电感耦合等离子体发射光谱法(ICP-AES)测定高铼酸钾中的19种杂质元素

建立了一种用稀盐酸溶解样品,标准工作溶液中匹配钾,ICP-AES测定高铼酸钾中19种杂质元素的方法。在选定的仪器工作条件下,样品加标回收率(%)分别为：钠94.4～101、钙98.8～102、铝98.1～102、镁95.8～99.1、钴98.4～101、钼97.3～103、钛97.6～102、钒96.6～106、锆96.2～97.7、铬97.8～101、铜98.1～108、铁92.9～104、锰95.5～98.4、镍93.6～101、钯93.3～101、铅96.5～103、锌95.2～103、铂95.9～99.9、铑94.5～96.3；方法精密度RSD%(n=7)分别为：钠2.0～5.5、镁1.1～3.5、铝0.9～2.5、钙1.5～7.3、钴1.1～3.1、钼0.9～4.5、钛1.0～2.8、钒1.6～4.0、锆1.4～3.6、铬0.77～4.6、铜0.74～1.8、铁1.3～3.8、锰1.1～2.0、镍0.99～5.0、钯1.1～2.4、铅1.3～9.1、锌0.80～6.7、铂1.2～10、铑0.78～8.6。方法简便、快速、准确, 满足生产分析要求。

Determination of 19 Impurity Elements in Potassium Perrhenate by Inductively Coupled Plasma Atomic Emission Spectrometry

A method for determination of 19 impurity elements in potassium perrhenate by ICP-AES was established, wish dissolution sample by dilute hydrochloric acid ,and the standard working solution matched potassium to eliminate potassium in the sample.Under the selected instrument working conditions, the recoveries were as follows: sodium 94.4% ~ 101%, calcium 98.8% ~ 102%, aluminum 98.1% ~ 102%, magnesium 95.8% ~ 99.1%, cobalt 98.4 %~ 101%, molybdenum 97.3% ~ 103%, titanium 97.6% ~ 102%, vanadium 96.6% ~ 106% , Zirconium 96.2% ~ 97.7%, chromium 97.8% ~ 101%, copper 98.1%~ 108%, iron 92.9 %~ 104%, manganese 95.5% ~ 98.4%, nickel 93.6% ~ 101%, palladium 93.3%~ 101%, lead 96.5% ~ 103%, zinc 95.2%~ 103%, platinum 95.9% ~ 99.9% , rhodium 94.5% ~ 96.3%.The RSD% (n = 7) of the method were as follows: sodium 2.0% ~ 5.5%, magnesium 1.1% ~ 3.5%, aluminum 0.9%~ 2.5%, calcium 1.5% ~ 7.3%, cobalt 1.1% ~ 3.1%, molybdenum 0.9% ~ 4.5%, titanium 1.0 %~ 2.8%, vanadium 1.6% ~ 4.0% , Zirconium 1.4% ~ 3.6%, chromium 0.77% ~ 4.6%, copper 0.74%~ 1.8%, iron 1.3 %~ 3.8%, manganese 1.15% ~ 2.0%, nickel 0.99% ~ 2.0%, palladium 1.1%~ 2.4%, lead 1.3% ~9.1%, zinc 0.80%~ 6.7%, platinum 1.2% ~ 10% , rhodium 0.78% ~ 8.6%.