• Title/Summary/Keyword: X선회절분석

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Asbestos Determination of Some Domestic Building-Materials Using X-ray diffraction (국내 건축자재에 함유된 석면의 함량에 대한 X-선회절분석 연구)

  • Hwang, Jin-Yeon;Lee, Hyo-Min;Oh, Ji-Ho;Park, Gi-Nam
    • Journal of the Mineralogical Society of Korea
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    • v.24 no.2
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    • pp.119-131
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    • 2011
  • The asbestos contents in some representative building materials were analyzed using JIS (Japanese Industrial Standard) X-ray diffraction (XRD) method. The changes in mineral composition during analysis process and problems in JIS method were also examined. XRD analysis of some representative domestic building materials used for roof, wall, ceiling, and floor indicates that slate have the highest asbestos content having 6.87~6.93% of chrysotile. Other building materials analyzed in this study also have 1.35~3.98% of chrysotile contents. The XRD analysis results of asbestos contents in some domestic building materials are presented in this study. This method is very effective for the asbestos content evaluation of building materials according to newly modified asbestos content regulation (Law of Industrial Safety and Health, 2007-26) that limits asbestos content less than 0.1% by Ministry of Employment and Labor. Small amount of tremolite as well as chrysotile were also observed in some samples. With consideration of crystal shape, contents and geological occurrence, it is considered that tremolite is an associated mineral of chrysotile and is not intentionally added. Complemental analyses with optical microscope and SEM/EDS are also necessary because XRD method cannot distinguish asbestiform from non-asbestiform. The XRD method applied in this study is very effective in the asbestos content analysis of building materials, specially building materials showing high asbestos concentration in residues due to the high loss rate with ashing and acid dissolution procedure.

Quantitative Determination of Cristobalite Content in Diatomite and Filtered Food (규조토와 여과식품 중 크리스토발라이트의 정량분석)

  • Jeong, Gi Young
    • Journal of the Mineralogical Society of Korea
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    • v.32 no.4
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    • pp.313-321
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    • 2019
  • Diatomite is a silicic porous sedimentary rock composed of diatom frustules, used for filtration aid, filler, absorbent, abrasive, carrier, insulator, and fertilizer. During the calcination of diatomite to improve physical properties for filtration-aid application, amorphous silica is transformed to cristobalite. X-ray diffraction and scanning electron microscopy studies were carried out for 17 diatomite samples, showing that 16 diatomite samples contain cristobalite in the range of 6~100 %. Concentration of respirable cristobalite in air is regulated as harmful substances, but the residual cristobalite in food is treated as generally safe substance. The determination procedure of cristobalite content in food was established for managing food safety. Calibration curve of cristobalite filtered on silver membrane were obtained by X-ray diffraction. The lower limit of quantification was evaluated as 2.7 mg. The cristobalite was not detected in the analyses of selected food samples using the established procedure.

Quantitative X-ray Diffraction Analysis of Synthetic Mineral Mixtures Including Amorphous Silica using the PONKCS Method (PONKCS 방법을 이용한 비정질 실리카 함유 인공광물혼합시료의 정량 X-선회절 분석)

  • Chon, Chul-Min;Lee, Sujeong;Lee, Sung Woo
    • Journal of the Mineralogical Society of Korea
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    • v.26 no.1
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    • pp.27-34
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    • 2013
  • X-ray powder diffraction is one of the most powerful techniques for qualitative and quantitative analysis of crystalline compounds. Thus, there exist a number of different methods for quantifying mineral mixtures using X-ray diffraction pattern. We present here the use of Rietveld and PONKCS (partial or no known crystal structure) methods for quantification of amorphous and crystallized mineral phases in synthetic mixtures of standard minerals (amorphous silica, quartz, mullite and corundum). Pawley phase model of amorphous silica was successfully built from the pattern of 100 wt% amorphous silica and internal standard-spiked samples by PONKCS approach. The average of absolute bias for quantities of amorphous silica was 1.85 wt%. The larger bias observed for lower quantities of amorphous silica is probably explained by low intensities of diffraction pattern. Averages of absolute bias for minerals were 0.53 wt% for quartz, 0.87 wt% for mullite and 0.57 wt% for corundum, respectively. The PONKCS approach achieved improved quantitative results compared with classical Rietveld method by using an internal standard.

