Determination of 10 major elements in magnesite by microwave digestion-inductively coupled plasma atomic emission spectrometry
YU Lei1,2, LIU Jun1,2, ZHANG Xiaoyi1,2, YIMANHAZI·Jialisen1,2
1. Xinjiang Research Institute of Mineral Resources, Urumqi 830000,China; 2. Key Laboratory of Rock and Mineral Analysis and Process Mineralogy of Xinjiang, Urumqi 830000,China
Abstract：The content range of ten major elements in magnesite (including magnesium, calcium, silicon, iron, aluminum, potassium, sodium, manganese, titanium, and phosphorus) has great difference. Therefore, the simultaneous analysis of multi-elements is relatively difficult. The sample was treated by microwave digestion in hydrochloric acid-nitric acid-hydrofluoric acid system. Yttrium was selected as the internal standard element. The contents of ten major elements in magnesite, including magnesium, calcium, silicon, iron, aluminum, potassium, sodium, manganese, titanium, and phosphorus, were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) with hydrofluoric acid resistant injection system. The linear correlation coefficients of calibration curves of elements were all higher than 0.999. The limits of detection were 0.000 5%-0.028%. The contents of magnesium, calcium, silicon, iron, aluminum, potassium, sodium, manganese, titanium, and phosphorus in five certified reference materials of magnesite were determined according to the experimental method. The relative standard deviations (RSD, n=6) of determination results were between 0.35% and 4.9%. The found results were consistent with the certified values. Ten elements in magnesite sample were determined according to the experimental method. Meanwhile, silicon was also determined by gravimetry, magnesium was determined by titration method, and other eight elements were determined by ICP-AES after open acid dissolution. The method comparison showed that the found results had no significant difference. The consumption of acid in microwave digestion was small. Moreover, no impurity was introduced and silicon could be remained in the solution, which solved the problem that silicon and other major elements could not be determined simultaneously. The use of internal standard method improved the determination precision of high content magnesium. The proposed method provided a new approach for the rapid and accurate determination of magnesite.
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