• 제목/요약/키워드: Proficiency testing materials (PTMs)

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BTEX 분석용 토양 숙련도 표준시료(PTMs) 개발에 관한 연구 (A Study on the Development of Soil-based PTMs for Analysis of BTEX)

  • 이민효;이군택;이법열;이원석;김금희;홍석영
    • 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.

Analysis of the influence of panel characteristics on odor measurement based on the air dilution olfactory method in Korea

  • Kim, Sun-Tae;Lee, Seokjun;Yim, Bongbeen
    • Environmental Engineering Research
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    • 제24권1호
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    • pp.91-98
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    • 2019
  • This study was to objectify differences in the results of odor testing according to the characteristics of panel members that participate in air dilution olfactory method (ADOM) testing. When differences in the results of olfactory testing were reviewed in relation to characteristics of the panelists, the result of entire panels for the site boundary Proficiency Testing Materials (PTMs) showed no difference according to panelist sex, age, smoking status, and past participation in ADOM tests. As for the outlet PTMs, distinct differences appeared in relation to the smoking status and age of panelists. The frequency distribution for all the panelists (Dev($D/T_{total}$)) showed a form similar to a normal distribution, so it is thought to be more appropriate for the review of effect of panelist characteristics on the result of air dilution olfactory tests. In addition, the ADOM testing method implemented as the standard method for odor compounds in Korea (Dev($D/T_3$)) will have to be implemented along with a concurrent assessment, for the purpose of identifying the effect of panelist characteristics on administrative dispositions against malodors.

실내공기질 VOCs 측정의 신뢰도 평가를 위한 연구 (Evaluation of confidence for measurement of VOCs in indoor air)

  • 김명옥;김영란;홍석영;허귀석;임현우;최성헌;이원석;한진석;김금희
    • 분석과학
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    • 제26권3호
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    • pp.165-173
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    • 2013
  • 본 연구는 실내공기질 분야에 대한 합리적인 숙련도 시험 프로그램 확립을 위해 기체상 표준 물질을 제조하고, 시료 채취 과정을 포함한 숙련도 평가가 타당한 것인지 여부를 검토하였다. 또한 숙련도시료(PTMs; proficiency testing materials)의 균질성 및 안정성 평가를 실시하였다. PTMs의 모든 항목에 대해 시료간 균질도가 $0.3{\sigma}p$ 값보다 낮은 값을 가지는 것으로 나타나 충분히 균질성이 확보 되었다고 판단할 수 있었다. 숙련도 평가를 실시한 결과 고압의 실린더에 제조된 VOCs (volatile organic compounds) 표준가스를 Tenax-TA에 흡착시켜 분배한 시료(A 방법)는 시료농도 50~320 ${\mu}g/m^3$에서 로버스트 상대표준편차(RSD)가 23~43% 이내로 나타났고, 시료채취 과정에 대한 숙련도 시험 포함 여부를 평가하기 위하여 고압의 실린더에 제조된 VOCs 표준가스를 기체상으로 테들라백에 담아 분배한 시료(B 방법)와 고압의 실린더에 제조된 VOCs 표준가스를 분배기를 통하여 시험기관이 직접 흡착관에 채취하게 한 시료(C 방법)는 자일렌을 제외하고, VOCs 각각의 농도 200~1200 ${\mu}g/m^3$, 100~450 ${\mu}g/m^3$에서 로버스트 상대표준편차(RSD)가 각각 13~42%, 16~31% 이내로 나타나 시료채취 과정을 포함한 경우 오히려 낮은 상대표준편차를 보였다. 이상의 결과로 볼 때 지속적으로 시료 채취 과정을 포함한 숙련도 평가를 실시하여도 타당할 것으로 사료된다.

Benzo[a]pyrene 분석용 토양 숙련도 표준시료 개발에 관한 연구 - 후보 표준물질의 인증을 위한 균질성, 안정성 평가를 중심으로 - (A Study on the Development of Soil-based PTMs for Analysis of Benzo[a]pyrene - Focusing on the Evaluation of Homogeneity and Stability for the Certification of Benzo[a]pyrenecandidate Reference Materials -)

  • 이민효;이군택;주창규;김용훈;이법열;최성헌;김명옥;홍석영;김금희;이원석
    • 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.

폴리프로필렌 수지 중 카드뮴과 납 측정 숙련도시험 (Proficiency testing of cadmium and lead in polypropylene resin)

  • 조경행;임명철;민형식;한명섭;송현주;박창준
    • 분석과학
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    • 제20권3호
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    • pp.183-192
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    • 2007
  • 최근의 전기전자제품 중 유해물질규제지침(RoHS)이나 폐전기전자제품 처리 지침(WEEE) 등의 각종 환경규제는 국제교역에 있어 실질적인 무역장벽으로 작용하고 있다. 한국표준과학연구원(KRISS)에서는 이와 같은 환경규제와 관련하여 국내시험연구기관 및 관련산업체실험실의 측정 신뢰성 확보를 위한 숙련도 시험을 실시하였다. 참여기관은 국내 전기전자 제품 및 자동차 관련 실험실 31개소이다. 숙련도시험용 시료는 pellet type 폴리프로필렌 소재 2 종이며, 측정대상원소는 유럽공동체의 RoHS 지침에서 규정하고 있는 6개 성분 중 카드뮴 (Cd)과 납 (Pb)이다. 시료는 2006년 9월 1일 각 참여실험실에 우편 송부하였으며 10월 10일까지 측정 결과를 접수하였다. 각 실험실의 측정 결과는 KRISS 기준값과의 비교, Robustic Z-score, Youden plot 등에 의해 비교 평가하고 전처리 방법에 따른 측정 결과도 비교 검토하였다. 전반적으로 기준값과의 10% 범위 내에서 일치되는 결과를 보고하였으나 일부 실험실은 심각한 bias를 보이고 있어 측정결과의 신뢰성 향상을 위한 품질보증 시스템을 갖추어야 할 필요가 있다.