微波消解样品-电感耦合等离子体原子发射光谱法测定铅精矿中铅、砷、镉、汞

采用微波消解样品-电感耦合等离子体原子发射光谱法同时测定铅精矿中主体元素铅及有毒有害元素砷、镉、汞的含量。0.20g试样置于消解罐中,先后加入硝酸9mL、盐酸3mL、氟硼酸2mL及过氧化氢2.5mL,密闭罐盖按设定的微波消解程序进行消解。试验选择铅、砷、镉和汞的分析线分别为220.351,189.042,228.802,184.950nm以消除基体干扰。铅、砷、镉、汞的检出限分别为16.0,2.2,0.4,0.8μg.g-1。方法用于铅精矿标准样品(GBW 07617)和铅精矿实际样品分析,此方法的测定值与认定值及原子吸收光谱法或原子荧光光谱法的测定值相一致。方法的相对标准偏差(n=10)在0.15%～3.9%之间。

ICP-AES Determination of Lead,Arsenic,Cadmium and Mercury in Lead Concentrates with Microwave Assisted Sample Digestion

The main element(Pb) and 3 poisonous and harmful elements(As,Cd and Hg) in lead concentrates were determined simultaneously by ICP-AES with microwave assisted sample digestion.0.20 g of the sample in a digestion vessel was mixed with 9 mL of HNO3,3 mL of HCl,2 mL HBF4 and 2.5 mL of H2O2 successively;after covering the vessel tightly,the sample was digested in microwave digestor under the pre-set program.Analytical spectral lines of 220.351 nm for Pb,189.042 nm for As,228.802 nm for Cd and 184.950 nm for Hg were chosen for the analysis.Values of detection limits(3s) of Pb,As,Cd and Hg found were 16.0,2.2,0.4 and 0.8 μg·g-1 respectively.The proposed method was applied to the analysis of a CRM(GBW 07617) and a sample of lead concentrate.The results of the elements found in the CRM by the present method were in consistency with the certified values,while the results of elements found in the concentrate sample were checked quite well with the results obtained by AAS and AFS.Values of RSD′s(n=10) found were in the range of 0.15%-3.9%.