• Title/Summary/Keyword: Solution NMR

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$^{17}O$ 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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Solution Nuclear Magnetic Resonance Spectral Characterization of Iron(II) Porphyrin Complexes of Weakly Coordinating Anions

  • Song, Byung-Ho;Park, Bong-Jin;Han, Chul-Hee
    • Bulletin of the Korean Chemical Society
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    • v.23 no.1
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    • pp.119-122
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    • 2002
  • Weakly coordinating anions show little affinity for binding to unfunctionalized iron(II) porphyrins. The electron-deficient 5, 10, 15, 20-tetrakis(pentafluorophenyl)porphinatoiron(II) compound is utilized in this study to demonstrate solution coordination by chloride, bromide and acetate ions. The binding strength of anions to the iron(II) porphyrin is reflected by a systematic change in pyrrole proton chemical shift in $^1H$ NMR spectra; the pyrrole resonance moves downfield when the ${\sigma}$-donor ability of anions is decreased.

A Study on Minimum Volume of Highly Homogeneous Superconducting Coil (균일자장 초전도코일의 체유최소화에 관한 연구)

  • 이승원;권영안
    • The Transactions of the Korean Institute of Electrical Engineers
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    • v.34 no.1
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    • pp.38-43
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    • 1985
  • Since the superconductor type II with high critical current and high critical magnetic field was discovered in 1961, there were many studies on the superconducting coil for high field and highly homogeneous field. The graphical method and the numerical method by Newton Raphson technique have been studied as the method for design of homogeneous superconducting coil. It is comparatively easy to get a compensating coil for any given main coil by the above methods, but it is too laborious to get a general solution for main coil dimension. This paper studies the optimal design method for minimum volume of superconducting coil under certain central field and highly homogeneous field. The present method makes use of the nonlinear programming for optimization. The optimal solution of NMR superconducting coils by this method are demonstrated very well.

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Partial Solution for Concomitant Gradient Field in Ultra-low Magnetic Field: Correction of Distortion Artifact

  • Lee, Seong-Joo;Shim, Jeong Hyun
    • Journal of the Korean Magnetic Resonance Society
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    • v.24 no.3
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    • pp.66-69
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    • 2020
  • In ultra-low field magnetic resonance imaging (ULF-MRI), the strength of a static magnetic field can be comparable to that of gradient field. On that occasion, the gradient field is accompanied by concomitant gradient field, which yields distortion and blurring artifacts on MR images. Here, we focused on the distortion artifact and derived the equations capable of correcting it. Its usefulness was confirmed through the corrections in both simulated and experimental images. This solution will be effective for acquiring more accurate images in low and/or ultra-low magnetic fields.

Operating characteristics of linear type magnetic flux pump (리니어타잎 초전도 전원장치의 동작특성)

  • Chung, Yoon-Do;Bae, Duck-Kweon;Yoon, Yong-Soo;Ko, Tae-Kuk
    • Proceedings of the KIEE Conference
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    • 2008.07a
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    • pp.665-666
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    • 2008
  • Inserted HTS (high temperature superconducting) coil is promisingly expected as a solution for achievement of higher fields such as GHz scale NMR magnet. However, HTS magnet causes persistent current decay in the persistent current mode and this decay should be compensated in order to keep stable magnetic field. As a solution for the decay in the HTS magnets, we proposed a new type superconducting power supply, i.e., linear type magnetic flux pump (LTMFP). The LTMFP mainly consists of DC bias coil, 3-phase AC coil and superconducting Nb foil. The compensating current in closed superconductive circuit can be easily controlled by the intensity of 3-phase AC current and its frequency. In this study, it has been investigated that the flux pump can effectively charge the current for various frequencies according to the different load magnets.

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Synthesis of Polycarbosilane for SiC Precursor (SiC의 Pricursor Polycarbosilan의 합성)

  • Han, Chul;Han, In-Seop;Lee, Hyung-Bock;Chung, Yun-Joong
    • Journal of the Korean Ceramic Society
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    • v.25 no.1
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    • pp.49-53
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    • 1988
  • Polycarbosilane was synthesized from the pyrolysis of polydimethylsilane, which is dechlorinated from dimethyldichlorosilane. The pyrolysis temperature was varied at 280-480$^{\circ}C$ for 2 hours. FT-IR, FT-NMR and GPC measurement were studied on the residue inside the reaction crucible and viscous solution inside the cooling zone respectively. From the viscous solution in the cooling zone at 420$^{\circ}C$, the synthesis of polycarbosilane wa well detected.

