气质校准用三组份混合溶液标准物质研制  

Development of a Certified Reference Material of Three-Component Mixed Solution for GC-MS Calibration

作　　者：李志丰 王晓冰 郭硕 宋增良 LI Zhifeng;WANG Xiaobing;GUO Shuo;SONG Zengliang(Institute of Metrology of Hebei Province,Shijiazhuang 050227,China)

机构地区：[1]河北省计量监督检测研究院,石家庄050227

出　　处：《计量科学与技术》2023年第7期68-73,44,共7页Metrology Science and Technology

摘　　要：为解决气相色谱-质谱联用仪(GC-MS)溯源问题,需用到标准物质。采用重量-容量法,对气质校准用的三组份混合溶液(异辛烷中八氟萘、二苯甲酮和硬脂酸甲酯三种物质)标准物质进行制备。制备的标准物质用气相色谱-氢火焰离子化检测器(GC-FID)进行分析。采用F检验和回归曲线法分别对均匀性和稳定性进行评估,并对最终结果进行不确定度评定。该混合标准物质中八氟萘、二苯甲酮和硬脂酸甲酯的定值结果均为3.00 ng/μL,相对扩展不确定度Urel=3%,k=2。经原料分析、标准物质制备、均匀性和稳定性分析、量值比较等试验,该标准物质符合国家二级标准物质的研制要求,目前已获批国家二级标准物质证书,证书编号为GBW(E)130677。作为量值传递的标准,本标准物质可用于气相色谱-质谱联用仪校准保留时间的重复性测试。To address the traceability issue in gas chromatography-mass spectrometry(GC-MS),standard substances are necessitated.A three-component mixed solution,comprising octafluoronaphthalene,benzophenone,and methyl stearate dissolved in isooctane,was meticulously prepared using the gravimetric method for the purpose of gas quality calibration.Analysis was carried out utilizing a gas chromatography equipped with a hydrogen flame ionization detector(GC-FID).Rigorous evaluation was conducted by employing F-tests and regression analysis to assess the homogeneity and stability of the prepared standard substances,as well as the associated uncertainty in the obtained results.Each component in the mixed standard substance yielded calibration values of 3.00 ng/μL with a relative expanded uncertainty Urel of 3%,at a coverage factor(k)of 2.Comprehensive experimentation involving raw material analysis,preparation of standard materials,assessment of uniformity and stability,and comparison of quantitative values confirmed that the developed standard material fulfills the criteria for national secondary standard substances.Consequently,it has been officially accredited with a certificate number GBW(E)130677,enabling its utilization in the calibration of GC-MS instruments,specifically for the repeatability testing of retention times.

关 键 词：计量学 八氟萘 二苯甲酮 硬脂酸甲酯 有证标准物质 不确定度 

分 类 号：TB99[一般工业技术—计量学]