• 제목/요약/키워드: trace analysis

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Determination of Trace Amounts of Lead and Copper in Water Samples by Flame Atomic Absorption Spectrometry after Cloud Point Extraction

  • Shemirani, Farzaneh;Abkenar, Shiva Dehghan;Khatouni, Asieh
    • Bulletin of the Korean Chemical Society
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    • 제25권8호
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    • pp.1133-1136
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    • 2004
  • The need for highly reliable methods for the determination of trace metals is recognized in analytical chemistry and environmental science. A method based on the cloud-point extraction (CPE) technique for the trace analysis of Pb and Cu in water samples is described in this study. The analytes in the initial aqueous solution are complexed with pyrogallol, and 0.1%(w/v) Triton X-114 is added as surfactant. Following phase separation at $50^{\circ}C$, based on the cloud point of the mixture and dilution of the surfactant-rich phase with acidified methanolic solution, the enriched analytes are determined by flame atomic absorption spectrometry. After optimization of the complexation and extraction conditions, the enrichment factors of Pb and Cu were found to be 72 and 85, respectively. Under optimum conditions, the preconcentration of 60 mL of samples in the presence of 0.1%(w/v) Triton X-114 permitted the detection of 0.4 ${\mu}gL^{?1}$ of Pb and 0.05 ${\mu}gL^{?1}$ of Cu. The proposed method was applied successfully to the determination of Pb and Cu in water samples.

Analysis of Minor Additives and Polymer in Used-stripper Using Pyrolysis-Gas Chromatography/Mass Spectrometry and Electrospray Mass Spectrometry

  • Koo, Jeong-Boon;Park, Chang-Hyun;Han, Cheol;Na, Yun-Cheol
    • Bulletin of the Korean Chemical Society
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    • 제30권2호
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    • pp.368-372
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    • 2009
  • The trace polymer and additives in used stripper solutions were analyzed by a combination of Py-GC/MS and ESI-MS. In the comparison of the pyrolysates produced by the pyrolysis of the pure stripper and photoresist at $500{^{\circ}C}$, the presence of novolac polymer in the used stripper was confirmed by the presence of the characteristic peaks of its pyrolysates, such as those of the methylphenol, di-methylphenol and methylenebis(methylphenol) isomers. The intact trace polymer was measured by ESI-MS, which showed the distribution of oligomers at intervals of 120 Da, indicating di-methylphenol to be the repeat unit. Additional MS/MS measurements demonstrated that the end group is methylphenol and the repeat groups are di-methylphenol. Some modified oligomers caused by the methylation or di-methylation of the repeat unit were also identified. Although the polymer is only present at a trace level in the used stripper, these combined analytical methods provided the means to qualify the stripper solution through the identification and structural determination of the polymer.

광산폐수 속의 중금속의 분석과 특성 (Analysis and Characteristics of Heavy Metals in Mines Waste Water)

  • 이경호
    • 동굴
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    • 제92호
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    • pp.9-18
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    • 2009
  • A number of closed metal mines act as point sources of contamination on nearby streams, soils and plants in our country. The contamination of twelve decomposed samples had earned from nine closed metal mines had been evaluated by TEA-3000. The contents of heavy metal with ion fraction exchange and carbonate fraction forms had been showed that the speciation of heavy metals represented with easy solubility, mobility and bioavailable of plants, and in case of sulfide compounds and organic residuals forms are related with the speciation of metals which may be stable forms because of strong bindable capacity. Also heavy metals elements in mosts of mines got with relative stable within crystal lattice, but results of trace element analyser showed that, in the most of tailings from mine areas, large portions of concentration of heavy metals were explained as stable from, sulfides/ organics and residual. In tailing from Imchun mines, the concentrations extracted by water were relatively high as compared with other mine areas whose total concentrations were very high because of large quantities of exchangeable ions and carbonates and low soil pH. Danger Index (D.I.) suggested in this study was based on the cumulative concentrations of step 1 and 2 from the result of trace element analyser. When the soil pH was considered, this index became better indicator to determine the priority for the remediation of mine area.

Toxic Trace and Earth Crustal Elements of Ambient PM2.5 Using CCT-ICP-MS in an Urban Area of Korea

