• Title/Summary/Keyword: CP/MAS

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Synthesis, Characterization and Enhanced Selectivity in RP-HPLC of Polar Carbonyl Group Embedded Poly (Vinyl Octadecanoate) Grafted Stationary Phase by Simple Heterogeneous "Graft from" Technique

  • Rana, Ashequl A.;Karim, Mohammad Mainul;Takafuji, Makoto
    • Bulletin of the Korean Chemical Society
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    • v.32 no.1
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    • pp.77-82
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    • 2011
  • A new high performance liquid chromatograpgy (HPLC) stationary phase that possesses an internal carbonyl functional group is synthesized by heterogeneous "graft from" method. This new stationary phase, poly (vinyl octadecanoate) grafted silica (Sil-2) is then characterized by different physico-chemical methods such as diffuse reflectance infrared fourier transform, suspension state $^1H$ NMR, solid state $^{13}C$ CP/MAS NMR, $^{29}Si$ CP/MAS NMR, elemental analysis and thermogravimetric analysis. Chromatographic properties of Sil-2 were evaluated under reversed phase condition by separating polycyclic aromatic hydrocarbons (PAHs) and comparing the chromatographic results with those on polymeric as well as monomeric octadecylated silica stationary phases.

Dynamics of Poly[oxy-1,4-phenyleneoxy-2-{6-(4-(4-butylphenylazo)phenoxy)hexyloxy}terephthaloyl] and Poly[oxy-1,4-phenyleneoxy-2-{10-(4-(4-butylphenylazo)phenoxy)decyloxy}terephthaloyl] Studied by $^{13}C$ CP-MAS NMR

  • 조경규;한옥희;진정일
    • Bulletin of the Korean Chemical Society
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    • v.19 no.2
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    • pp.178-183
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    • 1998
  • Carbon-13 CP-MAS NMR techniques were used to investigate dynamics of new combined type liquid crystalline polymers, poly[oxy-1,4-phenyleneoxy-2-{6-(4-(4-butylphenylazo)phenoxy)hexyloxy}terephthaloyl] and poly[oxy-1,4-phenyleneoxy-2-{10-(4-(4-butylphenylazo)phenoxy)decyloxy}terephthaloyl]. Noticeable mobility change of either aromatic groups or methylene groups is not detected between 25 ℃ and 82 ℃ from 13C spinlattice relaxation time in the rotating frame (T1ρ(C)) and contact time array experiments. However, line shape analysis shows the increase of mobility of methylene carbons in poly[oxy-1,4-phenyleneoxy-2-{6-(4-(4-butylphenylazo)phenoxy)hexyloxy}terephthaloyl] at higher temperature. The dynamics of side chanis does not seem to be affected in our experimental temperature range by the length of aliphatic chain which is connecting the side chain group to the main chain.

Preparation and Characterization of La0.8Ca0.2MnO3 (La0.8Ca0.2MnO3의 합성 및 특성연구)

  • 정미원;이지윤;김현정
    • Journal of the Korean Ceramic Society
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    • v.40 no.5
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    • pp.434-440
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    • 2003
  • The powders of L $a_{0.8}$C $a_{0.2}$Mn $O_3$ Colossal Magnetoresistance (CMR) materials were synthesized by sol-gel process. Lanthanum(H), Calcium(II) and Manganese(III) 2,4-Pentanedionate were dissolved in a mixed binary solution consisted of propionic acid and methanol with PEG (15 wt%) aqueous solution. The progress of reactions was monitored by FT-IR spectroscopy. The Lao scao.2Mn03 gel powders were annealed at various temperatures. The structural changes were investigated by FT-IR, CP/MAS $^{ 13}$C solid state NMR spectroscopy and XRD. The thermochemical property, particle characterization, microstructure of sintered sample, and cation composition of gel powder were studied by TG/DTA, FE-SEM and ICP-AES. The magnetic characterizations were identified through measurement of magnetic moment by VSM.

