Determination of germanium in tungsten molybdenum ore by inductively coupled plasma mass spectrometry
GAO Xiao-fei1,2,3, NI Wen-shan1,2,3, MAO Xiang-ju1,2,3, XIAO Fang*1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China; 3. Key laboratory of Evaluation and Multipurpose Utilization of Polymetallic Ores Ministry of Land and Resources, Zhengzhou 450006, China;
Abstract：The composition of tungsten molybdenum ore is relatively complex, and it usually contains several types of minerals including silicate, sulfides, oxide, and so on. Generally, the tungsten molybdenum ore is hardly dissolved. The sample was decomposed with hydrofluoric acid by microwave digestion. After adding nitric acid-perchloric acid-sulfuric acid, the solution was heated on high-temperature electric hot plate to further dissolve the sample. The wet salt formed after fuming at high temperature was redissolved with nitric acid. It was found that the sample could be completely dissolved. When the sample solution was clarified, the content of germanium in supernatant liquor was determined by inductively coupled plasma mass spectrometry (ICP-MS) using 45ng/mL rhenium as the internal standard. Thus the determination method of germanium in tungsten molybdenum ore was established. The experiments showed that the mass concentration of germanium in range of 5-100ng/mL had a linear relationship with the ratio of signal intensity between germanium and internal standard. The correlation coefficient was 0.9995, and the detection limit of method was 0.006ng/mL. The experimental method was applied for the determination of germanium in the certified reference material of molybdenum ore, the certified reference material of tungsten ore and the actual sample of tungsten molybdenum ore. The found results of certified reference materials were basically consistent with the certified values. The relative standard deviations (RSD, n=6) of determination results ranged from 0.30% to 2.8%. According to DZ/T 0130-2006 (The Specification of Testing Quality Management for Geological Laboratories), the calculated relative deviation of repeated analysis was less than the limit value. The standard solution of germanium was added into sample above for recovery test. The recoveries were between 93% and 106%.
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