溶媒抽出-原子吸光法による水中の微量カドミウム,亜鉛,鉛,銅の分析

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A method for the determination of ppb amounts of cadmium, zinc, lead and copper in water has been developed by combining atomic absorption spectrophotometry with solvent extraction with a volume ratio of aqueous phase/solvent as large as 5001000 ml/25ml. The following three procedures of extraction were compared. (A) To a sample water in a separatory funnel were added sodium-potassium tartrate (20%, 5 ml) and hydroxylamine hydrochloride (10%, 2 ml). This mixture was neutralized with ammonia using Thymol Blue indicator, and the buffer solution (NH4Cl-NH3, pH 10) was added to adjust the pH. It was extracted twice by shaking with dithizone-carbon tetrachloride solution (0.03%, 10 ml). The extract was washed with water and then shaken with hydrochloric acid (1N, 10 ml). This hydrochloric acid solution was aspirated in an atomic absorption spectrophotometer to determine cadmium, lead and zinc (For the determination of copper, 6N hydrochloric acid should be used to strip the element from the carbon tetrachloride extract). (B) To the dithizone-carbon tetrachloride extract in (A) was added methyl-isobutyl ketone (10 ml), and the mixture was aspirated. (C) To the sample water whose acidity was preliminarily adjusted to pH 45 was added ammonium pyrrolidine dithiocarbamate solution (1%, 5 ml). The mixture was shaken with methyl-isobutyl ketone (25 ml) and the extract was subjected to the measurement. All the three methods were applied satisfactorily to the determination of the four elements in various types of water samples. The method (C) showed the highest sensitivity because of the decreased volume of the extract due to an appreciable solubility (ca. 2%) of methyl-isobutyl ketone in water and also of the "solvent effect", but the apparent solubility of the solvent was a little different in sea water and in pure water. The standard addition method gave good results in this case.
社団法人日本分析化学会の論文

溶媒抽出-原子吸光法による水中の微量カドミウム,亜鉛,鉛,銅の分析

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