摘要
采用微波消解的方式,用逆王水将铅锌尾矿分解,加入硫脲-抗坏血酸作为还原剂,样品与硼氢化钾溶液进行氢化反应后生成的气态氢化物用氩气载入原子荧光光谱测定砷、锑和铋的含量。通过回收率试验验证王水-水浴、王水-电加热板、和逆王水-微波消解3种分解体系对铅锌尾矿样品的分解效率,试验结果显示,逆王水-微波消解体系样品的回收率在相对宽的含量范围内表现理想。用国家标准物质GBW07303、GBW07405、GBW07406、GBW07162进行验证试验,目标元素的最大相对偏差(RD)为砷-3.48%、锑3.89%和铋-4.79%,最大相对误差(RE)为砷4.13%、锑4.84%和铋-4.88%。用空白试验确定的方法检出为砷0.28μg/g、锑0.06μg/g、铋0.04μg/g。方法的测定范围为砷1.2μg/g~1.2mg/g、锑0.24μg/g~200μg/g、铋0.16μg/g~120μg/g。
The lead-zinc tailings were decomposed by reverse aqua regia by microwave digestion.Thiourea ascorbic acid was added as reducing agent.The gaseous hydride generated after hydrogenation of the sample with potassium borohydride solution was loaded with argon to determine the contents of arsenic,antimony and bismuth by atomic fluorescence spectrometry.The decomposition efficiency of lead-zinc tailings samples by aqua regia water bath,aqua regia electric heating plate and reverse aqua regia microwave digestion was verified by recovery test.The test results showed that the recovery of samples in reverse aqua regia microwave digestion system was ideal in a relatively wide content range.The verification test was carried out with national standard materials GBW07303,GBW 07405,GBW 07406 and GBW 07162.The maximum relative deviation(RD)of the target elements was arsenic-3.48%,antimony-3.89%and bismuth-4.79%,and the maximum relative error(RE)was arsenic-4.13%,antimony-4.84%and bismuth-4.88%.Arsenic was detected by the method determined by blank test as 0.28μg/g,antimony 0.06μg/g,bismuth 0.04μg/g.The determination range of the method is arsenic 1.2μg/g~1.2mg/g,antimony 0.24μg/g~200μg/g,bismuth 0.16μg/g~120μg/g。
作者
何绒
HE Rong(Central Laboratory of Lanzhou Mineral Exploration Institute,Gansu Nonferrous Metal Geological Exploration Bureau,Lanzhou 730046,China)
出处
《世界有色金属》
2022年第6期162-164,共3页
World Nonferrous Metals
