• 분석과학
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• 제13권3호
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• pp.297-303
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• 2000

저니토 시료 중의 미량 Cd, Cu, Pb, Ni, Zn 등의 분석을 위해 동위원소희석 질량분석법을 이용하였다. 시료는 마이크로파 혼합산(질산, 불산, 과염소산) 분해법을 이용하여 용해하였다. Ammonium pyrrolidenedithiocarbamate(APDC) 용매 추출법을 이용하여 알칼리 및 알칼리 토금속을 분리한 다음 Pb를 측정하고, 나머지 원소들은 이 용액에 $NH_4OH$ 첨가 후 원심 분리하여 Fe, Sn, Ti 등을 제거한 다음 측정하였다. 측정원소의 회수율은 다소 떨어지나 동중원소 방해를 일으키는 매질원소를 효율적으로 제거할 수 있었다. 2종의 저니토 인증표준물질 중의 미량원소 분석에 이 방법을 적용한 결과 인증값과 잘 일치하는 측정 결과를 얻을 수 있었다.

• 센서학회지
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• 제22권6호
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• pp.404-409
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• 2013

We devised calibration procedure for industrial thermometers by a comparison method at the boiling point of nitrogen (${\sim}-196^{\circ}C$). The uncertainty of the calibration was 4 mK (k = 2). As experimentally demonstrated in this work, the effect of the atmospheric pressure on the boiling point of nitrogen can be easily detected by the thermometer. Therefore, when the boiling point of nitrogen is used for calibration of thermometer by comparison, either a reference thermometer must be used to provide the reference temperature or the effect of atmospheric pressure should be carefully considered. The use of a copper block with a large thermal mass soaked into the liquid nitrogen was proven to be more reliable, and the stability of the temperature immersed into the copper block was 1.4 mK. The temperatures at the thermometer wells, evaluated by the crossed-measurement method to compensate for the inaccuracy of the thermometers and the linear drift of the temperature of the copper block, were equivalent within 0.23 mK of standard uncertainty.

• 분석과학
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• 제22권4호
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• pp.302-306
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• 2009

철강 중의 미량 붕소는 소재의 기계적, 물리적 특성에 중요한 영향을 준다. 즉발감마선 방사화 분석법에 의해 저합금강 시료 중의 미량 붕소를 측정하였다. 시료는 한국표준과학연구원에서 제조한 저합금강 표준물질KRISS 101-01-C21~C26을 이용하였으며, 측정방법의 유효성 확인을 위해 NIST SRM 362, 364, 1761, 1762를 정확도관리용 시료로 사용하였다. NIST SRM 362를 제외하고는 측정 농도가 인증값의 불확도 범위내에서 잘 일치하였다. 불확도는 ISO guideline에 따라 평가하였으며, 포함인자 2를 적용하여 확장불확도를 산출하였다. 붕소 농도 mg/kg수준에서 상대확장불확도는 3%에서 7% 사이였다. 그 결과를 용매추출-유도결합플라스마 방출분광분석결과와 비교하여 제시하였다.

• 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.

• Bulletin of the Korean Chemical Society
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• 제26권5호
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• pp.740-746
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• 2005

In this article, we report the tandem mass spectrometry investigations for the electron capture efficiencies of the protons belonging to the different locations (generations) in a poly(propylene imine) dendrimer with three layers of a repeat unit (named as the third generation dendrimer). The employed tandem mass spectrometry methods include SORI-CAD (sustained off-resonance irradiation collisional activation dissociation) and ECD(electron capture dissociation) mass spectrometry. We obtained SORI-CAD spectra for the dendrimer ions in the different charge states, ranging from 2+ to 4+. The analysis of fragmentation sites provides the information as to where the protons are distributed among various generations of the dendrimer. Based upon this, a new strategy to study the electron capture efficiencies of the protons is utilized to examine a new type of triplycharged ions by SORI-CAD, i.e., the 3+ ions generated from the charge reduction of the native 4+ ions by ECD: (M+4H)$^{4+}\;+\;e^-\;{\rightarrow}$ (M+4H)$^{3+\bullet}$ ${\rightarrow}\;({H^{\bullet}}_{ejected}$) + (M+3H)$^{3+}\;\rightarrow$ CAD. Interestingly, comparison of these four SORICAD spectra indicates that the proton distribution in the charge-reduced 3+ ions is very close to that in the native 4+ ions. It further suggests that in this synthetic polymer ($\sim$1.7 kDa) with an artificial architecture, the electron capture efficiencies of the protons are actually insensitive to where they are located in the molecule. This is somewhat contradictory to common expectations that the protons in the inner generations may not be well exposed to the incoming electron irradiation as much as the outer ones are, thus may be less efficient for electron capture. This finding may carry some implications for the case of medium sized peptide ions with similar masses, which are known to show no obvious site-specific fragmentations in ECD MS.