Mineralogy of Sepiolite from the Ulsan serpentine Mine (울산 사문석광산에서 산출하는 세피오라이트의 광물학적 연구)

  • 황진연
    • Journal of the Mineralogical Society of Korea
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    • v.4 no.2
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    • pp.108-118
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    • 1991
  • 경남 울산군 농소면의 울산사문석광산에서 세피오라이트(sepiolite)가 발견되었다. 그래서 이 세피오라이트시료에 대해 X-선회절분석, 열분석, 적외선분광분석, 투과전자현미경관찰 및 화학분석을 행하여 그 결과를 기술하였다. 본 세피오라이트는 사문암과 염기성암체와의 접촉부에 발달된 열극충진상 세맥에서 산출된다. 이 세맥내에서 많은 암편들이 포함되어 있는데, 그 기질부분은 회백색을 띠며 연질이고 부드러운 가죽같은 느낌을 준다. 이 기질부분이 거의 순수한 세피오라이트로 구성되어 있다. X-선회절분석의 결과로부터 이 광물시료가 결정도가 높은 {{{{ alpha }}-세피오라이트에 해당된다는 것이 밝혀졌다. 이 세피오라이트의 화학성분은 Mg를 많이 함유하는 일반적인 세피오라이트와 유사하였다. 산상 및 광물학적 특성으로 볼 때 이 세피오라이트는 열수용액에서 직접 침전하여 형성된 것으로 사료된다.

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A Study on the X-ray Diffractometry of Rock Minelals (주요암석광물(主要岩石鑛物)에 대(對)한 X 선적(線的) 특성(特性)에 관(關)한 연구(硏究))

  • Choi, Dae Ung;Hwan, Kyung Sun;Shin, Jae Sung
    • Korean Journal of Soil Science and Fertilizer
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    • v.6 no.4
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    • pp.199-204
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    • 1973
  • This work was carried out to establish the norm for identifying the rock forming minerals by the X-ray diffraction analysis with powdered rock samples. This study covered the eleven major rocks in Korea. The results are summarized as follows. 1. The norm for identifying the rock forming minerals based on X-ray diffraction data was established. 2. It was found that the rock forming minerals could be identified by the norm.

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Crystal Chemistry and Fine-scale Paragenesis of Chuncheon Nephrite (춘천 연옥의 결정화학과 미시적 공생관계에 관한 연구)

