The purpose of the document is to establish a general and uniform method for the determination of free caustic alkali in soap.
2.0 SCOPE
This standard testing procedure is suitable for the determination of free caustic alkali in soap.
3.0 RESPONSIBILITY
The expert and trained chemist are responsible for following this procedure. The technical manager is responsible for implementing this procedure.
4.1 Apparatus
4.1.1 Analytical balance
4.1.2 Water bath
4.1.3 Heating mantle
4.1.4 Oven
4.2 Glassware
4.2.1 Beaker-250 ml
4.2.2 Flask-250 ml
4.2.3 Burette-50 ml
4.2.4 Pipette-10 ml
4.2.5 Measuring cylinder-100 ml
4.2.6 Gooch crucible
4.3 Reagent
4.3.1 Ethyl alcohol
4.3.2 Barium chloride:10%(m/v)
4.3.3 Phenolphthalein:1 g in100 ml of 95% ethanol
4.3.4 Hydrochloric acid:0.1N
5.0 PROCEDURE
For Toilet Soaps and Unbuilt Laundry Soaps
5.1.1 Weigh 10 g of sample in a 250 ml conical flask.
5.1.2 Add about 100 ml of boiled and neutralized ethanol and reflux the solution.
5.1.3 Shaking frequently until soap is dissolved.
5.1.4 Add 5ml Barium chloride (10%m/v) solution to eliminate traces of carbonates.
5.1.5 Add a few drops of phenolphthalein indicator for titration.
5.1.6 Titrate the solution with standard 0.1N HCl.
5.1 For Soaps containing Builders And Filters
5.2.1 Weigh 2 g to 10 g of sample.
5.2.2 Digest with 200 ml of freshly boiled ethanol in the steam bath and dissolve the soap.
5.2.3 Filter into a filter flask through a tared, dried, and filter paper till neutral to phenolphthalein or through a tared and dried Gooch crucible dioxide and other acid fumes.
5.2.4 Filter paper and crucible must be dried on their own at 105 +2°C and weighed.
5.2.5 Wash it several times with hot ethanol to remove all alcohol soluble.
5.2.6 Heat the filtrate to boil.
5.2.7 Add about 0.5 ml of phenolphthalein indicator.
5.2.8 Titrate with standard hydrochloric acid.
6.0 CALCULATION
Free caustic alkali (as NaOH) % by mass = 4xVxN
V= Vol. of std. 0.1N HCl used in the sample
N= Normality of std. 0.1N HCl
M= Mass of the sample taken for test, in g
7.0 REVISION/CHANGE HISTORY: No
8.0 ATTACHMENTS
· Appendix-1: FLOW CHART FOR FREE CAUSTIC ALKALI
9.0 REFERENCES
· Clause 6.2 of IS 286:1978; Amendment 5,2011;RA 2013
END OF THE DOCUMENT
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