惰气熔融-热导法测定金属硅中氮

Inert gas fusion thermal conductivity method for the determination of nitrogen in silicon metal

研究了用TC600氧氮测定仪测定金属硅中氮的最佳工作条件。结果表明：在称样量为0.10 g,分析功率为4 750 W,比较器水平为6的条件下测定,可以得到满意的分析结果。应用硝酸钾标准溶液建立工作曲线,曲线的回归方程为y=0.985 8x＋0.000 017,相关系数r=0.999 8。用本方法测定金属硅试样10次,得到的相对标准偏差（RSD）≤4.3%,加标回收率在96.6%～108.2%之间。

The optimum conditions for the determination of nitrogen in silicon metal using TC 600 oxygen/nitrogen analyzer are developed. It is indicated that a satisfactively result is obtained when the determination is perfected in the following conditions. The sample mass is selected as 0.10 g. The power for analysis is 4 750 W. The comparator level is 6. Standard potassium nitrate solution is used in preparation of calibration curve. The linear regression equation is as follows： y = 0. 985 8x ＋ 0. 000 017, with the correlation coefficient of 0. 999 8. The method is employed in determination of nitrogen in silicon metal, giving the relative standard deviation ≤4.3 % and the addition standard recoveries of 99.6 %- 108.2%（n=10）.