mL 0.15% Triton X-100 solution are added by a burette,
10 mL 0.01 mol/L CTAB 4) 10 mL 0.01 CTAB solution are added by a second burette.
(Cetyltrimethylammonium bromide)
CTAB Standard solution (0.01 mol/L):
Titrant Dioctyl sodium sulfosuccinate Dissolve 3.64 g of reagent-grade CTAB (Cetyltrimethylammonim
(Aerosol OT) bromide, available from e.g. J.T. Baker, Cat. No. 7N121) in
900 mL distilled or deionized water. Add 100 mL of the pH 7.0
0.05 mol/L buffer solution. Warm the solution to a temperature
Standard --- between 22 and 25°C before using.
Instruments DL70ES, DL77 Aerosol OT (Dioctyl sodium sulfosuccinate):

water containing 2.5 mL/L of 37% formaldehyde, by swirling
AT261 Balance, printer vogourously with a magnetic stirrer for 48 h. Allow to stand an
Accessories 2 additional burette drive DV90, solution should be capped tightly and stored in a cool place
2 additional burette DV1010 (once opened, the solution should be store in a dessiccator).
Remarks
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
Calculation 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

ultrafiltration.
Results
All results are scaled by using the Industry Tint reference Black
Waste (ITRB) as a primary standard and taking its accessible surface
Aqueous waste area to be exactly 83.0 x 103 m2/kg.
disposal
Literature:
112
Results
113
Method
Method ALG3 ASTM3765: Sample det.
Version 24-Jan-1995 11:13
Title
Method ID . . . . . . . . . . . . . AL3
Title . . . . . . . . . . . . . . . ASTM3765: Sample det.
Date/time . . . . . . . . . . . . . 24-Jan-1995 11:13
Sample
Number samples . . . . . . . . . . . 3
Lower limit [g] . . . . . . . . . 0.15
Upper limit [g] . . . . . . . . . 0.25
ID1 . . . . . . . . . . . . . . . .
Molar mass M . . . . . . . . . . . . 100.0
Temperatur sensor . . . . . . . . . TEMP A
Stir
Speed [%] . . . . . . . . . . . . . 50
Time [s] . . . . . . . . . . . . . . 10
Titration
Titrant . . . . . . . . . . . . . . Aerosol OT
Sensor . . . . . . . . . . . . . . . DP550
Unit of meas. . . . . . . . . . . . mV
Predispensing 1 . . . . . . . . . mL
Volume [mL] . . . . . . . . . 1.0
dV[mL] . . . . . . . . . . . 0.1
Measure mode . . . . . . . . . . EQU
dE [mV] . . . . . . . . . . . 1.0
dt [s] . . . . . . . . . . . . 2.0
t(min) [s] . . . . . . . . . . 3.0
t(max) [s] . . . . . . . . . . 30.0
Threshold . . . . . . . . . . . . 500.0
n = . . . . . . . . . . . . . 1
Evaluation procedure. . . . . . . Minimum
Stop for reevaluation . . . . . . Yes
Condition . . . . . . . . . . neq=0
Calculation
Result name . . . . . . . . . . . . Consumption
Formula . . . . . . . . . . . . . . R=VEQ
Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . mL
Decimal places . . . . . . . . . . . 3
Record
Result last sample . . . . . . . . . Yes
Statistics
Ri (i=index) . . . . . . . . . . . . R1
Outlier test . . . . . . . . . . . . Yes
Record
All results . . . . . . . . . . . . Yes
114
METTLER TOLEDO M242
Determination of Amine Number

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

1) The sample mass depends on the amine number.
2) Recommended titrant consumption: 5-10 mL

Electrode cleaning:
1) Rinse the electrode after each titration withacetone
Chemicals 60 mL glacial acetic acid
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

Titrant Perchloric acid in glacial acetic acid: titration.
Standard THAM, 50-100 mg

DL70ES, DL77
Accessories 100 mL glass titration beaker

ME-101446, DV1010 burette, printer,
balance
Remarks
Indication 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.
Chemistry
If necessary , perform a blank value titration of the solvent.
Literature:
Application DL40RC No. 84-05.
Calculation Blank determination (Meth. blv):

