• 제목/요약/키워드: High-resolution NMR

검색결과 87건 처리시간 0.027초

Variable Temperature High-Resolution 19F MAS Solid-State NMR Characterization of Fluorocarbon Rubbers

  • Park, Tae-Joon;Choi, Sung-Sub;Kim, Ji-Sun;Kim, Yong-Ae
    • Bulletin of the Korean Chemical Society
    • /
    • 제32권7호
    • /
    • pp.2345-2350
    • /
    • 2011
  • Variable temperature high-resolution $^{19}F$ magic angle spinning (MAS) solid-state NMR spectroscopy was used to characterize fluorocarbon (FKM) rubbers. The high-resolution spectra of copolymers made from two monomers, vinylidene fluoride and hexafluoropropene, and terpolymers composed of vinylidene fluoride, hexafluoropropene, and tetrafluoroethylene, were obtained using MAS speeds of up to 18 kHz combined with high temperatures of up to 200 $^{\circ}C$ at a magnetic field strength of 9.4 Tesla. From these high resolution solid-state NMR spectra, we were able to assign the spectral peaks and differentiate the copolymer FKM from the terpolymer FKM. We also determined quantitatively the monomer compositions of each FKM rubber.

Nanoscale-NMR with Nitrogen Vacancy center spins in diamond

  • Lee, Junghyun
    • 한국자기공명학회논문지
    • /
    • 제24권2호
    • /
    • pp.59-65
    • /
    • 2020
  • Nitrogen-Vacancy (NV) center in diamond has been an emerging versatile tool for quantum sensing applications. Amongst various applications, nano-scale nuclear magnetic resonance (NMR) using a single or ensemble NV centers has demonstrated promising results, opening possibility of a single molecule NMR for its chemical structural studies or multi-nuclear spin spectroscopy for quantum information science. However, there is a key challenge, which limited the spectral resolution of NMR detection using NV centers; the interrogation duration for NV-NMR detection technique has been limited by the NV sensor spin lifetime (T1 ~ 3ms), which is orders of magnitude shorter than the coherence times of nuclear spins in bulk liquid samples (T2 ~ 1s) or intrinsic 13C nuclear spins in diamond. Recent studies have shown that quantum memory technique or synchronized readout detection technique can further narrow down the spectral linewidth of NMR signal. In this short review paper, we overview basic concepts of nanoscale NMR using NV centers, and introduce further developments in high spectral resolution NV NMR studies.

평면 경사자계 코일을 사용한 고분해능 NMR 생체 영상법에 관한 연구 (In Vivo High Resolution NMR Imaging by Using Surface Gradient Coil)

  • 이정한;오우진;조장희
    • 대한의용생체공학회:학술대회논문집
    • /
    • 대한의용생체공학회 1990년도 추계학술대회
    • /
    • pp.48-51
    • /
    • 1990
  • A new in vivo high resolution imaging method which is performed with a newly developed three channel surface gradient coil (SGC) is described. The surface gradient coil can produce more than an order of magnitude stronger gradient fields with good linearity within a limited imaging region. To increase the signal to noise ratio (SNR), we have developed an RF coil integrated surface gradient coil set. In this paper, the geometrical structures and characteristics of the proposed surface gradient coil are discussed and experimentally obtained high resolution images ($50\;{\mu}m$ to $100\;{\mu}m$) of a water filled phantom and a human volunteer's knee using the new surface RF coil integrated SGC set are presented for the demonstration of the in vivo high resolution imaging capability of the new imaging method.

  • PDF

Solid-State High-Resolution 1H-NMR Study for Ammonia Borane of Hydrogen Storage Material

  • Han, J.H.;Lee, Cheol-Eui;Kim, Se-Hun;Kim, Chang-Sam;Han, Doug-Young
    • 한국자기공명학회논문지
    • /
    • 제14권1호
    • /
    • pp.38-44
    • /
    • 2010
  • In liquids NMR, $^{1}H$ is the most widely observed nucleus, which is not the case in solids NMR. The reason is due to the strong homo-dipolar interactions between the hydrogen atoms which mask the useful chemical shift information. Therefore we must remove the strong homo-dipolar interactions in order to get structural information, which can be investigated by the isotropic chemical shift. There are two ways of obtaining it. One is the ultra-fast MAS of ca. 70 kHz spinning speed, which has become available only recently. The other way is devising a pulse sequence which can remove the strong homo-dipolar interaction. In the latter way, MAS with a moderate spinning rate of a few kHz, is enough to remove the chemical shift anisotropy. In this report, 1D-CRAMPS and 2D MASFSLG techniques are utilized and their results will be compared. This kind of highresolution $^{1}H$ NMR for solids, should become a valuable analytical tool in the understanding and the developing of a new class of hydrogen storage materials. Here ammonium borane $-NH_{3}BH_{3}$, whose hydrogen content is high, is used as a sample.

