还原蒸馏示波极谱法测定物料中微量硫

Determination of Trace Sulfer by Reduction-Destination and Oscillopolarography

本法用氢碘酸—盐酸—次亚磷酸为还原剂兼作溶剂,在蒸馏瓶中加热溶解试样,在不分离主体元素锡的条件下,直接将试样中硫还原呈硫化氢状态逸出。通过氮气载出,吸收于0.5N氢氧化钠溶液中。在示波极谱仪上,于-0.6～-1.1V进行扫描,记录峰值。本法适用于各种金属以及合金和金属氧化物中硫的测定。测定范围:0.0001～0.1％。

The sample is heated and dissolved in a reduction-destillation apparatus with hydroiodic acid-hydr-ochloric acid ( or glacial acetic acid)-sodium hypophosphite as both reducer and dissolvant. The sulfer contained in the sample is released in form of hydrogen sulfide which is carried by nitrogen and then absorbed in the solution of 0.5N sodium hydroxide. Thereafter it is scanned and the oscillopolarograph and the results show a good linear dependence between the peak of the wave and the concentration of sulfer within the range of 0-1.5g/ml. This method is rather sensitive and accurate, the measuring range is 0.0001-0.1%,