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介绍了原子荧光光谱法测定萤石中砷的协同试验验证。采用均匀水平设计,10个协同实验室和5个水平试样参与协同试验验证。协同试验验证前,水平试样进行了均匀性和稳定性检验。验证结果经曼德尔检验、科克伦检验和格拉布斯检验后,确定了测试方法的重复性和再限性。结果表明,As含量总平均值(m)在0.000011%~0.00766%范围内,方法重复性标准差(Sr)在2.31×10-6%~1.92×10-4%之间,Sr与m的函数关系为Sr=0.0246 m+2.76×10-6,相关系数R2=0.9998;方法再现性方差(SR)在0.0000255%~0.000415%之间,SR与m的函数关系为SR=0.0532 m+1.67×10-5,相关系数R2=0.9903。
The synergetic experimental verification of determination of arsenic in fluorite with atomic fluorescence spectrometry is introduced. Using a uniform level design, 10 collaborative laboratories and 5 horizontal samples were involved in the collaborative experiment. Before the verification of the collaborative test, the horizontal sample was tested for uniformity and stability. Verification results by the Mandel test, Cochrane test and Grabs test to determine the test method repeatability and further limit. The results showed that the average As content (m) was in the range of 0.000011% to 0.00766%, the method reproducibility standard deviation (Sr) was between 2.31 × 10-6% and 1.92 × 10-4%, the function of Sr and m The relationship between the two factors is Sr = 0.0246 m + 2.76 × 10-6, and the correlation coefficient R2 = 0.9998. The method reproducibility variance (SR) is between 0.0000255% and 0.000415%. The relationship between SR and m is SR = 0.0532 m + 1.67 × 10 -5, the correlation coefficient R2 = 0.9903.