• 환경영향평가
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• 제21권5호
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• pp.725-734
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• 2012

The outbreak of foot and mouth disease in November 2010 raised many social, economic and environmental issues and water contaminations by leachate from carcass disposal sites particularly emerged as a serious concern. In oder to efficiently handle these problems, a critical method is required to transport leachate to livestock manure and sewage treatment plants and purify it. This study aims to present the best applicable method to transport leachate from carcass disposal sites into livestock manure and sewage treatment facilities. We investigated the biological and chemical characteristics such as BOD, COD, SS, TN, TP and Total coliforms. Current conjugated treatments in livestock manure and sewage treatment plants was studied by surveying the operations of those facilities. The NIER-MASS(National Institute of Environmental Research - Mass Balance Evaluation System of Sewage Treatment Facilities) program was applied to present the best conjugated treatment method through estimating the maximum daily load to meet the water quality standards in effluent.

• 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.

• 센서학회지
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• 제12권6호
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• pp.258-264
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• 2003

본 연구에서는 영상처리를 통한 부액계의 교정방법을 연구한다. 이 방법은 부액계를 교정하기 위해 선정된 부액계의 측정눈금과 기준액체의 수평면을 교정자의 조작 없이 자동으로 일치시킨다. 이 시스템은 CCD카메라, frame grabber, 스텝모터, 영상처리를 포함한 시스템프로그램으로 구성된다. 영상처리프로그램은 부액계의 측정눈금부위와 기준액체의 수평면사이에서 발생하는 메니스커스를 검색하여 눈금을 일치시키는 부분과 스텝모터를 제어하는 부분으로 구성한다. 본 연구에서 개발한 시스템의 성능을 검증하기 위하여 교정자의 눈으로 직접 메니스커스와 측정눈금을 관측한 수동교정방법의 교정결과와 비교한다 각각의 교정값의 차이가 $0.004\;kg/m^3$ 이하로서 교정값의 측정 불확도 $0.06\;kg/m^3$을 고려하면 두 방법의 교정결과가 거의 같은 연구결과를 얻었다.

• Bulletin of the Korean Chemical Society
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• 제28권5호
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• pp.737-744
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• 2007

An isotope dilution-liquid chromatography/tandem mass spectrometric method was developed as a candidate reference method for the accurate determination of acrylamide in potato chips, starch-rich foodstuff cooked at high temperature. Sample was spiked with 13C3-acrylamide and then extracted with water. The extract was further cleaned up with an Oasis HLB solid-phase extraction (SPE) cartridge and an Oasis mixed-phase cation exchange (MCX) SPE cartridge. The extract was analyzed by using LC/ESI/Tandem MS in positive ion mode. LC with a medium reversed-phase (C4) column was optimized to obtain adequate chromatographic retention and separation of acrylamide. MS was operated to selectively monitor [M+H]+ ions of the analyte and its isotope analogue at m/z 72 and m/z 75, respectively. Sample was also analyzed by the LC/MS with selectively monitoring the collisionally induced dissociation channels of m/z 72 → m/z 55 and m/z 75 → 58. Compared to the LC/MS chromatograms, the LC/MS/MS chromatograms showed substantially reduced background chemical noises coming from solvent clusters formed during ESI spray processes and interferences from sample matrix. Repeatability and reproducibility studies showed that the LC/MS/MS method is a reliable and reproducible method which can provide a typical method precision of 1.0% while the LC/MS results are influenced by chemical interferences.

• Asian Journal of Atmospheric Environment
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• 제2권2호
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• pp.90-101
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• 2008

The chemical compositions of $PM_{2.5}$ and $PM_{10}$ and associated high-molecular-weight polycyclic aromatic hydrocarbons (PAHs) were investigated during winter and summer at a roadside and an urban background site in Saitama, Japan. The average concentrations of $PM_{2.5}$ exceeded the United States Environmental Protection Agency standards during both periods. Carbonaceous components were abundant in both the observed and calculated (by means of a mass closure model) chemical composition of $PM_{2.5}$. Traffic-related pollutants (elemental carbon and high-molecular-weight PAHs) were strongly associated with $PM_{2.5}$ rather than with larger particles. The mass concentrations of $PM_{2.5}$, as well as those of EC and PAHs associated with the particles, at the two sites were strongly correlated. Comparison of our data with source profile ratios indicates that diesel-powered vehicles were probably the main source of the measured PAHs. The PAHs concentrations were affected by meteorological conditions during our study. Our results highlight the need for the establishment of standards for $PM_{2.5}$ in Japan.