• Title/Summary/Keyword: X-ray spectrometry

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Impurity analysis and acid leaching purification of silica minerals (실리카광물의 산침출 정제와 불순물 분석법 연구)

  • Lee, Kil Yong;Yoon, Yoon Yeol;Cho, Soo Young;Chae, Young-Bae
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.516-523
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    • 2007
  • Purification of silica mineral has been investigated by acid leaching of pulverized silica. A series of studies has been carried out on the effect of leaching silica powder as a function of the leaching time at the constant temperature of $80^{\circ}C$ in oxalic acid, aqua regia, and two mixed acids of HF/HCl, $HF/HNO_3$. The impurities of silica and leachantes were measured by neutron activation analysis (NAA), inductively coupled plasma atomic emission spectrometry (ICP-AES), atomic absorption spectrometry, x-ray fluorescence (XRF) method and wet analysis (WA). Certain metals, such as sodium, calcium, iron, aluminium and titanium, have been found in concentrations of hundreds or even thousands of mg/kg. Comparison of purification processes of silica and analytical methods of impurities in the silica was conducted in this study.

Gemological Comparison between Gwangdong Tektite and Baikdusan Obsidian (텍타이트와 흑요석의 보석학적 특징비교 - 중국 광동 텍타이트와 백두산 흑요석을 중심으로 -)

  • Kim, Won-Sa
    • Journal of the Mineralogical Society of Korea
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    • v.20 no.3
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    • pp.181-191
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    • 2007
  • The gemological charateristics of Gwangdong tektites and Baikdusan obsidians were investigated, using microscopy, density and refractive index measurements, X-ray fluorescence spectrometry, Inductively Coupled Plasma Mass spectrometry, X-ray powder diffraction, and electron microprobe analysis. The Gwangdong tektites and Baikdusan obsidians are both black in colour and slightly trans-lucent with various shades of brown when cut into a few mm thick. Both the materials yield conchoidal fracture on broken surface. The tektites occur as tear-drop shapes, ranging from 4 to 10 cm long, and in spheres, from 3 to 5 cm in diameter. On the surface numerous shallow pits up to 3 mm in diameter are present. Mohs' hardness and specific gravity are 5 to 5.5 and 2.66, respectively. The tektites are singly refractive, with an refractive index of 1.51. Numerous spherical air bubbles are randomly scattered throughout the tektites, and silica-rich glass inclusions are occasionally seen. X-ray powder diffraction analysis verifies that they are non-crystalline. The Baikdusan obsidians show very similar properties to those of the Gwangdong tektites, especially in hardness, amorphous nature and fracture. Nevertheless, the Baikdusan obsidian can readily be distinguished from the Gwangdong tektites by refractive index ($1.49{\sim}1.50$), specific gravity (2.67 to 2.68), and inclusions (absence of bubbles and presence of sanidine and magnetite crystals).

A study on development of CRM by means of XRF analysis for fine ceramic ($BaTiO_3$) (티탄산바륨 소재의 XRF 분석용 CRM 개발에 관한 연구)

  • Kim, Young Man;Jeong, Chan Yee;Lim, Chang Ho;Song, Taek Yong;Lee, Dong Soo
    • Analytical Science and Technology
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    • v.9 no.4
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    • pp.382-391
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    • 1996
  • In this study, 12 different chemical species of fine ceramic($BaTiO_3$) were synthesized as the standard materials for the fast and accurate measurements of X-ray fluorescence spectrometry. Samples were diluted to sixteen times with the filling compound ($Li_2B_4O_7+LiBO_2$) in order to remove the matrix effect, and to get the convenient storage and homogeneity of ingredients. The matrix effects among the ingredients were corrected by the empirical coefficient method based on the Lucas-Tooth and Price model. The standard curve on 12 standard materials containing 15 elements were obtained by using X-ray fluorescence spectrometry at three different laboratories. The correlation factors of BaO, PbO, SrO, $Fe_2O_3$, $La_2O_3$, $SnO_2$, ZnO, $ZrO_2$, CaO indicated the relati vely good agreement over 0.995 among the three different laboratories. $SiO_2$ and $Al_2O_3$ showed the poor linearity because of their low fluorescence intensities.

