• Title/Summary/Keyword: FTIR spectroscopy

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Prediction of Precipitated Wax Amounts Using FTIR Spectroscopy (FTIR을 이용한 왁스 침전의 정량적 예측)

  • Oh, Kyeongseok
    • Korean Chemical Engineering Research
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    • v.51 no.3
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    • pp.376-381
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    • 2013
  • High molecular weight paraffinic waxes dissolved in oil phases can be precipitated when the surrounding temperature becomes lower than the wax appearance temperature (WAT). While the various methods of WAT determination have been developed, the determination of precipitated wax amount has not been comparably popular at temperatures below the WAT. It is important to predict how much solid wax content precipitates in temperature variance. The study develops the previous method which uses integrated areas determined at a wavenumber range of 735~715 $cm^{-1}$. This method uses two different wavenumber ranges, 735~715 $cm^{-1}$ and 1,402~1,324 $cm^{-1}$. The study shows how the method provides reliable data in the variety of applications regardless of FTIR spectral instability often occurred, such as volume reduction during cooling procedure and existence of emulsified water in oil phase.

Effect of boron doping on the chemical and physical properties of hydrogenated amorphous silicon carbide thin films prepared by PECVD (플라즈마 화학증착법으로 제조된 수소화된 비정질 탄화실리콘 박막의 물성에 대한 붕소의 도핑효과)

  • 김현철;이재신
    • Journal of the Korean Vacuum Society
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    • v.10 no.1
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    • pp.104-111
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    • 2001
  • B-doped hydrogenated amorphous silicon carbide (a-SiC:H) thin films were prepared by plasma-enhanced chemical-vapor deposition in a gas mixture of $SiH_4, CH_4,\;and\; B_2H_6$. Physical and chemical properties of a-SiC:H films grown with varing the ratio of $B_2H_6/(SiH_4+CH_4)$ were characterized with various analysis methods including scanning electron microscopy (SEM), X-ray diffractometry (XRD), Raman spectroscopy, Fourier-transform infrared (FTIR) spectroscopy, secondary ion mass spectroscopy (SIMS), UV absorption CH_4spectroscopy and electrical conductivity measurements. With the B-doping concentration, the doping efficiency and the micro-crystallinity were decreased and the film became amorphous when $B_2H_6/(SiH_4{plus}CH_4)$ was over $5{\times}10^{-3}$. The addition of $B_2H_6$ gas during deposition decreased the H content in the film by lowering the quantity of Si-C-H bonds. Consequently, the optical band gap and the activation energy of a-SiC:H films were decreased with increasing the B-doping level.

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Quantitative Analysis of Silanization Degree of Silica Nanoparticles Modified with Bis[3-(trimethoxysilyl)propyl]amine Coupling Agent (Bis[3-(trimethoxysilyl)propyl]amine 커플링제로 개질된 실리카 나노입자의 실란화도 정량 분석)

  • Jeon, Ha-Na;Kim, Jung-Hye;Ha, Ki-Ryong
    • Polymer(Korea)
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    • v.36 no.3
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    • pp.372-379
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    • 2012
  • In this study, we treated silica nanoparticles with bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify their surfaces. We investigated the effects of BTMA hydrolysis time, BTMA concentration and BTMA treatment time on the degree of silanization reaction of silica nanoparticles. We used Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to obtain quantitative data. We found the decrease of isolated Si-OH peak intensity at 3747 $cm^{-1}$ and the increase of $-CH_2 $stretching and bending peaks with increasing hydrolysis time, concentration and treatment time of BTMA. EA analysis results also supported this trend. We found a strong effect of BTMA concentration on the degree of silanization of the silica particles, but weak effects of the hydrolysis time and the treatment time.

Deposition of Polytetrafluoroethylene Thin Films by IR-pulsed Laser Ablation (Nd:YAG 레이저에 의한 폴리테트라플루오르에틸렌 박막 증착)

  • Park Hoon;Seo Yu-Suk;Hong Jin-Soo;Chae Hee-Baik
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.6 no.1
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    • pp.58-63
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    • 2005
  • PTFE (polytetrafluoroethylene) thin films were prepared from the pellets of the graphite doped PTFE via pulsed laser ablation with 1064 nm Nd:YAG laser. The graphite powder converts the absorbed photon energy into thermal energy which is transmitted to nearby PTFE. The PTFE is decomposed by thermal process. The deposited films were transparent and crystalline. SEM (scanning electron microscopy) and AFM (atomic force microscopy) analyses indicated that the film surface morphology changed to fibrous structure with increasing thickness. The fluorine to carbon ratios of the film were 1.7 and molecular axis was parallel with (100) Si-wafer substrate. These results obtained by XPS (X-ray photoelectron spectroscopy), FTIR (fourier transform infrared spectroscopy) and XRD (X-ray diffraction).

