Determination of antimony in antimony ore by flame atomic absorption spectrometry
WANG Xiaoqiang1,2,3, LIANG Qian*1,2,3, ZHAO Yanan1,2, ZHANG Hui1,2,3, ZHANG Liman1,2,3, YAN Huiyuan1,2,3
1. Henan Academy of Geology,Zhengzhou 450016,China; 2. General Institute for Non-ferrous Metals and Geological Exploration of Henan Province,Zhengzhou 450016,China; 3. Henan Nonferrous Metals Deep Prospecting Engineering Technology Research Center,Zhengzhou 450016,China
Abstract：The content of antimony in antimony ore is an important index for ore deposit evaluation and industrial beneficiation test. Therefore, the accurate determination of antimony content in antimony ore has an important guiding significance. The sample was dissolved by sulfuric acid smoking in sulfuric acid and nitric acid. Based on the characteristic that citric acid could react with antimony to form a complex, antimony was extracted by heating and boiling with citric acid-hydrochloric acid mixed acid. It solved the problem that antimony was easily hydrolyzed in hydrochloric acid, which caused low determination results. Thus, a method for determination of antimony in antimony ore was established by flame atomic absorption spectrometry(FAAS) with air-acetylene flame at wavelength of 231.147 nm. Arsenic and sulfur are often associated in antimony ores. The interference test of arsenic showed that its interference could be ignored. Since sulfur could react with hydrochloric acid in extracting solution to form hydrogen sulfide, which would be released and had no interference with the determination. The certified reference materials of antimony ore for composition analysis were treated according to the proposed method, and the contents of antimony in the test solution were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and flame atomic absorption spectrometry, respectively. The results showed that the measured values of FAAS were basically consistent with the certified values, while the measured values of ICP-AES were lower than the certified values. This might be related to the fact that the tube diameter of nebulizer injection capillary of ICP-AES was smaller than that of FAAS, and a small amount of sulfuric acid remained in test solution adhered to the inside of the nebulizer injection capillary, resulting in a smaller lifting volume of the test solution. Under the optimized experimental conditions, the mass concentration of antimony in range of 2-10 μg/mL showed a good linear relationship with its corresponding absorbance. The correlation coefficient was 0.999 6. The limit of detection of the method was 0.1 μg/g, and the limit of quantification was 0.3 μg/g. The proposed method was applied for determination of antimony content in the certified reference materials for composition analysis and the actual samples of antimony ore. The coefficient of variation (CV) of the determination results was 0.75%-2.2% for actual samples, and the relative error (RE) of the determination results was -0.76%-1.10% for the certified reference materials, which could meet the requirements for variable coefficient and relative error of determination results, specified in GB/T 27417-2017 and DZ/T 0130.3-2006, respectively.
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