• Title/Summary/Keyword: 고체 NMR

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Microscopic investigation on the binary ethanol + $CH_4$ Hydrate system (ethanol + $CH_4$ 하이드레이트 시스템의 미세 분광학적 연구)

  • Lee, Jong-Won;Kang, Seong-Pil
    • 한국신재생에너지학회:학술대회논문집
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    • 2010.11a
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    • pp.149.1-149.1
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    • 2010
  • 가스 하이드레이트는 작은 고체 부피 내에 막대한 양의 가스를 저장할 수 있다는 특징으로 인하여 최근 주목을 받고 있지만, 엔지니어링 분야에서는 천연가스 수송 파이프라인에 blockage problem을 일으키는 해로운 물질로 처음 관심을 받았다. 이러한 문제를 해결하기 위한 방법으로 초기에는 하이드레이트 형성영역을 벗어나도록 온도, 압력을 유지하기도 하였으나, 최근에는 다양한 형성 억제제가 사용되고 있다. 본 연구에서는 기존에 억제제로 알려져 있는 대표적인 알코올 화합물인 에탄올을 이용하여 고압의 메탄과 binary 하이드레이트의 형성 연구를 수행하였다. 다양한 농도의 에탄올을 이용하여 형성된 하이드레이트 샘플은 고체 NMR 분석을 통하여 분자 거동을 자세히 측정하였으며, 분말 XRD 분석을 통하여 헝성된 미세 결정 구조도 확인하였다. 본 연구에서 얻어진 결과는 에탄올 및 알코올 화합물의 가스 하이드레이트 형성 거동 및 binary guest 시스템에서의 tuning 효과에 대한 유용한 정보를 제시할 수 있을 것이라 판단된다.

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A Study on the Preparation of Hollow Microbeads Using Hydroxypropyl Chitosan (키토산 유도체를 이용한 화장품용 중공 마이크로비드의 제조에 관한 연구)

  • 하병조
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.24 no.1
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    • pp.7-24
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    • 1998
  • 게 껍질로부터 얻은 키틴을 탈아세틸화하여 키토산을 얻었으며, 얻어진 키토산의 유기용매에 대한 용해성을 향상시키기 위해 알칼리 조건에서 고압반응ㅇ기를 사용하여 프로필렌옥사이드와 반응시켜 치환율 3.5의 히드록시프로필 키토산을 합성하였다. 합성된 히드록시프로필 키토산은 고체상 CP/MAS 13C-NMR, 1H-NMR, FT-IR을 통해 반응이 키토산의 6번 탄소의 수산기와 2번 탄소의 아민기에 주로 일어났음을 알 수 있었다. 또한 X-선 회절분석을 통해 키토산의 결정성이 프로필렌옥사이드와의 반응에 의해 크게 감소하였음을 알 수 있었고, 그 결과 유기 용매에 대한 용해성이 현저히 증가되는 현상을 나타내었다. 한편, 히드록시프로필 키토산을 수상에 녹인 후 W/O 에멀젼상에 서 알칼리 촉매를 사용항 에피클로로히드린과 가교반응을 실시한 결과 내부가 비어있는 중공 마이크로비드를 얻을 수 있었다. 전자현미경을 통한 분석결과 중공 마이크로비드의 껍질의 내부에는 스킨층이 형성되어 있었으며, 외부 표면은 다공성이 높은 비대칭 막으로 되어 있음을 확인할 수 있었다.

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Microscopic analysis of gas hydrates using X-ray diffraction method (X-ray diffraction을 이용한 가스 하이드레이트 미세구조 분석)

  • Lee, Jong-Won;Seol, Ji-Woong;Koh, Dong-Yeun;Lee, Huen
    • 한국신재생에너지학회:학술대회논문집
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    • 2008.10a
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    • pp.178-181
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    • 2008
  • 다양한 조성을 갖는 $CH_4+CO_2$ 혼합 기체 하이드레이트 샘플의 미세 구조 분석을 위하여 X-ray 회절 방법을 이용하였다. X-ray 회절 분석을 이용할 경우, 하이드레이트로의 전환율과 같은 정성적인 분석뿐 아니라 각 객체별 cage occupancy와 같은 정량적인 분석까지도 가능한 것으로 나타났다. 또한 이렇게 얻어진 X-ray 회절 분석 결과 및 refinement 결과를 $^{13}C$ 고체 NMR 방법과 교차 비교함으로써 측정 결과의 신뢰도를 높이려 하였다. 얻어진 분석 결과는 이후 가스 하이드레이트를 이용한 다양한 연구 분야에서 저장용량 평가 및 객체 점유율과 같은 미세 구조 정보를 얻는 데에 유용하게 사용될 것으로 전망된다.

