• 제목/요약/키워드: Microwave Plasma

검색결과 398건 처리시간 0.02초

HPLC-AFS를 이용한 해산물 중 비소 화학종 분리정량 (Quantification of Arsenic Species in Some Seafood by HPLC-AFS)

  • 정승우;이채혁;이종화;장봉기
    • 한국환경보건학회지
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    • 제47권5호
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    • pp.496-503
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    • 2021
  • Background: Considering the expenses of and difficulties in arsenic speciation by high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS), alternative measurement methods should be useful, especially for large-scale research and projects. Objectives: A measurement method was developed for arsenic speciation using HPLC-atomic fluorescence spectrometry (HPLC-AFS) as an alternative to HPLC-ICP-MS. Methods: Total arsenic and toxic arsenic species in some seafoods were determined by atomic absorption spectrometry coupled with hydride vapor generation (AAS-HVG) and HPLC-AFS, respectively. Recovery rate of arsenic species in seafood was evaluated by ultra sonication, microwave and enzyme (pepsin) for the optimal extraction method. Results: Limits of detection of HPLC-AFS for As3+, dimethylarsinate (DMA), monomethylarsonate (MMA) and As5+ were 0.39, 0.53, 0.60 and 0.64 ㎍/L, respectively. The average accuracy ranged from 97.5 to 108.7%, and the coefficient of variation was in the range of 1.2~16.7%. As3+, DMA, MMA and As5+ were detected in kelp, the sum of toxic arsenic in kelp was 40.4 mg/kg. As3+, DMA, MMA and As5+ were not detected in shrimp and squid, but total arsenic (iAS and oAS) content in shrimp and squid analyzed by AAS-HVG were 18.1 and 24.7 mg/kg, respectively. Conclusions: HPLC-AFS was recommendable for the quantitative analysis method of arsenic species. As toxic arsenic species are detected in seaweeds, further researches are needed for the contribution degree of seafood in arsenic exposure.

Aluminum in rocks: Optimized microwave-assisted acid digestion and UV-Vis spectrophotometric measurement

  • Nguyen Thanh-Nho;Thai Huynh-Thuc;Le-Thi Anh-Dao;Do Minh-Huy;Le-Thi Huynh-Mai;Le Quang-Huy;Nguyen-Thi Kim-Sinh;Nguyen Cong-Hau
    • 분석과학
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    • 제36권5호
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    • pp.216-223
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    • 2023
  • Aluminium (Al) is one of the major elements in rocks and its concentration can be varied, depending on different rock types as well as sources. The present study aimed to propose an analytical method based on the UV-Vis as a cheap, simple, and common instrument equipped in most laboratories for Al quantification in rocks after the microwave assisted acid digestion. The aluminone and 8-hydroxyquinoline were investigated for the colorimetric assay. The results show that the 8-hydroxyquinoline reagent was more favorable in terms of the minimized affects of the potential interferences present in the digested solutions, i.e., Fe3+, Si4+ and F-. The calibration curve was constructed from 0.10 mg/L to 3.00 mg/L with the goodness of linearity (R2 = 0.9996). The limits of detection and quantification (LOD and LOQ) were estimated, i.e., 0.029 mg/L and 0.087 mg/L, respectively. The 8-hydroxyquinoline was applied to real rock samples, demonstrating favorable precision (RSD = 0.34 %-1.8 %) and no remarkable differences were found compared to the inductively coupled plasma-mass spectrometry (ICP-MS) as a reference measurement approach.

ICP-AES를 이용한 황기 속에 함유된 원소의 성분 분석과 Chemometrics를 이용한 한약재의 원산지 규명 (Elemental Analysis in Astragali Radix by Using ICP-AES and Determination of the Original Agricultural Place of Oriental Medicine by Using a Chemometrics)

  • 강미라;이익희;전형;김용성;이상천
    • 분석과학
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    • 제14권4호
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    • pp.311-316
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    • 2001
  • 본 연구는 한약재 중 우리 나라의 여러 지역에서 재배되고 있는 황기를 선택하여 유도결합 플라스마 분광분석법(inductively coupled plasma-atomic emission spectroscopy ; ICP-AES)을 이용한 미량성분을 분석하여 principal component analysis(PCA)와 pattern recognition의 원리를 이용한 chemometrics Analysis로 한약재에 함유된 미량 금속 성분 함량에 의한 원산지 판별의 가능성을 조사하였다. 황기와 토양시료는 각각 $HNO_3$$H_2O_2$ 그리고 $HNO_3$와 HCl를 첨가하여 microwave oven을 사용하여 전처리 하였다. ICP-AES를 사용하여 황기와 황기를 재배한 토양 속에 들어 있는 미량 금속 성분으로는 Mg, Al, K, Ca, Ti, Mn, Fe, Cu, Zn, and Ba 등이 있으며 그 중 Al과 Fe 그리고 Zn과 Ti의 함량으로는 PCA와 pattern recognition을 이용하여 각 재백지의 황기와 토양간의 연계성을 살펴보았다. 그 결과 국내산 황기와 중국산 황기를 PCA 방법으로 원산지 판별이 가능하였으며 구례, 예천, 제천, 그리고 정선의 국내산 황기의 원산지 판별이 가능하였다.