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A Working Standard Technique far Determination of Interference Correction Factors and Preparation of Standard Materials for CHIME Dating (CHIME 연대 측정의 간섭 보정 계수 결정과 표준 물질의 준비를 위한 실험실 표준법)

  • Cho, Deung-Lyong;Kato, Takenori;Suzuki, Kazuhiro
    • Journal of the Korean earth science society
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    • v.27 no.5
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    • pp.521-527
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    • 2006
  • The EPMA analysis for CHIME dating requires standard materials, which include nuclear fuel materials that are rare and sensitive to handle. Any laboratory that does not meet these standards has had difficulties adopting the CHIME dating method. We have developed a working standard technique for CHIME dating to prepare standard materials without use of nuclear fuel materials. Mineral samples, such as small pieces of monazite that are homogeneous in X-ray intensities, are calibrated using well-characterized primary standards in one laboratory. Once this procedure is done, they can be readily usable as working standards in the other laboratories, only with measurement of X-ray intensities. This method is applicable in preparing standard materials for both chemical compositions and determination of X-ray interference correction factors, and it is independent from chemical composition of mineral standard.

Studies on X-Ray Fluorescence Analysis of Sulfide Ores by Solution Technique (I). Analysis of Sulfur (용액법을 이용한 황화광석의 X-선 형광분석에 관한 연구 (제1보). 황의 분석)

  • Young-Sang Kim;Kee-Chae Park
    • Journal of the Korean Chemical Society
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    • v.26 no.4
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    • pp.229-234
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    • 1982
  • Using solution technique, sulfur in the sulfide ore was indirectly determined by X-ray fluorescence spectrometry. The sample was dissolved with the mixed solution of B$r_2$ and HN$O_3$, and Si$O_2$, a major constituent, was repelled from the solution by HF treatment several times, B$a^{2+}$ solution was added to the solution to precipitate the S$O^4_{2-}$ ion as BaS$O_4$. Measuring the fluorescent X-ray intensity of excess Ba2+ ion in the filtrate, the content of sulfur in the original ore was back-calculated. Comparing the results by this method with the gravimetric method, the mean difference was ${\pm}1.7%$ in the range of 20 to 40% of sulfur content and the method was tolerably reproducible.

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A Study on X-Ray Fluorescence Analysis of Ta$_2O_5,\;Nb_2O_5,\;SnO_2$ and ZrO$_2$ in Tin-slag Samples (희석 파라미터법에 의한 주석슬랙중 Ta$_2O_5,\;Nb_2O_5,\;SnO_2$ 및 ZrO$_2$의 X-선형광분석에 관한 연구)

  • Young Sang Kim
    • Journal of the Korean Chemical Society
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    • v.29 no.3
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    • pp.265-270
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    • 1985
  • Ta$_2$O$_5$, Nb$_2$O$_5$, SnO$_2$ and ZrO$_2$ in tin-slag samples were determined by X-ray fluorescence spectrometry using the dilution parameter method and the analytical results were compared with the data obtained by standard calibration curve method. Tin-slag samples and one standard sample having very similar composition to the tin-slags were diluted with a proper diluent (La$_2$O$_3$) to the ratio of 1: 1, 1 : 2, 1 : 3 and 1 : 4. After measuring the X-ray intensities of original and diluted samples, the values of dilution parameters were calculated by using the dilution parameter equation. Without any calibration curve, the analytical results were calculated from the equation including the dilution parameter term. The results were in good agreement with the reference data by the standard calibration curve method.

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DEGRADATION OF Zn$_3$$N_2$ FILMS PREPARED BY REACTIVE RF MAGNETRON SPUTTERING

  • Futsuhara, Masanobu;Yoshioka, Katsuaki;Takai, Osamu
    • Journal of the Korean institute of surface engineering
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    • v.29 no.5
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    • pp.563-569
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    • 1996
  • Degradation of $Zn_3N_2$ films is studied by using several analytical techniques. Polycrystalline $Zn_3N_2$ films prepared by reactie rf magnetron sputtering are kept in the air. Electrical and optical properties are measured by using van der Pauw technique and double-beam spectrometry. Structure and chemical bonding states are studied by X-ray diffraction(XRD), Fourier transfer infrared ray spectroscopy(FT-IR) and X-ray photoelectron specroscopy (XPS). Significant differences are observed in optical properties between the degraded film and the ZnO film. XRD analysis reveals that the degraded film contains very small ZnO grains because very weak and broad ZnO peaks are observed. XPS and FT-IR measurements reveal the formation of $Zn(OH)_2$ in the degraded film. The existence of N-H bonds in degraded films is exhibited from the N 1s spectra. $Zn_3N_2$ change into the mixture of ZnO, $Zn(OH)_2$ and an ammonium salt.