Preparation and Characterization of BaTiO3 Powders and Thin films (티탄산바륨 분말과 박막의 제조 및 특성 연구)

  • Jung, Miewon;Son, Hyunjin;Lee, Jiyun;Kim, Hyunjung
    • Analytical Science and Technology
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    • v.17 no.2
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    • pp.173-179
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    • 2004
  • The $BaTiO_3$ powders and thin films were prepared by an alkoxide modified sol-gel process (polymerization-complex route) using ethylene glycol. The stable starting (Ba-Ti)-mixed metal organic sol was made by addition of acetylacetone. The $BaTiO_3$ powders, which had a particle size of 40~77 nm, were crystallized from an amorphous to a tetragonal phase on annealing at 700 and $1100^{\circ}C$ for 1 h. From FT-IR, solid-state $^{13}C$ CP/MAS NMR spectroscopy and X-ray diffractometry, the trace of the Ba-Ti-oxycarbonate phase first appeared at $400^{\circ}C$. Hydrolyzed sol was spin coated on a quartz wafer at 3500 rpm for 60 s and pyrolyzed at $1100^{\circ}C$ for 1 h. After heat treatment, the coated layer became dense and smooth.

Molecular Dynamics in Paraelectric Phase of KH2PO4 Crystals Studied by Single Crystal NMR and MAS NMR

  • Paik, Younkee;Chang, Celesta L.
    • Journal of the Korean Magnetic Resonance Society
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    • v.17 no.1
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    • pp.19-23
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    • 2013
  • The temperature dependences of the NMR spectrum and the spin-lattice relaxation times in $KH_2PO_4$ were investigated via single-crystal NMR and MAS NMR. The stretched-exponential relaxation that occurred because of the distribution of correlation times was indicative of the degree of the distribution of the double-well potential on the hydrogen bond. The behaviors responsible for the strong temperature dependences of the $^1H$ and $^{31}P$ spin-lattice relaxation times in the rotating frame $T_{1{\rho}}$ in $KH_2PO_4$ are likely related to the reorientational motion of the hydrogen-bond geometry and the $PO_4$ tetrahedral distortion.

Changes in Body Function, Activity and Participation Following Task-oriented Training in Children with Cerebral Palsy (과제지향 훈련 후 뇌성마비아동의 신체기능, 활동 및 참여의 변화)

  • Yang, Hye-Yun;Kang, Soon-Hee
    • Journal of the Korean Society of Physical Medicine
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    • v.14 no.4
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    • pp.71-80
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    • 2019
  • PURPOSE: This study examined whether a task-oriented training program is an effective intervention to improve the body function, activity, and participation of children with cerebral palsy (CP). METHODS: Ten children with CP (7-13 years old) performed a task-oriented training program for eight weeks (three sessions per week, 30 minutes each). The taskoriented training program consisted of eight activities. The subjects' body function was assessed using a handheld dynamometer, goniometer, Modified Ashworth Scale (MAS), Balance Performance Monitor (BPM), and the Bruininks-Oseretsky Test of Motor Proficiency (BOTMP). The subjects' activity and participation were assessed using the Gross Motor Function Measure (GMFM) and Timed Up and Go (TUG) test. RESULTS: Task-oriented training provided significant improvements in the subjects' body function. The subjects improved the bilateral isometric muscle strength of the hip flexors, extensors and abductors, knee flexors and extensors, and ankle dorsi- and plantar flexors (p<.05). Bilateral passive hip flexion, abduction, and external rotation, knee flexion, and ankle dorsi- and plantar flexion were also increased (p<.05). In addition, the MAS score of the hip adductors decreased (p<.05) and the BOTMP score increased after training (p<.05). The subjects' activity and participation also improved significantly after training, increasing the GMFM score (p<.05) and decreasing the TUG score (p<.05). On the other hand, the BPM score did not change after training. CONCLUSION: This study suggests that a task-oriented training program can be an effective intervention to improve the body function, activity, and participation for children with CP.

Solid-State $^1H$ and $^{29}Si$ NMR Studies of Silicate and Borosilicate Gel to Glass Conversion

  • 양경화;우애자
    • Bulletin of the Korean Chemical Society
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    • v.17 no.8
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    • pp.696-699
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    • 1996
  • Silicate and borosilicate gels were prepared by the sol-gel process and thermally treated in the 150-850 ℃ temperature range. Solid-state 1H MAS and 29Si CP/MAS NMR spectroscopy were used to investigate the effects of heat treatments on the silicate gel to glass conversion process. The 1H NMR isotropic chemical shifts and the relative intensities of hydrogen bonded and isolated silanol groups have been used to access the information concerning the dehydration process on the silicate gel surface. The 29Si NMR isotropic chemical shifts affected by the local silicon environment have been used to determine the degree of crosslinking, i.e. the number of siloxane bonds. These NMR results suggest that the silicate gel to glass conversion process is occurred by two stages which are dependent on the temperature; (1) the formation of particles up to 450 ℃ and (2) the formation of large particles by aggregation of each separated single particle above 450 ℃. In addition, the effects of B atom on the formation of borosiloxane bonds in borosilicates have been discussed.

