• Title/Summary/Keyword: 스펙트럼 분리법

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Differences in Structural Characteristics and Eu(III) Complexation for Molecular Size Fractionated Humic Acid (분자량별 분류에 따른 휴믹산의 구조적 특성 및 Eu(III)과의 착물 반응 특성 비교에 대한 연구)

  • Shin, Hyun-Sang;Rhee, Dong-Seok;Kang, Kihoon
    • Analytical Science and Technology
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    • v.14 no.2
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    • pp.159-166
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    • 2001
  • A humic acid(HA, Aldrich Co) sample was subjected to ultrafiltration for molecular size fractionation and three fractions of different nominal size($F_1$: 1,000-10,000 daltons; $F_2$: 10,000-50,000 daltons; $F_3$: 100,000-300,000 daltons) were obtained. The structural characteristics of the size-fractionated HA were analyzed using their IR and solid state C-13 NMR spectral data, and the carboxylate group contents of the humic acids were determined using their pH titration data. The $^7F_0-{^5}D_0$ excitation spectra of Eu(III) complexes of the size-fractionated mgHA in aqueous solution were acquired($[Eu(III)]=1.0{\times}10^{-4}mol\;L^{-1}$, $(HA)=470-970mg\;L^{-1}$) at pH 5.0 using a pulsed tunable laser system, in which metal binding properties of the size-fractionated HA were elucidated and compared on another. Characterization of the IR and C-13 NMR spectral data indicated that the fraction($F_3$) with molecules of larger size were primarily aliphatic, while the fractions($F_1$, $F_2$) with smaller molecules of less than 50,000 daltons were predominantly aromatic. Titration data were consistent with an increase in the number of carboxylate groups per unit mass as molecular size became smaller. The $^7F_0-{^5}D_0$ excitation spectral data of Eu(III)-humate complexes showed that the peak maxima on these spectra were shifted toward lower energies with increasing molecular size of HA, indicating the higher degree of bindings of the Eu in the molecules of larger size. We also discussed the relationship of the lower energy shifts of the maximum peaks with increasing the molecular size of HA with the structural differences of the size-fractionated HA.

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A Photoreduction of Phenanthrenequinone by ESR and TRESR Spectroscopy(I)-Solvent Effect on Hyperfine-Splitting Constant of Radicals (ESR 및 TRESR 分光法에 의한 Phenanthrenequinone의 光環元反應(I). Radical의 超微細分離常數에 미치는 溶媒效果)

  • Daeil Hong;Chang Jin Kim
    • Journal of the Korean Chemical Society
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    • v.37 no.3
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    • pp.271-278
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    • 1993
  • The hyperfine splitting constants of phenanthrenequinone anion radical have been determined for the solution of triethylamine with 2-propanol, 2-pentanol or benzene by cwESR and time-resolved ESR methods. The radical anion was produced by photolysis using a pulsed excimer laser. The resulting hyperfine splitting constant A$_{H1}$ and A$_{H2}$ are 1.662, 0.378 in 2-propanol, 1.602, 0.361 in 2-pentanol and 1.518 in benzene respectively. The hyperfine coupling constants decrease with the decreasing of polarity of the mixed solvent. The tendency of the variation depends on the polarity of the solvents, thus, making it in impossible to observe the magnetic equivalent proton in a mixed solvent of nonpolar benzene. Particularly, time-resolved ESR spectrum of triethylamine radical (TEA${\cdot}$) has been observed in 0.15∼0.30 ${\mu}s$ from the solvent of 3 : 1 with 2-pentanol and triethylamine. Thus from the results of solvent effect, we can suggest that the identification of the unstable short-lived spin polarized phenanthrenequinone anion radical(*PQ${\cdot}^-$) proceed through photochemistry.

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Direct determination of gadolinium in urania-gadolinia nuclear fuels by inductively coupled plasma atomic emission spectrometry (유도결합플라스마 원자방출분광법을 이용한 UO2-Gd2O3 핵연료 중 가돌리늄 분석)

  • Choi, Kwang-Soon;Suh, Moo-Yul;Lee, Chang-Heon;Han, Sun-Ho;Jee, Kwang-Yong
    • Analytical Science and Technology
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    • v.20 no.2
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    • pp.131-137
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    • 2007
  • The urania-gadolinia fuels were dissolved with nitric acid. The analytical conditions of ICP-AES for the direct determinations of gadolinium in the uranium matrices without separation process were investigated. Based on the effect of uranium on gadolinium intensity, the best wavelength for gadolinium was 336.223 nm. The relative deviation of two methods, direct and indirect measurements with anion exchange chromatography, was less than 5 %. Therefore it was possible for this procedure directly to measure 5~10 wt.% of gadolinium in urania-gadolinia fuels without separation by ICP-AES.

