硫黄のスズ(II)-強リン酸を利用した気化分離-けい光X線分析法による定量

概要

論文の詳細を見る
The method is divided into three operations, the first being the evolution of hydrogen sulfide. the second being its fixing to a silver nitrate test paper, and the third is measurement of sulfur in the test paper by X-ray fluorescence spectrometry. Hydrogen sulfide was made by heating the sample with tin(II)-strong Phosphoric acid reagent (500g of reagent grade phosphoric acid was concentrated and heated to 270℃. To this 40g stanous chloride dihydrate was added and the mixture was heated again to 290℃). The method was applied to the determination of sulfur in iron and steels. Procedure : Place a sample containing up to 25μg of sulfur into the reaction tube. Add 10ml of tin(II)-strong phosphoric acid reagent and connect the capture part to which a test paper has been attached. Heat the contents for 15minutes in a stream of nitrogen(45ml/min) on a furnace whose temperature has been regulated at 400℃. Transfer the test paper to a sample holder and measure the intensity of SK_a line. The intensity was proportional to the sulfur amount (1 to 25μg). The coefficient of variation was 3.5% (with 10μg of sulfur) in five runs.
社団法人日本分析化学会の論文
1978-03-05