欢迎访问沈阳真空杂志社 Email Alert    RSS服务

真空 ›› 2022, Vol. 59 ›› Issue (4): 12-17.doi: 10.13385/j.cnki.vacuum.2022.04.03

• 测量与控制 • 上一篇    下一篇

质谱仪定量分析微量气体D2的校准因子研究*

李海洋1,2, 张占文1, 刘梅芳1, 栾旭1, 史瑞廷1, 易勇1   

  1. 1. 中国工程物理研究院 激光聚变研究中心,四川 绵阳 621900;
    2. 西南科技大学材料科学与工程学院,四川 绵阳 621000
  • 收稿日期:2021-07-04 出版日期:2022-07-25 发布日期:2022-08-09
  • 通讯作者: 张占文,研究员,博士。
  • 作者简介:李海洋(1995-),男,四川省德阳市人,硕士。
  • 基金资助:
    *环境友好能源材料国家重点实验室自主课题资助(20fksy04); 四川省重点研发计划项目(2019YFG0432)

Study on the Calibration Factor in Quantitative Analysis of Trace Gases D2 by Mass Spectrometer

LI Hai-yang1,2, ZHANG Zhan-wen1, LIU Mei-fang1, LUAN Xu1, SHI Rui-ting1, YI Yong1   

  1. 1. Laser Fusion Research Center, CAEP, Mianyang 621900, China;
    2. School of Materials Science and Engineering, Southwest University of Science and Technology, Mianyang 621000, China
  • Received:2021-07-04 Online:2022-07-25 Published:2022-08-09

摘要: 通过在质谱仪进气管路上安装的标定腔室与真空管路,实现了对与微球内气体含量相同范围的微量气体的获取。对质谱仪定量分析微量气体时的精密度及被测量氘气的压力对D2校准因子的影响进行了研究。结果表明:该四极质谱仪的精密度较高,不同压力下10次重复测量实验数据的相对标准偏差均小于0.004;校准后的一个月内质谱仪具有较高稳定性,其定量分析误差低于1%,准确度较高;D2和Ar的浓度校准因子在一年内的变化不超过3%,而D2的压力校准因子在一年内的变化超过8%;D2的压力校准因子η与被测量氘气的压力P1成反比,且η与logP1存在较好的线性关系,这种线性关系在半年内具有较高的稳定性。

关键词: 四极质谱, 校准因子, 定量分析, 微球, 微量气体

Abstract: Through the calibration chamber and vacuum tube installed on the intake pipe of the mass spectrometer, the trace gas with the same content range as the gas in microsphere can be obtained. The precision of quantitative analysis of trace gases by mass spectrometer and the effect of measured deuterium pressure on the calibration factor of D2 were studied. The results show that the precision of the quadrupole mass spectrometer is high, and the relative standard deviation of the 10 repeated measurements under different pressures is less than 0.004. The mass spectrometer has a high stability within one month after calibration, and it has a high accuracy with the quantitative analysis error is less than 1%. The concentration calibration factors for D2 and Ar varied no more than 3% within one year, while the pressure calibration factors for D2 varied more than 8% within one year. The pressure calibration factor η of D2 is inversely proportional to the pressure P1 of the measured deuterium gas, and there is a good linear relationship between η and logP1, which has a high stability in half a year.

Key words: Science and Engineering, Southwest University of Science and Technology, Mianyang 621000, China

中图分类号: 

