• Title/Summary/Keyword: X-ray Diffractometer

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Characteristics and Preparation of Calcium Acetate from Butter Clam (Saxidomus purpuratus) Shell Powder by Response Surface Methodology (반응표면분석법을 이용한 개조개(Saxidomus purpuratus) 패각분말로부터 가용성 초산칼슘의 제조 및 특성)

  • Lee, Hyun Ji;Jung, Nam Young;Park, Sung Hwan;Song, Sang Mok;Kang, Sang In;Kim, Jin-Soo;Heu, Min Soo
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.6
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    • pp.888-895
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    • 2015
  • For effective utilization of butter clam shell as a natural calcium resource, the optimal conditions for preparation of calcium acetate (BCCA) with high solubility were determined using response surface methodology (RSM). The polynomial models developed by RSM for pH, solubility, and yield were highly effective in describing the relationships between factors (P<0.05). Increased molar ratio of calcined powder (BCCP) from butter clam shell led to reduction of solubility, yield, color values, and overall quality. Critical values of multiple response optimization to independent variables were 2.70 M and 1.05 M for acetic acid and BCCP, respectively. The actual values (pH 7.04, 93.0% for solubility and 267.5% for yield) under optimization conditions were similar to predicted values. White indices of BCCAs were in the range of 89.7~93.3. Therefore, color value was improved by calcination and organic acid treatment. Buffering capacity of BCCAs was strong at pH 4.88 to 4.92 upon addition of ~2 mL of 1 N HCl. Calcium content and solubility of BCCAs were 20.7~22.8 g/100 g and 97.2~99.6%, respectively. The patterns of fourier transform infrared spectrometer and X-ray diffractometer analyses from BCCA were identified as calcium acetate monohydrate, and microstructure by field emission scanning electron microscope showed an irregular form.

On the Properties of TLCP/PBT Blends Prepared by In Situ Polymerization in PBT Solution (In situ 중합에 의해서 제조된 TLCP/PBT 블렌드의 특성 연구)

  • Choi, Jae-Kon;Park, Il-Soo;Kim, Sun;Choi, Yoo-Sung;Lee, Eung-Jae;Jo, Byung-Wook
    • Elastomers and Composites
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    • v.39 no.3
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    • pp.217-227
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    • 2004
  • A new thermotropic liquid crystalline polymer(TLCP) containing a triad aromatic ester type mesogenic unit and butylene terephthalate unit(BT) in the main chain was synthesized by polycondensation reaction. The TLCP synthesized showed nematic mesophasic behavior and its transition temperature from solid to mesophase was $260^{\circ}C$. The TLCP/PBT blends were prepared by in-situ polymerization in PBT solution and characterized by differential scanning calorimeter(DSC), thermogavimetric analyzer(TGA), scanning electron microscope(SEM), x-ray diffractometer(XRD), and dynamic mechanical thermal analyze, (DMTA). The blends showed well dispersed TLCP phases with domain sizes $0.05{\sim}0.2{\mu}m$ in the PBT matrix. As the increasing TLCP content from 5 to 20 wt%, ${\Delta}Hm$ values of pure PBT in the blend were increased because TLCP acts as a nucleating agent in the PBT matrix. The mechanical properties of the blends depended on the TLCP contents because the TLCP acted effectively as a reinforcing material in the PBT matrix. The blends showed good interfacial adhesion between the TLCP phase and PBT matrix.The blends prepared by in-situ polymerization showed higher mechanical properties and well dispersed TLCP domains than those of the blends prepared by melt blending.

Properties and Fabrication of Glass Fiber using Recycled Slag Materials (슬래그 재활용 원료를 이용한 유리섬유 제조 및 특성)