HR-MAS NMR Technique for Metabolic Profiling of Powdery Ginseng

  • Yoon, Dahye;Jo, Ick-Hyun;Kim, Suhkmann
    • 한국자기공명학회논문지
    • /
    • 제20권3호
    • /
    • pp.82-86
    • /
    • 2016
  • Ginseng is used as a medicinal ingredient. The quality control of species, age, origin and manufacturing process is important. The metabolome of ginseng about quality was studied in many reports. Almost studies carried out the extract of ginseng, however, the reproducibility cannot be obtained using extracted sample. In this study, powdery ginseng samples were analyzed using high resolution-magic angle spinning nuclear magnetic resonance (HR-MAS NMR)-based metabolomics except extraction step. Sample was measured three times using 600 MHz NMR spectrometer equipped with nano probe. Reproducibility can be enhanced using this method and the metabolic profiles of ginseng were identified and quantified.

High-resolution 1H NMR Spectroscopy of Green and Black Teas

  • Jeong, Ji-Ho;Jang, Hyun-Jun;Kim, Yongae
    • 대한화학회지
    • /
    • 제63권2호
    • /
    • pp.78-84
    • /
    • 2019
  • High-resolution $^1H$ NMR spectroscopic technique has been widely used as one of the most powerful analytical tools in food chemistry as well as to define molecular structure. The $^1H$ NMR spectra-based metabolomics has focused on classification and chemometric analysis of complex mixtures. The principal component analysis (PCA), an unsupervised clustering method and used to reduce the dimensionality of multivariate data, facilitates direct peak quantitation and pattern recognition. Using a combination of these techniques, the various green teas and black teas brewed were investigated via metabolite profiling. These teas were characterized based on the leaf size and country of cultivation, respectively.

고분해능 NMR 분석법에 의한 에틸렌글리콜과 1, 4-시클로헥산디메탄올의 테레프탈산 공중합체의 화학구조 연구 (Chemical Structure Study on Copolyterephthalates Based on Ethylene Glycol and 1, 4-Cyclohexane Dimethanol by High Resolution NMR Analysis)

  • 유희열;김상욱
    • 공업화학
    • /
    • 제4권4호
    • /
    • pp.770-775
    • /
    • 1993
  • 에틸렌글리콜과 1, 4-시클로헥산디메탄올의 테레프탈산 공중합체인, poly(ethylene terephthalate-co-1, 4-cyelohexylene dimethylene terephthalate), P(ET-CT)의 화학 구조를 고분해능 NMR 분석을 통하여 조사하였다. $^1H$ NMR 분석에서 메칠렌기에 의한 chemical shift가 ET, 트란스 CT, 및 시스 CT로 분리됨에 따라 공중합조성 및 이성질체의 비율을 구할 수 있었다. $^{13}C$ NMR 분석에서 카르보닐기에 연결된 벤젠기의 탄소가 diad로 분리됨에 따라 공중합 연쇄 분포(copolymer sequence distribution)를 구한 결과, P(ET-CT) 공중합체는 랜덤공중합체임이 판명되었다. 아울러 랜덤 통계식을 이용하여 공중합 연쇄의 분포 및 평균길이를 구할 수 있었다.

  • PDF

다성분계 현무암질 비정질 규산염의 원자 구조에 대한 고상핵자기 공명 분광분석연구 (Probing Atomic Structure of Quarternary Aluminosilicate Glasses using Solid-state NMR)

  • 박선영;이성근
    • 한국광물학회지
    • /
    • 제22권4호
    • /
    • pp.343-352
    • /
    • 2009
  • 특정 원자 중심의 정보를 제공해주는 고분해능 고상핵자기 공명 분광분석(NMR)은 현무암질 마그마를 포함한 대부분의 자연계의 다성분계 규산염 용융체의 원자 구조 분석에 적합하다. 본 연구에서는 일차원과 이차원 고상 NMR을 이용하여 현무암질 마그마의 모델 시스템인 CMAS (CaO-MgO-$Al_2O_3-SiO_2$) 비정질 규산염의 조성에 따른 원자 구조의 변화를 규명하였다. $^{27}Al$ MAS NMR 실험 결과 모든 조성에대해 $^{[4]}Al$ 피크가 지배적으로 나타나고 이는 $Al^{3+}$이 네트워크 형성 이온으로 작용한다는 것을 지시한다. $X_{MgO}$가 증가함에 따라 피크 위치가 음의 방향으로 4.7 ppm 이동하며 이는 조성에서 Si의 상대적인 양이 증가할수록 $Q^4$(4Si)가 증가하는 것을 의미하고 이를 통해 Al 주변의 산소가 모두 연결 산소(BO, bridging oxygen)임이 확인되었다. $^{17}O$ NMR 실험 결과 비정질 $CaMgSi_2O_6$에 있는 비연결 산소의 상대적 양이 $CaAl_2SiO_6$에 있는 비연결 산소보다 정성적으로 많은 것이 확인되었다. 모델 사성분계 비정질 알루미노규산염에 대한 $^{17}O$ 3QMAS NMR 실험결과 Al-O-Al, Al-O-Si, Si-O-Si의 연결 산소와 {Ca, Mg}-NBO의 원자 환경이 구별되며 이 실험 결과는 자연계에서 나타나는 다양한 조성의 다성분계 비정질에 대해서도 이차원 3QMAS NMR 실험을 이용하여 원자구조를 규명할 수 있는 가능성을 제시한다.