Feasibility of near-infrared spectroscopic observation for traditional fermented soybean production (전통 메주 제조과정에 있어서 근적외 모니터링 가능성 조사)

  • Jeon, Jae Hwan;Lee, Seon Mi;Cho, Rae Kwang
    • Food Science and Preservation
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    • v.24 no.1
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    • pp.145-152
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    • 2017
  • In this study, near infrared (NIR) spectroscopy known as a non-destructive analysis technique was applied to investigate peptide cleavage and consequent release of amino acids in soybean lumps as affected by its moisture content and incubation time during fermentation at 25 for 3 weeks. The NIR spectra of the soybean lump semi-dried and soaked in saline water showed that absorption intensity around 1,400 nm originating from hydrogen bonds of water decreased and absorption band shifted to 1,430 nm as moisture content decreased during incubation at 25 for 3 weeks. In addition, absorption around 2,050 nm which was assigned to amino groups increased as incubation time increased. NIR spectra data from 1,000 to 2,250 nm showed higher accuracy in the discriminant analysis between outside and inside parts of fermented soybean lumps than visible spectra result. NIR spectroscopy for the amino acid and moisture contents in traditional fermented soybean lumps showed relatively good accuracy with the multiple correlation coefficient ($R^2$) of 0.91 and 0.81, respectively, and root mean square error of cross validation (RMSECv) of 0.23 and 0.83%, respectively, in partial least square regression (PLSR). These results indicate that NIR spectral observations could be applicable to control the fermentation process for preparation of soybean products.

추가 열처리 공정에 의한 GaN계 LED소자의 광학 및 전기적 특성에 대한 연구

  • Han, Sang-Hyeon;Lee, Jae-Hwan;Song, Gi-Ryong;Lee, Seong-Nam
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.309.1-309.1
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    • 2014
  • III-N계 기반의 광 반도체는 직접 천이형 넓은 밴드갭 구조를 갖고 있기 때문에 자외선에서 가시광을 포함한 적외선까지 포함한 폭 넓은 발광이 가능하여 조명 및 디스플레이 관련 차세대 광원으로 많은 관심을 받고 있다. 하지만 p형 GaN의 경우, 상온에서 도펀트로 사용되는 마그네슘(Mg)이 수소(H)와 결합하여 보상 효과를 나타내기 때문에 높은 정공농도를 갖기에 어려움이 있다고 알려져 있다. 따라서, 대부분의 연구 그룹에서는 GaN계 LED 소자를 성장 후 rapid thermal annealing 공정이 요구되고 있고, 최근에는 박막 성장 후 반응로 내에서 자체적으로 열처리를 진행하고 있는 실정이다. 하지만, 열처리 조건은 LED 소자의 발광특성에 큰 영향을 주기 때문에 본 연구에서는 반응로에서 열처리가 된 LED 샘플에 대해 추가적인 열처리 공정의 유무에 따른 GaN계 LED소자의 광학적 및 전기적 특성에 대해 알아보고자 하였다. 금속유기화학증착법을 이용하여 c-면 사파이어 기판에 저온 GaN 완충층 및 $2.0{\mu}m$두께의 GaN 박막을 성장한 후, $3.0{\mu}m$두께의 n-형 GaN에피층과 InGaN/GaN 5주기의 양자우물구조를 형성하고 $0.1{\mu}m$두께의 p형 GaN층을 성장하였다. P-형 GaN층 성장 후 온도를 내리면서 $750^{\circ}C$, N2 분위기에서 5분간 Mg 활성화를 위한 열처리를 반응로에서 in-situ로 진행하였다. 그 후 급속열처리 장비에 장입하여 $650^{\circ}C$, N2 분위기에서 5분간 추가적인 열처리를 진행하여 추가 열처리 유무에 따른 LED소자의 특성을 분석하였다. 추가적인 열처리 유무에 따른 LED소자의 레이저 여기에 의한 포토루미네선스 스펙트럼과 전계발광 스펙트럼을 조사한 바, 포토루미네선스 스펙트럼의 경우 추가적인 열처리를 진행하였을 경우, 이전보다 발광 세기가 감소함을 나타내었다. 이는 추가적인 열처리에 의해 InGaN/GaN 활성층이 손상되었기 때문이라고 추측된다. 그러나 전계발광 스펙트럼에서는 활성층이 손상되었음에도 불구하고 전계 발광세기가 3배 가량 증가한 것을 확인할 수 있었다. 또한, 20 mA 인가 시 4.2 V 에서 3.7 V로 전압이 감소하였다. 상기 결과로 미루어 볼 때 열처리에 의한 InGaN/GaN 활성층 손상에도 불구하고 광 세기가 크게 증가한 것은 금속유기화학증착장치의 in-situ 열처리에 의한 Mg가 충분히 활성화되지 못하였고, 추가적인 열처리에 의하여 p형 GaN에서 Mg-H 복합체의 분리로 인한 Mg 활성화가 더욱더 효과적으로 이루어졌기 때문이라고 추측된다.