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Optimization of boric acid production process from boron ore (붕소원광으로부터 붕산제조 공정의 최적화)

  • 임형미;이옥란;이승호;최병현
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.03a
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    • pp.32-32
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    • 2003
  • Calcuim borate 화합물의 하나인 Colemanite 천연원광을 출발물질로 붕산을 제조하는 공정에 대한 연구로 황산 첨가량과 처리온도, 건조온도와 시간에 따라 생성되는 붕산의 결정상과 수득률, 순도 및 입자의 형상을 관찰하였다. 황산 첨가로 붕소 성분은 용해되어 액상에 남고, SO$_4$$^{2-}$ 와 결합하여 불용성 고체로 분리되고, 붕소의 온도에 따른 용해도 차를 이용하여 재결정화하는 방법으로 99% 이상의 순도를 갖는 붕산(H$_3$BO$_3$)을 얻었다. 공정의 각 단계에서 생성되는 화합물을 TG, NMR, IR, XRD, ICP 등의 방법으로 분석하여 최적 제조 조건을 찾았다.

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Solid Phase Synthesis of Lysine-exposed Peptide-Polymer Hybrids by Atom Transfer Radical Polymerization (ATRP를 이용한 Lysine 말단기를 가진 펩타이드-고분자 하이브리드 합성)

  • Ha, Eun-Ju;Kim, Mijin;Kim, Jinku;An, Seong Soo A.;Paik, Hyun-Jong
    • Polymer(Korea)
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    • v.38 no.4
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    • pp.550-556
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    • 2014
  • Recently, the peptide(or protein)-polymer hybrid materials (PPs) were sought in many research areas as potential building blocks for assembling nanostructures in selective solvents. In PPs, the facile routes of preparing well-defined peptide-polymer bio-conjugates and their specific activities in various applications are important issues. Our strategy to prepare the peptide-polymer hybrid materials was to combine atom transfer radical polymerization (ATRP) method with solid phase peptide synthesis. The standard solid phase peptide synthesis method was employed to prepare the PYGK (proline-tyrosine-glycine-lysine) peptide. PYGK is an analogue peptide, PFGK (proline-phenylalanine-glycine-lysine), which interacted with plasminogen in fibrinolysis. The peptide and the peptide-initiator were characterized with MALDI-TOF mass spectrometry and $^1H$ NMR spectrometer. The peptide-polymer, pSt-PYGK was characterized by GPC, IR, $^1H$ NMR spectrometer and TLC. Spherical micellar aggregates were determined by TEM and SEM. Current synthesis methodology suggested opportunities to create the well-defined peptide-polymer hybrid materials with specific binding activity.

Spectroscopic Analysis on Michael Addition Reaction of Secondary Amino Groups on Silica Surface with 3-(Acryloyloxy)-2-hydroxypropyl Methacrylate (2차 아미노기가 결합된 실리카 나노 입자 표면에 3-(Acryloyloxy)-2-hydroxypropyl Methacrylate의 마이클 부가 반응에 대한 분광학적 분석)

  • Lee, Sangmi;Ha, Ki Ryong
    • Polymer(Korea)
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    • v.38 no.2
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    • pp.257-264
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    • 2014
  • In this study, we modified silica nanoparticles with bis[3-(trimethoxysilyl)propyl]ethylenediamine (BTPED) silane coupling agent, which has two secondary amino groups in a molecule, to introduce amino groups on the silica surface. After modification of silica, we used acrylate group containing 3-(acryloyloxy)-2-hydroxypropyl methacrylate (AHM) to introduce polymerizable methacrylate groups by Michael addition reaction. We used Fourier transform infrared spectroscopy (FTIR), elemental analysis (EA) and liquid and solid state cross polarization magic angle spinning (CP/MAS) nuclear magnetic resonance spectroscopy (NMR) to understand the reactions between N-H groups of BTPED modified silica surface and acrylate groups of AHM monomer. We confirmed Michael addition reaction between BTPED modified silica and AHM completed in 2 hr reaction time. We also found increased methacrylate group introduction with increase of mol ratio of the acrylate group of AHM to N-H group of BTPED modified silica by increase of C=O peak area of measured FTIR spectra. These results were also supported by EA and solid state $^{13}C$ and $^{29}Si$ NMR results.