R1 = Q

R1 = (Q1 - H5)*C1/m
C1 = 56.1
Results
Waste Organic solvent waste

disposal
Author MSG
115
Results
DL40RC:
*** 17-FEB-84 ***
METHOD 8405 2114

IDENT. 530
SAMPLE NO. 3
*R * MG/G 198.71
Results:
Sample Weight Result St.Dev. n

in g mg KOH/g in %
MOCA ca. 0.1 415.58 0.11 2
ML-530 ca. 0.2 200.32 0.80 3
FCA-504 ca. 0.3 143.79 0.71 2
Statistics:
n 3
Mean: 200.32
Stand. dev% .80
116
Method
Method 40016 Amine number det. Method bv Blank value
Version 25-Mar-2002 10:00 Version 25-Mar-2002 10:30
Title Title
Method ID . . . . . . . . . . . . . 40016 Method ID . . . . . . . . . . . . . bl
Title . . . . . . . . . . . . . . . Amine number det. Title . . . . . . . . . . . . . . . Blank value
Date/time . . . . . . . . . . . . . 25-Mar-2002 10:00 Date/time . . . . . . . . . . . . . 25-Mar-2002 10:30
Sample Sample
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 120
EQP Titration Titrant . . . . . . . . . . . . . . HClO4
Titrant . . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . . 0.1
Predispensing . . . . . . . . . . . Yes Titrant addition . . . . . . . . . . Dynamic
Volume [mL] . . . . . . . . . . . 5.0 dE(set) [mV] . . . . . . . . . . 8.0
Titrant addition . . . . . . . . . . INC dV(min) [mL] . . . . . . . . . . 0.02
dV [mL] . . . . . . . . . . . . . 0.25 dV(max) [mL] . . . . . . . . . . 0.3
Measure mode . . . . . . . . . . . . Equilibrium Measure mode . . . . . . . . . . . . Equilibrium
controlled controlled
dE [mV] . . . . . . . . . . . . . 1.0 dE [mV] . . . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . . . 2.0 dt [s] . . . . . . . . . . . . . 1.0
t(min) [s] . . . . . . . . . . . 3.0 t(min) [s] . . . . . . . . . . . 3.0
t(max) [s] . . . . . . . . . . . 30.0 t(max) [s] . . . . . . . . . . . 30.0
Steepest jump only . . . . . . . No Steepest jump only . . . . . . . No
Range . . . . . . . . . . . . . . No Range . . . . . . . . . . . . . . No
Tendency . . . . . . . . . . . . Positive Tendency . . . . . . . . . . . . Positive
at potential . . . . . . . . . . No at potential . . . . . . . . . . No
at slope . . . . . . . . . . . . No at slope . . . . . . . . . . . . No
after number EQPs . . . . . . . . No after number EQPs . . . . . . . . No
comb. termination conditions . . No comb. termination conditions . . No
Procedure . . . . . . . . . . . . Standard Procedure . . . . . . . . . . . . Standard
Stop for reevaluation . . . . . . Yes Stop for reevaluation . . . . . . Yes
Condition . . . . . . . . . . neq=0 Condition . . . . . . . . . . neq=0
Formula . . . . . . . . . . . . . . R1=VEQ Formula . . . . . . . . . . . . . . R1=Q
Result unit . . . . . . . . . . . . ml Result unit . . . . . . . . . . . . mmol
Result name . . . . . . . . . . . . Consumption Result name . . . . . . . . . . . .
Statistics . . . . . . . . . . . . . No Statistics . . . . . . . . . . . . . Yes
Formula . . . . . . . . . . . . . . R2=(Q-H5)*C2/m Formula . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . . C2=M/z Constant . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . mg KOH/g Result unit . . . . . . . . . . . .
Result name . . . . . . . . . . . . Amine Number Result name . . . . . . . . . . . .
Statistics . . . . . . . . . . . . . Yes Statistics . . . . . . . . . . . . .
Calculation Auxiliary value
Formula . . . . . . . . . . . . . . ID text . . . . . . . . . . . . . . Blindwert
Constant . . . . . . . . . . . . . . Formula . . . . . . . . . . . . . . H5=x
Decimal places . . . . . . . . . . . 0 Report
Result unit . . . . . . . . . . . . Output unit . . . . . . . . . . . . Printer
Result name . . . . . . . . . . . . Results . . . . . . . . . . . . . . No
Statistics . . . . . . . . . . . . . All results . . . . . . . . . . . . Yes
Report Raw results . . . . . . . . . . . . No
Results . . . . . . . . . . . . . . No Sample data . . . . . . . . . . . . No
All results . . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes
Raw results . . . . . . . . . . . . No dE/dV - V curve . . . . . . . . . . Yes
Table of values . . . . . . . . . . Yes d2E/dV2 - V curve . . . . . . . . . No
Sample data . . . . . . . . . . . . No log dE/dV - V curve . . . . . . . . No
E - V curve . . . . . . . . . . . . Yes E - t curve . . . . . . . . . . . . No
dE/dV - V curve . . . . . . . . . . Yes V - t curve . . . . . . . . . . . . No
d2E/dV2 - V curve . . . . . . . . . No dV/dt - t curve . . . . . . . . . . No
E - t curve . . . . . . . . . . . . No
V - t curve . . . . . . . . . . . . No
dV/dt - t curve . . . . . . . . . . No
117
METTLER TOLEDO M243
Free available chlorine residual in water according to ASTM D 1253 - 86

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

1) 250 mL 0.4 M phosphate buffer pH 7.0:
Weight in 6.35 g KH 2PO4 and 21.5 g Na2HPO4 * 12 H2O and fill up to 250 mL with
dest. water.
2) 250 mL 0.3 M KI:

Substance OCl- and HOCl 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.
Chemicals 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) 4) 100 mL 0.1 M HCl:
NaOH (Merck Titrisol, 1 M); Acedic acid (Fluka puriss, 60.05 g*mol-1) Take 10 mL 1 M HCl and fill up to 100 mL with dest. water.
Phenylarsine Oxide (Sigma, min. 97%, 168.0 g*mol-1)
CHCl3 (Fluka purum, 119.38 g*mol-1); HCl (Merck Titrisol, 1 M)
5) 1L 0.0047 M KIO 3:
Weight in 1.0058 g KIO 3 and fill up to 1L with dest. water.
Titrant 0.00282 M Phenylarsine Oxide (PAO) 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
(= 0.00564 N PAO) 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.
Standard 0.0047 M KIO3 (= 0.0282 N KIO3) 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
Instruments DL5x before the titration) 1 pipette of concentrated acedic acid. Titrate this sample with
Rondo 60 with diaphragm pump 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.
Accessories KF Option Card ME-51 107 269
250 mL Titration beakers ME-23829
Printer
Remarks
Indication DM 143 The method is reliable down to a Cl2-concentration of about 100
ppb.
Below this concentration the relative standard deviation (rsd) of
Chemistry Titer:
KIO3 + 5 KI + 6H+ --> 3 I2 + 6 K+ + 3 H2O
a sample series increases dramatically.
C6H5AsIIIO + I2 + 2 H2O --> C6H7AsVO3 + 2 HI However, the method is well suitable to (qualitatively) detect
traces of free available chlorine in waste water.
Sample:
Cl2 in waste water --> HOCl, OCl-, Cl-, ClNR2, ...
C6H5AsIIIO + OCl- (HOCl) + H2O --> C6H7AsVO3 + Cl- (HCl) Measured sample series:
2 ppm Cl2: rsd = 0.082 % (3 samples)

Calculation free available chlorine - conc. in mmol / L 500 ppb Cl2: rsd = 7.402 % (3 samples, see results)
R1 = Q * C1 / m; C1 = 1000 / z 100 ppb Cl2: rsd = 3.442 % (4 samples)
50 ppb Cl2: rsd = 31.242 % (3 samples)
free available chlorine - conc. in mg / L
R2 = Q * C2 / m; C2 = 1000 * M / z
Method adjustment for different Cl2-Concentrations:
Titrant addition Termination

