METTLER TOLEDO

M051

Iodine Value of Edible Oils and Fats According to Wijs (AOAC Method
Method for the determination of iodine value (g I 2/100g) of edible oils and fats according to Wijs as indicated by AOAC Official Methods of Analysis (1984), Chapter 28.023 Sample
Fats and oils, approx. 25 g / expected Iodine value

Preparation and Procedures

1) Dissolve the sample in CCl4, add 25 mL Wijs solution and keep in the dark for approx. 1 hour to complete the reaction. 2) Add deionized water and titrate excess iodine with sodium thiosulphate.

Substance Chemicals

C-C double bonds, -CH=CH-

15 mL carbon tetrachloride, CCl4 ; 25 mL Wijs solution; 100mL water; 15 mL 10% potassium iodide, KI Sodium thiosulphate, Na2S2O3 c(Na2S2O3)=0.1 mol/L;

Wijs solution, c(ICl) = 0.1 mol/L: Dissolve 16.2 g iodine monochloride (ICl) in a 1 L volumetric flask with glacial acetic acid. Store the Wijs solution in amber bottle sealed with paraffin until it is used. Wijs solution is sensitive to temperature, moisture and light. Slight variations of the temperature considerably affect titer of the Wijs solution. Therefore it is essential that blanks and samples are titrated at the same time. The mean value of the blank determination (method 051b) is automatically stored as auxiliary value H3. Typical results: Blank = 4.94 mmol, srel = 0.04%, n = 5

Titrant

Standard Instruments

Potassium iodate, KIO3 DL70, ST20A, AT250, Matrix printer EPSON FX800 with serial interface

Accessories

250 mL Titration beakers ME-23829, Additional burette drive DV90

Remarks Indication Chemistry

DM140-SC at Sensor 2
The iodine value is defined as the weight of iodine absorbed by 100 g of an oil or fat. 1) The excess of Wijs solution should be 50-60% of the amount added, ie. 100-150% of amount reacted with the sample.

ICl3 + I2 = 3 ICl ICl + KI = I2 + KCl 2(SO3S)2- + I2 = 2 I- + (S2O6S2)2-

Calculation

Blank determination (Method 096B): R1 = Q R1 is stored as auxiliary value H3 Iodine value det. (Method 096A): R1 = (H3-Q1)*C1/m C1 = M/(10*z)

2) If the result will be assumed (e.g. in routinr quality control) the predispensing can be adjusted accordingly in volume or changed to % nominal content . This also shortens the titration time. 3) The addition of 10 mL 2.5% mercury (II) acetate in glacial acetic acid (after Wijs solution is added) shortens the reaction time to 5 minutes

Results

Waste disposal

Halogenated organic solvents.

Literature: AOAC Official Method of Analysis, 1984, Chapter 28.023

Author

Ruth von Rotz

Results
METTLER DL70 051a Titrator I2-value of oils and fats 25-June-1991 rvr PT 2 SW 2.0 3:37 pm

Measured User Titrator Version RESULTS No ID1 1/1 1/2 1/3 1/4 1/5

Weight 2.0267 2.0766 2.0892 2.031 2.0863 n x s srel = = = = g g g g g 5 11.85 0.013 0.107

Results 11.85 11.85 11.85 11.84 11.87 g I2/100 gI2-value g I2/100 gI2-value g I2/100 gI2-value g I2/100 gI2-value g I2/100 gI2-value