An NMR Study on the Phase Changes of Lipid Bilayers by Antimicrobial Peptides (항균성 펩타이드에 의한 지질 이중막의 상 변화에 대한 NMR 연구)

  • Kim, Chul
    • Journal of the Korean Chemical Society
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    • v.54 no.2
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    • pp.183-191
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    • 2010
  • The phase changes of 1-palmitoyl-$d_{31}$-2-oleoyl-sn-glycero-3-phosphatidylcholine (POPC_$d_{31}$) bilayers distorted by an antimicrobial peptide, a magainin 2 or an aurein 3.3 were investigated by using $^2H$ solid-state NMR (SSNMR) spectroscopy. From the theoretical simulation of the experimental $^2H$ solid-state NMR spectra the geometric structure constants and the lateral diffusion coefficients were obtained in the peptide-lipid mixture phases. Within five days of the peptide action on the lipid bilayers only the distorted alignment of the bilayers were measured but after 100 days an elliptic toroidal pore structure and an inverted hexagonal phase were formed in the presence of magainin 2 and aurein 3.3, respectively. In order to investigate the effect of an anionic lipid molecule on the actions of two peptides on the lipid bilayer, the same experiments were performed on the POPC_$d_{31}$/1-palmitoyl-2-oleoyl-sn-glycero-3-phosphatidylglycerol (POPG) bilayer and the significant differences in the actions of two peptides on two bilayers of POPC_$d_{31}$ and POPC_$d_{31}$/POPG were measured.

A solid-state NMR study on the hydration effect on the lipid phase change in the presence of an antimicrobial peptide (항균성 펩타이드와 혼합된 인지질 분자의 상 변화에 있어서 수화 효과에 대한 고체 핵자기 공명 연구)

  • Kim, Chul
    • Analytical Science and Technology
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    • v.26 no.6
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    • pp.395-400
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    • 2013
  • The hydration and antimicrobial peptide effects on the lipid alignment on the surface of a thin glass plate were investigated by using the solid-state nuclear magnetic resonance spectroscopy. Pure 1-palmitoyl-2-oleoyl-sn-glycero-3-phosphotidylcholine (POPC) lipid molecules were well aligned on the surface of a thin glass plate without direct hydration by placing the sample for a few days in the desiccator containing a saturated sodium phosphate dibasic solution, which provided 95% relative humidity. But there was a big difference between two lipid phases, the one of which was hydrated by placing the sample for a few days in the desiccator with 95% relative humidity without direct hydration and the other was directly hydrated by dropping water and then placed for a few days in the same desiccator. The surface mobility of POPC molecules in a lipid bilayer phase was much activated by water. While the time for the POPC to align on the glass plate surface was short, the time for the PG-1/POPC mixture to reach the its equilibrium state was long.

Synthesis of Methoxy Polyoxyethlene Dodecanoates (Methoxy Polyoxyethylene Dodecanoate의 합성)

  • Kang, Yun-Seog;Noh, Sueng-Ho;Choi, Seung-Ok;Nam, Ki-Dae
    • Applied Chemistry for Engineering
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    • v.9 no.5
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    • pp.749-753
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    • 1998
  • Methoxy polyoxyethylene dodecanoates, kinds of nonionic surfactants, could be obtained from addition of ethylene oxide (5, 7, 9, and 12mol) with fatty acid methyl ester utilizing solid catalyst, metal oxide. Because ethylene oxide (EO) couldn't react directly in acid or alkali catalyst with dodecanoic acid methyl ester (DME) that had no active hydrogen, the reaction to add EO was carried out using active solid catalyst. By using IR, HPLC and $^1H$ NMR analysis, structural confirmation of methyl polyoxy ethylene dodecanate showed high yield ranging from 93 to 97%. EO unit mol number of reacted products was 5.2, 7.1, 9.2 and 12.1 mol respectively. Also, EO adduct distrobution of ethoxylated methyl laurate (MPD) had normal distribution curve like polyoxyethylene alkyl ether (AE).

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Characterization of Fibroin Biosynthesis in the 5th Instar of Bombyx mori (5령 누에에 있어서 Fibroin 생합성의 특성)

  • 이인전;여주홍
    • Journal of Sericultural and Entomological Science
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    • v.38 no.2
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    • pp.180-185
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    • 1996
  • Biosynthesis tracing of the silk fibroin in Bombyx mori silkworm was examined in vivo with isotopic [1-13C] Gly. labeling by nuclear magnetic resonance method. The [1-13C] Gly. labeled silk fibroin yielded very sharp 13C NMR signal in the posterior silk gland as well as in aqueous solution and the amound of [1-13C] Gly. labeled signal in the silkworm increased gradually and rapidly to 5-th day of fifth instar. However, the decomposition or decrease of the [1-13C] Gly. labeled signal occured from 5-th to 9-th day of fifth instar unexpectedly. These findings suggest that a relative amount of ${\alpha}$-helical portion or amorphous silk II portion was formed without any further signal from 6-th day of fifth instar to pupation. Through peak separation of orientation spectrum, between the fiber axis and the molecular bond direction, N-H bond in Bombyx mori silk fiber as well as the orientation distribution around the silk fibroin axis were determined and two kinds of peaks were also obtained from this orientation spectrum.

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