• Title/Summary/Keyword: NMR spectrometer

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A Design for a Home-Built Solid State NMR Spectrometer

  • Yang Doo-Kyung;Zax David B.
    • Journal of the Korean Magnetic Resonance Society
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    • v.10 no.1
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    • pp.74-88
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    • 2006
  • Since the first commercial NMR spectrometer came out in 1953 from Varian, much of the hardware development has been improved and matured through commercial equipments. Many of magnetic resonance laboratories however still build and use home-built spectrometers, which are satisfactory even with the consideration of educational purpose only. The home-built NMR spectrometer could be further advantageous and could be often an only option for investigating new ideas with demanding experimental conditions or new hardware support. A solid state NMR spectrometer was designed with extra interest in stochastic experiment and built for an 8.93 T superconducting magnet from Oxford instrument. Super-heterodyned system was implemented for the transmitter and receiver parts. Intermediate frequency (IF) for the heterodyne system was chosen to 70 MHz for the first and the second channels, with additional 120 MHz for the third channel for maximum NMR frequency capability. We will show overall schematics, and discuss the designs with detailed diagrams, then demonstrate the applicability of home-built spectrometer with stochastic-excitation in solid state NMR and in applications to quadrupolar nuclear Spins.

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Constructing Overhauser Dynamic Nuclear Polarization-Nuclear Magnetic Resonance System Using Benchtop Electron Paramagnetic Resonance Spectrometer

  • Saun, Seung-Bo;Kim, JiWon;Han, Oc Hee
    • Journal of the Korean Magnetic Resonance Society
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    • v.22 no.2
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    • pp.34-39
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    • 2018
  • The Nuclear Magnetic Resonance (NMR) technique using Dynamic Nuclear Polarization (DNP) procedures is one of the promising techniques that enable overcoming low sensitivity problems in NMR spectroscopy. We constructed an ODNP-NMR system using a commercial benchtop EPR spectrometer. The $^1H$ NMR peak area of water in aqueous solutions of 4-hydroxy-TEMPO was enhanced more than 95 times in the ODNP-NMR experiments. Our signal enhancement results were about 55% of the previously reported result. This could be due to non-uniform microwave power over a sample and unwanted sample heating by microwave. However, this portable ODNP-NMR spectrometer will be eventually useful for site-specific detection with nano-scale spatial resolutions and molecular dynamics studies with significantly improved signal sensitivity.

The ALTADENA and PASADENA studies in benchtop NMR spectrometer

  • So, Howon;Jeong, Keunhong
    • Journal of the Korean Magnetic Resonance Society
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    • v.23 no.1
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    • pp.6-11
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    • 2019
  • Parahydrogen induced hyperpolarization (PHIP) technique is extensively studied to increase the sensitivity of the conventional NMR spectroscopy and recently try to apply this advanced technique into the revolutionary future of the MRI. The other hyperpolarization technique, which is widely utilized, is DNP (Dynamic Nuclear Polarization)-based hyperpolarization one. Despite its great advances in these fields, it contains several drawbacks to overcome: fast relaxation time, expensive equipment is needed, long build-up time is required (several hours), and batch scale material is hyperpolarized. To overcome all those limitations, one can effectively harness the hyperpolarized spin state of parahydrogen. One important step for utilizing the spin state of parahydrogen is doing well-developed experiments of ALTADENA and PASADENA. Based on those concepts, we successfully obtain the hydrogenation signals of ALTADENA and PASADENA from styrene by using benchtop NMR spectrometer. Also those signals were conceptually analyzed and confirmed with different mechanisms. To our best knowledge, those experiments using 1.4T (benchtop NMR) is the first reported one. Considering these experiments, we hope that parahydrogen-based hyperpolarization transfer studies in NMR/MRI will be broadened in Korea in the future.

FT-NMR as an analytical tool for identification of inert materials in crop protection products (농약제품분석의 정성분석도구로서 FT-NMR)

  • Choi, Dal-Soon;Kyung, Suk-Hun;Hong, Su-Myeong;Jin, Yong-Duk;Lee, Hea-Keun;Kim, Jin-Hwa;Ryu, Gab-Hee
    • The Korean Journal of Pesticide Science
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    • v.8 no.2
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    • pp.88-94
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    • 2004
  • In order to evaluate NMR spectrometer as the analytical tool for identification of individual adjuvant in crop protection products, the standard sample of individual adjuvant was analyzed by NMR spectrometer and then the formulation of crop protection products was also analyzed. Almost polymer system of surfactant was a co-polymer and there was an excess of ethylene. The most intense signal comes from long polyethylene blocks, 70.5 ppm. The carbonyl groups of ester group resonate at 173.5 ppm. Analytical sample was prepared in NMR tube without extraction, cleanup, concentration, or chromatographic separation. Identification of individual adjuvant in crop protection products was conducted by comparison of sample and reference spectra. NMR spectrometer was useful to analyze adjuvant in crop protection products without preparation process.

