论文部分内容阅读
目的通过对气相色谱法检测大米中溴氰菊酯残留量的测量不确定度来源的系统分析,提高对大米中溴氰菊酯残留量的检测水平和能力,并找出影响测量结果不确定度的主要因素。方法按照JJF 1059.1-2012(GUM)《测量不确定度评定和表示》和《CNAS-CL05:2011》的要求,找出分析不确定度的来源,建立测量模型,计算各不确定度分量,对其进行评定。结果大米中溴氰菊酯农药残留量的测量不确定度由标准曲线拟合、样品前处理后的回收率、标准溶液的逐级稀释、样品结果的重复性、样品称量、标准物质等引入的不确定度各组分合成。测量结果的扩展不确定度按公式U=k×u(合)计算。测定结果报告C=CX±U,以加入溴氰菊酯的标准物质的0.30 mg/kg的大米做气相色谱法检测残留量,报告为(0.30±0.062 2)mg/kg。结论从气相色谱法检测大米中溴氰菊酯残留量的测量不确定度分量汇总分析可以看出,影响不确定度的因素有很多,而样品的前处理及标准曲线拟合是最为关键的因素。
OBJECTIVE To improve the detection level and ability of deltamethrin residues in rice through the systematic analysis of the sources of uncertainty in measurement of deltamethrin residues in rice by gas chromatography and to find out the factors influencing the uncertainty of measurement results The main factor. Methods According to the requirements of JJF 1059.1-2012 (GUM) “Measurement Uncertainty Evaluation and Representation” and “CNAS-CL05: 2011”, the sources of the analysis uncertainty are found, the measurement model is established, and the components of each uncertainty are calculated. Its assessment. Results The uncertainty of the measurement of deltamethrin pesticide residues in rice was determined by standard curve fitting, recovery after sample preparation, gradual dilution of standard solution, repeatability of sample results, sample weight and reference materials The uncertainty of each component synthesis. Uncertainty of the expansion of the measurement results according to the formula U = k × u (together) calculation. Determination of the results reported in C = CX ± U, with deltamethrin standard substance of 0.30 mg / kg of rice do gas chromatography detection residue, reported as (0.30 ± 0.062 2) mg / kg. Conclusions From the summary analysis of the measurement uncertainty component of deltamethrin residue in rice by gas chromatography, it can be seen that there are many factors affecting the uncertainty, and the sample pre-treatment and standard curve fitting are the most crucial factors .