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Determination of Fission Products in Simulated Nuclear Spent Fuels by Cation.Anion Exchange Chromatography and Inductively Coupled Plasma Atomic Emission Spectrometry (양.음이온교환 크로마토그래피와 유도결합플라스마 원자방출분광법을 이용한 모의 사용후핵연료 중 핵분열생성물 분석)

  • Choi, Kwang Soon;Sohn, Se Chul;Pyo, Hyung Yeol;Suh, Moo Yul;Kim, Do Yang;Park, Yang Soon;Jee, Kwang Yong
    • Analytical Science and Technology
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    • v.13 no.4
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    • pp.446-452
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    • 2000
  • The simulated nuclear spent fuel (SIMFUEL) containing the platinum group elements which will not be dissolved in a nitric acid was completely dissolved with a acid digestion bomb. The metallic elements separated in the SIMFUEL were measured by inductively coupled plasma atomic emission spectrometry (ICP-AES). Because the peaks of metallic elements were spectrally interfered by uranium spectrum, uranium and metallic elements were separated by cation exchange resin for Mo, Pd, Rh and Ru and by anion exchange resin for Ba, Ce, La, Nd, Rh, Sr, Y and Zr, respectively. The recovery of Mo, Pd, Rh and Ru after separation by cation exchange chromatography found to be 99-103% and anion exchange separation showed 96.5-107% of recovery except Y with the simulated solution whose concentration was similar to the spent nuclear fuel. The relative standard deviation of this method showed 1.3-6.7% in the SIMFUEL whose concentrations of metallic elements were between several $10^2-10^3$ppm.

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Bioanalytical method validation for determination of arsenic speciation in dog plasma using HPLC-ICP/MS (Dog 혈장 중 HPLC-ICP/MS를 이용한 비소 화학종 분석법 검증)

  • Kim, Jong-Hwan;Kwon, Young Sang;Shin, Min-Chul;Kim, Su Jong;Seo, Jong-Su
    • Analytical Science and Technology
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    • v.29 no.5
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    • pp.234-241
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    • 2016
  • The approach presented in this article refers to the bioanalytical method validation for the detection and quantitative determination of arsenic species including arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA) and monomethylarsonic acid (MMA) in dog plasma by high-performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC-ICP/MS). The arsenic species were separated using an agilent As speciation column by a mobile phase of 2 mM sodium phosphate monobasic, 0.2 mM ethylenediaminetetraacetic acid disodium salt dehydrate, 10 mM sodium acetate, 3 mM sodium nitrate and 1 % ethyl alcohol at pH 11 (adjusted with 1M NaOH). The method validation experiment was obtained selectivity, linearity, accuracy, precision, matrix effect, recovery, system suitability, dilution integrity and various stabilities. All calibration curves showed good linearity (R2>0.999) within test ranges. The lower limit of quantitation (LLOQ) was 5 ng/mL for As(III), As(V) and DMA, and 20 ng/mL for MMA. The system suitability and dilution values were within 6.5 % and 7.7 %. Subsequently, the developed and validated HPLC-ICP/MS method was also successfully applied to determine the arsenic speciation in dog plasma samples, and the recoveries for the spiked samples were in the range of 91.5–102.2 %. Therefore, this method could be applied to the evaluation of arsenic exposure, health effect assessment and other bio-monitoring studies in biological samples.

