摘要
建立了硬质硬脂酸甲酯纯度定值分析方法,以高纯质硬脂酸甲酯为原料,研制得到10mg/L的异辛烷溶液标准物质。分别采用气相色谱(GC)法和高效液相色谱(HPLC)法对硬脂酸甲酯原料进行纯度分析,测定了原料中所含水分、杂质的含量,利用质量平衡法计算得到硬脂酸甲酯原料的纯度为99.2%,扩展不确定度为0.7%(κ=2)。异辛烷中硬脂酸甲酯溶液标准物质采用重量–容量法配制,并通过了均匀性和稳定性考察,经量值核验及不确定度评定,最终该溶液标准物质的量值为10.0mg/L,相对扩展不确定度为3%(κ=2)。该溶液标准物质已经批准为国家标准物质,编号为GBW(E)130528,可用于气相色谱–质谱联用仪(GC–MS)的质量准确性校准和硬脂酸甲酯日常分析和检测。
A method for purity determination of methyl stearate was established. The certified value of certified reference material (CRM) of methyl stearate in isooctane was 10.0 mg/L. The purity of methyl stearate was quantitative analysis by gas chromatography (GC) and high performance liquid chromatography (HPLC). The water content and impurity content in raw materials were determined at the same time. The purity of methyl stearate was 99.2% calculated by mass balance method, and the relative expanded uncertainty was 0.7%(κ=2). The certified reference material (CRM) of methyl stearate solution in isooctane was prepared by gravity–volume method. The homogeneity and stability of the standard solution were investigated. The uncertainty of the standard solution was evaluated after verification. The certified value was 10.0 mg/L, and the relative expanded uncertainty was 3.0%(κ=2). The standard solution has been approved as a national certified reference material (CRM) with No.GBW(E) 130528,which can be used for the quality accuracy calibration of gas chromatography–mass spectrometry (GC–MS),as well the daily analysis and detection of methyl stearate.
作者
花秀兵
陈玲
黄彦捷
周瑾艳
王世超
许俊斌
HUA Xiubing;CHEN Ling;HUANG Yanjie;ZHOU Jinyan;WANG Shichao;XU Junbin(Guangdong Provincial Key Laboratory of Modem Geometric and Mechanical Metrology Technology, Guangdong Provincial Institute of Metrology,Guangzhou 510405 China)
出处
《化学分析计量》
CAS
2019年第A01期6-10,共5页
Chemical Analysis And Meterage
基金
广东省科技厅项目计划(2017A040405034,2018B02020707)
广东省质量技术监督管理局科技项目(2018ZJ02,2016PJ15)
