高纯钼粉中超痕量杂质的质谱分析
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摘要
建立高纯钼粉中超痕量杂质测定的分析方法。采用电感耦合等离子体串联质谱(ICP-MS/MS)的MS/MS模式,选择H2为反应气,利用H2原位质量法测定Si和Ca;选择O2为反应气,利用O2原位质量法测定Cd,利用O2质量转移法测定P,As,Se,Ta,Sn,Sb,Ba和W;选择NH3/He作为反应气,利用原位质量法测定Na,Mg,Al,K和V,利用质量转移法测定Ti,Cr,Mn,Fe,Co,Ni,Cu,Zn;采用单四极杆(SQ)无气模式测定Pb,Bi,Th和U。与传统的带碰撞/反应池(CRC)电感耦合等离子体质谱(ICP-MS)相比,各元素的背景等效浓度(BEC)和检出限更低,消除质谱干扰更加彻底。在优化的工作条件下,28种元素的线性相关系数(R~2)≥0.999 7,线性关系良好,检出限为0.04~50.1ng·L~(-1),加标回收率为92.2%~107.4%,相对标准偏差(RSD)≤4.3%,表明所建立的分析方法具有极好的准确性和精密度。实际样品的分析结果显示,方法可用于纯度为5N(≥99.999%)高纯钼粉中28个杂质元素的测定。
An analytical method for the determination of ultra-trace impurities in high purity molybdenum was established by inductively coupled plasma tandem mass spectrometry(ICP-MS/MS).In MS/MS mode,H_2 was used as the reaction gas to measure Si and Ca through the H_2on-mass method.O_2 was employed as the reaction gas to measure the Cd via the O_2on-mass method,and P,As,Se,Ta,Sn,Sb,Ba,and W were measured by the O_2 mass-shift method.NH_3/He was adopted as the reaction gas,so that Na,Mg,Al,K,and V could be measured by NH_3/He on-mass method,and Ti,Cr,Mn,Fe,Co,Ni,Cu,and Zn could be measured by the NH_3/He mass-shift method.Pb,Bi,Th,and U were measured in single quadropole(SQ)mode without gas.Compared with conventional collision/reaction cell(CRC)inductively coupled plasma mass spectrometry(ICP-MS),the background equivalent concentration(BEC)and detection limit of analyte in this method were lower,and the mass spectrum interference could be eliminated more thoroughly.Under optimized working conditions,the calibration curves of analytes showed good linearity with linear correlation coefficient(R~2)≥0.999 7.The detection limit was 0.04~50.1ng·L~(-1),the spike recoveries were 92.2%~107.4%and the relative standard deviation(RSD)was≤4.3%,indicating that the proposal method has excellent accuracy and precision.The results of the sample analysis showed that the method can be used for the determination of 28impurity elements in high purity molybdenum powder with purity of 5N(≥99.999%).
An analytical method for the determination of ultra-trace impurities in high purity molybdenum was established by inductively coupled plasma tandem mass spectrometry(ICP-MS/MS).In MS/MS mode,H_2 was used as the reaction gas to measure Si and Ca through the H_2on-mass method.O_2 was employed as the reaction gas to measure the Cd via the O_2on-mass method,and P,As,Se,Ta,Sn,Sb,Ba,and W were measured by the O_2 mass-shift method.NH_3/He was adopted as the reaction gas,so that Na,Mg,Al,K,and V could be measured by NH_3/He on-mass method,and Ti,Cr,Mn,Fe,Co,Ni,Cu,and Zn could be measured by the NH_3/He mass-shift method.Pb,Bi,Th,and U were measured in single quadropole(SQ)mode without gas.Compared with conventional collision/reaction cell(CRC)inductively coupled plasma mass spectrometry(ICP-MS),the background equivalent concentration(BEC)and detection limit of analyte in this method were lower,and the mass spectrum interference could be eliminated more thoroughly.Under optimized working conditions,the calibration curves of analytes showed good linearity with linear correlation coefficient(R~2)≥0.999 7.The detection limit was 0.04~50.1ng·L~(-1),the spike recoveries were 92.2%~107.4%and the relative standard deviation(RSD)was≤4.3%,indicating that the proposal method has excellent accuracy and precision.The results of the sample analysis showed that the method can be used for the determination of 28impurity elements in high purity molybdenum powder with purity of 5N(≥99.999%).
引文
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