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Equimolar Carbon Dioxide Absorption by Ether Functionalized Imidazolium Ionic Liquids

  • Sharma, Pankaj;Park, Sang-Do;Park, Ki-Tae;Jeong, Soon-Kwan;Nam, Sung-Chan;Baek, Il-Hyun
    • Bulletin of the Korean Chemical Society
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    • v.33 no.7
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    • pp.2325-2332
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    • 2012
  • A series $[C_3Omim]$[X] of imidazolium cation-based ILs, with ether functional group on the alkyl side-chain have been synthesized and structure of the materials were confirmed by various techniques like $^1H$, $^{13}C$ NMR spectroscopy, MS-ESI, FTIR spectroscopy and EA. More specifically, the influence of changing the anion with same cation is carried out. The absorption capacity of $CO_2$ for ILs were evaluated at 30 and $50^{\circ}C$ at ambient pressure (0-1.6 bar). Ether functionalized ILs shows significantly high absorption capacity for $CO_2$. In general, the $CO_2$ absorption capacity of ILs increased with a rise in pressure and decreased when temperature was raised. The obtained results showed that absorption capacity reached about 0.9 mol $CO_2$ per mol of IL at $30^{\circ}C$. The most probable mechanism of interaction of $CO_2$ with ILs were investigated using FTIR spectroscopy, $^{13}C$ NMR spectroscopy and result shows that the absorption of $CO_2$ in ether functionalized ILs is a chemical process. The $CO_2$ absorption results and detailed study indicates the predominance of 1:1 mechanism, where the $CO_2$ reacts with one IL to form a carbamic acid. The $CO_2$ absorption capacity of ILs for different anions follows the trend: $BF_4$ < DCA < $PF_6$ < TfO < $Tf_2N$. Moreover, the as-synthesized ILs is selective, thermally stable, long life operational and can be recycled at a temperature of $70^{\circ}C$ or under vacuum and can be used repeatedly.

Spectroscopic Studies on the Reaction between Amino Groups on Silica Nanoparticle Surface and Glycidyl Methacrylate (실리카 나노입자 표면에 결합된 아미노기와 Glycidyl Methacrylate의 반응에 관한 분광학적 연구)

  • Lee, Sangmi;Ha, KiRyong
    • Polymer(Korea)
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    • v.37 no.6
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    • pp.777-783
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    • 2013
  • We used dipodal type bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to modify silica nanoparticles to introduce secondary amino groups on the silica surface. These grafted N-H groups were reacted with glycidyl methacrylate (GMA) to introduce polymerizable methacrylate groups on the silica surface. After modification reaction, we used several analytical techniques such as Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and solid state $^{13}C$ cross-polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to analyze the effects of reaction time, reaction temperature and used GMA concentration on the modification degree between N-H groups on the silica surface and epoxide groups of GMA. We found increased introduction of methacrylate groups on the silica surface by ring opening reaction of epoxide groups of GMA with N-H groups on BTMA treated silica with increased reaction time, reaction temperature and used GMA concentration within our experimental conditions.

Principal Component Analysis Based Two-Dimensional (PCA-2D) Correlation Spectroscopy: PCA Denoising for 2D Correlation Spectroscopy

  • Jung, Young-Mee
    • Bulletin of the Korean Chemical Society
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    • v.24 no.9
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    • pp.1345-1350
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    • 2003
  • Principal component analysis based two-dimensional (PCA-2D) correlation analysis is applied to FTIR spectra of polystyrene/methyl ethyl ketone/toluene solution mixture during the solvent evaporation. Substantial amount of artificial noise were added to the experimental data to demonstrate the practical noise-suppressing benefit of PCA-2D technique. 2D correlation analysis of the reconstructed data matrix from PCA loading vectors and scores successfully extracted only the most important features of synchronicity and asynchronicity without interference from noise or insignificant minor components. 2D correlation spectra constructed with only one principal component yield strictly synchronous response with no discernible a asynchronous features, while those involving at least two or more principal components generated meaningful asynchronous 2D correlation spectra. Deliberate manipulation of the rank of the reconstructed data matrix, by choosing the appropriate number and type of PCs, yields potentially more refined 2D correlation spectra.

