利用控制图法评定原子荧光光谱法测定土壤中总砷含量的测量不确定度  

Evaluation of measurement uncertainty in determination of total arsenic content in soil by atomic fluorescence spectrometry based on control chart method

作　　者：王茜 徐崇颖 杨嘉晖 陈超 祁春景 王旭东 WANG Qian;XU Chongying;YANG Jiahui;CHEN Chao;QI Chunjing;WANG Xudong(Hebei Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Baoding 071051,China;Hebei Research Center for Geoanalysis,Baoding 071051,China)

机构地区：[1]河北省矿产资源与生态环境监测重点实验室,河北保定071051 [2]河北省地质实验测试中心,河北保定071051

出　　处：《冶金分析》2023年第2期31-38,共8页Metallurgical Analysis

基　　金：保定市科技计划项目(2140ZZ034);河北省地质矿产勘查开发局科技计划项目(201936)。

摘　　要：地质环境检测领域的土壤样品检测项目多、检测过程较为冗长,给该领域检测实验室测量结果的不确定度评定工作带来了很大难度。采用GB/T 27411—2012中提出的Top-down技术,探讨了控制图法在原子荧光光谱法(AFS)测定土壤中总砷含量的测量不确定度评定工作中的应用。在期间精密度条件下,通过对土壤中总砷元素的实验室质控样品连续30周的全检测流程测量,进行了数据的异常值判别,以及正态性、独立性、分辨力检验,按照失控准则对建立的控制图进行了分析,最后对数据进行t检验,验证了所采用测量系统和测量过程均处于受控状态,测量不确定度可用期间精密度标准差(sR′)表示,并验证了采用实验方法评定不确定度的合理性。与GUM法相比,控制图法可操作性强,结果更为合理,在地质、环境、农业等土壤样品检测领域具有更为广泛的应用前景。In the field of geological environment testing, the soil sample testing usually has many items and long process, which brings great difficulties to the uncertainty evaluation of measurement results in testing laboratories. The Top-down technology proposed in GB/T 27411-2012 was used to discuss the application of control chart method in the evaluation of measurement uncertainty for the determination of total arsenic content in soil by atomic fluorescence spectrometry(AFS). Under the condition of period precision, through the whole detection process measurement of laboratory quality control samples of arsenic in soil for 30 weeks, the abnormal value discrimination, normality, independence and resolution test of the data were carried out. The established control chart was analyzed according to the out-of-control criterion. Finally, the t test of the data was conducted to verify that the measurement system and measurement process were under control. The measurement uncertainty could be expressed by the standard deviation of period precision(sR′), and the rationality of using the method to evaluate the uncertainty was verified. Compared with Guide to the Uncertainty in Measurement(GUM) method, the control chart method showed strong operability and more reasonable results. It had a wider application prospect in the field of soil sample detection in geology, environment and agriculture.

关 键 词：控制图 原子荧光光谱法(AFS) 总砷 土壤 测量不确定度 

分 类 号：O657.31[理学—分析化学] TP315[理学—化学]