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Induced Eye-detectable Blue Emission of Triazolyl Derivatives via Selective Photodecomposition of Chloroform under UV Irradiation at 365 nm

  • Lee, Byoung-Kwan;Yoon, Jun Hee;Yoon, Sangwoon;Cho, Byoung-Ki
    • Bulletin of the Korean Chemical Society
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    • v.35 no.1
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    • pp.135-140
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    • 2014
  • A bent-shape triazolyl derivative was synthesized via click chemistry, and its photophysical property was investigated in various solvents. In contrast to the invisible ultraviolet emission of other solutions, the chloroform solution exhibited a blue light emission at 460 nm. Furthermore, the blue fluorescence intensified as the UV exposure time at 365 nm increased. On the basis of $^1H$-NMR, pH paper, and acid-addition studies, we confirmed that chloroform was decomposed into HCl with the aid of the triazolyl derivative. The density functional theory calculations suggested that the eye-detectable blue fluorescence was attributed to an intramolecular charge transfer process of the protonated triazolyl derivative in the chloroform solution.

Well-Defined Thermoresponsive Copolymers with Tunable LCST and UCST in Water

  • Jung, Seo-Hyun;Lee, Hyung-Il
    • Bulletin of the Korean Chemical Society
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    • v.35 no.2
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    • pp.501-504
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    • 2014
  • A thermoresponsive polymer, poly(2-(dimethylamino)ethyl methacrylate) (PDMAEMA), was successfully synthesized by atom transfer radical polymerization (ATRP). Different amounts of 1,3-propanesultone were used as quaternization agent to transit the PDMAEMA into partially modified poly(zwitterions), resulting in p[DMAEMA-co-3-dimethyl(methacryloyloxyethyl)ammonium propanesulfonate] (PDMAEMA-co-PDMAPS). Molecular weight, molecular weight distribution, and degree of quarternization were determined by gel permeation chromatography (GPC) and 1H NMR spectroscopy. The transmission spectra of the 1.0 wt % aqueous solutions of the resulting polymers at 650 nm were measured as a function of temperature. Results showed that the lower critical solution temperature (LCST) and the upper critical solution temperature (UCST) could be easily controlled by the different composition of dimethylamino and zwitterion groups. The effect of partial quaternization on thermoresponsive properties was also studied by dynamic light scattering (DLS) with the same aqueous concentration (1.0 wt %) as employed for turbidimetry studies. The LCST and UCST values measured by DLS correlated well with those determined by turbidimetry.

The Photo-reproducibility and Stability of Long Chain Fatty Acid Containing Azobenzene (아조벤젠을 함유한 장쇄 지방산의 광재현성과 안정성에 관한 연구)

  • Par, Keun-Ho;Park, Tae-Gone
    • Journal of the Korean Applied Science and Technology
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    • v.12 no.1
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    • pp.109-114
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    • 1995
  • The Synthesis of long chain fatty acid containing azobenzene and $(C_{n}-Azo)$ was optimized, starting from p-(p'-hydroxy phenyl azo)-benzoic acid and the product of reaction containing azobenzene chromophores was investigated by ultraviolet spectrophotometery in chloroform solvent at the various temperature. In addition, Reversibility and stability of azo compounds have been measured by means of Ultraviolet and the structure of these compound were ascertained by means of FT-IR and NMR. Recrystallization of reaction product in the solvent results the experimental yield obtained about 62.93% p-(p'-octadecyloxy phenyl azo)-benzoic acid. Long chain azobenzene derivatives in chloroform solution are induced photoisomerization by u. v. and visible light irradiation. The solution of long chain fatty acids$(C_{n}-Azo)$ containing azobenzene are possible of being applied to functional molecular devices such as photomemory and light switching.

Synthesis and Solution Chemistry of Metal Hydrides from Cationic Rhodium(I) Catalyst Precursors [(L-L)Rh(NBD)]$ClO_4 (L-L=Fe({\eta}^5-C_5H_4PBu^t\;_2)_2,\;Fe{\eta}^5-C_5H_4PPhBu^t)_2)$

  • Tae-Jeong Kim
    • Bulletin of the Korean Chemical Society
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    • v.11 no.2
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    • pp.134-139
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    • 1990
  • The hydrogenation catalyst precursors $[(L-L)Rh(NBD)]ClO_4\;(L-L=Fe({\eta}^5-C_5H_4PBu^t\;_2)_2,\;Fe({\eta}^5-C_5H_4PPhBu^t)_2$; NBD = norbornadiene) react with $H_2(1\;atm,\;30^{\circ}C$, MeOH) to yield $[(L-L)HRh({\mu}-H)_3RhH(L-L)]ClO_4$. These hydrido species are fluxional, and variable temperature NMR studies show the existence of a number of equilibria involving both fluxional and non-fluxional species. The synthesis, solution structures, and fluxional behaviors of these hydrides are described.