  • Lee, Ji-Sun;Kim, Sun-Woog;Ra, Yong-Ho;Lim, Tae-Young;Lee, Youngjin;Jeon, Dae-Woo;Kim, Jin-Ho
    • Korean Journal of Materials Research
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    • v.28 no.12
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    • pp.763-768
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    • 2018
  • In this study, glass fibers are fabricated via a continuous spinning process using manganese slag, steel slag, and silica stone. To fabricate the glass fibers, raw materials are put into an alumina crucible, melted at $1550^{\circ}C$ for 2 hrs, and then annealed at $600^{\circ}C$ for 2 hrs. We obtain a black colored glass. We identify the non-crystalline nature of the glass using an XRD(x-ray diffractometer) graph. An adaptable temperature for spinning of the bulk marble glass is characterized using a high temperature viscometer. Spinning is carried out using direct melting spinning equipment as a function of the fiberizing temperature in the range of $1109^{\circ}C$ to $1166^{\circ}C$, while the winder speed is in the range of 100rpm to 250rpm. We investigate the various properties of glass fibers. The average diameters of the glass fibers are measured by optical microscope and FE-SEM. The average diameter of the glass fibers is $73{\mu}m$ at 100rpm, $65{\mu}m$ at 150rpm, $55{\mu}m$ at 200rpm, and $45{\mu}m$ at 250rpm. The mechanical properties of the fibers are confirmed using a UTM(Universal materials testing machine). The average tensile strength of the glass fibers is 21MPa at 100rpm, 31MPa at 150rpm, 34MPa at 200rpm, and 45MPa at 250rpm.

Surface Coating Treatment of Phosphor Powder Using Atmospheric Pressure Dielectric Barrier Discharge Plasma (대기압 유전체배리어방전 플라즈마를 이용한 형광체 분말 코팅)

  • Jang, Doo Il;Ihm, Tae Heon;Trinh, Quang Hung;Jo, Jin Oh;Mok, Young Sun;Lee, Sang Baek;Ramos, Henry J.
    • Applied Chemistry for Engineering
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    • v.25 no.5
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    • pp.455-462
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    • 2014
  • This work investigated the hydrophobic coating of silicate yellow phosphor powder in the form of divalent europium-activated strontium orthosilicate ($Sr_2SiO_4:Eu^{2+}$) by using an atmospheric pressure dielectric barrier discharge (DBD) plasma with argon as a carrier and hexamethyldisiloxane (HMDSO), toluene and n-hexane as precursors. After the plasma treatment of the phosphor powder, the lattice structure of orthosilicate was not altered, as confirmed by an X-ray diffractometer. The coated phosphor powder was characterized by scanning electron microscopy, fluorescence spectrophotometry and contact angle analysis (CAA). The CAA of the phosphor powder coated with the HMDSO precursor revealed that the water contact angle increased from $21.3^{\circ}$ to $139.5^{\circ}$ (max. $148.7^{\circ}$) and the glycerol contact angle from $55^{\circ}$ to $143.5^{\circ}$ (max. $145.3^{\circ}$) as a result of the hydrophobic coating, which indicated that hydrophobic layers were successfully formed on the phosphor powder surfaces. Further surface characterizations were performed by Fourier transform infrared spectroscopy and X-ray photoelectron spectrometry, which also evidenced the formation of hydrophobic coating layers. The phosphor coated with HMDSO exhibited a photoluminescence (PL) enhancement, but the use of toluene or n-hexane somewhat decreased the PL intensity. The results of this work suggest that the DBD plasma may be a viable method for the preparation of hydrophobic coating layer on phosphor powder.

