• Mass Spectrometry Letters
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• 제10권4호
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• pp.112-116
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• 2019

In this study, a chloroform consumer chemical product (CCP) reference material (RM) is successfully developed, with potential to be used in the proficiency testing of hazardous compounds in CCPs for analysis and testing agencies. Validation experiments are rigorously conducted to evaluate whether the RM meets the requirements set by the ISO 13528 and ISO Guide 35, using a reliable GC/MS method for the analysis of chloroform. The obtained calibration plot linearity, limit of detection (LOD), and limit of quantitation (LOQ) are excellent. The developed RM meets the homogeneity and stability requirements; the between-unit (s_bb) and within-unit (s_wb) standard deviations are less than 2.5%, and the stability is found to be guaranteed for 50 days.

• 한국지하수토양환경학회지:지하수토양환경
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• 제19권6호
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• pp.49-58
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• 2014

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.

• 농약과학회지
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• 제20권3호
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• pp.211-220
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• 2016

본 연구는 풋고추 시료를 이용하여 농약다성분 분석표준물질을 개발하기 위해 수행하였다. 10종의 농약성분을 풋고추 시료에 처리하여 균질하게 분포될 수 있도록 조제하였으며, 국제적인 지침서인 'ISO Guide 35', 'ISO Guide 13528' 그리고 'EURL-PT'에서 요구하는 균질성, 안정성, 인증값 및 표준불확도가 확립된 농약다성분 풋고추 분석표준물질을 개발하였다. 개발된 분석표준물질의 병간 표준편차와 병내 표준편차는 인증값의 1.7~3.7%로 매우 우수한 균질성을 나타냈으며, 불균질성에 의한 표준불확도는 인증값의 0.8~1.15% 매우 낮아 분석표준물질로 사용하기에 매우 적합하였다. 다양한 조건에서의 안정성을 확인한 결과, 실온 $20{\sim}30^{\circ}C$)에서는 7일, 냉동($-20^{\circ}C$)에서는 30일 동안 안정하였으며, 초저온 상태($-80^{\circ}C$)에서는 bifenthrin, Fenpropathrin을 제외한 8종이 245일 동안 안정하였다. 개발된 농약다성분 풋고추 분석표준물질을 사용하여 잔류농약을 분석하는 8기관의 시험소를 평가한 결과, 일부기관에서는 6성분을 검출하지 못하였으며 일부 농약성분에 대해서는 의심스러운(questionable) 또는 부적합(unacceptable)의 평가를 받았다. 동일한 분석표준물질에 대해서 각 기관마다 분석결과의 차이가 나타나는 것을 확인하였으며, 이런 결과를 통해서 잔류농약의 분석결과 신뢰성과 일관성을 향상시키기 위해 풋고추 분석표물질을 활용한 정도관리 또는 숙련도 평가시험이 필요할 것으로 보인다.

• 분석과학
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• 제23권5호
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• pp.485-491
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• 2010

토양 중 유해원소 분석용 인증표준물질 KRISS CRM 109-03-SSD를 개발하였다. 인증 대상 원소는 현행 토양환경보전법에서 규제하고 있는 비소, 카드뮴, 크로뮴, 구리, 수은, 니켈, 납, 아연이다. 인증표준물질 제조를 위한 출발물질은 강원도 상동의 텅그스텐 폐광 광미 더미에서 채취하였다. 출발물질은 선별, 건조, 분쇄, 체거름, 혼합, 병입, 살균의 일련의 과정을 거쳐 제조한 다음 ISO Guide 35의 절차를 준용하여 인증하였다. 측정에는 동위원소희석 질량분석법(ID-ICP/MS) 및 기기중성자방사화분석법(INAA)을 이용하였다. 균질도 평가는 ISO 13528의 부속서 B를 준용하여 실시하였다. 인증값은 서로 다른 두 가지 측정방법에 의한 분석 결과 또는 동일한 방법이지만 독립적으로 2회 반복 시행된 분석의 결과로부터 결정하였다. 최종으로 비소, 카드뮴, 크로뮴, 구리, 납, 니켈, 아연 7개 원소에 대한 인증값을 결정하였다. 수은은 낮은 농도로 인해 균질도 요건을 만족시키지 못해 철, 텅그스텐과 함께 참고값으로 제공된다. 환경감시목적으로 많이 이용되는 ISO 11466에 따른 왕수에 의한 용출시험 또한 실시하였다. 용출시험은 공립시험소 및 대학 시험소 등 6개 기관의 공동분석으로 수행되었다. 용출시험의 실험실간 편차는 인증값의 불확도에 비해 크게 나타났다. 용출시험에 대한 공동분석 결과는 참고값으로 제공된다.

• 한국지하수토양환경학회지:지하수토양환경
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• 제18권5호
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• pp.15-25
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• 2013

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.

• 한국환경농학회지
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• 제35권3호
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• pp.223-233
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• 2016

BACKGROUND: This study was to develop a analytical reference material including twenty pesticides in tomato. To use it for proficiency test, the suitability of homogeneity, storage stability, assigned values and uncertainty for analytical reference material were important.METHODS AND RESULTS: In order to develop a analytical reference material of tomato for multi-residue analysis of pesticides, twenty-pesticides were treated in tomato and the samples were frozen and homogenized. The homogeneity, stability, assigned value and uncertainty were calculated according to the requirements of the KS A ISO Guide 35, KS Q ISO 13528 and EURL-PT protocol. The values of the within-bottle standard variation(s_wb) and the between-bottle standard variation(s_bb) were 0.9~6.5% of assigned value and the uncertainty(u*_bb) due to inhomogeneity was also calculated as 0.6~1.9% for all pesticides. This indicated that it was satisfactory to be used as a analytical reference material. The storage stabilities of twenty-pesticides at room temperature and freezing conditions were assessed according to the requirement of the KS Q ISO Guide 35. All pesticides were stable at room temperature (20~30℃) for 8 days and freezing (-20℃) for 23 days.CONCLUSION: The feasibility of analytical reference material for pesticide multi-residue analysis in a tomato matrix was investigated. Homogeneity of within/between-bottle, uncertainty and stabilities at room temperature and freezing condition were satisfactory for a use of proficiency test and quality control. From these results, a analytical reference material would be applicable to monitor the proficiency test of pesticide analysis organizations to improve the reliability and consistency.