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국내에서 유통 중인 채소류의 중금속 함량에 관한 연구 (Heavy Metal Contents of Vegetables from Korean Markets)

  • 유하영;정진주;최은주;강성태
    • 한국식품과학회지
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    • 제42권4호
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    • pp.502-507
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    • 2010
  • 본 연구에서는 시판중인 일부 채소류의 중금속 함량을 조사해 국외기준과 비교하고 그 안전성을 검증해보고자 하였다. 전국에서 재배되어 시중에서 유통되고 있는 채소류 15종 243건을 시료로 하였다. 시료의 분석방법은 습식분해법 중 microwave 법을 이용하였으며 납, 카드뮴, 비소, 크롬, 구리, 망간, 아연을 유도결합 플라즈마 분광기(inductively coupled plasma spectrometer, ICP)를 이용하여 분석하였다. 조사결과 채소류의 평균 함량(최소-최대함량, mg/kg)은 Pb, 0.0026(ND-0.0313); Cd, 0.0017(ND-0.0280), As, 0.0005(ND-0.0332); Cr, 0.0156(0.0010-0.1798); Cu, 0.3767(0.0556-1.3980); Mn, 3.0214(0.0182-26.4100); Zn, 3.5796(0.830-14.46)으로 나타났다. 본 연구를 통해 얻어진 결과들 중 납, 카드뮴, 비소는 기존 연구결과들과 비슷하거나 낮은 수준이었으며 크롬, 구리, 망간, 아연은 비슷한 수준으로 나타났다. 또한 조사한 품목의 주간 섭취량을 FAO/WHO에서 안전성 평가를 위해 설정한 PTWI와 PMTDI 기준과 비교한 결과 그 수준이 매우 낮아 우리나라에서 재배되는 이들 채소류로부터 섭취하는 중금속 양은 안전한 수준으로 판단되었다. 본 연구결과는 아직 세부기준이 설정되지 않는 채소류의 중금속 기준을 설정하는데 있어 참고 자료로 활용될 수 있을 것으로 기대된다.

초경합금에 나노결정질 다이아몬드 코팅 시 금속 중간층의 효과 (Effect of Metal Interlayers on Nanocrystalline Diamond Coating over WC-Co Substrate)

  • 나봉권;강찬형
    • 한국표면공학회지
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    • 제46권2호
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    • pp.68-74
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    • 2013
  • For the coating of diamond films on WC-Co tools, a buffer interlayer is needed because Co catalyzes diamond into graphite. W and Ti were chosen as candidate interlayer materials to prevent the diffusion of Co during diamond deposition. W or Ti interlayer of $1{\mu}m$ thickness was deposited on WC-Co substrate under Ar in a DC magnetron sputter. After seeding treatment of the interlayer-deposited specimens in an ultrasonic bath containing nanometer diamond powders, $2{\mu}m$ thick nanocrystalline diamond (NCD) films were deposited at $600^{\circ}C$ over the metal layers in a 2.45 GHz microwave plasma CVD system. The cross-sectional morphology of films was observed by FESEM. X-ray diffraction and visual Raman spectroscopy were used to confirm the NCD crystal structure. Micro hardness was measured by nano-indenter. The coefficient of friction (COF) was measured by tribology test using ball on disk method. After tribology test, wear tracks were examined by optical microscope and alpha step profiler. Rockwell C indentation test was performed to characterize the adhesion between films and substrate. Ti and W were found good interlayer materials to act as Co diffusion barriers and diamond nucleation layers. The COFs on NCD films with W or Ti interlayer were measured as less than 0.1 whereas that on bare WC-Co was 0.6~1.0. However, W interlayer exhibited better results than Ti in terms of the adhesion to WC-Co substrate and to NCD film. This result is believed to be due to smaller difference in the coefficients of thermal expansion of the related films in the case of W interlayer than Ti one. By varying the thickness of W interlayer as 1, 2, and $4{\mu}m$ with a fixed $2{\mu}m$ thick NCD film, no difference in COF and wear behavior but a significant change in adhesion was observed. It was shown that the thicker the interlayer, the stronger the adhesion. It is suggested that thicker W interlayer is more effective in relieving the residual stress of NCD film during cooling after deposition and results in stronger adhesion.

