凝胶渗透色谱-液相色谱法测定沉积物中多环芳烃的不确定度评定

目的 对凝胶渗透色谱-液相色谱法测定沉积物中多环芳烃不确定度进行评定。分析不确定度来源,计算各不确定分量,以控制测定结果准确度。 方法 依据JJF 1059.1-2012 《测量不确定度评定与表示》和CNAS-GL06-2006 《化学分析中不确定度的评估指南》中有关规定,从标准溶液配制,样品前处理,仪器测定重复性等方面对测定结果的不确定来源进行评定。 结果 评定结果显示标准曲线,仪器测定的重复性和样品前处理是不确定度的主要来源。 结论 建立的凝胶渗透色谱-液相色谱法准确可靠,能应用于沉积物中多环芳烃的测定;优化仪器条件,规范实验操作提高回收率能减小方法不确定度。

Evaluation of uncertainty for determination of polycyclic aromatic hydrocarbons in sediment by gel permeation chromatography-high performance liquid chromatography

Objective To evaluate the uncertainty of measurement for the determination of polycyclic aromatic hydrocarbons (PAHs) in sediment by gel permeation chromatography (GPC)-high performance liquid chromatography (HPLC). To analyze the resources of the uncertainty in the determination process and to calculate each component of the uncertainty so as to control the accuracy of the determination results. Methods According to the relevant regulations given in JJF 1059.1-2012 Evaluation and Expression of Uncertainty in Measurement and CNAS-GL06-2006 Guidance on Evaluating the Uncertainty in Chemical Analysis, the measurement uncertainty items, including standard solution preparation, sample pretreatment and measurement repeatability were assessed. Results The results showed that the major factors of the uncertainty in the determination of PAHs in sediment by GPC-HPLC were standard curve, measurement repeatability and sample pretreatment. Conclusions The established method is accurate and reliable, which can be applied to detecting PAHs in sediment. Meanwhile, the values of the measurement uncertainty can be reduced by means of optimizing the instrument condition and standardizing the experimental operation.