氢还原重量法测定氯铱酸铵中的铱含量

Determination of Iridium in Ammonium Chloroiridate by HydrogenReduction Gravimetric Method

采用氢气为还原剂,将氯铱酸铵还原为铱并进行测定,建立了氢还原重量法测定氯铱酸铵中铱含量的实验方法。确立了电阻炉的最佳控温程序,考察了杂质元素对铱分析结果的影响。结果表明,氯铱酸铵在100℃碳化,350℃分解铵盐,750℃还原铱。用该方法测定铱含量,分析结果的极差和相对标准偏差(RSD,n=6)分别为0.05%、0.024%~0.044%。该方法具有准确度高,重复性好的特点,能够满足实际生产中氯铱酸铵铱含量的分析检测要求。

Ammonium chloroiridate was reduced to iridium by hydrogen as reducing agentand analyzed.The determination of iridium in ammonium chloroiridate by hydrogen reduction gravimetric method was established.The optimal temperature control procedure of reduction furnace was set up and the effect of impurities on the determination results of iridium was tested.It was found that ammonium chloroiridate was carbonized at 100℃firstly,then ammonium salt in was decomposed at 350℃,lastly the obtained matter was reduced into iridium at 750℃.The method was applied to determine iridium content.The rang and the relative standard deviation(RSD,n=11)were 0.03%and 0.063%,respectively.The recovery of standard addition was 99.5%~100.3%.The method had advantages of high accuracy and good reproducibility,can meet the requirement of iridium determination in ammonium chloroiridate.