모재/중간층/박막의 H/E ratio 구배에 따른 Cr계 경질 박막의 기계적 특성에 관한 연구

  • Kim, Hoe-Geun;Song, Myeon-Gyu;Lee, Sang-Yul
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2018.06a
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    • pp.135-135
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    • 2018
  • 천이금속 질화물 코팅은 우수한 기계적 특성들로 인해 공구 코팅으로 많이 사용 되어왔다. 그 중에서도 특히 Cr계 경질 코팅은 높은 경도와 낮은 표면조도, 우수한 마찰특성 등 뛰어난 기계적 특성을 나타내므로 공구 코팅으로의 적용 가능성이 크다. 그러나 최근 공구산업의 발전으로 인해 공구가 더욱 가혹한 환경에서 사용됨에 따라, 공구의 수명을 향상시키고 보호하기 위해 코팅의 높은 밀착력이 요구되고 있으며, 모재와 코팅 사이에 중간층을 합성함으로써 공구의 밀착력을 향상시키는 연구가 활발히 진행되고 있다. 이전 연구에서 모재/중간층/코팅간의 경도와 탄성계수 비율(H/E ratio)의 구배가 코팅의 밀착력에 큰 영향을 미치는 것으로 확인되었다. 그러므로, WC 모재와 Cr계 코팅의 중간값의 H/E ratio를 갖는 중간층의 합성을 통해 코팅의 밀착력을 향상시킬 수 있을 것으로 판단된다. 본 연구에서는, 코팅의 밀착력을 향상시키기 위해 다양한 중간층을 증착한 CrZrN, CrAlN 코팅을 비대칭 마그네트론 스퍼터링 장비를 이용하여 합성하였다. 모재로는 디스크 형상의 WC-6wt.%Co 시편을 사용하였고 Cr, Zr, Si, Al single 타겟을 이용하여 Cr, CrN, CrZrN, CrZrSiN 등의 중간층이 증착된 코팅을 합성했다. 코팅의 합금상, 경도 및 탄성계수, 미세조직 및 조성, 표면 조도을 확인하기 위해 X-ray diffractometer (XRD), Fischer scope, field-emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDS), atomic force microscopy를 사용하였고, 코팅의 밀착 특성을 분석하기 위해 scratch tester와 optical microscopy (OM)를 이용하였다. 코팅의 내열성을 확인하기 위해 코팅을 furnace에 넣어 공기중에서 500, 600, 700, 800, 900, $1,000^{\circ}C$로 30분 동안 annealing 한 후에 nano-indentation을 사용하여 경도를 측정하였다. CrZrN 및 CrAlN 코팅을 나노 인덴테이션으로 분석한 결과, 모든 코팅의 경도(33.4-35.8 GPa)와 탄성계수(384.1-391.4 GPa)는 중간층의 종류에 상관없이 비슷한 값을 보인 것으로 확인됐다. 그러나, 코팅의 마찰계수는 중간층의 종류에 따라 다른 값을 보였다. CrZrN 코팅의 경우 CrN 합금상 중간층을 갖을 때 가장 낮은 값을 보였으며, CrAlN 코팅의 경우 CrN/CrZrSiN 중간층을 증착하였을때 마찰계수는 0.34로 CrZrN 중간층을 증착하였을 때(0.41)에 비해 낮은 값을 보였다. 또한, 코팅의 마모율 및 마모폭도 비슷한 경향을 보인 것으로 보아, CrN/CrZrSiN 중간층을 합성한 CrAlN 코팅의 내마모성이 상대적으로 우수한 것으로 판단된다. 코팅의 밀착력의 경우도 마찰계수와 비슷한 경향을 보였다. 이것은 중간층의 H/E ratio가 코팅의 내마모성에 미치는 영향에 의한 결과로 사료된다. H/E ratio는 파단시의 최대 탄성 변형율로써, 모재/중간층/코팅의 H/E ratio 구배에 따라 코팅 내의 응력의 완화 정도가 변하게 된다. WC 모재 (H/E=0.040)와 CrAlN 코팅(H/E=0.089) 사이에서 CrN, CrZrSiN 중간층의 H/E ratio는 각각 0.076, 0.083으로 모재/중간층/코팅의 H/E ratio 구배가 점차 증가함을 확인 할 수 있었고, 일정 응력이 지속적으로 가해지면서 진행되는 마모시험중에 CrN과 CrZrSiN 중간층이 WC와 CrAlN 코팅 사이에서 코팅 내부의 응력구배를 완화시키는 역할을 함으로써 CrAlN 코팅의 내마모성이 향상된 것으로 판단된다. 모든 코팅을 열처리 후 경도 분석 결과, CrN/CrZrSiN 중간층을 증착한 CrAlN 코팅은 $1,000^{\circ}C$까지 약 28GPa의 높은 경도를 유지한 것으로 확인 되었고, 이는 CrZrSiN 중간층 내에 존재하는 SiNx 비정질상의 우수한 내산화성에 의한 결과로 판단된다.

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The Antimicrobial Effect of Water Soluble Chitosan (수용성 키토산의 항균효과)

  • Jung, Byung-Ok;Lee, Young-Moo;Kim, Jae-Jin;Choi, Young-Ju;Jung, Kyung-Ja;Kim, Je-Jung;Chung, Suk-Jin
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.660-665
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    • 1999
  • Structure of water soluble chitosan (WSC) was confirmed by Fourier transform infrared spectrometer (FT-IR), X-ray diffractometer and thermal analyser. The viscosity average molecular weight of WSC ranged from $3.0{\times}10^{4}$ to $4.5{\times}10^{4}$. Using the WSC having viscosity average molecular weight of $3.0{\times}10^{4}$, the antimicrobacterial effects against microorganism and oral microorganism showed 81.7% and 80.6% for Staphyloccus aureus and Bacillus subtilis, respectively, while the anitmicrobacterial effect exhibited 100% and 73.8% against Streptococcus mutans and Streptococcus sanguis, respectively. Therefore it is concluded that WSC is more effective against oral microorganism that microorganism in terms of antimicrobacterial effects. WSC sample with the viscosity average molecular weight of $4.5{\times}10^{4}$ exhibited a half of the antimicrobacterial effect of the low MW sample, indicating that the WSC with low MW was better than that with high MW. Chitin and chitosan showed a drastic decrease of acidity from pH 7.0 to 4.9 after 8 minute incubation time and reached an equilibrium after that. WSC, however, restrained pH of the sample from lowering up to about 16 minutes of incubation and reached an equilibrium after that. WSC obviously showed a buffering effect against pH change.