Results dV [mL] at maximum volume [mL]
Waste Collect all arsine containinig solutions 2 ppm Cl2: 0.3 3.0
disposal in a separate, designated tank 500 ppb Cl2: 0.06 1.2 (see method)
100 ppb Cl2: 0.012 0.2
50 ppb Cl2: 0.006 0.1
Author Mike Treyer
118
Results
Method 3333 Titer 0.00564 N PAO 31-May-2002 12:50 pm
Measured 31-May-2002 1:07 pm
User Mike Treyer
ALL RESULTS
1 KIO3 0.5 mL
R1 = 1.21625 Titer
2 KIO3 0.5 mL
R1 = 1.21086 Titer
3 KIO3 0.5 mL
R1 = 1.21383 Titer
4 KIO3 0.5 mL
R1 = 1.21313 Titer
STATISTICS
Mean value x = 1.21352 Titer
Standard deviation s = 0.00222 Titer
TITER
Titrant PAO 0.00564 mol/L
New titer t = 1.21352
Method 3341 free available chlorine residual 06-Jun-2002 2:50 pm

Measured 06-Jun-2002 3:20 pm
User Mike Treyer
ALL RESULTS
1 Waste water 200.0 mL

R1 = 0.007 mmol/L Cl2-Concentration
R2 = 0.521 mg/L Cl2-Concentration
STATISTICS
Mean value x = 0.008 mmol/L Cl2-Concentration
Standard deviation s = 0.00056 mmol/L Cl2-Concentration
Mean value x = 0.540 mg/L Cl2-Concentration
Standard deviation s = 0.03997 mg/L Cl2-Concentration
119
Method
Method 3333 Titer 0.00564 N PAO Method 3341 free available cholorine residual
Version 31-May-2002 12:50 pm Version 06-Jun-2002 2:50 pm
Title Title
Method ID . . . . . . . . . . . .3333 Method ID . . . . . . . . . . . .3341
Title . . . . . . . . . . . . . Titer 0.00564 N PAO
Title . . . . . . . . . . . . . free av. chl. rs.
Date/time . . . . . . . . . . . .31-May-2002 12:50
Date/time . . . . . . . . . . . .06-Jun-2002 2:50
Sample
Sample ID . . . . . . . . . . . . KIO3 Sample
Sample ID . . . . . . . . . . . . Waste water
Entry type . . . . . . . . . . . . Fixed volume
Volume [mL] . . . . . . . . . .0.5 Entry type . . . . . . . . . . . . Fixed volume
Molar mass M . . . . . . . . . . . 214.00 Volume [mL] . . . . . . . . . .200.0
Equivalent number z . . . . . . . 6 Molar mass M . . . . . . . . . . . 70.90
Titration stand . . . . . . . . . ST20A Equivalent number z . . . . . . . 2
Pump . . . . . . . . . . . . . No Titration stand . . . . . . . . . ST20A
Pump . . . . . . . . . . . . . No Pump . . . . . . . . . . . . . No
Rinse . . . . . . . . . . . . .Yes Pump . . . . . . . . . . . . . No
Solvent . . . . . . . . . .H2O Rinse . . . . . . . . . . . . .Yes
Volume[mL] . . . . . . . . 20.0 Solvent . . . . . . . . . .H2O
Conditioning . . . . . . . . . No Volume[mL] . . . . . . . . 20.0
Temperatur sensor . . . . . . . . Manual Conditioning . . . . . . . . . No
Stir Temperatur sensor . . . . . . . . Manual
Speed [%] . . . . . . . . . . . . 50 Stir
Time [s] . . . . . . . . . . . . . 30 Speed [%] . . . . . . . . . . . . 50
EQP Titration (Ipol/Upol) Time [s] . . . . . . . . . . . . . 20
Titrant/Sensor
EQP Titration (Ipol/Upol)
Titrant . . . . . . . . . . . .PAO
Concentration [mol/L] . . . . 0.00564 Titrant/Sensor
Sensor . . . . . . . . . . . . DM143 Titrant . . . . . . . . . . . .PAO
Indication . . . . . . . . . . . . Amperometric Concentration [mol/L] . . . . 0.00564
Upol [mV] . . . . . . . . . . .500.0 Sensor . . . . . . . . . . . . DM143
Predispensing . . . . . . . . . . to volume Indication . . . . . . . . . . . . Amperometric
Volume [mL] . . . . . . . . . . 1.5 Upol [mV] . . . . . . . . . . .500.0
Wail time [s] . . . . . . . . . 20 Predispensing . . . . . . . . . . No
Titrant addition Titrant addition
dV [mL] . . . . . . . . . . . . 0.05 dV [mL] . . . . . . . . . . . . 0.06
Measure mode . . . . . . . . . . . Equilibrium Measure mode . . . . . . . . . . . Timed increment
controlled dt [s] . . . . . . . . . . . . .20.0
dE [mV, µA] . . . . . . . . . . 0.2 Recognition
dt [s] . . . . . . . . . . . . 1.0 Threshold . . . . . . . . . . . 0.0
t(min) [s] . . . . . . . . . . 3.0 Steepest jump only . . . . . . .Yes
t(max) [s] . . . . . . . . . . 30.0 Range . . . . . . . . . . . . . .No
Recognition Tendency . . . . . . . . . . . .None
Threshold . . . . . . . . . . . 5.0 Termination
Steepest jump only . . . . . . .No at maximum volume [mL] . . . . . 1.2
Range . . . . . . . . . . . . . .No
at potential . . . . . . . . . .No
Tendency . . . . . . . . . . . .None
Termination at slope . . . . . . . . . . . .No
at maximum volume [mL] . . . . . 5.0 after number EQPs . . . . . . . .No
at potential . . . . . . . . . .No comb. termination conditions . .No
at slope . . . . . . . . . . . .No Evaluation
after number EQPs . . . . . . . .Yes Procedure . . . . . . . . . . . .Segmented
n = . . . . . . . . . . . . 1 Potential 1 . . . . . . . . . . .No
comb. termination conditions . .No Potential 2 . . . . . . . . . . .No
Evaluation Stop for reevaluation . . . . . .No
Procedure . . . . . . . . . . . .Minimum Calculation
Potential 1 . . . . . . . . . . .No Formula . . . . . . . . . . . . . .R1=Q*C1/m
Potential 2 . . . . . . . . . . .No Constant . . . . . . . . . . . . . .C1=1000/z
Stop for reevaluation . . . . . .Yes Decimal places . . . . . . . . . . .3
Condition . . . . . . . . . .neq=0 Result unit . . . . . . . . . . . .mmol/L
Calculation Result name . . . . . . . . . . . .Cl2-Concentration
Formula . . . . . . . . . . . . . .R1=m/(VEQ*c*C1)
Statistics . . . . . . . . . . . . .Yes
Constant . . . . . . . . . . . . . .C1=1/(H1*z)
{H1 = 0.0047 M = Conc. of standard KIO3-solution} Calculation
Decimal places . . . . . . . . . . .5 Formula . . . . . . . . . . . . . .R2=Q*C2/m
Result unit . . . . . . . . . . . . Constant . . . . . . . . . . . . . .C2=1000*M/z
Result name . . . . . . . . . . . .Titer Decimal places . . . . . . . . . . .3
Statistics . . . . . . . . . . . . .Yes Result unit . . . . . . . . . . . .mg/L
Titer Result name . . . . . . . . . . . .Cl2-Concentration
Titrant . . . . . . . . . . . . . .PAO Statistics . . . . . . . . . . . . .Yes
Concentration [mol/L] . . . . . . . 0.00564 Report
Formula t = . . . . . . . . . . . . x Output . . . . . . . . . . . . . . .Printer
Report
Results . . . . . . . . . . . . . .Yes
Output . . . . . . . . . . . . . . .Printer
Results . . . . . . . . . . . . . .Yes All results . . . . . . . . . . . .Yes
All results . . . . . . . . . . . .Yes Raw results . . . . . . . . . . . .No
Raw results . . . . . . . . . . . .No Table of values . . . . . . . . . .Yes
Table of values . . . . . . . . . .No Sample data . . . . . . . . . . . .No
Sample data . . . . . . . . . . . .No E - V curve . . . . . . . . . . . .Yes
E - V curve . . . . . . . . . . . .Yes dE/dV - V curve . . . . . . . . . .Yes
dE/dV - V curve . . . . . . . . . .No d2E/dV2 - V curve . . . . . . . . .Yes
d2E/dV2 - V curve . . . . . . . . .No log dE/dV - V curve . . . . . . . .No
log dE/dV - V curve . . . . . . . .No E - t curve . . . . . . . . . . . .No
E - t curve . . . . . . . . . . . .No V - t curve . . . . . . . . . . . .No
V - t curve . . . . . . . . . . . .No dV/dt - t curve . . . . . . . . . .No
dV/dt - t curve . . . . . . . . . .No
120
METTLER TOLEDO M244
Total residual chlorine in water according to ASTM D 1253 - 86

