• 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.

• 분석과학
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• 제25권6호
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• pp.402-409
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• 2012

연속흐름 수소화물 생성-유도결합 플라스마 원자 방출 분광기(FI-HG-ICP-AES) 이용하여 플라스틱 소재에 함유된 비소를 정량하기 위한 조건을 얻었다. 플라스틱 시료를 습식 산 분해 방법 및 마이크로파 산 분해 방법으로 전처리하여 시험 용액을 조제하였다. 인증표준물질(CRM)인 CRM-EC680k 및 CRM-EC681k를 사용하여 측정한 값과 인증값을 비교하여 분석 방법의 재현성 및 정확성을 확인하였다. 습식 산 분해 방법 및 마이크로파 산 분해 방법으로 전처리하여 FI-HG-ICP-AES로 측정한 결과 CRM-EC680k의 경우에는 4.1~4.3 mg/kg (인증값 $4.1{\pm}0.5$ mg/kg)이고, CRM-EC681k의 경우에는 28.9~30.6 mg/kg (인증값 $29.1{\pm}1.8$ mg/kg)이었다.

• The Korean Journal of Ceramics
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• 제4권4호
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• pp.311-322
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• 1998

American Society for Testing and Materials (ASTM) standard test method PS 070-97 has been created for measuring fracture toughness of advanced ceramics. PS 070-97 includes three test methods which use beams in bending: chevron notch (CNB), single-edged precracked beam (SEPB), and surface crack in flexure (SCF). Supporting data has been collected through several Versailles Advanced Materials and Standards round robins. This paper discusses the evolution of the standard including the rationale for the choice of the three methods and the specifications in the standard. Progress on Standard Reference material 2100 which will have certified values of fracture toughness is presented.

• Bulletin of the Korean Chemical Society
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• 제35권11호
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• pp.3275-3279
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• 2014

A mass balance method for purity assessment of thermolabile organic reference materials was established by combining several techniques, including liquid chromatography with UV/VIS detector (LC-UV), Karl-Fischer (K-F) Coulometry, and thermal gravimetric analysis (TGA). This method was applied to three fluoroquinolones like enrofloxacin, norfloxacin and ciprofloxacin. LC-UV was used to analyze structurally related organic impurities based on UV/VIS absorbance spectra obtained in combination with LC separation. For all three organic reference materials, the UV/VIS spectra of the separated impurities were similar to that of the major component of the corresponding materials. This indicates that the impurities are structurally related to the respective reference material sharing common chromophores. Impurities could be quantified by comparing their absorbances at the wavelength of maximum absorbance (${\lambda}_{max}$). The water contents of the reference materials were measured by K-F Coulometry by an oven-drying method. The total inorganic impurities contents were assayed from ash residues in TGA analysis with using air as a reagent gas. The final purities estimated from results of those analytical techniques were assigned as ($99.91{\pm}0.06$), ($97.09{\pm}0.17$) and ($91.85{\pm}0.17$)% (kg/kg) for enrofloxacin, norfloxacin and ciprofloxacin, respectively. The assigned final purities would be applied to the reference materials which will be used as calibrators for the certification of those compounds in matrix CRMs as starting points for the traceability of their certified values to SI units.

• 분석과학
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• 제23권1호
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• pp.74-82
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• 2010

휴대형 형광 분석기의 개발을 위한 사전 기초연구로서 탁상형 및 휴대형 X-선 형광분석기를 이용하여 플라스틱 중의 Cd, Pb, Hg, Cr (IV), polybrominated biphenyls (PBB) 및 polybrominated diphenyl ethers (PBDE)의 RoHS 규제 물질에 대하여 비교 분석하였다. 규제 물질이 0~1,200 mg/kg의 농도로 함유된 폴리에틸렌 및 폴리프로필렌 인증표준물질을 사용하여 측정시간에 따른 최적의 분석 조건을 확립하고, 각 규제 물질의 검량곡선을 작성하였다. 플라스틱 인증표준물질과 시료 중의 Pb, Hg, Cd, 총 Cr 및 총 Br 함량을 탁상형 X-선 형광분석기의 empirical (EM) 법 및 fundamental parameter (FP) 법으로 정량분석하고 그 결과를 휴대형 X-선 형광분석기와 비교 하였다.

• 분석과학
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• 제19권2호
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• pp.172-180
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• 2006

본 연구는 유해폐기물에 의한 환경오염을 예방하기 위해 폐기물 시험방법과 신규 항목을 설정하기 위해 수행하였다. 국내외 유해폐기물의 규제기준, 시험항목 등을 조사검토하여 유해물질에 대한 우선순위를 선정하였다. 선정한 Ba, Be, Cr(VI), F, Ni, Sb, Se, V 8종의 유해물질을 함유한 오니, 폐유, 소각재 등 폐기물 인증표준물질을 사용하여 전처리방법을 비교분석하였다. 이 결과를 통해 시험방법(안)을 확립하고, 관련 항목 배출 가능성이 있는 표본사업장을 선정하여 시료 37건을 채취분석하였다.

