火花放电原子发射光谱类型标准化校正方式的探讨

在国内,火花放电原子发射光谱分析广泛使用类型标准化进行方法校正。在国外,标准和文献中鲜见使用此方法的相关论述。类型标准化主要采用平移校正和转动校正两种方式,哪种方式更加合理也鲜见报道。国外设备类型标准化的默认设置优先采用转动校正方式,相关国内标准对最优校正方式的规定尚不明确,此默认设置的合理性有待探讨。实验选用低合金钢20CrNi2Mo、R407标准样品和不锈钢317L、0Cr18Ni9标准样品,引用国内相关标准,以正确度临界差为评判依据,模拟类型标准化样品和待测样品“十分接近”和“接近”两种情况下平移校正和转动校正的数据正确度。经数据统计分析,平移校正分析结果均满足要求,转动校正结果在“接近”情况下部分元素不满足要求。结合相关国家标准中元素含量范围和精密度数据进行分析,通过计算允许最大偏倚量并制作曲线图方式展开分析,得出如下结论:在满足文中类型标准化控制要点前提下,分析设置更适合于采用平移校正方式。

Discussion on the type standardization correction method of spark discharge atomic emission spectrometery

In China,the spark discharge atomic emission spectrometry widely uses type standardization for method calibration. In foreign countries, however, there are few relevant discussions about this method in standards and documents. There are two ways of calibration in type standardization, i.e., translation correction and rotation correction, but it is rarely reported that which one is more reasonable. The default setting of type standardization in foreign equipment gives priority to the rotation correction, but it is not clear about the optimal correction in relevant domestic standards. Moreover, the rationality of this default setting needs to be further discussed. Standard samples of low alloy steel (20CrNi2Mo and R407) and stainless steel (317L and 0Cr18Ni9) were selected. The relevant domestic standards were cited. The critical difference of trueness was used as judgment criteria. The trueness of data in translation correction and rotation correction was simulated under the conditions of "very close" and "close" between the standardized type samples and the samples to be tested. Through analyzing the statistical data, the analyzing results of translation correction could meet the requirements, while some elements did not meet the requirements when the rotation correction results were under the condition of "close". Based on the analysis of the element content range and precision data in relevant national standards, by calculating the maximum allowable bias and plotting the curve, the following conclusions were obtained: on the premise of meeting the control points of type standardization in the text, the analysis setting was more suitable for the translation correction.