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용존유기탄소의 δ<sup>13</sup>C : 분석시 고형화 전처리 방법 비교 알칼린 과황산칼륨산화 탄산침전과 동결건조
전병준,박현진,최우정,박용세,이상모,윤광식,Jeon, Byeong-Jun,Park, Hyun-Jin,Choi, Woo-Jung,Park, Yong-Se,Lee, Sang-Mo,Yoon, Kwang-Sik 한국환경농학회 2017 한국환경농학회지 Vol.36 No.2
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. 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.
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용존유기탄소의 δ<sup>13</sup>C 분석시 고형화 전처리 방법 비교: 알칼린 과황산칼륨산화-탄산침전과 동결건조
전병준 ( Byeong-jun Jeon ),박현진 ( Hyun-jin Park ),최우정 ( Woo-jung Choi ),박용세 ( Yong-se Park ),이상모 ( Sang-mo Lee ),윤광식 ( Kwang-sik Yoon ) 한국환경농학회 2017 한국환경농학회지 Vol.36 No.2
DOC의 δ<sup>13</sup>C은 수질 오염원 규명에 활용할 수 있는 매우 유용한 지표이다. 본 연구에서는 안정성동위원소비 질량분석기(EA-SIRMS)를 이용하여 DOC의 δ<sup>13</sup>C을 분석할 때 사용하는 두 가지 전처리방법(과황산칼륨산화-SrCO<sub>3</sub>침전법과 동결건조법)의 정확도를 비교 평가하였다. 표준물질로는 글루코스(δ<sup>13</sup>C; -12.0±0.02‰)와 돈분퇴비 침출액 건조분말(δ<sup>13</sup>C;-23.3±0.04‰)을 사용하였다. 과황산칼륨산화-SrCO<sub>3</sub>침전법에서는 용액의 알칼리성에 의해 DIC 제거가 어렵고 공기 중CO<sub>2</sub>의 영향에 의해 시료가 오염되어 분석결과의 정확도가 매우 낮았다. 반면, 동결건조법은 산 첨가에 의해 DIC 제거가 가능하였고, 측정값과 이론값의 상관관계가 매우 높아 실험조건별로 표준물질을 이용하여 측정값을 이론값에 근접하게 보정할 수 있는 것으로 나타났다. 따라서, EA-SIRMS를 이용하여 DOC의 δ<sup>13</sup>C 분석시 동결건조법으로 시료를 전처리하면 분석결과의 정확도를 증대시킬 수 있을 것으로 판단된다. BACKGROUND: The carbon (C) isotope ratio (δ<sup>13</sup>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 δ<sup>13</sup>C analysis, alkaline persulfate oxidation coupledwith 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 δ<sup>13</sup>C values were used for the experiments; chemical grade glucose (-12.0±0.02‰) and pig manure compost extract (-23.3±0.04‰). In the precipitation method, themeasured δ<sup>13</sup>C values were consistently lower than the theoretically calculated values as dissolved CO<sub>2</sub> could not be removed due to the alkaline property of the reagents and the dissolution of air CO<sub>2</sub> into the alkaline solution. The dryingmethod also resulted inmore negative δ<sup>13</sup>C than the calculated δ<sup>13</sup>C; however, the difference was systematic (3.9±0.3‰) and therewas a strong correlation (δ <sup>13</sup>C<sub>calculated</sub>=0.87×δ<sup>13</sup>C<sub>measured</sub>-0.624, r<sup>2</sup>=0.98) between the calculated andmeasured δ<sup>13</sup>C. Calibration of δ<sup>13</sup>C usingthe relationship between the calculated and themeasured δ<sup>13</sup>C values produced reliable and accurate δ<sup>13</sup>C values. CONCLUSION:Our results suggest that the dryingmethod is more accurate pre-treatment method to minimize the influence of air CO<sub>2</sub> compared to the precipitationmethod for the determination of δ<sup>13</sup>C of DOC.
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토양환경 분야PS-05 : 수질 시료 용존유기탄소의 탄소동위원소비 분석 방법: 알칼린 과황산 산화법과 동결건조 연소법 비교
전병준 ( Byeong Jun Jeon ),함종현 ( Jong Hyun Ham ),임상선 ( Sang Sun Lim ),이광승 ( Kwang Seung Lee ),이세인 ( Se In Lee ),박현진 ( Hyun Jin Park ),유서진 ( Seo Jin Yu ),이상모 ( Sang Mo Lee ),박용세 ( Yong Se Park ),윤광식 ( Kwa 한국환경농학회 2014 한국환경농학회 학술대회집 Vol.2014 No.-
Dissolved organic carbon (DOC) is a key parameter of water quality assessment as DOC is directly associated with biological oxygen demand (BOD). Carbon isotope composition (δ13C) of DOC can be used as an indicator of the DOC sources since organic materials have distinguished δ13C values affected by their source; for example C3 vs. C4. In this study, we compared two methods (alkaline persulfate oxidation and freeze drying-combustion). For the alkaline persulfate oxidation method, glucose (-12.0‰) was used as a standard material. Glucose solution (10 mg L-1) was oxidized with alkaline persulfate (10 mL) in the presence of SrCl2 (for precipitation of CO2) under a variety experimental conditions, and then the precipitates (SrCO3) were analyzed for δ13C. The measured δ13C were -25∼-17‰ and thus the precision and reproducibility were not satisfied. For the freeze drying-combustion method, five reference materials (-23.3∼-12.0‰) were prepared by mixing glucose (-12.0‰) and compost extracts (-23.3‰). The solutions (150 mL) containing the reference materials were freeze-dried after addition of 700 mg of K2SO4 (for increasing quantity) and then the powder was analyzed for δ13C. There was a linear relationship (y=1.1328x + 6.7348, r2=0.98, P<0.001) between the calculated values (y) and measured values (x). Therefore, our study suggests that freeze drying-combustion can produce more reliable δ13C measurement compared to the conventional alkaline persulfate oxidation method.
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