Determination of total residual chlorine (amount of available chlorine-induced oxidants present in water at
any specified period, subsequent to the addition of chlorine) in chlorine treated water by direct amperometric
titration
Sample Chlorine treated waste water Preparation and Procedures
1) 250 mL 9.8 M Acetate buffer pH 4.0
Weight in 36.625 g Sodium Acetate and 120 g Acedic acid and fill up to 250 mL
with dest. water
2) 250 mL 0.3 M KI:

Substance OCl-, HOCl, Cl3N, Cl2NR, ClNRR', ClNR2 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.
Chemicals Sodium acetate (anhydr., Fluka puriss, 82.04 g*mol-1)
Acedic acid (Fluka puriss, 60.05 g*mol-1)
KI (Fluka puriss, 166.01 g*mol-1); KIO3 (Fluka puriss, 214 g*mol-1) 4) 100 mL 0.1 M HCl:
NaOH (Merck Titrisol, 1 M); HCl (Merck Titrisol, 1 M) Take 10 mL 1 M HCl and fill up to 100 mL with dest. water.
Phenylarsine Oxide (Sigma, min. 97%, 168.0 g*mol-1)
CHCl3 (Fluka purum, 119.38 g*mol-1)
5) 1L 0.0047 M KIO 3:
Weight in 1.0058 g KIO 3 and fill up to 1L with dest. water.
Titrant 0.00282 M Phenylarsine Oxide (PAO) 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
(= 0.00564 N PAO) 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.
Standard 0.0047 M KIO3 (= 0.0282 N KIO3) 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
Instruments DL5x 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
Rondo 60 with diaphragm pump 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
Accessories KF Option Card ME-51 107 269 buffer pH 4.0 and 1 mL 0.3 M KI solution. To add one or both solutions long before
250 mL Titration beakers ME-23829 the titration starts will falsify the results.
Printer
Remarks
Indication DM 143 The method is reliable down to a Cl2-concentration of about 100
ppb.
Below this concentration the relative standard deviation (rsd) of
Chemistry Cl2 in waste water --> OCl-, HOCl, Cl3N, Cl2NR, ClNRR', ClNR2,Cl-
a sample series increases dramatically.
ClIxNR3-x + 2 x KI-I + x H+ --> x KCl-I + x I20 + HxNR3-x + x K+ However, the method is well suitable to (qualitatively) detect
and HOClI (OCl-) + 2 KI-I + H+ --> KCl-I + I20 + K+ + H2O (OH-) traces of chlorine in waste water.
1 mol Cl 2 corresponds to 1 mol I 2
C6H5AsIIIO + I2 + 2 H2O --> C6H7AsVO3 + 2 HI

Method adjustment for different Cl2-Concentrations:
Calculation free available chlorine - conc. in mmol / L Titrant addition Termination

R1 = Q * C1 / m; C1 = 1000 / z dV [mL] at maximum volume [mL]
2 ppm Cl2: 0.3 3.0

free available chlorine - conc. in mg / L
500 ppb Cl2: 0.06 1.2 (see method)
R2 = Q * C2 / m; C2 = 1000 * M / z
100 ppb Cl2: 0.012 0.2
50 ppb Cl2: 0.006 0.1
Results
Waste Collect all arsine containinig solutions

disposal in a separate, designated tank
Author Mike Treyer
121
Results
Method 3340 total chlorine residual 06-Jun-2002 1:50 pm
Measured 06-Jun-2002 5:20 pm
User Mike Treyer
ALL RESULTS

