• Title/Summary/Keyword: NMR measurements

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The Characterization of Borohydride-Stabilized Nanosilvers in Laponite Sol Using 1H NMR: Its Ligand Exchange Reactions with MUA and TOP

  • Seo, Jae-Seok;Son, Dong-Min;Lee, Han-Na;Kim, Jee-Kwang;Kim, You-Hyuk
    • Bulletin of the Korean Chemical Society
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    • v.30 no.11
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    • pp.2651-2654
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    • 2009
  • In borohydride-protected nanosilvers in laponite sol, the silver particles aggregate to form short chains and a dumbbell shape. The $^{1}H$ NMR measurements in this study represent, to our knowledge, the first observation of proton resonances of borohydride-protected nanosilvers in aqueous solution. Borohydride on nanosilver can be exchanged with 11-mercaptoundecanoic acid (MUA) or trioctylphosphine (TOP). Transmission electron microscopy and UV-Vis spectroscopy data show that the number of aggregated silver nanoparticles decreases upon addition of aforementioned ligands due to the formation of silver MPCs (monolayer-protected clusters). Adsorption of MUA or TOP on nanosilver is confirmed through the observation of broad proton resonances of MPCs in $^{1}H$ NMR spectra.

PMR in Organic Plastic Crystals (I). Pivalic Acid (유기플라스틱 결정체의 PMR 연구 (제 1 보). 피발산)

  • Stefan J. K. Choi;John D. Graham
    • Journal of the Korean Chemical Society
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    • v.19 no.3
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    • pp.149-155
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    • 1975
  • Pivalic acid, which has a globular shape and is a plastic crystal, has been examined by means of temperature-dependent with-line proton magnetic resonance spectroscopy. Results of temperature-dependent line width, second moment, and spin-lattice relaxation time studies of pivalic acid were interpreted in terms of dynamic behavior and hydrogen bonding. The dynamic behavior consists of superimposed reorientation of the methyl groups about their three-fold axes$(C_3) and of the molecule about the central C-C bond(C_3'),$ general molecular reorientation about the center of gravity, and molecular self-diffusion. Activation energies for the motional processes have been obtained from line width measurements using the modified Bloembergen, Purcell, and Pound theory and from spin-lattice relaxation time measurements. The results were compared with the Pople-Karasz theory of fusion and the agreement was found to be poor. The discrepancy was interpreted in terms of hydrogen bonding in this molecule.

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Analysis and reduction of thermal magnetic noise in liquid-He dewar for sensitive low-field nuclear magnetic resonance measurements

  • Hwang, S.M.;Yu, K.K.;Lee, Y.H.;Kang, C.S.;Kim, K.;Lee, S.J.
    • Progress in Superconductivity and Cryogenics
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    • v.15 no.2
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    • pp.20-23
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    • 2013
  • For sensitive measurements of micro-Tesla nuclear magnetic resonance (${\mu}T$-NMR) signal, a low-noise superconducting quantum interference device (SQUID) system is needed. We have fabricated a liquid He dewar for an SQUID having a large diameter for the pickup coil. The initial test of the SQUID system showed much higher low-frequency magnetic noise caused by the thermal magnetic noise of the aluminum plates used for the vapor-cooled thermal shield material. The frequency dependence of the noise spectrum showed that the noise increases with the decrease of frequency. This behavior could be explained from a two-layer model; one generating the thermal noise and the other one shielding the thermal noise by eddy-current shielding. And the eddy-current shielding effect is strongly dependent on the frequency through the skin-depth. To minimize the loop size for the fluctuating thermal noise current, we changed the thermal shield material into insulated thin Cu mesh. The magnetic noise of the SQUID system became flat down to 0.1 Hz with a white noise of 0.3 $fT/{\surd}Hz$, including the other noise contributions such as SQUID electronics and magnetically shielded room, etc, which is acceptable for low-noise ${\mu}T$-NMR experiments.

Wide-line NMR and DSC studies on intrinsically disordered p53 transactivation domain and its helically pre-structured segment

  • Tompa, Peter;Han, Kyou-Hoon;Bokor, Monika;Kamasa, Pawel;Tantos, Agnes;Fritz, Beata;Kim, Do-Hyoung;Lee, Chewook;Verebelyi, Tamas;Tompa, Kalman
    • BMB Reports
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    • v.49 no.9
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    • pp.497-501
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    • 2016
  • Wide-line 1H NMR intensity and differential scanning calorimetry measurements were carried out on the intrinsically disordered 73-residue full transactivation domain (TAD) of the p53 tumor suppressor protein and two peptides: one a wild type p53 TAD peptide with a helix pre-structuring property, and a mutant peptide with a disabled helix-forming propensity. Measurements were carried out in order to characterize their water and ion binding characteristics. By quantifying the number of hydrate water molecules, we provide a microscopic description for the interactions of water with a wild-type p53 TAD and two p53 TAD peptides. The results provide direct evidence that intrinsically disordered proteins (IDPs) and a less structured peptide not only have a higher hydration capacity than globular proteins, but are also able to bind a larger amount of charged solute ions.

