Top-Down法评定高频燃烧红外吸收法检测铁矿石中全硫的不确定度  

Top-Down Method Evaluation of Uncertainty of Total Sulfur in Iron Ore by High Frequency Combustion Infrared Absorption Method

作　　者：宋飞 丁仕兵 管嵩 刘静洁 冯丽丽 吴雅俊 李菲 SONG Fei;DING Shibing;GUAN Song;LIU Jingjie;FENG Lili;WU Yajun;LI Fei(Qingdao Customs Technology Center,Qingdao Shandong 266500,China)

机构地区：[1]青岛海关技术中心,山东青岛266500

出　　处：《江西化工》2025年第2期51-56,共6页Jiangxi Chemical Industry

摘　　要：利用4个不同硫含量的铁矿标样监控检测过程,通过监测值计算期间精密度和偏倚。经回归分析,期间精密度和偏倚均与硫含量的对数呈线性关系。t检验显示,各监控标样的偏倚均不显著,表明样品检测结果无需校正。对监测值进行标准化处理后的I进行正态性和独立性检验,统计量A_(S)^(2*)和A_(MR)^(2*)均小于1.0,接受检测结果正态性和独立性的假定。各I值均在上下行动限UCL和LCL之间,I的移动极差不大于上行动限UCL_(MR),t检验显示I平均值与假定值0没有显著性差异,表明测量系统一直处于可控状态。从期间精密度和偏倚两方面出发整体上评定测量不确定度,使不确定度最大限度地涵盖人员、仪器、样品、方法、环境等因素,具备简便性和操作性强等特点。本文对3个铁矿样品进行实测并评定了不确定度,1#样品全硫含量0.023%、扩展不确定度0.004%(测量1次),2#样品全硫含量0.141%、扩展不确定度0.007%(测量2次),3#样品全硫含量0.335%、扩展不确定度0.010%(测量2次)。Abstract:4 Iron ore reference samples with different sulfur content were used to monitor the whole test progress.Intermediate precision S_(R′)and bias b were calculated by monitor results.After regression,it was found that S_(R′)and b were all linear correlated to the logarithmic of sulfur content.It was showed that the biases of CRMs were nonsignificant by t-test,so no correction to the results of samples.A series of I were obtained through normality processed monitor results,statistics A_(S)^(2*)and A_(MR)^(2*)were less than 1.0,the pretending of normality and independence of test results was accepted.Every I was distributed between UCL and LCL,moving range of I was not greater than up limit UCLMR.t-test showed that average I was no significant difference with 0,measurement system was always under control.Uncertainty was evaluated from intermediate precision and bias,all the effects of personnel,equipment,sample,method and environment in the test progress were covered,simple and easy to operate.In this article,uncertainties of 3 samples’sulfur content were evaluated,S=0.023%and U=0.004%of 1#sample(test 1 time),S=0.141%and U=0.007%of 2#sample(test 2 times),S=0.335%and U=0.010%of 3#sample(test 2 times).

关 键 词：Top-Down法 铁矿石 全硫 不确定度 

分 类 号：O657.3[理学—分析化学] TF701.3[理学—化学]