STATISTICS
Mean value x = 0.007 mmol/L Cl2-Concentration
Standard deviation s = 0.00008 mmol/L Cl2-Concentration
Mean value x = 0.516 mg/L Cl2-Concentration
Standard deviation s = 0.00577 mg/L Cl2-Concentration
122
Method
Method 3340 total cholorine residual
Version 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 potential . . . . . . . . . .No
at slope . . . . . . . . . . . .No
after number EQPs . . . . . . . .No
comb. termination conditions . .No
Evaluation
Procedure . . . . . . . . . . . .Segmented
Potential 1 . . . . . . . . . . .No
Potential 2 . . . . . . . . . . .No
Stop for reevaluation . . . . . .No
Calculation
Formula . . . . . . . . . . . . . .R1=Q*C1/m
Constant . . . . . . . . . . . . . .C1=1000/z
Decimal places . . . . . . . . . . .3
Result unit . . . . . . . . . . . .mmol/L
Result name . . . . . . . . . . . .Cl2-Concentration
Statistics . . . . . . . . . . . . .Yes
Calculation
Formula . . . . . . . . . . . . . .R2=Q*C2/m
Constant . . . . . . . . . . . . . .C2=1000*M/z
Decimal places . . . . . . . . . . .3
Result unit . . . . . . . . . . . .mg/L
Result name . . . . . . . . . . . .Cl2-Concentration
Statistics . . . . . . . . . . . . .Yes
Report
Output . . . . . . . . . . . . . . .Printer
Results . . . . . . . . . . . . . .Yes
All results . . . . . . . . . . . .Yes
Raw results . . . . . . . . . . . .No
Table of values . . . . . . . . . .Yes
Sample data . . . . . . . . . . . .No
E - V curve . . . . . . . . . . . .Yes
dE/dV - V curve . . . . . . . . . .Yes
d2E/dV2 - V curve . . . . . . . . .Yes
log dE/dV - V curve . . . . . . . .No
E - t curve . . . . . . . . . . . .No
V - t curve . . . . . . . . . . . .No
dV/dt - t curve . . . . . . . . . .No
123
METTLER TOLEDO M258
Total Base Number according to DIN ISO 3771

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

General procedure:
1. Blank determ. of solvent 3771. The blank is stored as
auxiliary value H3 in mL (method b TBN).
Therefore, it is not necessary to determine the titer before running
the blank determination.
2. Titer determination of 0.1 mol/L HClO4 in acetic acid with
THAM (M524).
Chemicals DIN ISO 3771 solvent 3. Determination of the total base number, TBN (Method TBN)
Toluene/acetic acid/acetone
600:300:100 mL in 1 L Sample determination:
1) Weigh in a well homogenized oil sample in the titration
beaker. The sample size is selected according to the expected
Titrant Perchloric acid, HClO4 in acetic acid, base number:
c(HClO4) = 0.1 mol/L; BN until 1: 2g
BN 15-30: 1g
BN more than 30: 0.25 g
Standard THAM, see application M524 2) 60 mL solvent 3771 needed to dissolve the sample are
added automatically with a second burette.
Instruments DL55, DL58
DL70ES, DL77 3) The electrolyte for the DG113 sensor is TEAB (Tetraethyl
ammonium bromide)in ethylene glycol (EtG).To proceed with
this determination, the following steps are needed:
1. Titer determination of perchloric acid (application M524)
Accessories Glass titration beaker ME-101446 2. Blank of solvent 3771 (method )
1 additional burette DV90 3. Sample titration.
1 additional burette drive DV1010
AT261 Balance, Olivetti Artjet 20 printer
Remarks
Indication DG113-SC with 0.4 mol/L TEAB in EtG Total base number according to DIN ISO 3771
Consumption of mg KOH/g oil to the EQP.
Chemistry Conditioning
After every titration the electrode is conditioned in DIN ISO 3771.
Note:
This application does not replace the standard DIN ISO 3771
Calculation Base Number:

R1 = (VEQ-H3)*c*t*C/m ; C1 = 56.1
BN: mg KOH/g
R2 = VEQ ; mL
Results
Waste Special waste (aromatic compounds)

disposal
Author C. De Caro
124
Results
Market Support Laboratory
Method TBN TBN 30-04-2002 14:35

Measured 30-04-2002 15:40
User C. De Caro
RESULTS
1 01201 0.25725 g
R1 = 74.18 mg KOH/g TBN
R2 = 3.407 mL Consumption
2 01201 0.2323 g
3 01201 0.29195 g
STATISTICS
Mean value x = 74.10 mg KOH/gTBN
Standard deviation s = 0.07412 mg KOH/gTBN
Additional results:
Oil n TBN srel
01204 3 9.85 0.20