$^{13}C$ Nuclear Magnetic Resonance Study of Graphite Intercalated Superconductor $CaC_6$ Crystals in the Normal State ($CaC_6$ 결정에 대한 정상상태에서의 $^{13}C$ 핵자기공명 측정)

  • Kim, Sung-Hoon;Kang, Ki-Hyeok;Mean, B.J.;Ndiaye, B.;Lee, Moo-Hee;Kim, Jun-Sung
    • Progress in Superconductivity
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    • v.12 no.1
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    • pp.51-56
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    • 2010
  • $^{13}C$ NMR (nuclear magnetic resonance) measurements have been performed to investigate the local electronic structure of a superconducting graphite intercalation compound $CaC_6$ ($T_c$ = 11.4 K). A large number of single crystals were stacked and sealed in a quartz tube for naturally abundant $^{13}C$ NMR. The spectrum, Knight shift, linewidth, and spin-lattice relaxation time $T_1$ were measured in the normal state as a function of temperature down to 80 K at 8.0 T perpendicular to the c-axis. The $^{13}C$ NMR spectrum shows a single narrow peak with a very small Knight shift. The Knight shift and the linewidth of the $^{13}C$ NMR are temperature-independent around, respectively, +0.012% and 1.2 kHz. The spin-lattice relaxation rate, $1/T_1$, is proportional to temperature confirming a Korringa behavior as for non-magnetic metals. The Korringa product is measured to be $T_1T\;=\;210\;s{\cdot}K$. From this value, the Korringa ratio is deduced to be $\xi$ = 0.73, close to unity, which suggests that the independent-electron description works well for $CaC_6$, without complications arising from correlation and many-body effects.

A Review on nuclear magnetic resonance logging: fundamental theory and measurements (자기공명검층: 기본 이론 및 자료 측정)

  • Jang, Jae Hwa;Nam, Myung Jin
    • Geophysics and Geophysical Exploration
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    • v.15 no.4
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    • pp.235-244
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    • 2012
  • Nuclear magnetic resonance (NMR) logging has been considered one of the most complicated nevertheless, one of the most powerful logging methods for the characterization on of both rocks and natural fluids in formation. NMR measures magnetized signals (polarization and relaxation) between the properties of hydrogen nucleus called magnetic moment and applied magnetic fields. The measured data set contains two important petrophysical properties such as density of hydrogen in the fluids inside the pore space and the distinct decay rate for fluid type. Therefore, after the proper data processing, key petrophysical information, not only the quantities and properties of fluids but also supplies of rock characterization in a porous medium, could be archived. Thus, based on this information, several ongoing researches are being developed in estimating aspects of reservoir productivity information, permeability and wettability since it is the key to having correct interpretation. This study goes through the basic theory of NMR at first, and then reviews NMR logging tools as well as their technical characteristics. This paper also briefly discusses the basic knowledge of NMR simulation algorithm by using Random walk.

$^{17}O$ NMR Study On Water Excharge Rate of Paramagnetic Contrast Agents ($^{17}O$ NMR 기법을 이용한 상자성 자기공명조영제의 물분자 교환에 관한 연구)

  • Yongmin Chang;Sung Wook Hong;Moon Jung Hwang;Il Soo Rhee;Duk-Sik Kang
    • Investigative Magnetic Resonance Imaging
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    • v.5 no.1
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    • pp.33-37
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    • 2001
  • Purpose : The water exchange rate between bulk water and bound water is an important parameter in deciding the efficiency of paramagnetic contrast agents. In this study, we evaluated the water exchange rates of various Gd-chelates using oxygen-17 NMR technique. Material and Methods : The samples (Gd-DTPA, Gd-DTPA-BMA, Gd-DOTA, Gd-EOB-DTPA) were prepared by mixing 5% $^{17}O-enriched$ water (Isotech, USA). The pH of the samples was adjusted to physiological value [pH=7.0] by buffer solution. The variable temperature $^{17}O-NMR$ measurements were performed using Bruker-600 (14.1 T, 81.3 MHz) spectrometer. Bruker VT-1000 temperature control units were used to stabilize the temperature. The $^{17}O$ spin-spin relaxation times (T2) were measured using Carr-Purcell-Meiboom-Gill (CPMG)I pulse sequence with 24 echo trains. The variable temperature T2 relaxation data were then fitted into Solomon-Bloembergen equations using least square fit algorithm to estimate the water exchange times. Results : From the measured $^{17}O-NMR$ relaxation rates, the determined water exchange rates at 300K are $0.42{\;}{\mu}s$ for Gd-DTPA, $1.99{\;}{\mu}s$ for Gd-DTPA-BMA, $0.27{\;}{\mu}s$ for Gd-DOTA, and $0.11{\;}{\mu}s$ for Gd-EOB-DTPA. The Gd-DTPA-BMA showed slowest exchange whereas Gd-EOB-DTPA had fastest water exchange rate. In addition, it was found that the water exchange rates (${\tau}_m$) of all samples had exponential temperature dependence with different decay constant. Conclusion : $^{17}O-NMR$ relaxation rate measurements, when combined with variable temperature technique, provide a solid tool for studying water exchange rate, which is very important in investigating the detailed mechanism of relaxation enhancement effect of the paramagnetic contrast agents.

