首页|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

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

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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HJ 799-2016和HJ 800-2016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。50 mg/L~50。0 mg/L、NO3-在0。50 mg/L~50。0 mg/L、SO42-在0。50 mg/L~50。0 mg/L内线性关系良好,r均为0。999 9;NH4+在0。50 mg/L~10。0 mg/L 内拟合曲线为y=0。064 4+0。222 0x-0。005 8x2,r=0。999 4。各组分检出限在 0。003 μg/m3~0。016μgm3,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。
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
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 0.10 mg/L-5.0 mg/L,Cl-with-in 0.50 mg/L-50.0 mg/L,NO3-within 0.50 mg/L-50.0 mg/L,and SO42-within 0.50 mg/L-50.0 mg/L.All r values were 0.999 9;the fitted curve was y=0.064 4+0.222 0x-0.005 8x2(r=0.999 4)when NH4+was within 0.50 mg/L-10.0 mg/L.The detection limits of each component were within 0.003 μg/m3-0.016 μg/m3,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.

Ion chromatographyPM2.5Water-soluble ionsMethod validation

曹静、宋伟、于浩、郗德凤

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德州市疾病预防控制中心,山东 253016

泰安市疾病预防控制中心

离子色谱法 PM2.5 水溶性离子 方法验证

2023

中国卫生检验杂志
中华预防医学会

中国卫生检验杂志

影响因子:0.771
ISSN:1004-8685
年,卷(期):2023.33(23)
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