• Title/Summary/Keyword: XRD diffraction

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FT-IR and X-Ray Diffraction Characterization of Melanoidins Formed from Glucose and Fructose with Amino Acid Enantiomers in the Maillard Reaction

  • Kim, Ji-Sang;Lee, Young-Soon
    • Food Science and Biotechnology
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    • v.18 no.2
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    • pp.546-551
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    • 2009
  • The objective of this study was to investigate Fourier transform infrared (FT-IR) spectrometry and the X-ray diffraction (XRD) characterization of melanoidins formed from glucose and fructose with amino acid enantiomers in the Maillard reaction. Before dialysis, FT-IR spectroscopy of all the samples showed that the characteristic absorption intensities appeared as a broad and intense band of the stretching vibration of the -OH group at 3,400/cm for a high pH. The absorption bands of the melanoidins sharply decreased in intensity after dialysis as compared to those before dialysis. In particular, the absorption bands at 992 and 575/cm disappeared. The XRD confirmed that the crystal structure of the melanoidins disappeared after dialysis and a new crystal structure was formed at 9 and $28^{\circ}$ ($2{\theta}$. In particular, broad diffraction peaks were formed in the $10-21^{\circ}$ ($2{\theta}$) range for a high pH, while other sharp diffraction peaks disappeared.

Synchrotron X-Ray Diffraction Studies on Crystalline Domains in Urea-Formaldehyde Resins at Low Molar Ratio

  • WIBOWO, Eko Setio;PARK, Byung-Dae;CAUSIN, Valerio;HAHN, Dongyup
    • Journal of the Korean Wood Science and Technology
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    • v.50 no.5
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    • pp.353-364
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    • 2022
  • The crystalline domain of thermosetting urea-formaldehyde (UF) resins at low formaldehyde-to-urea (F/U) molar ratios (≤ 1.0) is known to be responsible for their poor performance as wood adhesives. Crystallization has been observed in 1.0 F/U UF resins during the addition reaction stage and at the end of the synthesis process (neat UF resins). The crystallinity and X-ray diffraction (XRD) spectra of the uncured neat UF resins, on the other hand, differed significantly from those of the cured neat UF resins, raising the possibility that their crystal structures were also different. This study demonstrates for the first time that the crystalline domains in 1.0 F/U UF resins generated from uncured and cured samples are identical. Despite having a lower crystallinity value, the synchrotron XRD patterns of purified neat UF resins were equivalent to the XRD patterns of cured neat UF resins. Transmission electron microscope images of the cured UF resins showed that the crystals were lamellar structures. This finding suggests that the crystal at low molar ratio UF resins are isotropic polycrystals with random orientation.

Polypropylene Reactive Nanocomposites with Functional Nanoclays

  • Phandee, Atinuch;Magaraphan, Rathanawan;Nithitanakul, Manit;Manuspiya, Hathaikarn
    • Proceedings of the Polymer Society of Korea Conference
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    • 2006.10a
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    • pp.280-280
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    • 2006
  • Na-bentonite (local clay mineral) and Na-montmorillonite were treated with quaternary alkylammonium cations. The effect of the molecular structure and functional groups of the surfactants on the organoclays was investigated by X-ray diffraction (XRD). For the preparation of nanocomposites, organoclays were melt-blended with polypropylene in a twin screw extruder and $Surlyn^{(R)$. ionomer was used as a reactive compatibilizer. The clay dispersions in the composites were investigated by X-ray diffraction (XRD). XRD spectra showed no peak at low angle indicated that the silicate clay layer has a nearly exfoliated dispersion in the polymer matrix. Thermal and mechanical properties of nanocomposites were higher than those of PP.

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The Synthesis of Maghemite and Hematite Nanospheres

  • Dar, Mushtaq Ahmad;Ansari, Shafeeque G.;Wahab, Rizwan;Kim, Young-Soon;Shin, Hyung-Shik
    • Proceedings of the Korean Powder Metallurgy Institute Conference
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    • 2006.09a
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    • pp.472-473
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    • 2006
  • Maghemite and hematite nanospheres were synthesized by using the Sol-gel technique. The structural properties of these nanosphere powders were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), and pore size distribution. Hematite phase shows crystalline structures. The mean particle size that resulted from BET and XRD analyses were 4.9 nm and 2 nm. It can be seen from transmission electron microscopy that the size of the particles are very small which is in good agreement with the FESEM and the X-ray diffraction. The BET and pore size method were employed for specific surface area determination.