02301 2 9.38 --
02302 2 10.90 --
01201 3 74.10 0.10
01202 2 17.13 --
01206 3 13.92 0.18
125
Method
Method TBN TBN Method b TBN Blank with EQP
Version 30-04-2002 14:35 Version 30-04-2002 9:59
Title Title
Method ID . . . . . . . . . . . . . TBN Method ID . . . . . . . . . . . . . b TBN
Title . . . . . . . . . . . . . . . TBN Title . . . . . . . . . . . . . . . Blank with EQP
Sample Sample
Sample ID . . . . . . . . . . . . . 01201 Sample ID . . . . . . . . . . . . . DIN ISO 3771
Entry type . . . . . . . . . . . . . Weight Entry type . . . . . . . . . . . . . Fixed volume
Upper limit [g] . . . . . . . . . 0.3 Molar mass M . . . . . . . . . . . . 100
Titration stand . . . . . . . . . . Stand 1 Temperature sensor . . . . . . . . . Manual
Temperature sensor . . . . . . . . . Manual Dispense
Dispense Titrant . . . . . . . . . . . . . . TBN DIN 3771
Titrant . . . . . . . . . . . . . . TBN DIN 3771 Concentration [mol/L] . . . . . . . 0.1
Concentration [mol/L] . . . . . . . 0.1 Volumen [mL] . . . . . . . . . . . . 60
Volumen [mL] . . . . . . . . . . . . 60 Stir
Stir Speed [%] . . . . . . . . . . . . . 50
Speed [%] . . . . . . . . . . . . . 50 Time [s] . . . . . . . . . . . . . . 10
Time [s] . . . . . . . . . . . . . . 240 EQP titration
EQP titration Titrant/Sensor
Titrant/Sensor Titrant . . . . . . . . . . . . . HClO4
Titrant . . . . . . . . . . . . . HClO4 Concentration [mol/L] . . . . . . 0.1
Concentration [mol/L] . . . . . . 0.1 Sensor . . . . . . . . . . . . . DG113
Sensor . . . . . . . . . . . . . DG113 Unit of meas. . . . . . . . . . . mV
Unit of meas. . . . . . . . . . . mV Predispensing . . . . . . . . . . . No
dE(set) [mV] . . . . . . . . . . 8.0 dV(min) [mL] . . . . . . . . . . 0.002
dV(min) [mL] . . . . . . . . . . 0.02 dV(max) [mL] . . . . . . . . . . 0.1
dV(max) [mL] . . . . . . . . . . 0.5 Measure mode . . . . . . . . . . . . Equilibrium controlled
Measure mode . . . . . . . . . . . . Equilibrium controlled dE [mV] . . . . . . . . . . . . . 0.5
dE [mV] . . . . . . . . . . . . . 1.0 dt [s] . . . . . . . . . . . . . 6.0
dt [s] . . . . . . . . . . . . . 5.0 t(min) [s] . . . . . . . . . . . 10.0
t(min) [s] . . . . . . . . . . . 10.0 t(max) [s] . . . . . . . . . . . 60.0
Recognition Threshold . . . . . . . . . . . . 200.0
Threshold . . . . . . . . . . . . 200.0 Steepest jump only . . . . . . . Yes
Steepest jump only . . . . . . . Yes Range . . . . . . . . . . . . . . No
Range . . . . . . . . . . . . . . Yes Tendency . . . . . . . . . . . . Positive
Limit A [mV,pH,...] . . . . . 550 Termination
Limit B [mV,pH,...] . . . . . 900 at maximum volume [mL] . . . . . 0.1
Tendency . . . . . . . . . . . . Positive at potential . . . . . . . . . . No
Termination at slope . . . . . . . . . . . . No
at maximum volume [mL] . . . . . 8.0 after number EQPs . . . . . . . . Yes
at potential . . . . . . . . . . No n = . . . . . . . . . . . . . 1
at slope . . . . . . . . . . . . No comb. termination conditions . . No
after number EQPs . . . . . . . . No Evaluation
comb. termination conditions . . No Procedure . . . . . . . . . . . . Standard
Evaluation Potential 1 . . . . . . . . . . . No
Potential 2 . . . . . . . . . . . No Calculation
Stop for reevaluation . . . . . . No Formula . . . . . . . . . . . . . . R1= VEQ
Formula . . . . . . . . . . . . . . R1=(VEQ-H3)*c*t*C/m Decimal places . . . . . . . . . . . 3
Constant . . . . . . . . . . . . . . C1=56.1 Result unit . . . . . . . . . . . . mL
Decimal places . . . . . . . . . . . 2 Result name . . . . . . . . . . . . Blank
Result unit . . . . . . . . . . . . mg KOH/g Statistics . . . . . . . . . . . . . Yes
Result name . . . . . . . . . . . . TBN Calculation
Statistics . . . . . . . . . . . . . Yes Formula . . . . . . . . . . . . . .
Constant . . . . . . . . . . . . . . Result unit . . . . . . . . . . . .
Result unit . . . . . . . . . . . . mL Statistics . . . . . . . . . . . . . No
Result name . . . . . . . . . . . . Consumption Auxiliary value
Statistics . . . . . . . . . . . . . No ID . . . . . . . . . . . . . . . . . Blank
Formula . . . . . . . . . . . . . . Report
Decimal places . . . . . . . . . . . 0 Results . . . . . . . . . . . . . . Yes
Result name . . . . . . . . . . . . Raw results . . . . . . . . . . . . No
Statistics . . . . . . . . . . . . . No Table of measured values . . . . . . Yes
Results . . . . . . . . . . . . . . Yes dE/dV - V curve . . . . . . . . . . Yes
Raw results . . . . . . . . . . . . No log dE/dV - V curve . . . . . . . . No
Table of measured values . . . . . . Yes E - t curve . . . . . . . . . . . . No
dE/dV - V curve . . . . . . . . . . Yes
d2E/dV2 - V curve . . . . . . . . . No
E - t curve . . . . . . . . . . . . No
V - t curve . . . . . . . . . . . . No
dV/dt - t curve . . . . . . . . . . No
126
METTLER TOLEDO M259
CTAB Surface Area on Amorphous Silica

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

General procedure:
1) Titration of a known amount of CTAB solution (meth. 00032)
2) The silica sample is prepared as indicated in the patent, and
unadsorbed CTAB is titrated (1 mL sample size, meth. 00033).
Substance Amorphous precipitated silica,
3) Calculation of the surface area, ACTAB (m2/g)
CTAB surface area: 85-275 m2/g
CTAB Standard solution
Chemicals 50 mL distilled water (Cetyltrimethylammonium bromide, CAS 57-09-0)
pH buffers 7 and 10. Dissolve 11.000 +/- 0.001 g of reagent-grade CTAB in distilled
water in a 2 L volumetric flask. record the value as C.
Aerosol OT titrant solution

Titrant Aerosol OT, (Sodium di(2-ethylhexyl) sulfosuccinate, CAS 577-11-7):
c(Aerosol OT) = 3.7 g / 2 L Dissolve 3.70 g of Aerosol OT in distilled water in a 2 L flask.
Both solutions are kept in the dark for at least 12 days before
use (storage lives of the solutions: 2 months after preparation)
Standard ---
Instruments DL50Graphix, DL53/DL55/DL58 Sample preparation:

