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  • P-ISSN1225-0163
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GC/AED를 이용한 HFC-134a의 미량 불순물 분석

Determination of trace impurities of HFC-134a by gas chromatograph with atomic emission detector (GC/AED)

분석과학 / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
2017, v.30 no.5, pp.240-251
https://doi.org/10.5806/AST.2017.30.5.240
김명자 (과학기술연합대학원대학교)
임정식 (과학기술연합대학원대학교)
이정순 (과학기술연합대학원대학교)
이진복 (한국표준과학연구원)
윤두현 (과학기술연합대학원대학교)
김예라 (과학기술연합대학원대학교)
김명자, 임정식, 이정순, 이진복, 윤두현, & 김예라. (2017). GC/AED를 이용한 HFC-134a의 미량 불순물 분석. 분석과학, 30(5), 240-251, https://doi.org/10.5806/AST.2017.30.5.240
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초록

1,1,1,2-수소불화탄소(HFC-134a)는 에어컨에 주로 사용되는 냉매로, 최근 온실가스로 규제되어정제를 통한 재사용 방법이 권장되고 있다. 폐냉매의 재사용 기준 평가를 위해서는 폐냉매에 존재하는미량 성분의 정량분석이 매우 중요하다. 본 연구에서는 표준 물질이 없어서 정량화하기 어려웠던 C, H, Cl, F가 포함된 미량 성분들을 GC/AED (gas chromatograph-atomic emission detector)를 이용하여 정량분석하였다. 이를 위하여 GC/MSD (mass selective detector)를 통한 정성분석을 선행하였다. 또한 성분의 원자 수와 비례하여 반응하는 AED의 특성을 조사하기 위하여, 탄화수소 혼합 표준물질을 이용하여 선형성을 확인하였다. 시료 중 C, H, Cl, F가 포함된 미량 성분의 정성 분석 결과, 주성분인 HFC-134a와 유사 냉매류들을 포함한 총 15개의 성분이 검출되었다. MSD 결과를 토대로 AED를 이용한 미량 성분들을 정량 분석한 결과, 한 시료는 CHClF2 성분(45438.38 μmol/mol), 또 다른 시료는 C2H2ClF3 성분(1311.47 μmol/mol)이 가장 높은 몰분율을 나타냈다. 본 연구에서는 이 분석법을 기반으로 하여, 표준 물질이 존재하지 않아 정량화하기 어려운 복합 성분들의 정성 및 정량 분석의 확장 적용이 가능할 것으로 보인다.

keywords
gc/aed, trace impurity, linearity test, certified reference material, matrix effect

Abstract

1,1,1,2-Tetrafluoroethane (HFC-134a), which is used as refrigerant in air conditioners, has been recently regulated as a greenhouse gas and is recommended for reuse by refining. It is very important to quantitatively analyze trace impurities present in the refrigerant to evaluate the criteria for reuse. In this study, trace impurities including C, H, Cl, and F, which are difficult to quantify because there are no reference materials, were quantitatively analyzed by a gas chromatograph-atomic emission detector (GC/AED); for this analysis, this was preceded by a qualitative analysis with a GC-mass selective detector (GC/MSD). In addition, the AED response was investigated using a hydrocarbon mixed reference material, which was proportional to the number of atoms in the component. Fifteen refrigerant components were detected as trace impurities in HFC- 134a by qualitative analysis of trace impurities including C, H, Cl, and F in the samples. Based on the results of the qualitative analysis, quantitative analysis of trace impurities using AED showed that the highest mole fractions were for the CHClF2 component (45438.38 μmol/mol) in one sample and for the C2H2ClF3 component (1311.47 μmol/mol) in another sample. From this study, it has been shown that it is possible for this analytical method to be applied to the qualitative and quantitative analysis of trace compounds in refrigerants, which are difficult to quantify because of the absence of reference materials.

keywords
gc/aed, trace impurity, linearity test, certified reference material, matrix effect


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