Pulsed ECR PECVD를 이용한 $SiO_x$ 박막의 성장 및 특성분석 (Growth and Chrarcterization of $SiO_x$ by Pulsed ECR Plasma)

  • 이주현;정일채;채상훈;서영준;이영백
    • 한국재료학회지
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    • 제10권3호
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    • pp.212-217
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    • 2000
  • 일반적으로 TFT(thin film transistor)의 유전체막으로 실리콘 질화막($Si_3$$N_4$)이나 실리콘 산화막(SiO$_2$)을 $200-300^{\circ}C$의 온도에서 증착을 하게 되는데 본 연구에서는 비정질 실리콘과 유전체막 사이의 계면 특성 특히 계면의 거칠기를 향상시키기 위해서 기존의 증착법이 아니라 비정질 실리콘(a-Si:H)과 산소 ECR 플라즈마의 반응에 의한 산화 막의 성장법을 시도했는데, 이때 기판은 의도적으로 가열하지 않았으며 특히 본 연구에서는 기존의 시도와는 달리 ECR 플라즈마를 형성할 때 마이크로파 전력에 pulse를 가하는 방법을 최초로 시도했고, 계면에 불순물의 혼입을 최대한으로 줄이기 위해서 진공을 파괴하지 않은 상태로 산화막을 연속적으로 성장시키는 방법을 이용했다. Pulse를 가했을 경우에는 pulse를 가하지 않은 경우에 비해서 화학양론적 측면, 유전상수, 산화막의 표면 평탄도 등에서 우수한 산화막이 성장했으며, 특히 비정질 실리콘과 유전체막 사이의 계면 특성을 반영하는 산화막의 표면 평탄도가 1/3정도로 획기적으로 줄어들었다.

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RF and Optical properties of Graphene Oxide

  • 임주환;;윤형서;오주영;정영모;박형구;전성찬
    • 한국재료학회:학술대회논문집
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    • 한국재료학회 2012년도 춘계학술발표대회
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    • pp.68.1-68.1
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    • 2012
  • The best part of graphene is - charge-carriers in it are mass less particles which move in near relativistic speeds. Comparing to other materials, electrons in graphene travel much faster - at speeds of $10^8cm/s$. A graphene sheet is pure enough to ensure that electrons can travel a fair distance before colliding. Electronic devices few nanometers long that would be able to transmit charge at breath taking speeds for a fraction of power compared to present day CMOS transistors. Many researches try to check a possibility to make it a perfect replacement for silicon based devices. Graphene has shown high potential to be used as interconnects in the field of high frequency electrical devices. With all those advantages of graphene, we demonstrate characteristics of electrical and optical properties of graphene such as the effect of graphene geometry on the microwave properties using the measurements of S-parameter in range of 500 MHz - 40 GHz at room temperature condition. We confirm that impedance and resistance decrease with increasing the number of graphene layer and w/L ratio. This result shows proper geometry of graphene to be used as high frequency interconnects. This study also presents the optical properties of graphene oxide (GO), which were deposited in different substrate, or influenced by oxygen plasma, were confirmed using different characterization techniques. 4-6 layers of the polycrystalline GO layers, which were confirmed by High resolution transmission electron microscopy (HRTEM) and electron diffraction analysis, were shown short range order of crystallization by the substrate as well as interlayer effect with an increase in interplanar spacing, which can be attributed to the presence of oxygen functional groups on its layers. X-ray photoelectron Spectroscopy (XPS) and Raman spectroscopy confirms the presence of the $sp^2$ and $sp^3$ hybridization due to the disordered crystal structures of the carbon atoms results from oxidation, and Fourier Transform Infrared spectroscopy (FTIR) and XPS analysis shows the changes in oxygen functional groups with nature of substrate. Moreover, the photoluminescent (PL) peak emission wavelength varies with substrate and the broad energy level distribution produces excitation dependent PL emission in a broad wavelength ranging from 400 to 650 nm. The structural and optical properties of oxygen plasma treated GO films for possible optoelectronic applications were also investigated using various characterization techniques. HRTEM and electron diffraction analysis confirmed that the oxygen plasma treatment results short range order crystallization in GO films with an increase in interplanar spacing, which can be attributed to the presence of oxygen functional groups. In addition, Electron energy loss spectroscopy (EELS) and Raman spectroscopy confirms the presence of the $sp^2$ and $sp^3$ hybridization due to the disordered crystal structures of the carbon atoms results from oxidation and XPS analysis shows that epoxy pairs convert to more stable C=O and O-C=O groups with oxygen plasma treatment. The broad energy level distribution resulting from the broad size distribution of the $sp^2$ clusters produces excitation dependent PL emission in a broad wavelength range from 400 to 650 nm. Our results suggest that substrate influenced, or oxygen treatment GO has higher potential for future optoelectronic devices by its various optical properties and visible PL emission.