• Journal of Radiation Protection and Research
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• 제41권4호
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• pp.359-367
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• 2016

Background: As new legislation has come into force implementing radiation safety management for the use of naturally occurring radioactive materials (NORM), it is necessary to establish a rapid and accurate measurement technique. Measurement of $^{238}U$ and $^{232}Th$ using conventional methods encounter the most significant difficulties for pretreatment (e.g., purification, speciation, and dilution/enrichment) or require time-consuming processes. Therefore, in this study, the applicability of ED-XRF as a non-destructive and rapid screening method was validated for raw materials and by-product samples. Materials and Methods: A series of experiments was conducted to test the applicability for rapid screening of XRF measurement to determine activity of $^{238}U$ and $^{232}Th$ based on certified reference materials (e.g., soil, rock, phosphorus rock, bauxite, zircon, and coal ash) and NORM samples commercially used in Korea. Statistical methods were used to compare the analytical results of ED-XRF to those of certified values of certified reference materials (CRM) and inductively coupled plasma mass spectrometry (ICP-MS). Results and Discussion: Results of the XRF measurement for $^{238}U$ and $^{232}Th$ showed under 20% relative error and standard deviation. The results of the U-test were statistically significant except for the case of U in coal fly ash samples. In addition, analytical results of $^{238}U$ and $^{232}Th$ in the raw material and by-product samples using XRF and the analytical results of those using ICP-MS ($R^2{\geq}0.95$) were consistent with each other. Thus, the analytical results rapidly derived using ED-XRF were fairly reliable. Conclusion: Based on the validation results, it can be concluded that the ED-XRF analysis may be applied to rapid screening of radioactivities ($^{238}U$ and $^{232}Th$) in NORM samples.

• 분석과학
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• 제18권1호
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• pp.51-58
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• 2005

A comparison of the analytical data obtained by three $k_0$-NAA software programs was carried out using both the airborne particulate matter collected from an urban site and the certified reference materials of the air filter and urban dust to evaluate the performance of the analysis. The individual $k_0$-NAA standardization methods of three countries, Korea, China and Vietnam which had been modified from the well established $k_0$-program were used for the comparative analysis. The measured concentrations of 30 elements from the two kinds of air samples based on this software were in agreement with each other within about 20% analytical error except for a few elements. By contrast, the results of China and Vietnam were moderately higher than that of Korea due to a systematic error associated with the detection efficiency, gamma peak analysis and geometric effect.

• Mass Spectrometry Letters
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• 제14권4호
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• pp.166-172
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• 2023

The utilization of methyl 2-aminobenzoate as a biocide and pesticide has raised concerns regarding its potential toxicity. To assess its safety, it is crucial to determine its quantity and related toxicity using reference materials (RMs) or certified reference materials (CRMs). As an RM and CRM containing methyl 2-aminobenzoate within a biocidal product matrix is currently unavailable, this study aimed to produce a high-quality RM containing methyl 2-aminobenzoate, ensuring its homogeneity and stability, following the ISO Guide 35 and ISO 17034. The study determined that the produced RM exhibited homogeneity, as indicated by a calculated F-value (1.91) smaller than the critical F-value (3.02). In the assessment of isochronous short-term stability, the slope of the linear regression for the RM showed no statistically significant difference from zero when stored at temperatures of 4, 18, and 60 ℃ for 4 weeks. Regarding classical long-term stability, the RM demonstrated sustained stability over the course of one year when stored at 4 ℃. This study has successfully developed an RM for monitoring methyl 2-aminobenzoate in biocides and pesticides. Its quality underwent rigorous evaluation, confirming both homogeneity and stability.

• Nuclear Engineering and Technology
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• 제54권5호
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• pp.1754-1759
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• 2022

The activity of gamma-ray emitting nuclides is calculated assuming that each gamma-ray is detected individually; thus, the magnitude of the coincidence summing signal must be considered during activity calculations. Here, the correction factor for the coincidence summing effect was calculated, and the detection efficiencies of two HPGe detectors were compared. The CANBERRA Inc. GC4018 high-purity Ge detector provided an estimate for the peak-to-total ratio using a point source to determine the coincidence summing correction factor. The ORTEC Inc. GEM60 high-purity Ge detector uses EFFTRAN in LVis to obtain the parameters of the detector and source model and the gamma-gamma and gamma-X match estimates, in order to determine the coincidence summing correction factor. Nuclide analyses, radioactivity comparisons, and analyses of reference material samples were performed utilizing certified reference materials to accurately determine the detection efficiencies. For both Co-60 and Y-88, the detection efficiency for a point source increased by an average of at least 12-13%, whereas the detection efficiency determined using LVis increased by an average of at least 13-15%. The calculated radioactivity values of the certified reference material and reference material samples were accurate to within 3% and 6% of the measured values, respectively.