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《化学分析计量》 2017年第04期
DOI:10.3969/j.issn.1008-6145.2017.04.002
氮中丙烯腈气体标准物质的研制
许思思1,郑鹏1,李锋丽1,郭波1,张冬霞2,高捷1,周宁宁1
1. 山东省计量科学研究院; 2. 济南德洋特种气体有限公司 
Preparation of Reference Material of Acrylonitrile in Nitrogen
Xu Sisi1,Zheng Peng1,Li Fengli1,Guo Bo1,Zhang Dongxia2,Gao Jie1,Zhou Ningning1
1. Shandong Institute of Metrology, Jinan 250014, China; 2. Jinan Deyang Special Gas Co., Ltd., Jinan 250100, China 
摘要:
以高纯丙烯腈和高纯氮气为原料,采用称量法配制氮中丙烯腈气体标准物质。对配制的气体标准物质 分别进行机械混匀试验、压力均匀性和时间稳定性试验。经F 检验,2.00 μmol/mol 及5.00 μmol/mol 两种浓度 的样品在0.5~10 MPa 范围内标准值无显著变化,具有较好的压力均匀性;在-20℃和40℃条件下保存7 d,其量值 无显著变化,可满足运输环节量值稳定;在常温下贮存9 个月量值无显著变化,表明其稳定性良好,满足国家二级标 准物质对有效期的要求。对定值结果的不确定度进行评定。配制的氮中丙烯腈气体标准物质标准值为(2~5)×10-6 mol/mol,相对扩展不确定度为9%(k=2)。该标准物质达到国家二级标准物质的相关技术要求,可用于对丙烯腈 气体报警器的校准。
 
Abstract:The reference material of acrylonitrile in nitrogen was prepared by gravimetric method with high purity acrylonitrile and nitrogen as raw material. The mechanical homogeneity test, pressure uniformity and stability test were carried out by using gas chromatography. The F test results showed that the reference value of 2.00 μmol/mol and 5.00 μmol/mol samples exhibited good uniformity with the change of the pressure from 0.5 MPa to 10 MPa, and that exhibited good stability after being stored for 9 months at room temperature and after being stored for 7 days at -20℃and 40℃, respectively. It could satisfy the requirements of transport and long-term stability of two grade reference material. The uncertainty of certified value was evaluated. The standard value of the reference material of acrylonitrile in nitrogen was (2-5)×10-6 mol/mol with the relative expanded uncertainty of 9%(k=2). The reference material meets the technical requirements of the national reference material, and can be used for the calibration of the acrylonitrile gas alarm. 
关键词:丙烯腈;制备;气体标准物质 
Keywords:acrylonitrile; preparation; gas reference material 
本文引用格式:
许思思,郑鹏,李锋丽,等.氮中丙烯腈气体标准物质的研制[J].化学分析计量,2017,26(4):9-12.
XU S S,ZHENG P,LI F L,et al.Preparation of Reference Material of Acrylonitrile in Nitrogen[J]. Chemical analysis and meterage,2017,26(4):9-12. 

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