1. Shandong Dongyi Photoelectric Instruments Co.,Ltd.,Yantai 264670,China; 2. China Institute of Atomic Energy,Beijing 102413,China; 3. Technical Center for Industrial Product and Raw Material Inspection and Testing of Shanghai Customs,Shanghai 200135,China
Abstract:The contents of CaF2 and CaCO3 in fluorite are usually determined by EDTA titration method. However, the operation process of this method is complicated. The end point of titration is difficult to be judged, which affects the determination accuracy of CaF2 and CaCO3. Moreover, the contents of CaCO3 and CaF2 cannot be simultaneously determined by the traditional method, which hardly meet the rapid analysis requirements in industrial production. In this study, calcium acetic acid solution was selected to dissolve the sample, which could inhibit the decomposition of CaF2 in the dissolution process of CaCO3. Under the conditions of optimizing the position parameters of the light source and the analytical spectral line, Ca II 315.886 9 nm with high signal-to-background ratio was selected as the analytical line. The contents of CaF2 and CaCO3 in fluorite were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The linear range of calibration curves was 0.2-100 μg/mL, and the linear correlation coefficient was 0.999 8. The limits of detection of CaCO3 and CaF2 were 0.019 9% and 0.015 6%, respectively. The contents of CaF2 and CaCO3 in six fluorite standard samples were determined according to the experimental method. The relative standard deviations (RSD, n=6) of CaF2 and CaCO3 were 0.20%-0.55% and 1.7%-3.8%, respectively. The contents of CaF2 and CaCO3 in actual fluorite samples were determined according to the experimental method and JC/T 1021.6-2007, and the found results were consistent.
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