直流辉光放电质谱法检测三氧化钼中痕量元素含量

Analysis of trace elements content in molybdenum trioxide by direct current glow discharge mass spectrometry

建立了直流辉光放电质谱(dc-GDMS)测定三氧化钼中痕量元素含量的方法,优化了辉光放电参数,考察了三氧化钼制样面积对放电稳定性和灵敏度的影响。在优化条件下,测定2个三氧化钼标准样品BS ZZ42001和BS ZZ42003的相对灵敏度因子RSF_(1)和RSF_(2),计算得到平均相对灵敏度因子RSF_(A),对三氧化钼标准样品BS ZZ42002的测定结果进行校正,与BS ZZ42002的标准值比较,除Ti和Cd外,校正后得到的各元素测定值相对误差在±9.5%以内。对未知的三氧化钼样品测定结果进行校正,并与电感耦合等离子体原子发射光谱法(ICP-AES)和电感耦合等离子体质谱法(ICP-MS)结果对比。t检验结果表明,RSF_(A)校正值与ICP-AES/ICP-MS法测定值无显著性差异。该方法可为三氧化钼中多种痕量元素的快速定量分析提供参考。

A method was established to determine the trace elements content in molybdenum trioxide by direct current glow discharge mass spectrometry(dc-GDMS).The glow discharge parameters were optimized,and the effects of sample preparation area of molybdenum trioxide on discharge stability and sensitivity were investigated.Under the optimized conditions,two molybdenum trioxide standard samples BS ZZ42001 and BS ZZ42003 were analyzed to obtain two groups of relative sensitivity factors(RSF_(1) and RSF_(2)),and the average relative sensitivity factor RSF_A was calculated.The RSF_A was used to correct the determination results of molybdenum trioxide standard sample BS ZZ42002.Compared with the certified values of BS ZZ42002,the relative error of the measured values of various elements after correction with RSF_(A) was within±9.5%,except Ti and Cd.The determination results of an unknown molybdenum trioxide sample were corrected by RSF_(A).The inductively coupled plasma atomic emission spectrometry(ICP-AES)and inductively coupled plasma mass spectrometry(ICP-MS)were used as comparison methods.The results of t-test showed that there were no significant differences between the corrected values of RSF_(A) and the values determined by ICP-AES and ICP-MS.This method could provide a reference for the rapid quantitative analysis of trace elements contents in molybdenum trioxide.