Abstract:0.4 g of tin particles and 0.3 g of pure iron were put on the bottom of crucible, and 0.15 g of sample was added, then they were covered with 1.5 g of tungsten particles for determination. Or 1.50 g of sample was added on the bottom of crucible, and then it was covered with 1.8 g of iron-tungsten-tin mixed flux for determination. Consequently, a method for determination of total carbon in silicon powder by high frequency combustion infrared absorption method was established. Three calibration curves for carbon mass fraction in the range of 0.001%-0.01%, 0.01%-0.10% and 0.1%-1.0% were prepared respectively with the certified reference materials of anhydrous sodium carbonate and steel. The experimental results showed that the linear regression coefficients of calibration curves were all higher than 0.99. For the same silicon powder sample, the determination results which were based on the calibration curve with the certified reference materials whether anhydrous sodium carbonate or steel were consistent. The NIST57b silicon powder certified reference material was determined with the calibration curve prepared by steel certified reference material. The determination result was 0.021 4%. The relative error was 7.0%, which satisfied the guidance range of relative error between the determination result and true value. The verification tests of method were conducted in five laboratories using the silicon powder samples with three carbon content level. The statistics and examination for the results were performed according to GB/T 6379.2-2004. The results indicated that the founds determined by five laboratories were had good consistence, and there were no outliers, indicating that the dispersity of determination results of total carbon in silicon powder was within the acceptable range. The recoveries were between 95% and 120%.
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XU Min-xiu, HE Li, YAO Feng-hua, YUAN Kai-di, YANG Jun, JIANG Wei. Determination of total carbon in silicon powder by high frequency combustion infrared absorption method. , 2015, 35(9): 25-31.
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