Composition and structure analysis of natural gas hydrates

  • 박영준;김도연;박제성;이흔
    • 한국신재생에너지학회:학술대회논문집
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    • 2005.06a
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    • pp.660-662
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    • 2005
  • 본 연구에서는 미 인근 해저에서 ODP로 확인된 부존 하이드레이트 샘플을 다양한 분광학 및 실험적 분석 방법을 통해 시료의 물성 및 특성을 파악하여 부존된 하이드레이트 자원의 성분 파악을 목적으로 하고 있다. 일반적으로 가스 하이드레이트 연구에 있어서 X-ray diffractometer, NMR stectrometer, Raman spectrometer 등 분광학적 분석기기를 이용하여 가스 하이드레이트의 구조 및 성분을 규명한다. 본 연구에서는 실험실에서 인위적으로 만들어진 메탄 하이드레이트와 심해저 천연가스 하이드레이트 층에서 채취된 샘플의 비교 분석을 통하여 심해에 매장되어 있는 천연가스 하이드레이트의 구조 및 성분을 규명하였다 XRD 결과로부터 천연가스 하이드레이트는 sI의 구조를 가지며 NMR 및 Raman 결과에 의하면 하이드레이트 내에 포집되어 있는 가스의 주 성분은 메탄인 것으로 밝혀졌다. 또한 천연가스 하이드레이트를 이용한 이산화탄소의 치환 실험을 통하여 심해저 천연가스 하이드레이트 층의 이산화탄소 저장 매체로의 활용 가능성을 조사하였다.

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NEAR INFRARED TRANSFLECTANCE SPECTROSCOPY (NIRS) IN PHYTOCHEMISTRY

  • Huck, C.W.;W.Guggenbichler;Bonn, G.K.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.3114-3114
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    • 2001
  • During the last years phytochemistry and phytopharmaceutical applications have developed rapidly and so there exists a high demand for faster and more efficient analysis techniques. Therefore we have established a near infrared transflectance spectroscopy (NIRS) method that allows a qualitative and quantitative determination of new polyphenolic pharmacological active leading compounds within a few seconds. As the NIR spectrometer has to be calibrated the compound of interest has at first to be characterized by using one or other a combination of chromatographic or electrophoretic separation techniques such as thin layer chromatography (TLC), high performance liquid chromatography (HPLC), capillary electrophoresis (CE), gas chromatography (GC) and capillary electrochromatography (CEC). Both structural elucidation and quantitative analysis of the phenolic compound is possible by direct coupling of the mentioned separation methods with a mass spectrometer (GC-MS, LC-MS/MS, CE-MS, CEC-MS) and a NMR spectrometer (LC-NMR). Furthermore the compound has to be isolated (NPLC, MPLC, prep. TLC, prep. HPLC) and its structure elucidated by spectroscopic techniques (UV, IR, HR-MS, NMR) and chemical synthesis. After that HPLC can be used to provide the reference data for the calibration step of the near infrared spectrometer. The NIRS calibration step is time consuming, which is compensated by short analysis times. After validation of the established NIRS method it is possible to determine the polyphenolic compound within seconds which allows to raise the efficiency in quality control and to reduce costs especially in the phytopharmaceutical industry.

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Development of Remote Data Analysis System for the Joint Use of Equipments (분석기기지원을 위한 원격 데이터 분석 시스템 개발)

  • 최인식
    • Journal of Korea Technology Innovation Society
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    • v.2 no.3
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    • pp.94-106
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    • 1999
  • In Korea Basic Science Institute(KBSI) the remote data analysis system is developed for the joint use of advanced equipments. This system enables the researchers to access the datas which are produced at KBSI and analyse them by Java program on the Web,. Except Web browser such as Internet Explorer or Netscape Navigator no additional softwares are required for analysing data. We have developed remote data analysis systems for five major equipments which KBSI supports for the researchers, The systems which are developed are those for NMR spectrometer High Reso-lution Tandem mass Spectrometer Microscopic Imaging System DNA Sequencer and Natural Ra-dioactivity Measruement System, These programs work on any computer platform and any operat-ing system only if the internet is available. This remote data analysis system will be served as a part of Collaboratory the remote collaborative system.