DL70ES, DL77 The sample must be prepared according to the procedure by
Swift at al. indicated in the US Patent 5.888.467 (1999).
AT261 Balance, printer
For more details, see under remarks.
Remarks
Indication DP550 with adapter cable ME-89600 Silica sample preparation:
DG111 1) Add 0.500+/- 0.001 g silica as received in a 200 mL wide
mouth glass bottle. Record the value as S (g).
Chemistry 2) 100 mL standard CTAB solution is added into the bottle.
3) Add a stirring bar, close the bottle, stir gently for 15 minutes
4) Place a calibrated pH electrode into the bottle and adjust the
pH value to between 9.0 and 9.5.
5) Cover the bottle with aluminium foil, and stir for 1 hour.
6) The mixture is filtrated (0.2 or 0.45 µm filter). Note: the
original patent indicates to filtrate the sample for 30 minutes.
Calculation 7) 1 mL from the filtrated clear solution is taken and diluted with
ACTAB = (V1-V2)*C*A*28.92/(V1*S*B)
50 mL distilled water in a titration beaker.
V1 = Titr. consumption for CTAB 8) The sample is titrated with Aerosol OT solution to a turbidity
V2 = Titr. consumption for CTAB-Silica maximum endpoint ito determine the unadsorbed CTAB after
C = CTAB mass for standard sol. (g) removal of the colloidally dispersed silica.
A, B = Mass of a 1 g silica sample
before/after drying (2 hours, 105°C). The method has been modified with respect to the original
titration procedure: Instead of performing a two-phase titration as
S = Silica sample mass (g)
Results described by the patent, a direct turbidimetric titration was done.
Automated two-phase titration did not provide any result, since
Waste the samples were too milky for an efficient EP recognition by the
Aqueous waste photometric sensor.
disposal
Literature:
US Patent 5.888.467, 30th March 1999, Swift et al.
Author C. De Caro
127
Results
Method 00032 CTAB 15-04-2002 17:13
Measured 15-04-2002 18:06
User Cosimo
ALL RESULTS
No. ID Sample amount and results
1 CTAB 1.0 mL
R1 = 3.707 ml Consumption
2 CTAB 1.0 mL
3 CTAB 1.0 mL
4 CTAB 1.0 mL
STATISTICS
Mean value x = 3.636 mL Comsumption --> V 1
Standard deviation s = 0.02019 mL Comsumption
Sample No. 1 deleted
Method 00033 Silica 2 + CTAB 19-04-2002 10:47

Measured 19-04-2002 11:54
User Cosimo
ALL RESULTS
No. ID Sample amount and results
1 Silica2CTAB 1.0 mL
STATISTICS
Mean value x = 3.047 mL Comsumption --> V 2
Standard deviation s = 0.02255 mL Comsumption
128
Method
Method 00032 CTAB Method 00033 Silica 2 + CTAB
Version 15-04-2003 17:13 Version 19-04-2003 10:47
Title Title
Method ID . . . . . . . . . . . . . 00032 Method ID . . . . . . . . . . . . . 00033
Title . . . . . . . . . . . . . . . CTAB Title . . . . . . . . . . . . . . . Silica 2 + CTAB
Sample Sample
Sample ID . . . . . . . . . . . . . CTAB Sample ID . . . . . . . . . . . . . Silica2CTAB
Volume [mL] . . . . . . . . . . . 1.0 Volume [mL] . . . . . . . . . . . 1.0
Equivalent nuber z . . . . . . . . . 1 Equivalent nuber z . . . . . . . . . 1
Stir Stir
Speed [%] . . . . . . . . . . . . . 40 Speed [%] . . . . . . . . . . . . . 40
Time [s] . . . . . . . . . . . . . . 5 Time [s] . . . . . . . . . . . . . . 5
EQP Titration EQP Titration
Titrant/Sensor Titrant/Sensor
Titrant . . . . . . . . . . . . . Aerosol OT Titrant . . . . . . . . . . . . . Aerosol OT
Concentration [mol/L] . . . . . . 1.0 Concentration [mol/L] . . . . . . 1.0
Sensor . . . . . . . . . . . . . DP550 Sensor . . . . . . . . . . . . . DP550
Unit of meas. . . . . . . . . . mV Unit of meas. . . . . . . . . . mV
Predispensing . . . . . . . . . . . No Predispensing . . . . . . . . . . . No
Titrant addition Titrant addition
Titrant addition . . . . . . . . Dynamic Titrant addition . . . . . . . . Dynamic
dE(set) [mV] . . . . . . . . 8.0 dE(set) [mV] . . . . . . . . 8.0
dV(min) [mL] . . . . . . . . 0.02 dV(min) [mL] . . . . . . . . 0.02
dV(max) [mL] . . . . . . . . 0.2 dV(max) [mL] . . . . . . . . 0.2
Measure mode . . . . . . . . . . Equilibrium controlled Measure mode . . . . . . . . . . Equilibrium controlled
dE [mV] . . . . . . . . . . . 0.5 dE [mV] . . . . . . . . . . . 0.5
dt [s] . . . . . . . . . . . . 2.0 dt [s] . . . . . . . . . . . . 1.0
t(min) [s] . . . . . . . . . . 10.0 t(min) [s] . . . . . . . . . . 10.0
t(max) [s] . . . . . . . . . . 30.0 t(max) [s] . . . . . . . . . . 30.0
Threshold . . . . . . . . . . 600.0 Threshold . . . . . . . . . . 600.0
Steepest jump only . . . . . . Yes Steepest jump only . . . . . . Yes
Range . . . . . . . . . . . . No Range . . . . . . . . . . . . No
Tendency . . . . . . . . . . . Negative Tendency . . . . . . . . . . . Negative
at maximum volume [mL] . . . . 5.0 at maximum volume [mL] . . . . 3.5
at potential . . . . . . . . . No at potential . . . . . . . . . No
at slope . . . . . . . . . . . No at slope . . . . . . . . . . . No
after number EQPs . . . . . . No after number EQPs . . . . . . No
comb. termination conditions . No comb. termination conditions . No
Procedure . . . . . . . . . . Minimum Procedure . . . . . . . . . . Minimum
Stop for reevaluation . . . . Yes Stop for reevaluation . . . . Yes
Condition . . . . . . . . . neq=0 Condition . . . . . . . . . neq=0
Formula . . . . . . . . . . . . . . R1=VEQ Formula . . . . . . . . . . . . . . R1=VEQ
Result unit . . . . . . . . . . . . mL Result unit . . . . . . . . . . . . mL
Result name . . . . . . . . . . . . Consumption Result name . . . . . . . . . . . . Consumption
Statistics . . . . . . . . . . . . . Yes Statistics . . . . . . . . . . . . . Yes
Formula . . . . . . . . . . . . . . Formula . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . Result unit . . . . . . . . . . . .
Result name . . . . . . . . . . . . Result name . . . . . . . . . . . .
Statistics . . . . . . . . . . . . . Statistics . . . . . . . . . . . . .
Formula . . . . . . . . . . . . . . Formula . . . . . . . . . . . . . .
Result unit . . . . . . . . . . . . Result unit . . . . . . . . . . . .
Result name . . . . . . . . . . . . Result name . . . . . . . . . . . .
Statistics . . . . . . . . . . . . . Statistics . . . . . . . . . . . . .
Report Report
Output . . . . . . . . . . . . . . . Printer Output . . . . . . . . . . . . . . . Printer
Results . . . . . . . . . . . . . . No Results . . . . . . . . . . . . . . No
All results . . . . . . . . . . . . Yes All results . . . . . . . . . . . . Yes
Raw results . . . . . . . . . . . . Yes Raw results . . . . . . . . . . . . Yes
Tables of measured values . . . . . Yes Tables of measured values . . . . . Yes
Sample data . . . . . . . . . . . . No Sample data . . . . . . . . . . . . No
E - V curve . . . . . . . . . . . . Yes E - V curve . . . . . . . . . . . . Yes
dE/dV - V curve . . . . . . . . . . Yes dE/dV - V curve . . . . . . . . . . Yes
d2E/dv2 - V curve . . . . . . . . . No d2E/dv2 - V curve . . . . . . . . . No
log dE/dV -V curve . . . . . . . . . No log dE/dV -V curve . . . . . . . . . No
E - t curve . . . . . . . . . . . . No E - t curve . . . . . . . . . . . . No
V - t curve . . . . . . . . . . . . No V - t curve . . . . . . . . . . . . No
dv/dt - t curve . . . . . . . . . . No dv/dt - t curve . . . . . . . . . . No
129
This application bulletin represents selected, possible application examples. These have been tested with all possible
care in our lab with the analytical instrument mentioned in the bulletin. The experiments were conducted and the
resulting data evaluated based on our current state of knowledge.
However, the application bulletin does not absolve you from personally testing its suitability for your intended methods,
instruments and purposes. As the use and transfer of an application example are beyond our control, we cannot accept
responsibility therefore.
When chemicals and solvents are used, the general safety rules and the directions of the producer must be
observed.