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Microstructural ananalysis of AlN thin films on Si substrate grown by plasma assisted molecular beam epitaxy (RAMBE를 사용하여 Si 기판 위에 성장된 AIN 박막의 결정성 분석)

  • 홍성의;한기평;백문철;조경익;윤순길
    • Journal of the Korean Vacuum Society
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    • v.10 no.1
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    • pp.22-26
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    • 2001
  • Microstructures of AlN thin films on Si substrates grown by plasma assisted molecular beam epitaxy were analyzed with various growth temperatures and substrate orientations. Reflection high energy electron diffraction (RHEED) patterns were checked for the in-situ monitoring of the growth condition. X-ray diffraction(XRD), double crystal X-ray diffraction (DCXD), and transmission electron microscopy/diffraction (TEM/TED) techniques were employed to characterize the microstructure of the films after growth. On Si(100) sub-strates, AlN thin films were grown mostly along the hexagonal c-axis orientation at temperature higher than $850^{\circ}C$. On the other hand the AlN films on Si(111) were epitaxially grown with directional coherencies in AlN(0001)/Si(111), AlN(1100)/Si(110), and AlN(1120)/Si(112). The microstructure of AlN thin films on Si(111) substrates, with a full width at half maximum of almost 3000 arcsec at 2$\theta$=$36.2^{\circ}$, showed that the single crystal films were grown, even if they includ a lot of crystal defects such as dislocations and stacking faults.

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Estimation Study of Firing Temperature for Fired Clay Brick Relics Excavated from Buddhist Temple in Karatepa Using Analytical Method of High Temperature X-ray Diffraction (고온 XRD 분석법을 이용한 카라테파 불교사원 출토 점토벽돌의 소성온도 추정연구)

  • Han, Min Su;Lee, Jang Jon;Kim, Jae Hwan
    • Journal of Conservation Science
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    • v.32 no.4
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    • pp.511-520
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    • 2016
  • The purpose of this study was to estimate the firing temperature of fired clay brick by applying high temperature X-ray diffraction(XRD) analysis. The clay bricks, which were excavated from a Buddhist temple in Karatepa, Uzbekistan were composed of quartz, plagioclase, alkali feldspar, mica, chlorite, limestone, hornblende, etc. Some clay bricks contained gypsum, which was presumed to have been used to improve the adhesive strength of the brick. Estimating the firing temperature using a geologic thermometer, the UZ-1 sample was identified as being in the quartz, plagioclase, pyroxene series, and the firing temperature was estimated to be $900-1200^{\circ}C$. On the other hand, applying the high temperature XRD method to the UZ-5 sample, it was found that the limestone was destroyed at $1000^{\circ}C$ and the diffraction peak of chlorite was weakened at $1050^{\circ}C$. Moreover, pyroxene series minerals developed at $1050^{\circ}C$ in the reproduction experiment. These results indicate that the clay bricks used in the temple were produced in a kiln that reached a temperature of more than $1000^{\circ}C$. Thus, high temperature XRD analysis can more accurately estimate firing temperatures as compared to the firing temperature mineral identification method and it can be used to determine the creation and extinction temperature range of minerals.

X-ray Diffraction Patterns of Activated Carbons Prepared under Various Conditions

