[논문]초저온 냉각 트랩을 결합한 비활성기체 동위원소 희석 질량분석 시스템의 제작

홍봉재; 신동엽; 박기홍; 함도식

doi:10.7850/jkso.2022.27.3.144

[국내논문] 초저온 냉각 트랩을 결합한 비활성기체 동위원소 희석 질량분석 시스템의 제작
Development of a Noble Gas Isotope Dilution Mass Spectrometric System Combined with a Cryogenic Cold Trap 원문보기

바다 : 한국해양학회지 = The sea : the journal of the Korean society of oceanography, v.27 no.3, 2022년, pp.144 - 157

홍봉재 (부산대학교 해양학과) , 신동엽 (부산대학교 해양학과) , 박기홍 (극지연구소 해양연구본부) , 함도식 (부산대학교 해양학과)

초록
AI-Helper

비활성기체는 화학적, 생물학적 반응을 하지 않는 보존적인 특성을 가지고 있어 해양에서 수온과 염분 변화, 기체 주입, 해수의 혼합과 빙하 융해수의 분포와 같은 물리적인 변화의 추적자로 활용되고 있다. Ne, Ar과 Kr을 정밀하게 분석하기 위해 사중극자 질량 분석기, 고진공 전처리 라인, 초저온 냉각 트랩과 동위원소 표준기체로 구성된 분석 시스템을 제작했다. 고진공 라인은 시료의 용존 기체를 추출하여 동위원소 표준기체와 혼합하는 시료추출부, 합금 물질을 이용하여 반응성 기체를 제거하고 초저온 냉각 트랩으로 비활성기체를 기화점에 따라 분별 증류하는 기체 준비부, 비활성기체를 원소별로 측정하는 기체 측정부로 구성하였다. 기체준비부에 결합한 초저온 냉각 트랩은 질량분석기 내 Ar와 CO₂의 부분압을 현저히 낮추어 Ne 동위원소 분석의 오차를 감소시켰다. 동위원소 표준기체는 ²²Ne, ³⁶Ar과 ⁸⁶Kr를 혼합하여 제작하였고, 혼합 표준 기체의 원소별 양은 대기를 반복 측정하여 역동위원소 희석법으로 결정했다. 대기 평형수 반복 분석의 상대 오차는 Ne, Ar과 Kr에 대해 각각 0.7%, 0.7%, 0.4%이었다. 반복 측정한 대기 평형수의 농도와 포화 농도의 차이로 확인한 분석시스템의 정확도는 Ne, Ar, Kr에 대해 각각 0.5%, 1.0%, 1.7%이었다.

Abstract ▼ AI-Helper

Noble gases, which are chemically inert and behave conservatively in marine environments, have been used as tracers of physical processes such as air-sea gas exchange, mixing of water masses, and distribution of glacial meltwater in the ocean. For precise measurements of Ne, Ar, and Kr, we developed a mass spectrometric system consisting of a quadrupole mass spectrometer (QMS), a high vacuum preparation line, an activated charcoal cryogenic trap (ACC), and a set of isotope standard gases. The high vacuum line consists of three sections: (1) a sample extraction section that extracts the dissolved gases in the sample and mixes them with the standard gases, (2) a gas preparation section that removes reactive gases using getters and separates the noble gases according to their evaporation points with the ACC, and (3) a gas analysis section that measures concentrations of each noble gas. The ACC attached to the gas preparation section markedly lowered the partial pressures of Ar and CO2 in the QMS, which resulted in a reduced uncertainty of Ne isotope analysis. The isotope standard gases were prepared by mixing 22Ne, 36Ar, and 86Kr. The amounts of each element in the mixed standard gases were determined by the reverse isotope dilution method with repeated measurements of the atmosphere. The analytical system achieved precisions for Ne, Ar, and Kr concentrations of 0.7%, 0.7%, and 0.4%, respectively. The accuracies confirmed by the analyses of air-equilibrated water were 0.5%, 1.0%, and 1.7% for Ne, Ar, and Kr, respectively.

주제어

표/그림 (10)

그림 Fig. 1. Diagram showing the effect of different physical processes on saturation anomlies of Ne and Ar. Saturation anomaly of gas C is defined as ΔC(%)=(C_obs/C_sat-1)×100, where C_obs and C_sat are the observed and air-saturated concentrations at the observed potential temperature and salinity. Refer to Hamme et al.(2019) for the explanation of each process.
그림 Fig. 2. Schematic of the mass spectrometric system. The system is divided into gas measurement section, gas preparation section and sample release section. CTO: copper tube opener, WVC: water vapor cryo-trap, T/C: thermocouple gauge, AP: air pipette, SP: spike pipette, GP: glass pipette, BG: Baratron gauge, CF: charcoal finger, ACC: activated charcoal cryogenic trap, IP: ionization pump, QMS: quadrupole mass spectrometer.
그림 Fig. 3. Percentage of ⁴He, ²⁰Ne and ²²Ne release as a function of ACC temperature.
그림 Fig. 4. The difference in intesities of He, Ne, Ar and CO₂ between Ne analyses with and without activated charcoal cryogenic trap (ACC). The intensities are from the measurements of air and isotope spike mixture. The use of the ACC markedly reduces the partial pressures of ⁴⁰Ar and CO₂ in the QMS, resulting in negligible interference by doubly charged ⁴⁰Ar (⁴⁰Ar⁺⁺) on ²⁰Ne.
그림 Fig. 5. Schematic of the vacuum line for mixed isotope spikes.
표 Table 1. The measured isotopic ratios of the air, isotope spikes and air mixed with isotope spikes
그림 Fig. 6. Temperature change of the traps during analysis. The arrows indicate trapping and releasing of gases. Refer to Fig. 2 for the locations of the traps.
그림 Fig. 7. An example of Kr measurements for air-equilibrated water spiked with ⁸⁶Kr. The intensities of ⁸⁴Kr and ⁸⁶Kr and the ratio of ⁸⁴Kr/⁸⁶Kr at the start of the measurement are determined as the intercepts (at t = 0) of the linear regression lines. The first 10-minute data points (open circles) are excluded from linear regression.
표 Table 2. The concentrations of Ne, Ar and Kr in deionized water equilibrated with air at temperature of 24.9℃, atmospheric pressure of 1001.5 hPa, and relative humidity of 35.9%
표 Table 3. Comparison of isotope dilution mass spectrometric systems for the analysis of noble gases

참고문헌 (21)

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