Study on noise prediction by classification of noise sources of a tip-jet driven rotor (팁젯 로터의 소음원 구분을 통한 소음 예측 기법 연구)

  • Ko, Jeongwoo;Kim, Jonghui;Lee, Soogab
    • The Journal of the Acoustical Society of Korea
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    • v.37 no.2
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    • pp.83-91
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    • 2018
  • The noise sources of a tip-jet driven rotor can be separated by rotor blade noise and jet noise. The rotor blade noise consists of thickness noise, loading noise, nonlinear quadrupole noise, and jet noise is divided into nozzle momentum noise and jet radiation noise. The flow analysis for the prediction of rotor blade noise is performed by CFD (Computational Fluid Dynamics) analysis, and the noise source of the rotor blade noise is identified by simultaneously applying the permeable and impermeable surface based FW-H (Ffowcs Williams-Hawkings) acoustic analogy. The nozzle momentum noise is obtained by permeable surface FW-H, and jet radiation noise is predicted by using empirical method for the fixed-wing jet. Both of jet noises use nozzle exit condition for noise analysis. The accuracy of the technique is verified based on the noise measurements of the tip-jet driven rotor, and the unique noise characteristics of the tip-jet driven rotor is confirmed by spectrum analysis.

Comparative Photoluminescence Study of Single-Layer MoS2 Annealed in Hydrogen and Vacuum

  • Ryu, Ye-Jin;Park, Min-Gyu;Ryu, Sun-Min
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.195.1-195.1
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    • 2014
  • 최근 반자성 물질인 $MoS_2$를 수소 기체 속에서 열처리하게 되면 약한 강자성이 유발된다는 연구가 보고되었다. 본 연구에서는 강자성 발현을 수반하는 물리적 및 화학적 변화를 이해하기 위해서 단일층 $MoS_2$에 대한 라만분광 및 광발광 연구를 수행하였다. 기계적 박리법을 이용하여 $MoS_2$ 결정으로부터 단일층 및 이중층 $MoS_2$를 분리하여 $SiO_2/Si$ 기판에 전사한 후, $200^{\circ}C{\sim}500^{\circ}C$ 영역의 특정 온도에서 1시간 동안 열처리하였다. 배경 기체가 열처리 도중 $MoS_2$에 미치는 영향을 이해하기 위하여 수소 속 반응을 진공 상태와 비교하였다. 라만 스펙트럼에서는 큰 변화가 없었으나, 광발광의 세기는 수소 속 반응 후에 감소하고 진공 속 반응 후에는 증가하는 대조적인 결과를 보였다. AFM 측정으로부터는 열처리 후에 $MoS_2$ 표면에 뚜렷한 변화가 일어나지 않는다는 사실을 확인하였다. 본 발표에서는 수소와 진공 조건에서 관찰된 상이한 광발광 특성과 그래핀/$SiO_2/Si$에서 관찰된 p-형 도핑과의 상관관계를 설명하고자 한다.

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A study on surface photovoltage characteristics of $IN_{0.03}Ga_{0.97}AS/GaAs$ epilayer ($IN_{0.03}Ga_{0.97}AS/GaAs$에피층의 표면 광전압 특성에 관한 연구)

  • 최상수;김기홍;배인호
    • Journal of the Korean Vacuum Society
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    • v.10 no.1
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    • pp.81-86
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    • 2001
  • We have investigated surface photovoltage characteristics of InGaAs grown by metalorganic chemical vapor deposition (MOCVD) method on semi-insulating GaAs. The splitted SPV signals from the substrate and epilayer were observed. The band gap energy of InGaAs was about 1.376 eV, The In composition(x) was determined by Pan's composition formula. The photovoltage gradually decreases with increasing frequency. This is because the transfer of charge from the surface states reduces. From the temperature dependent SPV measurement, we obtained Varshni and temperature coefficients. In spectrum of etched sample at 300 K, the 'A' peak below $E_o(GaAs)$ is related with residual impurity during sample growth.

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