Top-down法评定X射线荧光光谱法测定车用柴油中总硫含量的测量不确定度  

Evaluating Uncertainty of Determination of sulfur content in diesel fuel by X-ray fluorescence with Top-down Strategy

作　　者：张鑫[1] 王硕 段卫宇 吴丹[2,3,4] 李响 王桂萱 ZHANG Xin;WANG Shuo;DUAN Wei-yu;WU dan;LI Xiangg;WANG Gui-xuan(Dalian University,Dalian Liaoning 116622,China;Liaoning Inspection,Examination&Certification Centre,Shenayng Liaoning 110032,China;Liaoning Province Product Quality Supervision and Inspection Inspection Institute,Shenayng Liaoning 110032,China;National Quality Supervision&Testing Center of Petroleum Products(Shenyang),Shenayng Liaoning 110144,Chin)

机构地区：[1]大连大学,辽宁大连116622 [2]辽宁省检验检测认证中心,辽宁沈阳110032 [3]辽宁省产品质量监督检验院,辽宁沈阳110032 [4]国家石油产品质量监督检验中心(沈阳),辽宁沈阳110144

出　　处：《当代化工》2022年第12期3017-3020,共4页Contemporary Chemical Industry

基　　金：辽宁省自然科学基金计划重点项目(项目编号:20170520108);辽宁省检验检测认证中心青年人才创新创业项目(项目编号:SC20210120);辽宁省检验检测认证中心科技成果转化项目(项目编号:CGZH202102)。

摘　　要：采用Top-down技术评定X射线荧光光谱法测定车用柴油中总硫含量的测量不确定度。在对车用柴油检测结果的偏倚和精密度验证后证明数据受控,车用柴油稳定性较好,以多次重复测试结果计算实验室内期间相对标准偏差(S_(p,rel))和重复性相对标准偏差(S_(r,rel)),通过外部质量控制的能力验证结果计算测定结果的偏倚和实验室间精密度相对标准偏差(S_(bias,rel)),通过以上数据评定测量不确定度,来评估测定方法和精密度的控制情况。以Top-down精密度法评定测量不确定度,可以反映出检测人员的检测能力、测量仪器的重复性以及试验环境等因素对不确定度的干扰,不需要识别和建立测量不确定度分量,但Top-down法无法识别出对测量不确定度有较大影响的测量不确定度分量。结果表明,实验室间精密度对扩展不确定度的贡献最大,实验室可通过能力验证结果数据评估检测过程精密度控制情况。The Top-down technique was used to evaluate the measurement uncertainty of the determination of total sulfur content in vehicle diesel fuel by X-ray fluorescence spectrometry.After verifying the bias and precision of the test results of vehicle diesel,it was proved that the data were controlled and the vehicle diesel had good stability.The relative standard deviation(S_(p,rel))and the repeatability relative standard deviation(S_(r,rel))in the laboratory were calculated from the repeated test results.The bias of the test results and the relative standard deviation(S_(bias,rel))of the precision between laboratories were calculated from the verification results of the external quality control ability.The measurement uncertainty was evaluated from the above data,to evaluate the control of measurement method and precision.The Top-down precision method was used to evaluate the measurement uncertainty,which could reflect the interference of such factors as the detection ability of the tester,the repeatability of the measuring instrument,and the test environment on the uncertainty.It was not necessary to identify and establish the measurement uncertainty components,but the Top down precision method could not identify the measurement uncertainty components that had greater impact on the measurement uncertainty.The results showed that the inter laboratory precision contributed the most to the expanded uncertainty,and the laboratory could evaluate the precision control of the testing process through the data of the capability validation results.

关 键 词：测量不确定度 X射线荧光光谱法 总硫含量 Top-down法 车用柴油 

分 类 号：O657.34[理学—分析化学]