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증착 압력이 a-Si:H막의 전도도와 광학적 특성에 미치는 영향 (Effect of Deposition Pressure on the Conductivity and Optical Characteristics of a-Si:H Films)

  • 전법주;정일현
    • 공업화학
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    • 제10권1호
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    • pp.98-104
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    • 1999
  • 본 연구에서는 ECR플라즈마 화학증착법을 이용하여 반응기내 압력의 변화에 따라 수소화된 무정형 실리콘막을 증착하고 박막내 수소의 함량과 결합구조 및 전기적 특성을 조사하였다. 일반적인 CVD에 의해 제조된 a-Si:H막은 증착속도가 증가할수록 광감도는 감소하지만 ECR플라즈마의 경우 증착속도가 증가할수록 광감도가 향상되었다. 마이크로파 출력과 사일렌/수소 희석비, 반응기내 압력등이 동일한 실험 조건에서 증착시간에 따른 막의 두께는 선형적으로 증가하고 막내에 함유된 수소의 농도는 일정하지만, 반응시간이 짧은 경우 막내에 $SiH_2$결합이 SiH결합보다 많이 형성되어 광전도도를 저하시킬 수 있다. 반응기내 압력이 증가함에 따라 박막내에 SiH결합이 증가하여 광학 에너지 갭을 줄여 광전도도를 향상시킬 수 있었으나 암전도도의 증가로 광감도는 감소하였다. 따라서 양질의 박막을 얻기 위해서는 압력이 낮고 수소기체의 양이 적은 조건에서 성장시켜야 한다.

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저온 증착된 불소도핑 주석 산화 박막의 광학적·전기적 특성 (Optical and Electrical Properties of Fluorine-Doped Tin Oxide Prepared by Chemical Vapor Deposition at Low Temperature)

  • 박지훈;전법주
    • 한국재료학회지
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    • 제23권9호
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    • pp.517-524
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    • 2013
  • The electrical and optical properties of fluorine-doped tin oxide films grown on polyethylene terephthalate film with a hardness of 3 using electron cyclotron resonance plasma with linear microwave of 2.45 GHz of high ionization energy were investigated. Fluorine-doped tin oxide films with a magnetic field of 875 Gauss and the highest resistance uniformity were obtained. In particular, the magnetic field could be controlled by varying the distribution in electron cyclotron deposition positions. The films were deposited at various gas flow rates of hydrogen and carrier gas of an organometallic source. The surface morphology, electrical resistivity, transmittance, and color in the visible range of the deposited film were examined using SEM, a four-point probe instrument, and a spectrophotometer. The electromagnetic field for electron cyclotron resonance condition was uniformly formed in at a position 16 cm from the center along the Z-axis. The plasma spatial distribution of magnetic current on the roll substrate surface in the film was considerably affected by the electron cyclotron systems. The relative resistance uniformity of electrical properties was obtained in film prepared with a magnetic field in the current range of 180~200A. SEM images showing the surface morphologies of a film deposited on PET with a width of 50 cm revealed that the grains were uniformly distributed with sizes in the range of 2~7 nm. In our experimental range, the electrical resistivity of film was able to observe from $1.0{\times}10^{-2}$ to $1.0{\times}10^{-1}{\Omega}cm$ where optical transmittance at 550 nm was 87~89 %. These properties were depended on the flow rate of the gas, hydrogen and carrier gas of the organometallic source, respectively.

동위원소희석 질량분석법에 의한 혈액 중 Cd, Pb 성분의 측정 : 국제공동분석 (Determination of Cd and Pb in Human Blood by Isotope Dilution Inductively Coupled Plasma Mass Spectrometry : International Comparison)

  • 박창준;서정기;이상화
    • 분석과학
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    • 제9권2호
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    • pp.145-160
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    • 1996
  • 한국표준과학연구원 무기분석그룹에서는 1994년과 1995년도에 카나다 퀘백주 독성센터에서 실시한 혈액시료의 국제공동분석프로그램에 참여하였다. 이 프로그램의 목적은 생체시료에 있는 미량의 독성원소에 대해 참여하는 각국 실험실의 재현성과 정확도의 평가이다. 본 실험실에서는 3개 농도수준의 Pb과 Cd이 함유된 혈액시료를 동위원소희석 유도결합플라스마 질량분석법으로 분석하였다. 0.5mL의 혈액시료에 농축 동위원소를 첨가하고 질산 2mL와 함께 마이크로파 가압분해장치에서 분해한 후 약 10mL로 묽힌 후 ICP-MS에 주입하였다. 각국 실험실에서 보고한 Pb과 Cd의 농도를 나타내고 서로 비교하였으며 본 실험실에서 보고한 값은 모두 목표값에 매우 가까운 값을 얻었다.

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