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EFFECT OF HYDROGEN PEROXIDE CONCENTRATION ON THE WHITENING AND PHYSICAL PROPERTIES OF HYDROXYAPATITE DISCS (Hydrogen Peroxide 농도와 적용시간이 Hydroxyapatite Discs의 미백과 물리적 성질에 미치는 영향)

  • Yang, Yeon-Mi;Lee, Doo-Cheol;Baik, Byeong-Ju;Kim, Jae-Gon;Shin, Jeong-Geun
    • Journal of the korean academy of Pediatric Dentistry
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    • v.34 no.1
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    • pp.1-12
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    • 2007
  • The purpose of this study was to evaluate the effect that various concentration and application time of hydrogen peroxide had on tooth whitening and physical properties. The hydroxyapatite (HA) discs of $12mm({\Phi}){\times}1.2mm(t)$ in dimensions were made by compression $(100kg/cm^2)$ and sintering (at $1350^{\circ}C$ for 2 hours) All specimens were polished sequentially with '240 through '2000 emery paper and one side of each specimen was polished finally with $0.3{\mu}m$ alumina paste. The discs were placed in sterile whole stimulated saliva overnight at $37^{\circ}C$ in order to form an in vitro pellicle layer. Then the discs were rinsed with distilled water and soaked into staining broth at $37^{\circ}C$ for 7 days. These stained specimens were bleached with hydrogen peroxide according to the change of concentration $(3{\sim}30%)$ and application time ($3{\sim}10$ days). The specimens were analyzed with a spectrophotometer, X-ray diffractometer (XRD), scanning electron microscope (SEM), surface roughness tester, microhardness tester and biaxial flexural strength. The results of present study can be summarized as follows : 1. The bleaching effect was increased with the increased concentration and the extended application time of hydrogen peroxide. 2. The surface roughness was significantly increased from the specimen bleached with 15% hydrogen peroxide for 10 days and with 30% for 7 and 10 days respectively (p<0.05). 3. The changes of crystal phase observed by XRD between before and after bleaching weren't shown of any difference, but microporous structure of surface observed by SEM was shown of increase with the increased concentration and the extended application. 4. The biaxial flexural strength was significantly decreased from bleaching of specimen with 30% hydrogen peroxide for 7 and 10 days respectively (p<0.05) 5. Microhardness was significantly decreased from bleaching with 15% hydrogen peroxide for 10 days and with 30% for 3, 7 and 10 days respectively (p<0.05). Although the tooth bleaching effect was greater when the high concentration was applied, further in vivo experiment will be needed to prove it's safety.

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A Mineralogical Study on the Arsenic Behavior in the Tailings of Nakdong Mine (낙동광산의 광미 내 비소 거동에 대한 광물학적 연구)

  • Lee, Woo-Chun;Cho, Hyen-Goo;Kim, Young-Ho;Kim, Soon-Oh
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.4
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    • pp.359-370
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    • 2009
  • Arsenic and heavy metals leached out as a result of oxidation of tailings exposed to the surface pose a serious environmental contamination of mine areas. This study investigated how arsenic behavior is controlled by a variety of processes, such as oxidation of sulfides and formation or alteration of secondary minerals, based on mineralogical methods. The study was carried out using the tailing samples obtained from Nakdong mine located in Jeongseongun, Gangwondo. After separating magnetic and non-magnetic minerals using pretreated tailing samples, each mineral sample was classified according to their colors and metallic lusters observed by the stereoscopic microscope. Subsequently, the mineralogical properties were determined using various instrumental analyses, such as x-ray diffractometer (XRD), energy dispersive spectroscopy (EDS), and electron probe micro analyzer (EPMA). The literature review confirmed that various ore minerals were identified in the Nakdong ore deposits. In this study, however, there were observed a few original ore minerals as well as secondary and/or tertiary minerals newly formed as a result of weathering including oxidation. In particular, we did not recognize pyrrhotite which has been known to originally exist in a large abundance, but peculiarly colloform-type iron (oxy)hydroxides were identified, which indicates most of pyrrhotite has been altered by rapid weathering due to its large reactivity. In addition, a secondary scorodites filling the fissure of weathered primary arsenopyrites were identified, and it is speculated that arsenic is immobilized through such a alteration reaction. Also, we observed tertiary iron (oxy)hydroxides were formed as a result of re-alteration of secondary jarosites, and it suggests that the environment of tailing has been changed to high pH from low pH condition which was initiated and developed by oxidation reactions of diverse primary ore minerals. The environmental change is mainly attributed to interactions between secondary minerals and parental rocks around the mine. As a result, not only was the stability of secondary minerals declined, but tertiary minerals were newly formed. As such a process goes through, arsenic which was immobilized is likely to re-dissolve and disperse into surrounding environments.

