アンチモンの気化分離-けい光X線分析法による定量

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A method was presented for the determination of antimony in pig lead. The method consisted of the evolution of stibine, its fixing on a chloroauric acid test paper, and the measurement by X-ray fluorescence spectrometry. Procedure: Transfer a sample solution containing up to 200μg of antimony into an evolution vessel (200-ml Erlenmeyer flask). Add 15 ml of 12 M hydrochloric acid, and dilute the mixture to 50 ml with water. Add 5 g of granular zinc, and immediately connect a capture vessel to which a test paper has been attached. After standing for an hour, remove the test paper, set it on a sample holder, and count the X-ray fluorescence intensity of the SbK_a line (2θ=13.47°) in a vacuum using a tungsten target X-ray tube (50kV-20mA) and a LiF crystal. The intensity of the X-ray fluorescence was almost proportional to the antimony amount (up to 200μg). The standard deviation was 2.6% (with 1OOμg of antimony) in five runs.
社団法人日本分析化学会の論文
1976-01-10