顶空气相色谱法测定生活饮用水中三卤甲烷的不确定度评定

    Uncertainty evaluation for determination of trihalomethanes in drinking water using headspace gas chromatography

    • 摘要:
      目的 对顶空毛细管柱气相色谱法测定生活饮用水中三卤甲烷(trihalomethanes, THMs),包括三氯甲烷(chloroform, TCM)、二氯一溴甲烷(bromodichloromethane, BDCM)、一氯二溴甲烷(dibromochloromethane, DBCM)、三溴甲烷(tribromomethane, TBM)的不确定度进行评定,以评估检测结果的质量。
      方法 利用全自动顶空进样器进样,采用电子捕获检测器,测定水中三卤甲烷含量,通过建立测量模型,量化求出各分量不确定度,最后评定顶空毛细管柱气相色谱法测定生活饮用水中三卤甲烷的不确定度。
      结果 TCM、BDCM、DBCM和TBM测定按不确定度来源分别为:标准曲线拟合引入的相对标准不确定度分别为0.067、0.051、0.051和0.056;样品重复性测量引入的相对标准不确定度分别为0.012、0.012、0.009和0.010;样品取样过程引入的相对标准不确定度均为9.6×10-4;标准物质引入的相对标准不确定度均为0.015;标准曲线配制过程引入的相对标准不确定度均为0.006。顶空气相色谱法测定TCM、BDCM、DBCM和TBM的含量分别为(1.44±0.20)、(2.50±0.27)、(2.61±0.28)和(2.69±0.32)μg/L。
      结论 顶空毛细管柱气相色谱法测定生活饮用水THMs不确定度的主要来源是标准曲线拟合残差。实验操作时应注意规范操作,提高标准曲线的检测次数,降低曲线拟合不确定度。

       

      Abstract:
      Objective To evaluate the uncertainty in the determination of trihalomethanes (THMs) including chloroform (TCM), bromodichloromethane (BDCM), dibromochloromethane (DBCM), and tribromomethane (TBM) in drinking water using headspace capillary gas chromatography (HS-GC) to assess the quality of measurements.
      Methods An automated headspace sampler was used for sample injection, and an electron capture detector (ECD) was employed to measure THMs levels in water. A measurement model was established to quantify the uncertainty of components, ultimately assessing the uncertainty of HS-GC in determining THMs in drinking water.
      Results According to the sources of uncertainty, relative standard uncertainties (RSUs) from standard curve fitting of TCM, BDCM, DBCM and TBM were 0.067, 0.051, 0.051, and 0.056, respectively; RSUs from repeated sample measurements of TCM, BDCM, DBCM and TBM were 0.012, 0.012, 0.009, and 0.010, respectively; RSUs from sampling, reference standards and standard curve preparation of THMs were all 9.6×10-4, 0.015, and 0.006, respectively. The contents of TCM, BDCM, DBCM and TBM determined by HS-GC were (1.44±0.20), (2.50±0.27), (2.61±0.28) and (2.69±0.32)μg/L, respectively.
      Conclusion The primary source of uncertainty in the determination of THMs in drinking water HS-GC is the residual error from standard curve fitting. Standardized operations should be strictly followed, and the number of calibration curve measurements should be increased to reduce uncertainty in curve fitting.

       

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