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BTEX 분석용 토양 숙련도 표준시료(PTMs) 개발에 관한 연구
이민효,이군택,이법열,이원석,김금희,홍석영,Lee, Minhyo,Lee, Guntaek,Lee, Bupyoel,Lee, Wonseok,Kim, Gumhee,Hong, Sukyoung 한국지하수토양환경학회 2013 지하수토양환경 Vol.18 No.5
In this study, two kinds of soil-based proficiency testing materials (PTMs), NICE-012L and NICE-012R were prepared and certified for Benzen, Toluene, Etylbenzene and Xylene with evaluation of uncertainties. In order to analyse BTEX (Benzen Toluene Etylbenzene Xylene) for the candidate materials, GC/MS was used after pretreatment according to methods of soil analysis by Ministry of Environment. For the homogeneity test among bottles in terms of candidate materials, ISO 13528 and IUPAC Protocol were used and according to the result, both candidate materials showed sufficient homogeneity. Also, the stability test over the candidate materials was accessed according to the ISO Guide 35 by classifying short-term and long-term stability and the result showed that both candidate materials showed decent stability. The reference values of the two candidate materials depending on BTEX components were derived from the average of the 11 samples that were used for verification of the samples' homogeneity. Uncertainty of measurement was combined by uchar that was caused by a characteristic value, $u_{bb}$ that was caused by between-bottle homogeneity, and $u_{stab}$ that was caused by stability, and then combined uncertainty ($u_{PTM}$) was multiplied to the coverage factor (k) derived from the effective degree of freedom from each factor that leads to expanded uncertainty (U) in about 95% of confidence level. The proficiency testing materials developed through this study were supplied to National Institute of Environmental Research (NIER) and utilized as an external proficiency testing materials for evaluating analysis capacity of soil agencies with specialty in terms of soil analysis approved by Minister of Environment.
Comparing Bioavailability of Cadmium and Arsenic in Agricultural Soil Under Varied pH Condition
오세진,김성철,옥용식,오승민,이법열,이상환,양재의 한국토양비료학회 2015 한국토양비료학회지 Vol.48 No.1
Bioavailability of cadmium (Cd) and arsenic (As) can be different depending on soil pH. For this reason, main purpose of this research was to compare bioavailability of Cd and As in agricultural field under varied soil pH and different extractants. Bioavailable fraction of Cd and As in soil was extracted with CaCl2, NaNO3, DTPA, EDTA, and low molecular weight organic acids (LMWOAs). Soil samples and cultivated crops were collected at the range of soil pH 4.5-8.5 and correlation analysis was conducted between bioavailable fraction of Cd and As in soil and total concentration of Cd and As in crops. Results showed that concentration of Cd and As in acidic soil was ranged 0.002-0.462 mg kg-1 and 0.041-4.903 mg kg-1 respectively. In alkaline condition, concentration of Cd and As were ranged 0.006-0.351 mg kg-1 and 0.039-2.807 mg kg-1 respectively. Comparing bioavailable fraction of Cd and As in acidic and alkaline soil condition, higher concentration was measured in acidic condition. Similarly, higher average concentration of Cd and Asin crops was observed in acidic condition (0.398 and 0.751 mg kg-1 respectively) than alkaline condition (0.248 and 0.264 mg kg-1). Among different extractants, LMWOAs method showed higher correlation (r2=0.545) for Cd in acidic condition indicating that LMWOAs method could be applied for evaluating bioavailability of Cd in acidic soil. However, no high correlation was observed for As in both acidic and alkaline condition. Overall, bioavailable fraction of Cd and As can be higher in acidic condition of soil than alkaline condition resulting higher uptake of Cd and As from soil to crops. Therefore, efficient best management practice (BMPs) for Cd and As in acidic soil should be conducted for minimizing uptake of Cd and As into crops.
Benzo[a]pyrene 분석용 토양 숙련도 표준시료 개발에 관한 연구 - 후보 표준물질의 인증을 위한 균질성, 안정성 평가를 중심으로 -
이민효,이군택,주창규,김용훈,이법열,최성헌,김명옥,홍석영,김금희,이원석,Lee, Minhyo,Lee, Guntaek,Joo, Changkyu,Kim, Yonghun,Lee, Bupyoel,Choe, Sunghun,Kim, Myeongock,Hong, Sukyoung,Kim, Gumhee,Lee, Wonseok 한국지하수토양환경학회 2014 지하수토양환경 Vol.19 No.6
This study was implemented as a part of the experiment to develop two kinds of soil-based Benzo[a]pyrene (BaP) proficiency testing materials (PTMs) for soil analysis. A test was carried out for the check of solubility of the reference material (high purity reagent) using several solvents. Another test was also conducted for the evaluation of homogeneity and stability of two kinds of candidate soil reference materials. The test analysis of BaP in terms of the candidate materials was conducted according to the Standard Soil Analytical Methods by Ministry of Environment. Dissolution of the reference material was shown to vary depending on solvent type and was higher in the order of Dichloromethane > Acetone > Acetone/MeOH (9 : 1) > N-hexane. In addition, the slope on calibration curve for BaP standard solutions was largest on BaP standard solutions prepared with dichloromethane of the tested solvents. Such tendency appeared egually in the commercial BaP standard solution. Therefore, it is thought to be reasonable to use dichloromethane as the solvent in case of the standard stock solution that is used for the measurement of BaP concentration in soil. ISO 13528 and IUPAC protocol were used for verification of homogeneity on the two kinds of soil candidate materials, Both candidate materials were sufficiently homogeneous. Stability assessment of the two candidate materials was made according to ISO Guide 35 and the result showed that both batches did not have any long-term and short term stability issues that might occur during shipping. However, monitoring results of BaP concentration in soil showed that BaP concentration of the two batches measured at 15 days after the sample preparation was reduced by about 24~37% compared with that of the samples measured on 0 day of the sample preparation. Identification was done with several treatments such as irradiation and sterilization etc. The major cause was shown to be irradiation to the samples.