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    微波消解-电感耦合等离子体原子发射光谱法测定铜精矿中银、铅、镉、汞和砷的含量

    Determination of Silver, Lead, Cadmium, Mercury and Arsenic in Copper Concentrate by Inductively Coupled Plasma Atomic Emission Spectrometry with Microwave Digestion

    • 摘要: 建立了微波消解-电感耦合等离子体原子发射光谱法(ICP-AES)测定铜精矿中银、铅、镉、汞和砷含量的方法。将已烘至恒重的铜精矿样品0.2 g用盐酸6 mL、硝酸2 mL和氢氟酸0.5 mL按微波消解程序进行消解,结束后冷却至室温,所得溶液用水定容至100 mL,此外,个别碳含量高的样品须干过滤除碳。以银328.068 nm、铅220.353 nm、镉214.438 nm、汞194.227 nm和砷193.759 nm为分析谱线,采用ICP-AES测定其中品质指标银元素和环保指标铅、镉、汞和砷元素的含量。通过铁、铜基体匹配消除铁、铜元素的干扰。结果表明,银、铅、镉、汞、砷的质量浓度在一定范围内与其对应的发射强度呈线性关系,检出限(3s)依次为0.001 5,0.030,0.014,0.006 0,0.037 mg·L-1。按上述方法分析国家标准物质、能力验证样品,测定值与认定值或中位值一致,相对标准偏差(n=11)为0.63%~1.8%。按此法分析铜精矿实际样品,所得结果与标准方法的一致。

       

      Abstract: A method for determination of silver, lead, cadmium, mercury and arsenic in copper concentrate by inductively coupled plasma atomic emission spectrometry (ICP-AES) with microwave digestion was established. Copper concentrate sample of 0.2 g that had been dried to constant weight was digested with 6 mL of hydrochloric acid, 2 mL of nitric acid and 0.5 mL of hydrofluoric acid according to the microwave digestion procedure. After that, it was cooled to room temperature, and the resulting solution was made its volume up to 100 mL with water, moreover, individual samples with high carbon content must be dry filtered to remove carbon. 328.068 nm of silver, 220.353 nm of lead, 214.438 nm of cadmium, 194.227 nm of mercury and 193.759 nm of arsenic were used as analytical spectral lines, and silver content of quality index and the contents of lead, cadmium, mercury and arsenic of environmental protection indexes were determined by ICP-AES. The interference of iron and copper elements was eliminated by iron and copper matrix matching. It was showed that the linear relationships between mass concentrations of silver, lead, cadmium, mercury and arsenic and their corresponding emission intensities were kept in the definite ranges, with detection limits (3s) of 0.001 5, 0.030, 0.014, 0.006 0 and 0.037 mg·L-1, respectively. The proposed method was used for analyzing the national reference materials and capability verification samples, and the determined values were consistent with the certified values or median values, with RSDs (n=11) in the range of 0.63%-1.8%. The actual samples of copper concentrate were analyzed by this method, and the results were consistent with that of the standard methods.

       

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