应用能力验证结果评定火花源原子发射光谱法测定低合金钢中镍的方法精密度研究

Study on the precision evaluation in determination of nickel in low alloy steel by spark source atomic emission spectrometry based on proficiency testing results

应用能力验证结果,研究一种分析方法精密度的评定方法。利用6个轮次能力验证中,采用火花源原子发射光谱法(SS-AES)测定不同含量水平的低合金钢中Ni含量的结果数据,对方法的精密度进行评定,建立了重复性限r和再现性限R的拟合计算公式。采用组内相关系数(ICC)法,对拟合公式计算结果与国家标准中的精密度公式计算结果的一致性进行了评价,重复性限r和再现性限R的组内相关系数分别为ICC_r=0.99,ICC_R=0.94,表明拟合公式信度良好,拟合公式与国家标准方法的精密度公式非常一致。

The evaluation method of precision in analysis was studied based on proficiency testing results.In six rounds of proficiency testing,the precision of method was evaluated using the determination results of Ni with various content levels in low alloy steel by spark source atomic emission spectrometry(SS-AES).The fitting calculation formula of repeatability limit(r)and reproducibility limit(R)was established.The consistency between the calculation results by fitting formula and precision formula in national standard was evaluated using intra-class correlation coefficient(ICC)method.The intra-class correlation coefficient of repeatability limit(r)and reproducibility limit(R)was ICC_r=0.99 and ICC_R =0.94,respectively.It indicated that the reliability of fitting formula was good.The fitting formula was consistent with the precision formula in national standard method.