  • O6-33
[1] 陈鹏玮, 厉彦忠, 丁岚, 等. 低温冷冻靶微管燃料充注流动冷凝特性[J]. 强激光与粒子束, 2017, 29(12): 17-27.
[2] SCHMITT M L, SHELBY J E, HALL M M.Preparation of hollow glass microspheres from sol-gel derived glass for application in hydrogen gas storage[J]. Journal of Non Crystalline Solids, 2006, 352(6/7): 626-631.
[3] HOPPE M L, STEINMAN D A.New developments in glass shells from SiGDP-residual gases, gas filling and tailored half-lives[J]. Fusion Science and Technology, 2007, 51(4): 606-610.
[4] LEE B H, LOPEZ-HI, FIKER F D, et al.An iodide-adduct high-resolution time-of-flight chemical-ionization mass spectrometer: application to atmospheric inorganic and organic compounds[J]. Environmental Science & Technology, 2014, 48(11): 6309-6317.
[5] DIAZ J A, PIERI D, WRIGHT K, et al.Unmanned aerial mass spectrometer systems for in-situ volcanic plume analysis[J]. Journal of the American Society for Mass Spectrometry, 2015, 26(2): 292-304.
[6] FRANZ H B, TRAINER M G, MALESPIN C A, et al.Initial SAM calibration gas experiments on Mars: quadrupole mass spectrometer results and implications[J]. Planetary and Space Science, 2017, 138: 44-54.
[7] TEOLIS B D, NIEMANN H, WAITE J, et al.A revised sensitivity model for Cassini INMS: results at Titan[J]. Space Science Reviews, 2015, 190(1): 47-84.
[8] TURNER P, TAYLOR S, CLARKE E, et al.Calibration effects during natural gas analysis using a quadrupole mass spectrometer[J]. TrAC Trends in Analytical Chemistry, 2004, 23(4): 281-287.
[9] BASFORD J A, BOECKMANN M D, ELLEFSON R E, et al.Recommended practice for the calibration of mass spectrometers for partial pressure analysis[J]. Journal of Vacuum Science & Technology A, 1993, 11(1): A22-A40.
[10] BLESSING J E, ELLEFSON R E, RABY B A, et al.Recommended practice for process sampling for partial pressure analysis[J]. Journal of Vacuum Science 8t Technology A, 2007, 25(1): 167-186.
[11] ELLEFSON R E.Methods for in situ QMS calibration for partial pressure and composition analysis[J]. Vacuum, 2014, 101: 423-432.
[12] GRANEY J R, KESLER S E.Factors affecting gas analysis of inclusion fluid by quadrupole mass spectrometry[J]. Geochim Cosmochim Acta, 1995, 59(19): 3977-3986.
[13] ANDRAWES F F, GIBSON E K.Release and analysis of gases from geological samples[J]. Am Mineral, 1979, 64: 453-463.
[14] WILLIAMS A E.Mass spectrometric analysis of volatiles in fluid inclusions: aliquot calibration valve to simulate inclusion rupture[J]. Chem Geol, 1996, 131(1-4): 155-165.
[15] NORMAN D I, SAWKINS F J.Analysis of volatiles in fluid inclusions by mass spectrometry[J]. Chem Geol, 1987, 61: 1-10.
[16] NEWMAN B D, NORMAN D I, GUNDIMEDA M, et al.Understanding the genesis of nonmarine calcite deposits through quadrupole mass spectrometric analysis of fluidinclusion gases[J]. Chem Geol, 1996, 132(1): 205-213.
[17] BLAMEY N J F, PARNELL J, MCMAHON S, et al. Evidence for methane in Martian meteorites[J]. Nat Commun, 2015, 6(1): 1-7.
[18] MORRISON C F.Partial pressure calibration for residual gas analyzers[J]. Journal of Vacuum Science and Technology, 1969, 6(1): 79-82.
[19] KENDALL B.Pulsed gas injection for on-line calibration of residual gas analyzers[J]. Journal of Vacuum Science & Technology A, 1987, 5(1): 143-148.
[20] SANTELER D J.Gas dynamics in residual gas analyzer calibration[J]. Journal of Vacuum Science & Technology A, 1987, 5(1): 129-133.
[21] 代彦伟. 微量气体超高灵敏度四极质谱检测分析[D]. 南京: 东南大学, 2016.
[22] SUN W, WU C, CHENG Y, et al.Study on calibrating the quadrupole mass spectrometers with gas mixture[J]. Measurement, 2020, 164: 108099.
[23] 王朝阳,张占文,李波,等.靶丸内混合气体的质谱法测量技术[J].强激光与粒子束,2005(5):711-714.
[1] 李静, 谭张华, 刘星星, 陈颖琳, 李豪文, 杨浩, 王昌林, 王江涌, 徐从康. 利用遗传算法定量分析Ni/Cr多层膜俄歇深度谱*[J]. 真空, 2021, 58(4): 6-11.
[2] 刘燕文, 孟宪展, 田 宏, 李 芬, 石文奇, 朱 虹, 谷 兵, 王小霞 . 空间行波管极高真空的获得与测量[J]. 真空, 2018, 55(5): 25-28.
Viewed
Full text


Abstract

Cited

  Shared   
  Discussed   
No Suggested Reading articles found!