• Bulletin of the Korean Chemical Society
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• 제26권3호
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• pp.440-446
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• 2005

A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

• Bulletin of the Korean Chemical Society
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• 제29권7호
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• pp.1391-1394
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• 2008

Polymer materials are very difficult to decompose for the purpose of chemical analysis. Nondestructive analysis without pretreatment provides a suitable solution that will overcome this obstacle. In this study, CRM candidate samples that contained toxic elements such as As, Cd, Cr and Zn in a polypropylene (PP) were analyzed using instrumental neutron activation analysis (INAA). The analytical results were obtained from ten samples selected by random sampling at two different concentration levels (low and high). Particular attention was paid to reducing analytical errors and evaluating the associated uncertainty.

• 분석과학
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• 제16권1호
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• pp.90-93
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• 2003

The standard uncertainties of two different approaches using the same data set are compared and evaluated using an example of gravimetric standard gas preparation. It is shown that the correlation between input quantities should be taken into account for the proper evaluation of uncertainty resulting from random effects.

• 분석과학
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• 제15권6호
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• pp.580-583
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• 2002

New approach is developed employing the overall uncertainty obtained from multiple measurements to evaluate the statistical significance for the difference between a given reference value and its measured value determined in a lab. The overall uncertainty is determined by separate combinations of the uncertainties arising from systematic and random effects. It is shown that the uncertainty term in regular t-test can be underestimated by n measurements.

• 분석과학
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• 제18권6호
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• pp.475-482
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• 2005

화학분석 분야에는 ISO 17025에 따른 체계적 품질 관리/보증의 요구가 커지면서, 측정 불확도의 표기가 크게 요구되고 있다. 측정품질의 정량화를 위하여, 화학분석의 QA/QC 문헌들로부터 화학분석 품질에 영향을 미치는 중요한 불확도 요소를 선정하였고, 이것을 측정결과 평가 요소의 기본인 7개의 품질요소로서 반복성, 직선성, 소급성, 변동성, 매질효과, 균질성, 안정성으로 구분하였다. 화학분석의 QA/QC를 위한 이 7대 품질 요소의 측정 모델화, 표준불확도의 계산 및 합성방법을 각각 예로서 제시하였다.

• 분석과학
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• 제16권1호
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• pp.82-89
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• 2003

Isotope dilution mass spectrometry (IDMS) was applied to the determination of Ni, Cr, Mo in low alloy steel reference materials. The Mo isotope ratio measurement was performed by dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP/MS) using ammonia as a reaction cell gas. In the case of Ni and Cr measurement, all data were obtained at medium resolution mode (m/${\Delta}m=3000$) of double focusing sector field high resolution inductively coupled plasma mass spectrometry (HR-ICP/MS). For the method validation of the technique was assessed using the certified reference materials such as NIST SRM 361, NIST SRM 362, NIST SRM 363, NIST SRM 364, NIST SRM 36b. This method was applied to the determination of Ni, Cr and Mo in low alloy steel sample (CCQM-P25) provided by NMIJ for international comparison study.

• Bulletin of the Korean Chemical Society
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• 제31권5호
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• pp.1149-1154
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• 2010

Liquid chromatography/mass spectrometry using isotope dilution method has been established as a primary method for the measurement of cortisol in human serum. Verification of this method was accomplished by the participation in Consultative Committee for Amount of Substance-Metrology in Chemistry (CCQM) pilot study. Two levels of cortisol certified reference materials were prepared and certified by the established method. They were used as sample materials for the proficiency testing. The expanded uncertainty in the measurement of cortisol in human serum was approximately 1.2% at 95% confidence level. The results of the proficiency testing showed a good precision among the participants, but some bias to the certified values. This means that commercial field laboratories should keep traceability chain to SI unit through available reference measurement procedures and/or available reference materials.

• 한국안전학회지
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• 제23권5호
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• pp.30-34
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• 2008

To evaluate the mechanical properties of in-service materials, tensile properties measurement using small-scaled specimen has been carried out. Tensile testing specimens with various dimensions, including standard and sub-size specimen specified in ASTM and ISO and small-scaled specimen, were prepared. Tensile strain in small-scaled specimen was measured using micro-ESPI system set up in this study. This system was used in the specimen with the parallel length of 2 mm and in subsequently measuring the strain under tensile loading. From each type of tensile specimen, stress-strain curves were determined. The dimension effect of the tensile properties was investigated comparing the tensile results obtained from standard specimens and small-scaled specimens. It was shown that the tensile strength for the small-scaled specimen is lower by 15% than those for the standard specimen.

• 분석과학
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• 제12권4호
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• pp.332-340
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• 1999

본 연구에서는 canister에 채집한 대기시료 중의 VOC 성분을 농축하기 위해 home-made 저온농축장치를 제작하였다. 제작한 저온농축장치와 GC-MS 분석장치를 이용하여 대기 시료 중에 ppb 농도로 존재하는 EPA의 TO-14 법에서 규정한 성분들을 정량하였다. 제작한 homemade 농축장치에 의한 분석의 결과를 종전에 사용해 오던 흡착관법의 결과와 비교함으로써 제작한 system의 성능을 평가하였고 그 결과 benzene, toluene, ethylbenzene 및 xylene류의 농도가 잘 일치하였다.

• 한국세라믹학회지
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• 제43권1호
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• pp.4-9
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• 2006

To test the fracture toughness of alumina; a Surface-Crack-in-Flexure (SCF) method, a Single-Edge-Precracked-Beam (SEPB) method and a Single-Edge-V-Notched-Beam (SEVNB) method were used at crosshead rates ranging from 0.005 mm/min to 2 mm/ min and relative humidity ranging from $15\%\;to\;80\%$. The results show that the fracture toughness tested by the SCF method increases with either an increasing loading rate or decreasing relative humidity; in contrast, the toughness by the SEPB method and the SEVNB method does not depend on the loading rate or the relative humidity. Theoretical analysis of the way slow crack growth affects the apparent fracture toughness indicates that the three testing methods have different effects with respect to the loading rate and the relative humidity; moreover, these differences are attributable to differences in the size of the cracks or notches.