活性炭管中三氯乙烯标准物质的研制

    Research and preparation of reference materials of trichloroethylene in activated charcoal tubes

    • 摘要:
      目的 研制活性炭管中三氯乙烯标准物质。
      方法 采用动态配气, 用活性炭管吸附气体, 制备两个水平(70和140 μg)的三氯乙烯标准物质, 采用气相色谱-氢火焰离子化检测器法对其进行均匀性和稳定性检验, 联合7家实验室对其进行定值并进行不确定度评定。
      结果 两个水平样品测定结果的相对标准偏差分别为1.6%和1.1%, 均 < 3%, 说明样品均匀性良好; 长期和短期稳定性结果均显示线性回归方程斜率|β1| < t0.95, 3 × s (β1), 说明常温条件(10~35 ℃)储存, 样品可稳定保存12个月, 在≤50 ℃条件下运输, 样品在7 d内稳定; 标准物质的标准量值及扩展不确定度分别为(70.1±4.6)和(140.2±9.0)μg(k=2)。
      结论 研制的标准物质均匀性、稳定性、量值及不确定度等各项指标均符合国家标准物质研制技术要求, 可用于三氯乙烯检测的质量控制。

       

      Abstract:
      Objective To develop and prepare reference materials of trichloroethylene in activated charcoal tubes.
      Methods Two levels of reference materials of trichloroethylene (70 and 140 μg) were prepared by dynamic gas distribution and adsorption with activated charcoal tubes. The homogeneity and stability of the samples were tested by the gas chromatography-hydrogen flame ionization detector method. Certification was carried out by seven independent laboratories, and the uncertainty of the reference materials was evaluated.
      Results The relative standard deviations of the results for the two-level samples were 1.6% and 1.1%, respectively, both less than 3%, indicating the homogeneity of the two-level samples was good.Both the long-term and short-term stability results showed that the slope of the linear regression equation |β1| < t0.95, 3× s (β1), indicating that the samples were stable for 12 months at room temperature (10 ℃ to 35 ℃) and stable for 7 days at ≤50 ℃. The certified value and expanded uncertainty of reference materials were (70.1±4.6) and (140.2±9.0) μg, respectively (k=2).
      Conclusion The homogeneity, stability, certified values, and uncertainty of the prepared reference materials met the technical requirements for preparation of reference materials of China, indicating that the materials can be used for quality control in trichloroethylene detection.

       

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