Determination of disperse elements of gallium, indium, thallium, germanium, tellurium and cadmium in geological samples by inductively coupled plasma mass spectrometry with high-pressure microwave digestion
LI Xiao-jing, BIAN Peng-sha*, JIN Qian, CHEN Qing-zhi, SUN Meng-hua, SHEN Yu-min
Hebei Research Center for Geoanalysis, Baoding 071051, China
Abstract：The establishment of a highly sensitive and accurate analytical method for disperse elements has aways been the focus of geological sample analysis. The samples were treated by high-pressure microwave digestion in HF-HNO3 system. 205Tl, 125Te, 69Ga, 74Ge, 115In, 114Cd were selected as the measured isotopes. The isobaric interference of 74Ge and 115In was corrected by the online calibration equation, while the isobaric interference of 114Sn to 114Cd were corrected by offline interference correction. A method for the determination of disperse elements of Ga, In, Tl, Ge, Te and Cd in geological samples by inductively coupled plasma mass spectrometry (ICP-MS) has been developed. The mass of samples, conditions of high-pressure microwave digestion, and leaching acid species were optimized. The results show that under the optimized experimental conditions, the correlation coefficient of the calibration curve is not less than 0.9997, with the detection limit ranges from 0.005 to 0.093μg/g, and the low limit of determination from 0.017 to 0.31μg/g. The proposed method was applied for the 12 times parallel determination of Ga, In, Tl, Ge, Te and Cd in the composition analysis standard substances of soil, water sediment, and andesite rock. The analytical results were basically consistent with the certified values, with the relative standard deviations (RSD) were not more than 8.5% and the relative errors were not more than 9.1%. The soil samples were analyzed by experimental methods. The results were basically consistent with the determination of Ga, In and Tl by closed acid dissolution-ICP-MS, determination of Ge by hydride generation atomic fluorescence spectrometry, determination of Te by ethanol sensitization-ICP-MS and the determination of Cd by graphite furnace atomic absorption spectrometry.
李晓敬, 边朋沙, 金倩, 陈庆芝, 孙孟华, 申玉民. 高压微波消解-电感耦合等离子体质谱法测定地质样品中分散元素镓铟铊锗碲镉[J]. 冶金分析, 2019, 39(4): 38-44.
LI Xiao-jing, BIAN Peng-sha, JIN Qian, CHEN Qing-zhi, SUN Meng-hua, SHEN Yu-min. Determination of disperse elements of gallium, indium, thallium, germanium, tellurium and cadmium in geological samples by inductively coupled plasma mass spectrometry with high-pressure microwave digestion. , 2019, 39(4): 38-44.
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