摘要:
建立了王水溶矿-电感耦合等离子体发射光谱法测定砷矿石和锑矿石中主、次量元素砷、锑、硫及含量范围在100 μg/g以上的铜、铅、锌等元素的方法。研究了放置时间、溶液酸度、氧化剂与络合剂对砷、锑、硫及其他元素测定的影响。不同王水浓度酸度对可同时测定的其他元素的影响不明显;当溶液酸度较小时,不能放置,应及时测定;如需放置,应在溶液定容前加入酒石酸防止水解。样品中砷、锑、硫的含量在0.74%~39.7%时,相对误差(RE)在-0.17%~7.74%,5次独立测定的相对标准偏差(RSD)均小于2%;含量在100~500 μg/g以下的Sb,RE在-2.5%~4.79%,5次独立测定的RSD均小于2%。由于稀释倍数较大(DF=1000),不能准确测定含量在100 μg/g以下的铜、铅、锌;含量在100 μg/g以上的铜、铅、锌的RE在-10.3%~10.3%,5次独立测定的RSD基本小于5%。经标准物质验证获得满意结果。方法也可应用于砷、锑含量较高的硫化矿的测定。
Abstract:
The method for determining concentrations of As, Sb, S, and Cu, Pb, Zn which are above 100 μg/g, within arsenic ore and stibium ore by inductively coupled plasma-atomic emission spectrometry(ICP-AES)with aqua regia digestion is reported in this paper. The experimental conditions such as placement time, solution acidity, and the influence of oxidant and complexing agents on As, Sb, S and the other elements were studied. The relative error (RE) was determined to be between -0.17% and 7.74% with a RSD (n=5) of <2% if the concentrations of As, Sb, S in the samples were in the range of 0.74-39.7%. However, the RE was from -2.5% to 4.79% and RSD(n=5) was <2% if the Sb concentration is lower than 100-500 μg/g. The RE was determined to be between -10.3% and 10.3% with a RSD(n=5) of generally less than 5% if the Cu, Pb and Zn concentrations were more than 100 μg/g. No accurate data were obtained for Cu, Pb and Zn if the concentrations were lower than 100 μg/g, limited by the large dilution factor of 1000. The accuracy and precision of the method were validated by reference materials.
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