Ultraviolet-ozone irradiation of HPMC thin films: Structural and thermal properties

  • Abdel-Zaher, Nabawia A.;Moselhey, Manal T.H.;Guirguis, Osiris W.
    • Advances in materials Research
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    • v.6 no.1
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    • pp.1-12
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    • 2017
  • The aim of the work was to evaluate the effect of ultraviolet-ozone ($UV-O_3$) irradiation with different times on the structure and thermal properties of hydroxypropyl methylcellulose (HPMC) in the form of a thin film to be used as bioequivalent materials according to their important broad practical and medical applications. HPMC thin films were exposed to $UV-O_3$ radiation in air at a wavelength of 184.9 nm.The beneficial effects of this treatment on the crystallinity and amorphousity regions were followed by X-ray diffraction technique and FTIR spectroscopy. Differential scanning calorimetry, thermogravimetric and differntial thermal analyses were used in order to study the thermal properties of HPMC samples following the process of photodegradation. The obtained results indicated that the rate of degradation process was increased with increasing the exposure time. Variations in shape and area of the thermal peaks were observed which may be attributed to the different degrees of crystallinity after exposing the treated HPMC samples. This meant a change in the amorphousity of the treated samples, the oxidation of its chemical linkages on its surface and its bulk, and the formation of free radical species as well as bond formation.

Potential degradation of methylene blue (MB) by nano-metallic particles: A kinetic study and possible mechanism of MB degradation

  • Singh, Jiwan;Chang, Yoon-Young;Koduru, Janardhan Reddy;Yang, Jae-Kyu
    • Environmental Engineering Research
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    • v.23 no.1
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    • pp.1-9
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    • 2018
  • The degradation of methylene blue (MB) in an aqueous solution by nano-metallic particles (NMPs) was studied to evaluate the possibility of applying NMPs to remove MB from the wastewater. Scanning electron microscopy (SEM), Fourier-transform infrared (FTIR) spectroscopy and X-ray photoelectron spectroscopy (XPS) were used to characterize the synthesized NMPs before and after the reaction. The effects of the NMP dosage, the initial pH, the initial concentration of MB and the amount of $H_2O_2$ on the MB degradation outcomes were studied. The highest removal rate of MB was achieved to be 100% with an initial MB concentration of 5 mg/L, followed by 99.6% with an initial concentration of 10 mg/L under the following treatment conditions: dose of NMP of 0.15 g/L, concentration of $H_2O_2-100mM$ and a temperature of $25^{\circ}C$. The SEM analysis revealed that the nano particles were not spherical in shape. FTIR spectra shows occurrence of metal oxides on the surfaces of the NMPs. The XPS analyses results represent that Fe, Zn, N, Ca, C and O were occurred on the surfaces of the NMPs. The degradation of MB was suitable for the pseudo-first-order kinetics.

Spectroscopic Studies on Electroless Deposition of Copper on Hydrogen-Terminated Si(111) Surface in NH4F Solution Containing Cu(II) Ions

  • Lee, In-Churl;Bae, Sang-Eun;Song, Moon-Bong;Lee, Jong-Soon;Paek, Se-Hwan;J.Lee, Chi-Woo
    • Bulletin of the Korean Chemical Society
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    • v.25 no.2
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    • pp.167-171
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    • 2004
  • The electroless deposition of copper on the hydrogen-terminated Si(111) surface was investigated by means of attenuated total reflection Fourier transform infrared (ATR-FTIR) spectroscopy, scanning tunneling microscopy (STM), and energy-dispersive spectroscopy (EDS). The hydrogen-terminated Si(111) surface prepared was stable under air atmosphere for a day or more. It was found from ATR-FTIR that two bands centered at 2000 and 2260 $cm^{-1}$ appeared after the H-Si(111) surface was immersed in 40% $NH_4F$ solution containing 10 mM $Cu^{2+}$. On the other hand, STM image included the copper islands with a height of 5 nm and a diameter of 10-20 nm. The EDS data displayed the presence of copper, silicon and oxygen species. The results were rationalized in terms of the redox reaction of surface Si atoms and $Cu^{2+}$ ions in solutions, which are changed into $Si(OH)_x(F)_y$ containing $SiF_6^{2-}$ ions and neutral copper islands.