  • Lee, Jin-Hong;Jeong, Jin-Hee;Lim, Joung-Myung
    • Environmental Engineering Research
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    • 제18권1호
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    • pp.3-8
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    • 2013
  • Collision cell technology-inductively coupled plasma-mass spectrometry (CCT-ICP-MS) was used to measure the concentrations of approximately 19 elements associated with airborne PM2.5 samples that were collected from a roadside sampling station in Daejeon, Korea. Standard reference material (SRM 2783, air particulate on filter media) of the National Institute of Standards and Technology was used for the quality assurance of CCT-ICP-MS. The elemental concentrations were compared statistically with the certified (or recommended) values. The patterns of distribution were clearly distinguished between elements with their concentrations ranging over four orders of magnitude. If compared in terms of enrichment factors, it was found that toxic trace elements (e.g., Sb, Se, Cd, As, Zn, Pb, and Cu) of anthropogenic origin are much more enriched in PM2.5 samples of the study site. To the contrary, the results of the correlation analysis showed that PM2.5 concentrations can exhibit more enhanced correlations with the elements (e.g., Fe, K, Si, and Ti) arising from earth's crust. The findings of strong correlations between PM2.5 and the elements of crustal origin may be directly comparable with the dominant role of those species by constituting a major fraction of even PM2.5 as well as PM10 at the roadside area.

Studies on Solvent Extraction and Flotation Technique Using Metal-Dithizone Complexes(II). Determination of Trace Elements in Water Samples by Solvent Sublation

  • 김영상;최윤석;최희선
    • Bulletin of the Korean Chemical Society
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    • 제19권10호
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    • pp.1036-1042
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    • 1998
  • The preconcentration and determination of trace elements in water samples were studied by a solvent sublation utilizing dithizonate complexation. After metal dithizonates were formed, trace amounts of cadmium, cobalt, copper and lead were floated and extracted into small volume of a water-immiscible organic solvent on the surface of sample solution and determined in the solvent directly by GF-AAS. Several experimental conditions as formation condition of metal-dithizonate complexes, pH of solution, amount of dithizone, stirring time, the type and amount of surfactants, N2 bubbling rate and so on were optimized for the complete formation and effective flotation of the complexes. And also four kinds of light solvents were compared each other to extract the floated complexes, effectively. After the pH was adjusted to 4.0 with 5 M HNO3, 8.0 mL of 0.05% acetone solution of dithizone was added to 1.00 L water sample. The dithizonate complexes were flotated and extracted into the upper methyl isobutylketone (MIBK) layer by the addition of 2.0 mL 0.2% ethanolic sodium lauryl sulfate solution and with the aid of small nitrogen gas bubbles. And this solvent sublation method was applied to the analysis of real water samples and good results of more than 85% recoveries were obtained in spiked samples.

퇴적물 내 석영의 광여기 루미네선스 특성과 미량원소 조성 (Trace Element Compositions and Optically Stimulated Luminescence Characteristics of Sedimentary Quartz)

  • 정기영;최정헌;길영우
    • 한국광물학회지
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    • 제23권4호
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    • pp.357-365
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    • 2010
  • 석영의 광여기 루미네선스(OSL)를 이용한 제4기 퇴적물의 연대측정이 최근 널리 적용되고 있다. 그러나 모든 석영시료가 OSL 연대측정에 적합하지는 않다는 사실도 잘 알려져 있다. OSL 연대측정의 신뢰도를 향상시키고 적용범위를 넓히기 위해서는 석영시료별로 다양한 OSL 신호 특성의 원인에 대한 광물학적 규명이 필요하다. 본 연구는 그러한 광물학적 연구의 일환으로 전혀 다른 지질 및 지표 환경에서 채취한 퇴적물 시료로부터 분리한 석영을 대상으로 OSL 신호특성 분석과 레이저삭마 유도결합플라즈마질량분석(LA-ICP-MS)을 이용한 미량원소 조성분석을 실시하였다. OSL 신호분석 결과, 석영시료는 연대 측정에 적합한 신호특성을 갖는 시료와 부적합한 시료로 명확히 분리할 수 있었다. 미량원소조성분석 결과, Al (평균 73~267 ppm)과 Ti (평균 61~248 ppm)의 함량이 가장 높았으며, 그 외 Li, Mg, Cr, Mn, Fe 등이 40 ppm 미만으로 함유되어 있었다. 석영 시료간 OSL 특성의 명확한 차이에도 불구하고, 그에 상응하는 미량원소함량의 뚜렷한 차이는 발견할 수 없었다. 이는 시료별로 다양한 OSL 신호 특성이 미량원소가 아닌 석영의 다른 광물학적 원인에 기인되었을 가능성을 시사하지만, 향후 보다 많은 시료 분석으로 확인되어야 한다.

