Determination of cadmium in copper concentrate by inductively coupled plasma atomic emission spectrometry combined with internal standard method
ZENG Jing1, HU Jun-kai1, FENG Zhao-jun*2
1. Daye Non-Ferrous Design & Research Institute Co., Ltd.,Huangshi 435000, China; 2.The First Geological Brigade of Hubei Geological Bureau, Huangshi 435100, China
Abstract：The sample was dissolved with hydrochloric acid, nitric acid, hydrofluoric acid and perchloric acid under covering conditions, and the analytical line and internal standard line was Cd 226.502 nm and Y 371.029 nm, respectively. Thus, a determination method of cadmium in copper concentrate was established by inductively coupled plasma atomic emission spectrometry(ICP-AES) combined with internal standard method. The effect of acid dosages and covering conditions was investigated. The results indicated that when 10.0 mL of hydrochloric acid, 10.0 mL of nitric acid, 3.0 mL of hydrofluoric acid and 3.0 mL of perchloric acid was added to dissolve sample with covering and smoking for removing fluorine, and 2.0 mL of perchloric acid was added successively until smoke was disappear, the common sample could be dissolved completely. For specific samples, the addition of perchloric acid and smoking were repeated until the samples were completely dissolved. The effect of internal standard method and matrix matching method on elimination of matrix interference, instrument and environment fluctuation was compared. The determination precision of cadmium by internal standard method was basically consistent with that of matrix matching method under the same conditions. The relative standard deviations (RSD, n=11) were between 0.9% and 1.1%. Moreover, the interference tests of coexisting elements in copper concentrate were conducted. It was found that the determination results of cadmium gradually decreased with the addition of copper and iron matrix. This influence could be eliminated by internal standard method. The mass concentration of cadmium in range of 0.025-10.0 μg/mL showed linearity to its corresponding emission intensity with correlation coefficient of r=0.999 8. The detection limit of method was 0.000 2% (mass fraction). The determination range of cadmium was 0.001 1% and 2.0% (mass fraction). The content of cadmium in certified reference material of copper concentrate (VS2891-84) was determined according to the experimental method. The results were consistent with the certified values. The relative error (RE) was 0.34%.
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