Abstract:The determination method of barium carbonate and barium sulfate contents in barite by inductively coupled plasma atomic emission spectrometry (ICP-AES) was discussed with different sample treatment methods. Pure barium sulfate was dissolved with different concentration acetic acids. The results showed that when it was dissolved with 1.7mol/L acetic acid at room temperature for 1h, the dissolution rate of barium sulfate was consistent with that obtained with water for dissolution. Therefore, the following procedures were adopted for the determination of barium carbonate in sample: the sample was dissolved with water, and the content of barium in sample solution was determined by ICP-AES, thus the content of water soluble barium in sample was obtained; the sample was dissolved with 1.7mol/L acetic acid, and the content of barium in sample solution was determined by ICP-AES, thus the content sum of water soluble barium and that in the form of barium carbonate in sample was obtained; then the content of barium in the form of barium carbonate could be calculated by subtraction from the latter from the former, thus the content of barium carbonate could be obtained by further conversion. Therefore,the determination of barium carbonate in barite by ICP-AES could be realized. The sample was treated with 1.0mol/L hydrochloric acid by heating and boiling for 30min, the barium-containing impurities such as barium chloride and barium carbonate could be effectively dissolved. The dissolution tests of pure barium sulfate with 1.0mol/L hydrochloric acid showed that the dissolution rate of barium sulfate by 1.0mol/L hydrochloric acid was only 0.090%, which could be ignored compared to the mass fraction of barium sulfate in barite (higher than 10%). Therefore, the following procedures were adopted for the determination of barium sulfate in sample: the sample was treated with 1.0mol/L hydrochloric acid; after filtration, the precipitate was treated by sodium peroxide fusion-sodium carbonate solution for leaching; the content of barium in leaching solution was determined by ICP-AES to obtain the content of barium in the form of barium sulfate; then it was converted to the content of barium sulfate, realizing the determination of barium sulfate in barite sample by ICP-AES. Considering that the content of barium carbonate in barite sample was low while the content of barium sulfate was relatively high, Ba 455.403nm with highest sensitivity and Ba 230.424nm with low sensitivity was selected as analytical line for the determination of barium carbonate and barium sulfate, respectively. The linear correlation coefficients of calibration curves were 0.9991-0.9999 and 0.9995-1.0000, respectively. The content of barium carbonate and barium sulfate in barite sample was determined according to the experimental method. The detection limit was 0.001% and 0.003%, respectively. The relative standard deviations (RSD, n=12) for barium carbonate and barium sulfate were less than 21% and 1.0%, respectively. The experimental method was applied for the determination of barium carbonate in sample. Meanwhile, barium carbonate was added for standard addition recovery test. The recoveries were between 90% and 110%. The proposed method was applied for the determination of barium sulfate in certified reference material of barite for composition analysis. The results were consistent with the certified values.
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