Validation of Bulk Analysis with Simulated Swipe Samples Containing Ultra-Trace Amounts of Uranium and Plutonium Using MC-ICP-MS

  • Lim, Sang Ho;Han, Sun-Ho;Park, Jong-Ho;Park, Ranhee;Lee, Min Young;Park, Jinkyu;Lee, Chi-Gyu;Song, Kyuseok
    • Mass Spectrometry Letters
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    • 제6권3호
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    • pp.75-79
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    • 2015
  • Suitable analytical procedures for the bulk analysis of ultra-trace amounts of uranium and plutonium have been developed using multi-collector inductively coupled mass spectrometry (MC-ICP-MS). The quantification and determination of the isotopic ratios of uranium and plutonium in three simulated swipe samples, a swipe blank, and a process blank were performed to validate the analytical performance. The analytical results for the simulated swipe samples were in good agreement with the certified values, based on the measurement quality goals for the analysis of bulk environmental samples recommended by the International Atomic Energy Agency (IAEA)

스마트 안전도시 플랫폼 구축을 위한 드론 시스템의 분석 및 설계 (Analysis and Design of Dron System for Smart Safety-City Platform Construction)

  • 조병호
    • 한국인터넷방송통신학회논문지
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    • 제20권4호
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    • pp.93-99
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    • 2020
  • 드론 기술의 발전으로 감시, 재난사고 예방 및 구호 등 공공임무 수행에도 지능화된 드론 활용이 급속히 늘어날 것으로 본다. 드론이 스마트 안전도시 플랫폼에 구축에 사용되기 위해서는 목표물 탐지 및 추적기술, 드론비행 시에 비행 조정 및 장애물 회피기능, 착륙지점 탐지 및 제어 기능 등의 주요 기술 구현이 필요하다. 드론 시스템 은 기술적 파급효과가 크고 신기술 분야의 산업화를 촉진한다. 본 논문에서는 이와 같은 드론 개발을 위하여 객체지향 분석/설계 방법을 이용한 요구사항 분석 및 플로우차트, 화면 설계 등을 보여여줌으로 효과적인 드론 시스템의 소프트웨어 분석 및 설계 방법을 제시하고자 한다.

도.토기의 화학조성-경주 황남대총 출토 도.토기를 중심으로 (The scientific analysis of potteries excavated from Kyong-ju relics-In terms of potsherds excavated from Wangkyong, Walsung, Hwangnam great tomb)

  • 홍종욱;문환석;황진주;조남철
    • 보존과학연구
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    • 통권20호
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    • pp.91-120
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    • 1999
  • This paper presents the results of investigation on crystal, firing temperature and trace elements analysis of fragments 4~8 centriesexcavated from Kyong ju historical sites such as Wang kyong,Walsung, Hwangnam great tomb by application of optical microscope, neutron activation analysis and X-ray diffraction. Temper analysis of clay for identification of local or foreign production; Trace elements is not presented a unique chemical composition. That’s data have to be treated a statistical process in order to normalize. The results followed ;(1) Firing temperature could be estimated $700^{\circ}C$ on some softness pottery at Walsung and most of hardness others are $1,000^{\circ}C$ to $1,200^{\circ}C$.(2) Crystal structures are divided into three kinds of mineralogical composition(Quartz, Mullite, Feldspar).(3) Considering of the results of statistical data, chemical composition of Walsung is more similarly Wang kyong than Hwangnam great tomb.

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부채널 분석에 안전한 하드웨어 이진 스칼라 곱셈 알고리즘에 대한 단일 파형 비밀 키 비트 종속 공격 (Key Bit-dependent Attack on Side-Channel Analysis-Resistant Hardware Binary Scalar Multiplication Algorithm using a Single-Trace)

  • 심보연;강준기;한동국
    • 정보보호학회논문지
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    • 제28권5호
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    • pp.1079-1087
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    • 2018
  • 타원 곡선 암호 시스템의 주요 연산이 스칼라 곱셈 알고리즘은 부채널 분석에 취약함이 보고되어 왔다. 특히 알고리즘이 수행되는 동안 소비되는 전력 패턴 및 방출되는 전자파 패턴을 활용하는 부채널 분석에 취약하다. 이에 다양한 대응 기법이 연구되어 왔으나 데이터 종속 분기 유형, 중간 값에 따른 통계 특성 또는 데이터 간의 상호 관계 기반 공격에 대한 대응 기법 등 주 연산에 대한 대응 기법만 연구되어 왔을 뿐 비밀 키 비트 확인 단계에 대한 대응 기법은 연구되지 않았다. 이에 본 논문에서는 하드웨어로 구현된 이진 스칼라 곱셈 알고리즘에 대한 단일 파형 비밀 키 비트 종속 공격을 수행하여 전력 및 전자 파형을 이용하여 100% 성공률로 비밀 스칼라 비트를 찾을 수 있음을 보인다. 실험은 차분 전력 분석 대응 기법이 적용된 $Montgomery-L{\acute{o}}pez-Dahab$ ladder 스칼라 곱셈 알고리즘[13]을 대상으로 한다. 정교한 사전 전처리가 필요하지 않고 단일 파형만으로도 공격이 가능한 강력한 공격으로 기존 대응 기법을 무력화 시킬 수 있다. 따라서 이에 대한 대응 기법을 제시하고 이를 적용해야 함을 시사한다.