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以空气PM2.5中5种水溶性离子的方法验证为例浅谈实验室新方法的开展

A study on the development of new laboratory methods-taking the experimental verification of 5 kinds of water-soluble ions in PM2.5 as an example
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摘要 目的为满足实验室不断开展新项目,应用新方法的需要,以测定环境空气颗粒物PM2.5中5种水溶性离子项目开展为例,通过对HJ799—2016和HJ800—2016进行方法验证,探讨实验室开展新项目的具体试验流程。方法采集环境空气颗粒物PM2.5的石英滤膜(空白滤膜及自制加标滤膜),按照标准方法要求经高温处理、恒温恒湿处理、称重、粉碎、超纯水超声提取、离心过滤等一系列实验操作,用离子色谱法测定5种水溶性离子含量。结果F^(-)在0.10 mg/L~5.0 mg/L、Cl在0.50mg/L~50.0mg/L、NO;在0.50 mg/L~50.0 mg/L、S02~在0.50 mg/L~50.0 mg/L内线性关系良好,r均为0.9999;NH4在0.50mg/L~10.0mg/L内拟合曲线为y=0.0644+0.2220x-0.0058x^(2),r=0.9994。各组分检出限在0.003μg/m^(3)~0.016μg/m^(3),加标回收率为89.0%~106.0%,RSD为0.05%~1.66%(n=6)。结论通过对标准方法的线性关系、空白实验、检出限、定量线、准确度、精密度等参数的测定,可以验证实验室是否具备开展该项新实验的能力,以及该标准实验方法在现有试验条件下是否能满足具体工作开展要求。 Objective In order to meet the requirements of the laboratory to carry out new projects and apply new methods,taking the project of measuring five water-soluble ions in ambient air particulate matter PM2.5 as an example,the specific experimental process for the laboratory to carry out new projects was explored through the experimental verification of HJ 799-2016 and HJ 800-2016.Methods The quartz filter membranes(including blank filter membranes and self-made standard added filter membranes)were subjected to a series of experimental procedures,such as high-temperature treatment,constant temperature and humidity treatment,weighing,crushing,ultrapure water ultrasonic extraction,centrifugal filtration,etc.,in accordance with the requirements of the standardized method.Subsequently,the content of five water-soluble ions was deter-mined using ion chromatography.Results Good linearity was obtained when F^(-)was within O0.10 mg/L-5.0 mg/L,Cl~with-in 0.50 mg/L-50.0 mg/L,NO;within 0.50 mg/L-50.0 mg/L,and S02-within 0.50 mg/L-50.0 mg/L.All r values were 0.9999;the fied curve was y=0.0644+0.2220x-0.0058x^(2)(r=0.9994)when NH_(4)^(+)was within 0.50 mg/L-10.0 mg/L.The detection limits of each component were within 0.003μg/m^(3)-0.016μg/m^(3),the recoveries were within 89.0%-106.0%,and RSD was within 0.05%-1.66%(n=6).Conclusion The measurement of linear relationship,blank experiment,detection limit,quantitative line,accuracy,precision and other parameters of the standard method can verify whether the laboratory has the ability to carry out the new experiment,and whether the standard experimental method can meet the requirements of specific work under the existing experimental conditions.
作者 曹静 宋伟 于浩 郗德凤 CAO Jing;SONG Wei;YU Hao;CHI De-feng(Dezhou Municipal Center for Disease Control and Prevention,Shandong 253016,China;不详)
出处 《中国卫生检验杂志》 CAS 2023年第23期2833-2836,共4页 Chinese Journal of Health Laboratory Technology
关键词 离子色谱法 PM2.5 水溶性离子 方法验证 Ion chromatography PM2.5 Water-soluble ions Method validation
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