Determination of 9 major and minor elements in phosphate rock by inductively coupled plasma atomic emission spectrometry with microwave digestion
FAN Lei1,2,3, GUO Xiaorui1,2,3, WANG Tiantian1,2,3, NI Wenshan1,2,3, MAO Xiangju*1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources,CAGS, Zhengzhou 450006,China; 2. Key Laboratory for Polymetallic Ores′ Evaluation and Utilization,MNR,Zhengzhou 450006,China; 3. China National Engineering Research Center for Utilization of Industrial Minerals,Zhengzhou 450006,China
Abstract：The accurate determination of various elements in phosphate rock plays an important guiding role in the development and utilization of phosphate rock. The phosphorus rock sample was treated in hydrochloric acid, nitric acid and hydrofluoric acid with microwave digestion. After digestion, 20 mL of saturated boric acid solution was added to neutralize the residual hydrofluoric acid to avoid impurities introduced by etching glass. The contents of phosphorus, potassium, sodium, calcium, magnesium, silicon, aluminum, iron and titanium were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Thus, a method for determination of 9 major and minor elements in phosphate rock was established by ICP-AES with microwave digestion. The acid for microwave digestion was investigated. The results showed that the phosphate rock sample could not be completely digested with hydrochloric acid and nitric acid, but the sample could be fully digested with hydrochloric acid, nitric acid and hydrofluoric acid. The dosage of hydrofluoric acid was optimized, and 2 mL of hydrofluoric acid was selected. Under the optimized experimental conditions, the mass concentrations of elements had good linear relationships with their corresponding emission spectral intensities. The linear correlation coefficients were all not less than 0.999 7. The limits of detection for elements were between 0.003% and 0.078% (mass fraction). The certified reference materials of phosphate rock were determined according to the proposed method. The results were consistent with the certified values. The relative standard deviations (RSD, n=5) were all less than 3%. The proposed method was applied for determination of phosphate ore samples. The relative standard deviations (n=5) of determination results were between 0.26% and 1.9%. The recoveries were between 90% and 105%.
樊蕾, 郭晓瑞, 王甜甜, 倪文山, 毛香菊. 微波消解-电感耦合等离子体原子发射光谱法测定磷矿石中9种主次元素[J]. 冶金分析, 2023, 43(9): 56-61.
FAN Lei, GUO Xiaorui, WANG Tiantian, NI Wenshan, MAO Xiangju. Determination of 9 major and minor elements in phosphate rock by inductively coupled plasma atomic emission spectrometry with microwave digestion. , 2023, 43(9): 56-61.
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