Spectroscopic Analysis on the Michael Addition Reaction between Secondary Amino Group Containing Silica Nanoparticles with (Meth)acrylate Monomers (2차 아미노기를 갖는 실리카 나노입자와 (메타)아크릴레이트 단량체와의 마이클 부가반응에 대한 분광학적 분석)

  • Jeon, Ha-Na;Ha, Ki-Ryong
    • Polymer(Korea)
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    • v.36 no.5
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    • pp.668-676
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    • 2012
  • In this study, we modified silica nanoparticles with bis[3-(trimethoxysilyl)propyl]amine (BTMA) silane coupling agent to introduce secondary amino groups on the silica surface. After modification of silica, we investigated effects of different types of (meth)acrylate group containing monomers on the Michael addition reaction to introduce reactive (meth)acrylate groups on the BTMA modified silica surface. We used two kinds of (meth)acrylate monomers, trimethylolpropane ethoxylate triacrylate (TMPET) which has three identical acrylate groups, and 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) which has one acrylate and one methacrylate group. 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 understand reactions between NH groups on the silica surface with (meth)acrylate groups of TMPET and AHM monomers. We found almost complete Michael addition reaction between all three acrylate groups of TMPET with NH groups on the BTMA modified silica. But, for the AHM treatment of BTMA modified silica, we found Michael addition reaction occurred only between acrylate groups of AHM and NH groups of silica surface, not between methacrylate groups of AHM and NH groups of BTMA modified silica surface.

Synthesis and Physical Properties of Biocompatible and Biodegradable Chitin Derivatives III. -Synthesis and Solubility of Ester Chitin Derivatives- (생체적합성과 생분해성을 갖는 키틴유도체의 합성 및 물성 III -에스테르 키틴 유도체의 합성과 용해 특성-)

  • Kim, Seon-Jeong;Lee, Young-Moo;Sung, Yong-Kiel;Kang, Inn-Kyu;Park, Young-Hoon
    • Applied Chemistry for Engineering
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    • v.4 no.4
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    • pp.785-790
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    • 1993
  • Three ester-type chitin derivatives were synthesized by reacting chitin with acetic anhydride, propionic anhydride and n-butyric anhydride to form acetyl chitin(AC), propionyl chitin(PC) and n-butyryl chitin(BC). Methanesulfonic acid was used as a catalyst. FT-IR spectra and solid state CP/MAS $^{13}C-NMR$ spectra of three chitin derivatives showed that the substituents were mainly incorporated in the $C_6$ position of chitin. The ester-type chititn derivatives were dissolved well in formic acid and swollen in aqueous acidic solution.

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Nanocomposites from Epoxy Resin and Layered Minerals (에폭시 수지와 층상광물로부터 나노복합재료의 합성)

  • 강재현;유성구;서길수
    • Polymer(Korea)
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    • v.24 no.4
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    • pp.571-577
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    • 2000
  • A new type of filler for epoxy-clay nanocomposites has been prepared by the reaction of octadecyltrimethylammonium bromide and layered sodium montmorillonite (MMT) via an ion-exchange reaction. The gallery space was further modified by grafting the aminopropyl groups via a reaction between a octadecyltrimethylammonium-MMT and 3-aminopropyltriethoxysilane (APS). The interlayer modification of MMT was confirmed by XRD, IR, and solid-state $^{29}$ Si CP/MAS NMR. Furthermore, clay-polymer nanocomposites have been synthesized by the polymerization of diglycidyl ether of bisphenol A(DGEBA) and $C_{18}$ H$_{37}$ N($CH_3$)$_3$-APS-MMT. The resulting hybrid nanocomposites were characterized by XRD, transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The results proved that the organomontmorillonite could be exfoliated and uniformly dispersed in the epoxy matrix.

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