• Title/Summary/Keyword: High-resolution NMR

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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
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    • v.32 no.7
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    • pp.2345-2350
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    • 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
    • Journal of the Korean Magnetic Resonance Society
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    • v.24 no.2
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    • pp.59-65
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    • 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.

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

  • Yi, Jeong-Han;Oh, Woo-Jin;Cho, Zang-Hee
    • Proceedings of the KOSOMBE Conference
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    • v.1990 no.11
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    • pp.48-51
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    • 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.

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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
    • Journal of the Korean Magnetic Resonance Society
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    • v.14 no.1
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    • pp.38-44
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    • 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
    • Journal of the Korean Magnetic Resonance Society
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    • v.20 no.3
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    • pp.82-86
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    • 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
    • Journal of the Korean Chemical Society
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    • v.63 no.2
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    • pp.78-84
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    • 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.

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

  • Yoo, Hee-Yeoul;Kim, Sang-Wook;Okui, Norimasa
    • Applied Chemistry for Engineering
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    • v.4 no.4
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    • pp.770-775
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    • 1993
  • Chemical structure of poly(ethylene terephthalate-co-1, 4-cyclohexylene dimethylene terephthalate), P(ET-CT) copolyesters was investigated by High Resolution NMR analysis. The copolymer composition and isomeric ratio were determined by methylene resonance peaks which were separated into three peaks corresponding to ET, trans CT and cis CT units, respectively. The copolymer sequence distribution was evaluated from the carbon resonance peaks connected to carbonyl groups in benzene, indicating died distribution. According to statistics model, these copolyesters are almost random copolymers. The copolymer sequence distribution could be simulated and its averaged length was calculated by random copolymer statistics.

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

  • Park, Sun-Young;Lee, Sung-Keun
    • Journal of the Mineralogical Society of Korea
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    • v.22 no.4
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    • pp.343-352
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    • 2009
  • High-resolution Solid-state NMR provides element specific and quantitative information and also resolves, otherwise overlapping atomic configurations in multi-component non-crystalline silicates. Here we report the preliminary results on the effect of composition on the structure of CMAS (CaO-MgO-$Al_2O_3-SiO_2$) silicate glasses, as a model system for basaltic magmas, using the high-resolution 1D and 2D solid-state NMR. The $^{27}Al$ MAS NMR spectra for the CMAS silicate glasses show that four-coordinated Al is predominant, demonstrating that $Al^{3+}$ is network forming cation. The peak position moves toward lower frequency about 4.7 ppm with increasing $X_{MgO}$ due to an increase in $Q^4$(4Si) fraction with increasing Si content, indicating that Al are surrounded only by bridging oxygen. $^{17}O$ MAS NMR spectra for $CaAl_2SiO_6$ and $CaMgSi_2O_6$ glasses qualitatively suggest that NBO fraction in the former is smaller than that in $CaMgSi_2O_6$ glasses. As $^{17}O$ 3QMAS NMR spectrum of model quaternary aluminosilicate glass resolved distinct bridging and non-bridging oxygen environments, atomic structure for natural magmas can also be potentially probed using high-resolution 3QMAS NMR.