  • 노진환;최진범
    • Journal of the Mineralogical Society of Korea
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    • v.13 no.2
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    • pp.96-114
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    • 2000
  • 춘천 연옥은 색깔에 따라 세가지 유형 (연녹색, 암녹색, 및 회색 연옥)으로 구분되고 이들은 각기 서로 다른 조직과 조성을 나타낸다. 연녹색 연옥이 이중에서 가장 일반적인 유형이다. 연옥은 주로 극미립의 연옥질 투각섬석으로 구성되고 여기에 미량의 휘석, Mg-녹니석 및 방해석이 불순물로서 수반된다. 연옥질 투각섬석 결정들은 그 폭이 5$\mu\textrm{m}$ 이하의 극미립질 침상 결정형을 이루며 서로 치밀하게 얽혀있는 연옥 특유의 조직을 나타낸다. 주사전자현미경 하에서 (110)의 벽개면의 발달이 현저하고, 주사탐침현미경 하에서는 벽개면을 가로지르는 방향으로 특징적인 조선이 나타나는 것이 특징이다. 연옥질 투각섬석은 투과전자현미경 하에서 흔히 단쇄형과 복쇄형이 결합한 3중쇄형 격자가 복쇄형의 투각섬석 구조 내에서 불규칙적으로 협재되는 혼성격자 구조가 발달하는 것이 특징이다. 드물지만 5중쇄형 격자와 4중쇄형 격자도 관찰되는데, 이 같은 불규칙한 격자 혼재상은 회색 연옥에서 보다 현저한 경향을 보인다. 이와 같은 혼성격자 구조형의 존재는 춘천 연옥이 열역학적으로 비평형 상태에서 형성되었음을 시사하는 것으로 여겨진다. 리트벨트법에 의한 구조검증을 통해서 구해진 연옥질 투각섬석들의 격자상수 값들은 X-선회절의 경우, a=9.837(1)~9.9804(4)$\AA$, b=18.046(2)~18.062(1)$\AA$. c=5.2765(7)~5.2803(3)$\AA$, $\beta$=104.717(9)~104.786(3)$^{\circ}$로 계산되었다. 이에 비해서 중성자 회절법에 의해서 측정되 격자 상수 값은 a=9.8841(6)~9.8933(7)$\AA$, b=18.1429(7)~18.161(2)$\AA$, c=5.3024(3)~5.3060(7)$\AA$, $\beta$=104.698(7)~104.771(4)$^{\circ}$로서 X-선회절에 의한 값들과 약간의 차이를 보인다. 연옥질 투각섬석은 Ca에 대한 Mg의 치환에 의해 M(4) 자라의 크기가 작아지면서 b축의 단위포도 함께 줄어드는 결정화학적 특징을 나타낸다. 이는 중성자 회절분석에 의해서 구해진 M(4)의 자리점유율과 M(4)-O의 원자간 거리에 의해서도 확인된다. 그러나 연옥질 투각섬석에 대한 리트벨트법에 구조검증 결과는 연옥의 유형별 미시적 광물상과 혼성격자 구조형의 특징에 별다른 연계성이 없는 것으로 나타났다.

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Phase Constitution of the Palladium and Tellurium System (팰래듐과 테루리움계의 상평형 연구)

  • ;G.Y.Chao, L.J.Cabri
    • Korean Journal of Crystallography
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    • v.1 no.2
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    • pp.66-75
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    • 1990
  • The Pd-Te system has been investigated by differential thermal analysis, X-ray diffration, electron probe microanalysis and reflected light microscopy. New phase relations in 0-50at% Te portion of the binary system are proposed. Eight binary phases exist in the system:Pd17Te4, Pd20Te7.PdsTe3, P477e3, P497e4, P637e2, PeTe and PaTe2. Of these, P677e3 is a newly reported phase. P4177e4 is cubic, space group Fd3c, with a=12.678(5)A. The X-ray powder data of PdsTe3, indexed on an orthorhombic cell, give a= 12.843(3), b=15.126(3), c: 11.304(2)A and those of PdTTe.1, indexed on a monoclinic cell, give a=7.444(1), b= 13.918(2) , c=8.873(2)A. p =92.46(2). Some physical and optical properties of synthetic phases in the system are also reported.

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Synthesis and characterization of LiCoO2 thin film by sol-gel process (Sol-gel법에 의한 LiCoO2 박막의 합성과 특성평가)

  • Roh, Tae-Ho;Yon, Seog-Joo;Ko, Tae-Seog
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.24 no.3
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    • pp.94-98
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    • 2014
  • $LiCoO_2$ thin film has received diverse attention as cathodes material of thin-film micro-batteries. In this study, $LiCoO_2$ thin films were synthesized on Au substrates by sol-gel spin coating method and an annealing process. Their structures were studied using X-ray diffraction and Raman Spectroscopy. The particle morphologies of these thin films were observed by Scaning electron microscope. From the results of X-ray diffractometry and Raman Spectroscopy analyses, it was found that as-grown films had the structure of spinel (LT-$LiCoO_2$) and layered-Rock-salt (HT-$LiCoO_2$) at $550^{\circ}C$ and $750^{\circ}C$ respectively. The annealed films at $650^{\circ}C$ were presumed to be the mixed state of these two types. Throlugh the scanning electron microscope, It was estimated that the particle size in as-grown films at $750^{\circ}C$, were larger crystilline particle than in those at the other lower temperature and well distributed in the film.