Korean Journal of Environmental Agriculture (한국환경농학회지)

The Korean Society of Environmental Agriculture (한국환경농학회)
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Comparison of Solidification Pre-treatment Methods for the Determination of δ13C of Dissolved Organic Carbon: Alkaline Persulfate Oxidation-Carbonate Precipitation vs. Freeze Drying

용존유기탄소의 δ13C : 분석시 고형화 전처리 방법 비교 알칼린 과황산칼륨산화 탄산침전과 동결건조

  • Jeon, Byeong-Jun (Department of Rural & Biosystems Engineering, Chonnam National University) ;
  • Park, Hyun-Jin (Department of Rural & Biosystems Engineering, Chonnam National University) ;
  • Choi, Woo-Jung (Department of Rural & Biosystems Engineering, Chonnam National University) ;
  • Park, Yong-Se (National Instrumentation Center for Environmental Management, Seoul National University) ;
  • Lee, Sang-Mo (National Instrumentation Center for Environmental Management, Seoul National University) ;
  • Yoon, Kwang-Sik (Department of Rural & Biosystems Engineering, Chonnam National University)
  • 전병준 (전남대학교 지역.바이오시스템공학과) ;
  • 박현진 (전남대학교 지역.바이오시스템공학과) ;
  • 최우정 (전남대학교 지역.바이오시스템공학과) ;
  • 박용세 (서울대학교 농생명과학공동기기원) ;
  • 이상모 (서울대학교 농생명과학공동기기원) ;
  • 윤광식 (전남대학교 지역.바이오시스템공학과)
  • Received : 2017.04.25
  • Accepted : 2017.06.07
  • Published : 2017.06.30
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Abstract

BACKGROUND: The carbon (C) isotope ratio (${\delta}^{13}C$) of dissolved organic C (DOC) is an indicator of water pollution source. In this study, the potential use of two pre-treatments for the ${\delta}^{13}C$ analysis, alkaline persulfate oxidation coupled with carbonate precipitation (precipitation) and freeze drying (drying), were compared to suggest a more feasible pre-treatment method. METHODS AND RESULTS: Two reference materials with different ${\delta}^{13}C$ values were used for the experiments; chemical grade glucose ($-12.0{\pm}0.02$‰) and pig manure compost extract ($-23.3{\pm}0.04$‰). In the precipitation method, the measured ${\delta}^{13}C$ values were consistently lower than the theoretically calculated values as dissolved $CO_2$ could not be removed due to the alkaline property of the reagents and the dissolution of air $CO_2$ into the alkaline solution. The drying method also resulted in more negative ${\delta}^{13}C$ than the calculated ${\delta}^{13}C$; however, the difference was systematic ($3.9{\pm}0.3$‰) and there was a strong correlation (${\delta}^{13}C_{calculated}=0.87{\times}{\delta}^{13}C_{measured}-0.624$, $r^2=0.98$) between the calculated and measured ${\delta}^{13}C$. Calibration of ${\delta}^{13}C$ using the relationship between the calculated and the measured ${\delta}^{13}C$ values produced reliable and accurate ${\delta}^{13}C$ values. CONCLUSION: Our results suggest that the drying method is more accurate pre-treatment method to minimize the influence of air $CO_2$ compared to the precipitation method for the determination of ${\delta}^{13}C$ of DOC.

DOC의 ${\delta}^{13}C$은 수질 오염원 규명에 활용할 수 있는 매우 유용한 지표이다. 본 연구에서는 안정성동위원소비 질량분석기(EA-SIRMS)를 이용하여 DOC의 ${\delta}^{13}C$을 분석할 때 사용하는 두 가지 전처리방법 (과황산칼륨산화-$SrCO_3$침전법과 동결건조법)의 정확도를 비교 평가하였다. 표준물질로는 글루코스(${\delta}^{13}C$; $-12.0{\pm}0.02$‰)와 돈분퇴비 침출액 건조분말(${\delta}^{13}C$; $-23.3{\pm}0.04$‰)을 사용하였다. 과황산칼륨산화-$SrCO_3$ 침전법에서는 용액의 알칼리성에 의해 DIC 제거가 어렵고 공기 중 $CO_2$의 영향에 의해 시료가 오염되어 분석결과의 정확도가 매우 낮았다. 반면, 동결건조법은 산 첨가에 의해 제거가 가능하였고, 측정값과 이론값의 상관관계가 매우 높아 실험조건별로 표준물질을 이용하여 측정값을 이론값에 근접하게 보정할 수 있는 것으로 나타났다. 따라서, EA-SIRMS를 이용하여 DOC의 ${\delta}^{13}C$ 분석시 동결건조법으로 시료를 전처리하면 분석결과의 정확도를 증대시킬 수 있을 것으로 판단된다.

Keywords

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