  • Girgis, Badie S.;Temerk, Yassin M.;Gadelrab, Mostafa M.;Abdullah, Ibrahim D.
    • Carbon letters
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    • v.8 no.2
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    • pp.95-100
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    • 2007
  • A series of activated carbons (ACs) were derived from sugarcane bagasse under two activation schemes: steam-pyrolysis at $600-800^{\circ}C$ and chemical activation with $H_3PO_4$ at $500^{\circ}C$. Some carbons were treated at 400, $600^{\circ}C$, or for 1-3 h, and/or in flowing air during pyrolysis of acid-impregnated mass. XRD profiles displayed two broad diffuse bands centered around $2{\theta}=23$ and $43^{\circ}$, currently associated with diffraction from the 002 and 100/101 set of planes in graphite, respectively. These correspond to the interlayer spacing, Lc, and microcrystallite lateral dimensions, La, of the turbostratic (fully disordered) graphene layers. Steam pyrolysis-activated carbons exhibit only the two mentioned broad bands with enhancement in number of layers, with temperature, and small decrease in microcrystallite diameter, La. XRD patterns of $H_3PO_4$-ACs display more developed and separated peaks in the early region with maxima at $2{\theta}=23$, 26 and $29^{\circ}$, possibly ascribed to fragmented microcrystallites (or partially organized structures). Diffraction within the $2{\theta}=43^{\circ}$ is still broad although depressed and diffuse, suggesting that the intragraphitic layers are less developed. Varying the conditions of chemical activation inflicts insignificant structural alterations. Circulating air during pyrolysis leads to enhancement of the basic graphitic structure with destruction and degradation in the lateral dimensions.

Estimation of Phase Ratio for TiO2 Powders by XRD and XAS (XRD와 XAS에 의한 TiO2 분말의 상분율 결정)

  • Rha, Sa-Kyun;Lee, Youn Seoung
    • Journal of the Korean Ceramic Society
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    • v.49 no.5
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    • pp.469-474
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    • 2012
  • The crystallinity and phase ratio of anatase to rutile in $TiO_2$ were estimated by x-ray diffraction (XRD) and x-ray absorption spectroscopy (XAS). Traditionally, the structural characterization of $TiO_2$ powders has been carried out by XRD techniques, which are comparatively easy in use and analysis. However, materials with amorphous phase, nano-sized or nano-structured crystallinities cannot be fully characterized by XRD because XRD analysis has a limit for abnormal contributions of the nano-crystal such as the surface contribution. From the comparison with the experimental and calculated Ti K-edge XAS spectra, we found the possibility of efficient estimation in the crystalinites and the phase ratio of anatase to rutile for nano-sized $TiO_2$ mixture.

Determination of mixing ratios in a mixture via non-negative independent component analysis using XRD spectrum (XRD 스펙트럼의 비음독립성분분석을 통한 혼합물 구성비 결정)

  • You, Hanmin;Jun, Chi-Hyuck;Lee, Hyeseon;Hong, Jae-Hwa
    • Analytical Science and Technology
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    • v.20 no.6
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    • pp.502-507
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    • 2007
  • X-ray diffraction method has been widely used for qualitative and quantitative analysis of a mixture of materials since every crystalline material gives a unique X-ray diffraction pattern independently of others, with the intensity of each pattern proportional to that material's concentration in a mixture. For determination of mixing ratios, extracting source spectra correctly is important and crucial. Based on the source spectra extracted, a regression model with non-negativity constraint is applied for determining mixing ratios. In some mixtures, however, X-ray diffraction spectrum has sharp and narrow peaks, which may result in partial negative source spectrum from independent component analysis. We propose several procedures of extracting non-negative source spectra and determining mixing ratios. The proposed method is validated with experimental data on powder mixtures.

Mineralogical Properties of Asian Dust in April 6 and 15, 2018, Korea (2018년 4월 6일과 15일 황사의 광물학적 특성)

  • Jeong, Gi Young
    • Journal of the Mineralogical Society of Korea
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    • v.31 no.2
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    • pp.103-111
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    • 2018
  • Mineralogical properties of two Asian dust (Hwangsa) samples collected during dust events in April 6 and 15, 2018 were examined by X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD analyses showed that Asian dusts were dominated by phyllosilicates (62 wt%) comprising illite-smectite series clay minerals (ISCMs) (55%), chlorite (3%) and kaolinite (4%). Nonphyllosilicate minerals were quartz (18%), plagioclase (9%), K-feldspar (3%), calcite (3%), and gypsum (2-4%). Mineral compositions determined by SEM chemical analyses were consistent with XRD data. ISCMs occur as submicron grains forming aggregate particles or coating coarse mineral grains such as quartz, plagioclase, K-feldspar, chlorite, and calcite. The ISCMs are often associated with calcite nanofibers and gypsum blades. Mineralogical properties of 2018 dusts were similar to those of previous dusts although clay contents were higher than that of coarse 2012 dust.