Determination of silicon, ferric, magnesium, potassium, sodium, phosphorus and sulphur in fluorite by microwave digestion-inductively coupled plasma atomic emission spectrometry
NIAN Ji-qiang, GU Feng, ZHU Chun-yao, LU Na-ping
Analysis and Characterization Center, Institute of Research of Iron and Steel, Jiangsu Province/Sha-Steel, Zhangjiagang 215625, China
Abstract：The fluorite sample was pretreated by closed microwave digestion technology. The analysis method of silicon, iron, magnesium, potassium, sodium (in oxide), phosphorus and sulfur in fluorite by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The dissolution of sample was investigated. The results showed that the sample could be fully decomposed by hydrochloric acid, nitric acid and hydrofluoric acid under microwave digestion conditions. Moreover, the volatilization loss of nonmetallic elements such as sulfur, phosphorus and silicon could be avoided. During the preparation of calibration curve, proper amount of standard solution of potassium oxide, sulfur and phosphorus was added into some standard sample solutions. Moreover, the foreign standard samples of potassium oxide, sulfur, phosphorus and magnesium oxide with wide content range were used. Therefore, the analytical range of potassium oxide, sulfur, phosphorus and magnesium oxide was enlarged. The proposed method was applied to the analysis of standard and actual samples of fluorite. The found results were consistent with the certified values or those obtained by X-ray fluorescence spectrometry (XRF). The relative standard deviations (RSD, n=10) were less than 5.0% except for phosphorus. The recovery test of each component was conducted. The recovery rates were between 91.5% and 109.0%.
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