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Synthesis of $Zn(BH_4)_2$ powders by mechanochemical reaction and study of thermal decomposition behavior (기계 화학적 반응법을 이용한 $Zn(BH_4)_2$ 분말의 합성과 열분해 특성)

  • Jeon Eun;Jo Yeong Hwan
    • 한국전기화학회:학술대회논문집
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    • 2005.07a
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    • pp.373-378
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    • 2005
  • [ $Zn(BH_4)_2$ ] ($8.4\;wt\%$ theoretical hydrogen storage capacity) powders have been successfully synthesized by mechanochemical reaction from mixtures of $ZnCl_2$ and $NaBH_4$ powders in a 1:2 molar ratio in different times. $$ZnCl_2\;+\;2NaBH_4\rightarrow\;Zn(BH_4)_2\;+\;2NaCl\;(1)$$ $Zn(BH_4)_2$ powders were characterized by X-ray diffractometry(XRD), and Furier Transform Infrared spectrometry(FT-IR). The thermal stabilities of $Zn(BH_4)_2$ powders were studied by Differential scanning calorimetry(DSC), Thermogravimetry analysis(TGA), and Mass spectrometry(MS). $Zn(BH_4)_2$ can be tested for hydrogen evolution without further purification. The reaction to yield hydrogen is irreversible, the other products being compounds of Zn, and borane. $Zn(BH_4)_2$ thermally decomposes to release borane and hydrogen gas between about 85 and $150^{\circ}C$.

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Study of Self Texturing on ZnO:Al TCO surface for Thin-Film Solar Cell (박막태양전지용 ZnO:Al 투명전도막 표면 Self-Texturing 연구)

  • Oh, Kyoung Suk;Yoon, Soon Gil;Lee, Jeong Chul
    • 한국신재생에너지학회:학술대회논문집
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    • 2011.05a
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    • pp.127.2-127.2
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    • 2011
  • 본 연구에서는 RF Magnetron Sputtering System을 이용하여 ZnO계 투명전도막 증착시 Vaporization된 MeOH를 유입함으로써 박막증착과 동시에 표면의 Roughness를 제어하여 이에따른 전기적 특성 및 광학적 특성의 개선에 대하여 연구하였다. 실험방법으로 기존의 RF Magnetron Sputtering System에 Vaporization이 가능한 Ultrasonic을 이용하여 MeOH를 Vaporized시켜 MFC Controll을 통해 챔버에 유입하여 ZnO계 투명전도막의 박막증착과 동시에 표면 Texturing을 하였다. ZnO계 투명전도막의 박막증착시 Vaporized MeOH의 유입에 따른 광학적 특성변화를 UV-visible-nIR spectrometry로 조사하였으며, 전기적 특성 변화를 4-Point-Probe로 조사하였으며, 표면적 특성 변화를 Atomic Force Microscope(AFM), Scanning Electron Microscopy(SEM)를 조사하였으며, 박막의 결정성장특성 변화를 X-ray Diffraction(XRD)으로 조사하였으며, Vaporized MeOH 유입에 따른 박막의 성분분석을 Secondary Ion Mass Spectrometry (SIMS)로 조사함으로써 최적의 조건 및 공정을 확립하였다.

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고에너지 이온선을 이용한 분석 기술

  • 김효배;송종한;김희중
    • Journal of the Korean Magnetics Society
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    • v.6 no.2
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    • pp.122-129
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    • 1996
  • Fig. 1에서 보는 바와 같이 수 MeV의 에너지를 가진 입사이온이 고체 시료표면과 충돌했을 때 여러 가지의 상호작용과 과정들이 일어난다. 입사 아온이 표적원자의 원자가전자나 내각전자와 상호작용을 하였을 때 원자를 여기시키거나 이온화시키게 되며 입사 이온이 표적 핵과 매우 가까이 접근했을 때 입사이온과 표적 핵사이에 쿨롱상호작용이나 핵 상호작용이 일어나게 된다. 이러한 여러가지 상호작용의 결과들로부터 분석하고자 하는 시료의 성분, 구조, 상호작용 과정에 대한 정보를 얻을 수 있다. 이러한 고에너지 이온선을 이용한 분석기술로는 Fig. 1에서 보는 바와 같이 후방산란법(BS : Backscattering Spectrometry), 전방산란법(FRS : Forward Recoil Spectrometry), 핵반응법(NRA : Nuclear Reaction Analysis), 양성자여기X선검출법(PIXE : Proton Induced X-ray Emission)등과 이러한 방법들과 같이 조합하여 사용하는 이온 채널링(ion channeling)등이 있다. 본 해설에서는 이러한 분석법중에서도 널리 사용되고 있는 후방산란법과 이온 채널링에 대하여 주로 기술하고자 한다.

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