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The method described below can be used to identify and determine organo-mercury derivatives employed as preservatives in cosmetic products for the eyes. It is applicable to thiomersal (INN) (sodium 2-(ethylmercuriothio)benzoate) and phenylmercury and its salts.
The organomercury compounds are complexed with l,5-diphenyl-3-thiocarba-zone. After extraction of the dithizonate with carbon tetrachloride, silica gel, thin-layer chromatography is carried out. The spots of the dithizonates appear as an orange colour.
All the reagents should be of analytical purity.
sodium 2-(ethylmercuriothio)benzoate,
ethylmercury chloride or methylmercury chloride,
phenylmercury nitrate or phenylmercury acetate,
mercury dichloride or mercury di(acetate).
For example, the following Rf values are obtained:
Rf | Colour | |
---|---|---|
Thiomersal | 0,33 | Orange |
Ethylmercury chloride | 0,29 | Orange |
Methylmercury chloride | 0,29 | Orange |
Phenylmercury salts | 0,21 | Orange |
Mercury (II) salts | 0,10 | Orange |
Mercury di(acetate) | 0,10 | Orange |
1,5-diphenyl-3-thiocarbazone | 0,09 | Pink |
The content of organomercurial compounds determined by this method is expressed as the percentage by mass (m/m) as mercury in the sample.
The method consists in measuring the quantity of total mercury present. It is thus necessary to have first made sure that no mercury in an inorganic state is present and to have identified the organomercurial derivative contained in the sample. After mineralization, the mercury liberated is measured by flameless atomic absorption.
All the reagents should be of analytical purity.
Take all normal precautions for trace mercury analysis.
Let:
=
the mass (in milligrams) of the test sample.
=
the quantity of mercury (in μg) read on the instrument.
The quantity of mercury, expressed as mercury, as percentage by mass, is calculated by the formula:
In the case of mercury concentrations of 0,007 %, the difference between the results of two determinations carried out in parallel on the sample should not exceed an absolute value of 0,00035 %.
Norm ISO 5725.
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