电感耦合等离子体发射光谱法测定硫化物矿中的高含量铅

摘要

铅含量高的硫化物矿在氧化性酸的存在下极易形成硫酸铅沉淀而影响样品中铅的准确测定.文章通过王水-双氧水分解和高温灼烧后王水分解两种不同的样品处理方法,有效地去除样品中的硫,配合使用高盐雾化器采用电感耦合等离子体发射光谱法对硫化物矿石中的高含量铅进行测定.王水-双氧水分解可以测定硫化物矿中的铅、银和锑,高温灼烧后王水分解只能测定铅;两种样品处理方法均操作简便,具有准确度好、精密度高、分析速度快等优点.用这两种样品处理方法10次测定铅精矿(GBW 07167)中的铅,精密度(RSD)分别为0.38%和0.56%,相对误差分别为-0.41%和0.14%;测定方铅矿(GBW 07269)中铅精密度分别为0.76%和0.66%,相对误差分别为0.82%和0.45%.%The high content lead hosted in sulfide ore is easily formed PbSO4 precipitation with sulfur under the strong rnoxidizing acids , which effected the determination of Pb. This experiment established the two methods for determination of rnhigh content Pb in sulfide ore by inductively coupled plasma-atomic emission spectrometry ( ICP-AES) , being dissolved rnby aqua regia and H2O2 and by aqua regia after calcination at high lemperature. The aqua regia-H2O2 decomposition rnmethod can be used to simultaneously determine Pb, Ag and Sb in samples, but calcination at high temperature-aqua rnregia decomposition method only can be used to determinate Pb. The two methods are both simple and fast with high rnaccuracy and precision. The precision and accuracy of the two methods were demonstrated by analyzing reference rnmatenals GBW 07167 and GBW 07269. The RSD ( n = 10) of Pb for CBW 07167 were 0. 38％ and 0. 56％ , and rnrelative error were -0.41％ and 0. 14％ , respectively. The analytical results of Pb for reference material GBW 07269 rnwere determinated by the same methods, whose RSD (n = lO) were 0. 76％ and 0. 66％ , and relative error were rn0. 82％ and 0. 45％ , respectively.