电感耦合等离子体发射光谱法同时测定铅锌矿中银铜铅锌
Simultaneous Quantification of Silver, Copper, Lead and Zinc in Lead-Zinc Ores by Inductively Coupled Plasma-Atomic Emission Spectrometry
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摘要: 采用盐酸-硝酸-硫酸混合酸分解样品,全谱直读电感耦合等离子体发射光谱法同时测定铅锌矿石中的银、铜、铅和锌。基于改善和提高测定结果准确度和精密度的要求,分析了溶液稀释因子和酸度等实验条件对测定结果的影响。结果表明,当溶液的稀释因子为1000,盐酸的体积分数在5%~10%时,测定结果最佳。采用内标法,通过加入钴内标测量分析谱线的相对强度,抵消了由于实验条件的波动引起的影响。方法检出限银为1.96 μg/g,铜为6.00 μg/g,铅为9.00 μg/g,锌为3.00 μg/g,精密度(RSD, n=10)为1.41%~7.50%。方法经国家标准物质分析验证,测定值与标准值相符,结果准确可靠。Abstract: Lead-zinc ore samples were digested with HCl-HNO3-H2SO4 mixed acid. Silver, copper, lead and zinc in sample solutions were directly determined by inductively coupled plasma-atomic emission spectrometry. Based on the requirement of improving and enhancing the accuracy and precision, the external conditions such as the dilution factor and the acidity of the solution were systematically studied. The results showed that the quantification is most accurate when the dilution factor of the solution is 1000 and the volume fraction of HCl is between 5% and 10%. The internal element of cobalt was added to measure the relative intensity of the spectral line in order to offset the effect of fluctuations in experimental conditions. The detection limits of the method were 1.96 μg/g for Ag, 6.00 μg/g for Cu, 9.00 μg/g for Pb and 3.00 μg/g for Zn with a precision in the range of 1.41%-7.50% (RSD, n=10). The reliability of the method has been tested by quantification of the elements in National Standard Reference Materials and the results were in agreement with the certified values.
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