氯菊酯纯度标准物质的定值及不确定度评定

Certification and uncertainty evaluation of permethrin reference material certified for purity

研制了氯菊酯纯度标准物质。采用红外光谱、质谱和熔点法对氯菊酯进行定性鉴定。深入研究并优化了高效液相色谱-二极管阵列检测器(HPLC-DAD)与气相色谱-氢火焰离子化检测器(GC-FID)对氯菊酯主成分的定值方法。采用卡尔费休法、电感耦合等离子体质谱法、灼烧法等方法进行无机杂质的分析。均匀性和稳定性结果表明,研制的氯菊酯纯度标准物质均匀性良好,稳定时间至少20个月,纯度值为99.5%,扩展不确定度为0.4%(k=2)。

Permethrin is prepared and certified as pure refer- ence material. IR spectrum,MS and melting point method are used to qualitative identify the structure of the permethrin. The methods of high performanee liquid chromatography-diode array detector （HPLC-DAD） and gas chromatography-hydro- gen flame ionization detector （GC-FID） are used to measure the eomponent. With Karl Fischer method,inductively coupled plasma mass spectrometry and burning methods, inorganic im- purities are analyzed. Permethrin has good homogeneity and stability which can maintain at least 20 months. The purity of permethrin is （99.5±0. 4）% and the expanded uncertainly is 0.4% （k =2）.