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STATISTICS Number results R1 Mean value Standard deviation Rel. standard deviation Various Samples Sample Coconut fat Margarine "light" Lard Olive oil Margarine Rape oil Sunflower oil Weight (g) 2.00-2.10 0.40-0.45 0.40-0.45 0.20-0.25 0.50-0.55 0.20-0.25 0.20-0.25

g I2/100 gI2-value g I2/100 gI2-value %

n 5 3 5 5 3 4 3

Iodine value (gI2/100g) 11.8 37.3 57.6 82.5 86.1 113.4 132.7

RSD (%) 0.11 0.26 0.13 0.16 0.21 0.15 0.06

t (min) 5 5 5 6 3 5 4

Table of measured values

Titration curve

Method
Method 051a Version I2 - value of oils and fats 19-June-1991 16:21 . . . . 051a . . . . I2 - value of oils and . . . . 19-June-1991 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Stand 1 Weight m 0.02 1.5 254 2 16:21 Method 051b Version Blank I2 - value 19-June-1991 16:15 . . . . 051b . . . . Blank I2 - value . . . . 19-June-1991 16:15 . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 Stand 1 Fixed volume U 25.0 Blank 0.0 1 Title Method ID . . . . . . . . . Title . . . . . . . . . . . fats Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Lower limit [g] . . . . . Upper limit [g] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . Predispensing 2 . . . . . slope [mV,pH, .../mL] Titrant addition . . . . dE (set)[mV] . . . . . Limits dV . . . . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t (min) [s] . . . . t (max) [s] . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . E - V curve . . . . . . . . Table of measured values . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . . Title Method ID . . . . . . . . . Title . . . . . . . . . . . Date/time . . . . . . . . . Sample Number samples . . . . . . . Titration stand . . . . . . Entry type . . . . . . . . . Volume [mL] . . . . . ID1 . . . . . . . . . . . . Molar mass M . . . . . . . . Equivalent number z . . . . Dispense Titrant . . . . . . . . . . Concentration [mol/L] . . . Volume [mL] . . . . . . . . Stir Speed [%] . . . . . . . . . Time [s] . . . . . . . . . . Titration Titrant . . . . . . . . . . Concentration [mol/L] . . . Sensor . . . . . . . . . . . Unit of meas. . . . . . . . Titration mode . . . . . . . Predispensing 1 . . . . . Volume [mL] . . Predispensing 2 . . . . . slope [mV,pH, .../mL] Titrant addition . . . . dE (set)[mV] . . . . . Limits dV . . . . . . dV(min) [mL] . . . dV(max) [mL] . . . Measure mode . . . . . . dE [mV] . . . . . . . dt [s] . . . . . . . . t (min) [s] . . . . t (max) [s] . . . . Threshold . . . . . . . . Maximum volume [mL] . . . Termination after n EQPs n = . . . . . . . . . Evaluation procedure . . Calculation Result name . . . . . . . . Formula . . . . . . . . . . Constant . . . . . . . . . . Result unit . . . . . . . . Decimal places . . . . . . . Record Output unit . . . . . . . . Raw results last sample . . E - V curve . . . . . . . . Table of measured values . . Statistics Ri (i=index) . . . . . . . . Standard deviation s . . . . Rel. standard deviation srel Outlier test . . . . . . . . Auxiliary value ID text . . . . . . . . . . Formula . . . . . . . . . . Record Output unit . . . . . . . . All results . . . . . . . .

. . . . KI 10% . . . . 10.0 . . . . 15.0 . . . . 50 . . . . 45 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3H2O 0.1 DM140-SC mV EQP mL 20.0 To slope 4.0 DYN 0.02 Absolute 0.02 0.5 EQU 1.0 1.0 6.0 30.0 50.0 50.0 Yes 1 Standard I2 - value R=(H3-Q)*C/m C=M/(10*z) g I2/100g 2 Printer Yes Yes Yes R1 Yes Yes Yes

. . . . KI 10% . . . . 10.0 . . . . 15.0 . . . . 50 . . . . 45 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Na2S2O3H2O 0.1 DM140-SC mV EQP mL 40.0 To slope 4.0 DYN 4.0 Absolute 0.02 0.5 EQU 1.0 1.0 6.0 30.0 50.0 60.0 Yes 1 Standard Blank I2 - value R1=Q[1] mmol 4 Printer Yes Yes Yes R1 Yes Yes Yes I2 - value

. . . . Blank . . . . H3=x . . . . Printer . . . . Yes

. . . . Printer . . . . Yes