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Fourth Commission Directive of 11 October 1985 on the approximation of the laws of the Member States relating to methods of analysis necessary for checking the composition of cosmetic products (85/490/EEC)

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Changes over time for: Division B.

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B.DETERMINATIONU.K.+E.U.

1.DEFINITIONU.K.+E.U.

The sulphite or hydrogen sulphite content of the sample as determined by the method is expressed as percentage by mass of sulphur dioxide.

2.PRINCIPLEU.K.+E.U.

After acidification of the sample, sulphur dioxide liberated is distilled into a solution of hydrogen peroxide. Sulphuric acid formed is titrated against a standardized sodium hydroxide solution.

3.REAGENTSU.K.+E.U.

All reagants should be of analytical purity.

3.1.Hydrogen peroxide 0,2 % (m/v). Prepare daily.U.K.+E.U.
3.2.Orthophosphoric acid (
).U.K.+E.U.
3.3.Methanol.U.K.+E.U.
3.4.Sodium hydroxide (0,01 M) standardized solution.U.K.+E.U.
3.5.Nitrogen.U.K.+E.U.
3.6.Indicator: mixture 1: 1 (v/v) of methyl red (0,03 % m/v in ethanol) and methylene blue (0,05 % m/v in ethanol). Filter the solution.U.K.+E.U.
4.APPARATUSU.K.+E.U.
4.1.Normal laboratory equipment.U.K.+E.U.
4.2.Distillation apparatus (see figure).U.K.+E.U.
5.PROCEDUREU.K.+E.U.
5.1.Weigh accurately about 2,5 g of sample into the distillation flask A (see figure).U.K.+E.U.
5.2.Add 60 ml of water and 50 ml of methanol (3.3) and mix.U.K.+E.U.
5.3.Place 10 ml of hydrogen peroxide (3.1), 60 ml of water and a few drops of indicator (3.6) in the distillation receiver D (see figure). Add a few drops of sodium hydroxide (3.4) until the indicator turns green.U.K.+E.U.
5.4.Repeat 5.3 for the wash bottle E (see figure).U.K.+E.U.
5.5.Assemble the apparatus and adjust the nitrogen (3.5) flow to about 60 bubbles per minute.U.K.+E.U.
5.6.Run 15 ml of orthophosphoric acid (3.2) from the funnel into the distillation flask A.U.K.+E.U.
5.7.Heat rapidly to boiling and then simmer gently for a total time of 30 minutes.U.K.+E.U.
5.8.Detach the distillation receiver D. Rinse the tube and then titrate with sodium hydroxide solution (3.4) until the indicator turns green (3.6).U.K.+E.U.
6.CALCULATIONU.K.+E.U.

Calculate the content of sulphite or hydrogen sulphite by mass in the sample by the expresssion:

where

M

=

molar concentration of sodium hydroxide solution (3.4),

V

=

volume of sodium hydroxide (3.4) required for titration (5.8), in millilitres,

m

=

mass of sample (5.1) in grams.

7.REPEATABILITY(1) U.K.+E.U.

For a content of 0,2 % m/m of sulphur dioxide the difference between two parallel determinations done on the same sample should not be greater than 0,006 %.

Sulphurdioxide distillation apparatus according to Tanner All dimensions in mmU.K.+E.U.
(1)

ISO 5725.

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