Mettler-Toledo GmbH METTLER TOLEDO on the WWW
Analytical
CH-8603 Schwerzenbach, Schweiz You can also reach us on the World Wide Web. There you
Telefon (01) 806 77 11, Fax (01) 806 73 50 will find information on other products and services of
Internet: http://www.mt.com METTLER TOLEDO and interesting information about our
company.
The address is http://www.mt.com
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Tel. +7-095-921 92 11, Fax +7-095-921 63 53
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For all other countries:

Mettler-Toledo GmbH
PO Box, VI-400, CH-8606 Greifensee, Schweiz Subject to technical changes
Tel. (01) 944 22 11, Fax (01) 944 31 70 © 12/03 Mettler-Toledo GmbH

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METTLER TOLEDO Titrators

Dedicated to Mr. Kees Mooibroek

M086 Epoxide Values ................................................................................................. 19

M087 Bromine Number of Petroleum Distillates and Aliphatic Olefins ............................... 25

M090 Determination of Saponification Value ................................................................. 31

M096 Iodine Value in Resins and Oils According to Wijs ................................................. 49

M206 Determination of Carboxyl Groups in PET ............................................................ 58

M238 Determination of Permanganate Index in Waste Water .......................................... 67

METTLER TOLEDO Titrators Characteristic Values

M099 Conductometric Base Number Titration of Motor Oil............................................... 94

M061 pH, Acidity, Lactone and Formol Value of Honey................................................. 100

M242 Determination of Amine Number ....................................................................... 115

Characteristic Values METTLER TOLEDO Titrators

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

3) The titration can also indicated photometrically by a

Accessories 1 additional burette DV1005,

Calculation The whole acidic components are neutralized, including half of

Waste Organic solvent waste (chlorinated and

Author Kees Mooibroek

Method 084B Acid Values (non aqueous) 15-Apr-1994 14:35

Table of measured values Titration curve

Acid Number of Castor Oil

Sample Castor oil, 9-11 g Preparation and Procedures

Substance Acidic components

Titrant KOH in Ethanol:

Standard Potassium hydrogen phthalate

Instruments DL50Graphix, DL53/55/58

Accessories 100 mL titration beaker ME-101974

Chemistry 2) The first equivalent point is due to the neutralization of 1 mL

Calculation Blank determination (Meth. SZ-bw):

Acid value det. (Meth: SZtit):

Author Dieter Rehwald

Method SZtit Säurezahl Rizinulöl/DAB 22-Feb-1999 19:42

No ID Sample amount and results

Table of measured values Titration curve

Acid Number of Cosmetic Creams

Sample Cosmetic creams, 1-2 g Preparation and Procedures

2) To ensure complete dissolution, the sample solution is

Titrant KOH in Ethanol:

Standard Potassium hydrogen phthalate

Instruments DL50Graphix, DL53/55/58

Accessories 100 mL titration beaker ME-101974

2) In addition, an EQP titration was performed. Two equivalence

3) The arrows in the titration curve indicate two equivalence

Acid value det. (Meth: 40012):

Waste Organic solvent waste Literature:

Author U. Büchi/P. Schauwecker

*** 17-NOV-81 ***

PROV. 11321 1321

Table of measured values Titration curve

Neutralizing Value of Baking Powder

Sample Baking powder, 10 g Preparation and Procedures

Method 40013 (sample deter.):

Waste Aqueous waste (after neutralization)

Author K. Mooibroek/P. Schauwecker

*** 20-NOV-81 ***

METHOD 118 1521

Table of measured values Titration curve

Acid Number of Polyester

Sample Polyester, 0.2-0.4 g Preparation and Procedures

Substance Acidic components

Titrant KOH in Ethanol:

Standard Potassium hydrogen phthalate

* 17-NOV-81 *

* 20-NOV-81 *

Free Fatty acid FFA = atM/(100*m) %