Influence of sample dissolution method on the determination of six elements in regional geochemical survey sample by inductively coupled plasma mass spectrometry
FENG Hai-yuan, MA Hai-ping
Anhui Geological Research Laboratory,Hefei 230001,China
Abstract：The regional geochemical survey sample was dissolved with HCl-HNO3-HClO4-HF. After extraction by aqua regia, the content of six microelements (including Co, Ni, Cu, Zn, Cd and Pb) was determined by inductively coupled plasma mass spectrometry (ICP-MS) using 59Co, 60Ni, 65Cu, 66Zn, 114Cd and 208Pb as determination isotopes. The mass spectrometry interference was corrected by indirect empirical formula. Three sample dissolution methods (i.e., HCl-HNO3-HClO4-HF digestion method, aqua regia digestion method and microwave digestion method) were compared. The determination data of certified reference materials of soil, stream sediment and rock were analyzed. The results indicated that the determination results of HCl-HNO3-HClO4-HF digestion and microwave digestion were consistent with the certified values. The treatment amount of sample in microwave digestion method was little, which was not suitable for the analysis of bulk geological samples. Therefore, the samples were dissolved with HCl-HNO3-HClO4-HF digestion method in this study. The correlation coefficients of calibration curves of Co, Ni, Cu, Zn, Cd and Pb were higher than 0.999 9. The detection limit of method (μg/g) was Co 0.04, Ni 0.69, Cu 0.89, Zn 1.31, Cd 0.029 and Pb 0.34, respectively. The proposed method was applied to the determination of six metal elements in standard sample of soil, stream sediment and rock for composition analysis. The found results were basically consistent with the certified values. The relative standard deviations (RSD, n=12) were less than 8%. The method was also used in the analysis of actual regional geochemical survey samples, and the results were consistent with those obtained by X-ray fluorescence spectrometry (XRF).
凤海元, 马海萍. 溶样方法对电感耦合等离子体质谱法测定区域地球化学调查样品中6种元素的影响[J]. 冶金分析, 2016, 36(8): 18-24.
FENG Hai-yuan, MA Hai-ping. Influence of sample dissolution method on the determination of six elements in regional geochemical survey sample by inductively coupled plasma mass spectrometry. , 2016, 36(8): 18-24.
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