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顶空-气相色谱法测定烟用接装纸中乙酸丁酯的不确定度

Uncertainty in Determination of Butyl Acetate in Tipping Paper by Headspace Gas Chromatography

  • 摘要: 为提高测量结果的准确性,依据JJF 1059.1-2012《测量不确定度评定与表示》,建立相关数学模型,分析了顶空-气相色谱法测定接装纸中乙酸丁酯含量的不确定度,并计算了影响测量的各个不确定度分量。结果表明:①影响测量不确定度的因素有试样制备、标准工作溶液制备、重复性考察、标准工作曲线拟合等,其中拟合标准工作曲线所引入的不确定度最大;②当接装纸样品中乙酸丁酯残留量为0.54 mg/m2时,其合成不确定度为0.024 mg/m2,扩展不确定度为0.05 mg/m2(P=95%,k=2)。通过改变标准工作曲线逐级稀释制备方法和减小标准工作溶液浓度范围可进一步提高分析的精准度。

     

    Abstract: In order to improve the accuracy of measurement results, the uncertainty in determination of butyl acetate in tipping paper by headspace gas chromatography (HS-GC) was analyzed on the basis of JJF 1059.1-2012 "Evaluation and Expression of Uncertainty in Measurement", and the uncertainty of individual component affecting measurement was calculated. The results showed that: 1) The factors influencing measurement uncertainty included sample preparation, standard solution preparation, repeatability examination, calibration curve fitting, etc., particularly the calibration curve fitting. 2) When the residue of butyl acetate in tipping paper sample was 0.54 mg/m2, the combined uncertainty and the expanded uncertainty of measurement results were 0.024 and 0.05 mg/m2 (P=95%, k=2), respectively. Therefore, the analysis accuracy could be improved by means of abandoning stepwise dilution method during the solution preparation of standard working curve or reducing the concentration range of standard working solution.

     

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