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Composition and Temperature Dependence of Structural Changes in Borosilicate Glasses by Spectrometer (분광계에 의한 Borosilicate계 글라스의 조성 및 온도의존성 평가)

  • Park Sung-Je;Ryu Bong-Ki
    • Korean Journal of Materials Research
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    • v.15 no.12
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    • pp.786-790
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    • 2005
  • We investigated the particularity of temperature and composition changes in $xNa_2O{\cdot}(52.5-x)B_2O_3{\cdot}47.5SiO_2$ glasses by use of FT-IR, $^{11}B$ NMR, Raman spectrometer. From FT-IR and $^{11}B$ NMR spectrometer, we thought that tetrahedral boron, $BO_4$ units are created $N_4$ increasing tendency generated near $600^{\circ}C$. It's expected that composition ana heat treatment directly contributed to structural changes, this changes are following to $Na_2O$ increasing or decreasing. caused by $N_4\;and\;BO_4$ units are caused by relatively increasing or decreasing in the glasses' structure. Particularly, $BO_4$ units are converted to $BO_3$ units after $600^{\circ}C$ heat treatment for 50h in the composition of $x<18(R<0.5,\;R=Na_2O/B_2O_3\;mol\%)$. On the order hand, $BO_3$ units are converted to, $BO_4$ units after $600^{\circ}C$ heat treatment for 50h in the composition of $x{\geq}18\;(R>0.5)$. This particularity of composition and temperature dependence of structural changes are similarly represented by Raman analysis results.

1H-NMR Analysis according to the Storage Period after the Use of Iopamidol and Ioversol Formulations Contrast Agents (Iopamidol과 Ioversol 제제 조영제의 사용 후 보관 기간에 따른 1H-NMR 분석)

  • Han, Beom-Hee
    • Journal of radiological science and technology
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    • v.44 no.3
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    • pp.239-245
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    • 2021
  • Since the side effects of contrast agents occur in many ways, hospitals must clearly identify the contrast agents and know how to manage them. Storage of contrast media It is common practice to store contrast media in a warm room to reduce viscosity and improve patient comfort. However, it is important to recognize that long-term storage at high temperatures can shorten the shelf life of a product. Therefore, in this study, the presence or absence of chemical changes according to the storage period after using the contrast medium was analyzed. As the analysis equipment, a 500 MHz Nuclear Magnetic Resonance Spectrometer of Bruker Avance (Germany) possessed by Korea Basic Science Institute (KOREA BASIC SCIENCE INSTITUTE; KBSI) was used. For the X-ray iodide contrast medium, Pamiray contrast medium of Iopamidol and Optiray contrast medium of Ioversol, samples remaining after 7 days, 20 days, 30 days, and 1 year were collected, By acquiring the spectrum from the 1H-NMR spectrometer of the contrast medium stimulated by It was compared and analyzed with the standard sample. In conclusion, depending on the storage period of the contrast medium, no peaks of physical and chemical changes were observed in both the Pamiray contrast medium of Iopamidol and the Optiray contrast medium of Ioversol after 7 days, 20 days, 30 days, and 1 year after use.

A Study on the 300MHz NMR Transceiver (300MHz급 NMR Transceiver 설계 및 제작)

  • Park, Yang-Ha;Jin, Seung-Oh;Won, Jin-Im;Huh, Young
    • Proceedings of the KIEE Conference
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    • 2000.07d
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    • pp.3210-3212
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    • 2000
  • We designed and manufactured 300MHz NMR RF Transceiver. NMR system is composed of NMR Spectrometer, Superconductive Magnet and Pulse Programmer, GUI. NMR RF Transceiver is composed of transmitter, receiver, frequency synthesizer. T/R switch, main power amp., RF coil. To phase modulation, transmitter is composed of mixer, splitter and combiner et al. To weak signal detection, receiver is composed of pre-amp., filter, mixer et al. Each module is manufactured PCB. And installed NMR system to detect chemical component of specimen. In result, we can get the information of specimen.

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