气相色谱-质谱联用仪校准质量准确性用异辛烷中硬脂酸甲酯溶液标准物质研制及不确定度评定  

Preparation of standard material of methyl stearate in isooctane used for quality accuracy calibration of GC-MS and uncertainty evaluation

作　　者：刘淑华 王冰玥 王骏 吴红 赵海波 Liu Shuhua;Wang Bingyue;Wang Jun;Wu Hong;Zhao Haibo(Beijing Institute of Metrology,Beijing 100029,China)

机构地区：[1]北京市计量检测科学研究院,北京100029

出　　处：《化学分析计量》2021年第7期1-7,共7页Chemical Analysis And Meterage

基　　金：国家质量基础专项支持(2019YFF0216700);北京市计量检测科学研究院自主项目(KJ 2019-22)。

摘　　要：制备了气相色谱-质谱联用仪校准质量准确性用异辛烷中硬脂酸甲酯溶液标准物质,并进行了不确定度评定。采用气相色谱-质谱联用仪和傅立叶红外光谱仪对硬脂酸甲酯纯品进行定性分析,采用质量平衡法对原料硬脂酸甲酯进行纯度核验,采用气相色谱(配FID检测器)峰面积归一法测定主成分含量,采用卡尔·费休水分仪测定原料中所含水分,采用电感耦合等离子体质谱法测定无机元素的含量,采用GC-FID-顶空进样法分析微量挥发性溶剂残留。采用重量-容量法制备质量浓度为10.0 ng/μL的气相色谱-质谱联用仪校准质量准确性用的异辛烷中硬脂酸甲酯溶液标准物质,对其进行均匀性和稳定性检验。结果表明其均匀性和稳定性均良好,定值相对扩展不确定度U_(rel)=3%(k=2),有效期为12个月。Standard material for methyl stearate in isooctane used for the quality accuracy calibration of gas chromatography-mass spectrometry(GC-MS)was developed,and the uncertainty was evaluated accordingly.The acquired methyl stearate was well characterized by GC-MS and Fourier transform infrared spectrometer(FTIR).The purity of methyl stearate was calculated by mass balance method with principle component content quantitatively analyzed by GC-FID with area normalization method,water content was determined by Karl Fischer moisture titrator,inorganic impurity was analyzed by inductively coupled plasma mass spectrometry(ICP-MS),and trace solvent residue was determined by headspace GC-FID.Standard material for methyl stearate in isooctane was prepared by gravity-volume approach,which was then thoroughly evaluated in the aspects of homogeneity and stability.The results confirmed that standard material of methyl stearate in isooctane with certified value of 10.0 ng/μL was fairly homogeneous and stable,and the relative expanded uncertainty was 3.0%(k=2)with 12 month validity.

关 键 词：硬脂酸甲酯 标准物质 气相色谱-质谱联用仪 不确定度评定 

分 类 号：O657[理学—分析化学]