微波消解-电感耦合等离子体原子发射光谱法测定铂铑系列合金中铑

提出了试样经微波消解后用电感耦合等离子体原子发射光谱法（ICP AES）测定铂铑系列合金中铑的分析方法。对试样的微波消解条件、基体和谱线干扰等进行研究。结果表明，在230℃温度下，以盐酸和少许过氧化氢、硝酸和氢氟酸为消解试剂，试样在密闭容器中分两次进行消解60 min可以完全溶解。消解液用ICP AES测定时，通过选择合适的分析谱线可避免基体和光谱干扰。用本方法测定了系列铂铑合金的模拟试样，测定结果与行业标准方法的分析结果相一致，相对误差在010%～030%之间，相对标准偏差小于066%（n=6）。该法可以用于铂铑系列合金中铑含量的测定。

Determination of rhodium in platinum-rhodium series alloy by microwave digestion-inductively coupled plasma atomic emission spectrometry

An analysis method for the determination of rhodium in platinum-rhodium series alloy by inductively coupled plasma atomic emission spectrometry(ICP-AES) after microwave digestion was proposed.The microwave digestion conditions of sample,interference of matrix and spectral line were investigated.The results showed that the sample could be fully dissolved in a mixed acid of hydrochloric acid,hydrogen peroxide,nitric acid and hydrofluoric acid by microwave digestion twice for 60 min in closed container at 230℃.During determination of the digestion solution by ICP-AES,the interference of matrix and spectrum could be avoided by selecting proper analytical lines.The proposed method was applied to the determination of platinum-rhodium alloy simulation sample with relative error in the range of 0.10 %-0.30 % and relative standard deviation below 0.66 %(n=6),in addition the determination results were consistent with those obtained by industrial standard method.This method was applicable for the determination of rhodium in platinum-rhodium series alloy.