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Magnetic Field Standards Using Magnetic Resonance

  • Park, Po Gyu;Kim, Wan-Seop;Joo, Sung Jung;Lee, Hyung Kew
    • Journal of the Korean Magnetic Resonance Society
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    • v.21 no.1
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    • pp.7-12
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    • 2017
  • The nuclear magnetic resonance (NMR) and atomic magnetic resonance (AMR) plays a fundamental role in achieving a high accuracy of magnetic field measurements. Magnetic field unit (T) was realized based on the shielded proton gyromagnetic ratio (${\gamma}^{\prime}_P$), helium-4 gyromagnetic ratio (${\gamma}_{4He}$) and related techniques. The magnetic field standard system has been disseminated by the NMR magnetometer and electromagnet, a Helmholtz coil system, and AMR magnetometer in the nonmagnetic laboratory. A magnetic field standard below 1 mT has been developed by using Cs and Cs- $^4He$ AMR with automatic compensation of an external magnetic field noise. The standards serve for the calibration of magnetometers and support the test of sensors and materials in the range from $5{\mu}T$ to 2.0 T with (1 to 50) ${\mu}T/T$ uncertainty (k=2).

Experimental study of unsteady thermally stratified flow (비정상 열확산 현상 의 실험적 연구)

  • 이상준;정명균
    • Transactions of the Korean Society of Mechanical Engineers
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    • v.9 no.6
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    • pp.767-776
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    • 1985
  • Unsteady thermally stratified flow caused by two-dimensional surface discharge of warm water into a oblong channel was investigated. Experimental study was focused on the rapidly developing thermal diffusion at small Richardson number. The basic objective were to study the interfacial mixing between a flowing layer of warm water and an underlying body of cold water and to accumulate experimental data to test computational turbulence models. Mean velocity field measurements were carried out by using NMR-CT (Nuclear Magnetic Resonance-Computerized Tomography). It detects quantitative flow image of any desired section in any direction of flow in short time. Results show that at small Richardson number warm layer rapidly penetrates into the cold layer because of strong turbulent mixing and instability between the two layers. It is found that the transfer ofheat across the interface is more vigorous than that of momentum. It is also proved that the NMR-CT technique is a very valuable tool to measure unsteady three dimensional flow field.

NMR Microimaging for Noninvasive Investigation of Polymers (고분자의 비파괴 연구를 위한 핵자기 공명 현미영상법)

  • Lee, D.H.;Ko, R.K.;Moon, C.H.;Cho, Z.H.
    • Proceedings of the KOSOMBE Conference
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    • v.1995 no.11
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    • pp.253-256
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    • 1995
  • Polymers have been one of the emerging biomedical materials in the area of biomedical research which are applicable to the human body. For human applications, noninvasive characterization of the biomedical polymers has been one of the important topics, and is valuable information. Among others, the swelling rate is one of the important measurements needed for the hydrophilic polymers. NMR imaging has been a suitable method for the noninvasive study of such a material since it is sensitive to many physical and biochemical changes of the specimens. In addition, NMR techniques possess many useful intrinsic properties such as the relaxation and diffusion effects. The present study has provided a noble and noninvasive method of measuring the process of swelling as well as volumetric changes occurred in polymers and drug delivery processes in a drug delivery system (DDS) together with changes of released drug. This gives information, relating with both water ingress process, volumetric changes of polymer specimens and the visualization of sequential drug delivery process. Also, this study provides more reliable method to ascertain the time dependent swelling process compared to the conventional method. The important aspects is that the proposed method is truly noninvasive and is able to ascertain time dependent processes.

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