作者：郑力文, 董了瑜, 邓凡锋, 袁娇阳

作者单位：四川中测标物科技有限公司, 四川 成都 610021

关键词：气相质谱仪;气体标准物质;注射称量法;不确定度

摘要：

介绍0.1 mol/mol气相质谱仪校准用氮气中4组分混合气体标准物质的研制方法。标准气体的组分为溴氯甲烷、1，4-二氟苯、氯苯-D5和4-溴氟苯，所采用的制备及分析方法分别为注射称量法和GC-MS法。通过瓶内压力及各组分浓度随时间的变化考察其浓度的均匀性和稳定性。对标准气体的制备过程及均匀性和稳定性引入的不确定度进行评定。实验结果表明，4组分混合气体标准物质在0.5~10 MPa范围内具有较好的压力均匀性和稳定性，其相对扩展不确定度为5.0%（k=2），使用有效期为1年。

The development of gas chromatography-mass spectrometry calibration for 4 components in nitrogen mixture gas reference material

ZHENG Liwen, DONG Liaoyu, DENG Fanfeng, YUAN Jiaoyang

Sichuan Zhongce Biaowu Technology Co., Ltd., Chengdu 610021, China

Abstract: The development method of gas chromatography-mass spectrometry calibration of 4 components that containing bromochloromethane, 1,4-difluorobenzene, chlorobenzene-D5 and 4-bromofluorobenzene at 0.1 μmol/mol in nitrogen gas reference material is described．The gas standard is prepared by gravimetric preparation method and is intercompared to the existing gas cylinder standard using gas chromatography with a mass spectrometry detector. Relationships between time or pressure and homogeneity or stability were also investigated. The paper also evaluated the uncertainties from preparation using gravimetric method, uniformity and stability. All the research results indicated that have been better homogeneity and stability between 0.5 MPa and 10 MPa and an estimated relative expanded uncertainty of 5% (k=2) with one year shelf life have been achieved.

Keywords: gas chromatography-mass spectrometry;gas reference material;gravimetric method;uncertainty

2018, 44(11): 110-115  收稿日期: 2018-09-05;收到修改稿日期: 2018-10-10

基金项目: 四川省科技服务业示范项目（2017GFW0713）

作者简介: 郑力文(1987-),男,四川遂宁市人,助理研究员,硕士,主要从事标准物质制备方法及分析方法研究

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