Inorganic-organic nano-hybrid; Preparation of Nano-sized TiO$_2$ Paste Trapped OMC Nano-emulsion and it's Application for Cosmetics (OMC Nano-emulsion을 포집하고 있는 Nano-TiO$_2$-Paste의 합성과 화장품의 응용)

  • Byung Gyu, Park;Jong Heon, Kim;Jin Hee, Im;Kyoung Chul, Lee
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.30 no.2
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    • pp.181-187
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    • 2004
  • Preparations of mesoporous materials using various templates and their applicability have been intensively investigated for many years. We studied on synthesizing mesoporous Ti02 with pores in which sensitive compounds having weak physico-chemical properties such as thermal or UV irradiation and low solubility in solvent are trapped. Prior to trapping OMC in the pores of mesoporous titania, OMC was nano-emulsified in O/W system using Lecithin. Thereafter the OMC was trapped in the pores of mesoporous titania using sol-gel method. Main focus of this work is to prepare OMC-trapped mesoporous titania and to trace the stability and solubility of nano-emulsified OMC in the pores of mesoporous titania, and compared with that of mesoporous silica. OMC-trapped mesoporous Inorganic-Organic hybrid titania showed higher factors in sun protecting and a skin penetration phenomenon was reduced.

Chemical and Optical Absorption Spectroscopic Study of Colored Tourmalines (유색 전기석의 화학적 및 광학흡수 분광학적 연구)

  • Kim, Hee-Jong;Kim, Soo-Jin
    • Journal of the Mineralogical Society of Korea
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    • v.6 no.1
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    • pp.1-16
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    • 1993
  • The chemical and optical absorption spectroscopic characters of pink and colorless tourmalines from San Diego mine in California, U.S.A., blue/green tourmalines from anonymous mine, Brazil, and brownis black tourmalines from Uncheon and Haksan mines in Korea have been studied using X-ray diffractometer, electron microprobe, optical absorption spectroscopy, and heat treatment. Least-squares refinements give unit cell diminsions : a = 15.96-16.01 ${\AA}$, c = 7.15-7.16 ${\AA}$ for the brownish black tourmalines, a = 15.82 - 15.87 ${\AA}$, c = 7.09 - 7.10 ${\AA}$ for pink tourmalines, and a = 15.88 - 15.94 ${\AA}$, c = 7.12 - 7.15 ${\AA}$ for blue green tourmalines. The colors of tourmalines are responsible for the transition elements. The pink color is attributed to the $Mn^{3+}$ ions, the blue-green to $Fe^{2+}$ and $Mn^{2+}$, bluish green to $Cu^{2+}$, and the brownish black to $Fe^{2+}$, $Fe^{2+}$ - $Fe^{3+}$, and $Fe^{2+}$ - $Ti^{4+}$. The $Mn^{3+}$ ions of pink color tourmalines are stabilized in the Y sites compressed along the O(1)H-O(3)H axis by Jahn-Teller distortion. Heating removes the pink or red component from tourmalines, producing the colorless stones from the pink and red ones. The bluish green samples change into the greenish blue ones and a certain yellowish green samples change into the light green ones by heat treatment. In the elbaite-schorl series, the concentration of Fe and Mn are variable depending on the color zones. The green zone is characterrized by the high content of Fe and Mn are variable depending on the color zones. The green zone is characterized by the high content of Fe, whereas the pink zone by the high content of Mn. Mn increases in deep yellow zone compared with yellow or colorless zones.

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