锗烟尘中锗的测定——碘酸钾容量法

The Determination of Gemenium in Gemenium Soot——Potassium Iodate Titrimetry

文章采用硝酸-高氯酸-氢氟酸冒烟使锗烟尘中的大量碳、硫去除.试样经高锰酸钾-硝酸-磷酸溶样后,在盐酸-磷酸介质中蒸馏分离锗,使大部分干扰元素经蒸馏分离,以次亚磷酸钠还原四价锗为二价,以淀粉为指示剂,在20℃以下,用碘酸钾标准溶液滴定.该法滴定终点明显,准确率高.标准回收率为95.00％～108.00％,变异系数为0.73 ％～1.37％,适用于锗烟尘中锗的测定分析.

In the paper, Nitric Acid - Perchloric Acid - Hydrofluoric Acid fumes are used to remove large amounts of Carbon and Sulfur in the Gemenium Soot. The sample is dissolved in the Potassium Permanganate - Nitric Acid - Phosphoric Acid solution, then it is destilled to separate Germaniumin from the co-exist elements in the media of Hydrochloric Acid- Phosphoric Acid. Under 20 ℃, Gemenium was titrated by Potassium Iodate standard solution, using starch as indicator. This method has a distinct titration end point and high accuracy.The standard recovery is in the range of 95.00 %-108.00 %. The relative standard deviation （RSD） is in the range of 0.73 %-1.37 %. It can be used to determine the amount of Gemenium in Gemenium Soot.