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镍精矿样品中铝、钙、钴、铬、铜、锰、镁、镍、铅、锌等10种金属元素的含量。0.200 0 g试样置于消解罐中,先后加入盐酸2 mL、硝酸6 mL及氢氟酸1 mL,密闭罐盖按设定的微波消解程序进行消解。试验选择铝、钙、钴、铬、铜、镁、锰、铅、锌和镍的分析线分别为308.215,317.933,228.616,267.716,324.745,279.079,257.610,220.353,206.200,231.604 nm,配制工作曲线时采用基体匹配的方法消除基体干扰。方法用于镍钴矿标准样品(GBW 07283)和镍精矿实际样品的分析,此方法的测定值与认定值及国标方法的测定值相一致。方法的回收率在95.8%~103.1%之间,相对标准偏差(n=6)均小于4.5%。

Ten elements, i.e., Al, Ca, Co, Cr, Cu, Mn, Mg, Ni, Pb and Zn, in nickel concentrate were determined simultaneously by ICP-AES with microwave assisted sample digestion. 0.200 0 g of the sample in a digestion vessel was mixed with 2 mL of HCl, 6 mL of HNO3 and 1 mL of HF successively; after covering the vessel tightly, the sample was digested in microwave digestor under the pre-set programe. Analytical spectral lines of 308.215 nm (for Al), 317.933 nm (for Ca), 228.616 nm (for Co), 267.716 nm (for Cr), 324.745 nm (for Cu), 279.079 nm (for Mg), 257.610 nm (for Mn), 220.353 nm (for Pb), 206.200 nm (for Zn) and 231.604 nm (for Ni) were chosen for the analysis. Matrix effect was compensated by the matching method in preparation of calibration curves. The proposed method was applied to the analysis of a CRM (GBW 07283) and a sample of nickel 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 the GB methods. Values of recovery found were in the range of 95.8%-103.1% with RSD′s (n=6) less than 4.5%.