电感耦合等离子体-质谱法测定高纯硫粉末中17种痕量杂质

Determination of 17 trace impurities in high purity sulfur powder by inductively coupled plasma mass spectrometry

建立电感耦合等离子体-质谱(ICP-MS)法测定高纯硫粉中Si、P、V、Cr、Mn、Ni、Co、Cu、As、Zn、Zr、Cd、In、Sb、Te、Pb、Bi等17种痕量金属杂质含量的方法。样品用HClO4溶解后挥发硫基体,使样品中杂质元素得到富集,各杂质元素的方法检出限为0.1～50ng/g。方法加标回收率为83%～117%。各杂质元素均为10ng/mL的混合标准溶液平行7次测定的相对标准偏差均小于5%。该方法能够满足纯度为99.999%～99.9999%的高纯硫样品中杂质测定的需要。

Seventeen trace impurities in high purity sulfur powder such as manganese,nickel were determined by inductively coupled plasma mass spectrometry in this paper.Samples were dissolved by concentrated perchloric acid.After solution was evaporated,the impurities were enriched.The method detection limits were in the range from 0.1 to 50ng/g.Good spiked recoveries from 83% to 117% were obtained.The relative standard deviations（RSDs） calculated from seven consecutive injections of 10ng/mL standard mixtures were less than 5%.The operation is simple and the impurities are concentrated efficiently.It can meet the demand for the analysis of high purity sulfur powder from 99.999% to 99.9999%.