Determination of Sodium

Benzoate

From: Official Methods of

Analysis of the Association
of Official Analytical
th
Chemists 14 Edition

20.024-20.025
Benzoic Acid in Food Titrimetric Method (The presence of Vanillin interferes)

1. Thoroughly mix the sample

2. Transfer 150 ml or 150 grams to 500ml Volumetric Flask.

3. Add enough pulverized NaCl to saturate the H2O in the sample

4. Make alkaline to litmus paper using 10% NaOH solution or milk of lime and
dilute to volume with saturated NaCl solution.

5. Shake thoroughly and let stand for more than 2 hours, shaking frequently.
Filter

6. Pipette 100-200 ml of filtrate into separator. Neutralize to litmus paper with

HCL, then add 5 ml in excess.

7. Extract carefully with CHCl3 using successive portions of 70,50,40 and 30 ml.
Shake cautiously using rotary motion each time to avoid emulsion. The CHCl3
layer usually separates readily after standing for a few minutes. If and
emulsion forms, break it by stirring CHCl3 layer with glass rod, by drawing off
into a second separator and giving 1 or 2 sharp shakes from one end of the
separator to the other, or by centrifugation for a few minutes.
As this is a progressive extraction, carefully drain as much clear CHCl3
solution as possible after each extraction, but do not drain any of the emulsion
with CHCl3 layer. If this precaution is taken the CHCl3 extraction need not be
washed.

8. Transfer combined CHCl3 extracts to a porcelain evaporating dish, rinse

container several times with a few mls CHCL3 and evaporate to dryness at
room temperature in a current of dry air.

9. Dry residue overnight in desiccator.

10. Dissolve residue of benzoic acid in 30-50 ml alcohol, neutralize to

phenolphthalein.

11. Add approximately ¼ of this volume of H2O and 1 or 2 drops of

phenolphthalein

12. Titrate with 0.05N NaOH.

1ml 0.05 N NaOH = 0.0072g anhydrous Na benzoate.