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600 MHz FT-NMR (Varian) | 600 MHz 핵자기 공명 분광기

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보유장비 관련 정보
Laboratory/Field
  • Materials Characterization Lab
  • Spectroscopic Analysis
Model VNMRS600
Maker Varian
Technician Sun-Phil Han
Contact 052-217-4174 / okno1234@unist.ac.kr
Status for Reservation 가능
Reservation Unit 10min Maximum Time (per day) 24hr
Open(~ago) 5일전 Cancel (~ago) 1시간전
Equipment location 102동 B119호

  • Description

    핵자기 공명 분광기는 유기분자, 고분자 물질 및 생체 분자 등의 화합물 구조를 결정하는 기기이며, 정성 및 정량 분석에 이용된다. 자기장 내에서 일정한 회전축을 갖는 원자핵에 라디오파를 가해주면 무질서하게 있던 핵들이 높은 에너지 준위로 여기된다. 이때 발생하는 원자핵의 핵자기 공명 현상을 이용하여 시료 내 핵 주위의 화학적 환경 및 이웃 원자와의 스핀 결합에 대한 정보를 얻을 수 있다.

    NMR is a technique for determining the structure of most organic and some inorganic molecules. NMR studies a magnetic nucleus by aligning it with a very powerful external magnetic field and disturbing this alignment using an electromagnetic field. Different atoms within a molecule resonate at different frequencies at a given field strength.

    https://ucrf.unist.ac.kr/en/category/data/technical-library/
    1) Varian 600 MHz FT-NMR Operation Manual
    2) DOSY NMR Manual
    3) 2D NMR Manual
    4) SOP of Bruker 400 MHz FT-NMR

    https://ubts.co.kr/
    NMR 이론 및 실습관련 동영상 교육자료 (NMR Theory and Practice video)
    - 이론, 장비사용법, Mnova processing 등

  • Specifications

    • Premium shielded 14.09 T (600 MHz) magnet

    • 3 channel console

    Ch1: 100 Watt

    Ch2: 300 Watt

    Ch3: 300 Watt

    • Available probes

    - 5mm Dual broad band auto X probe

    Ch1: 1H, 19F

    Ch2: 15N ~ 31P

    Sample amount: 400 ~ 700 µl

    Temperature: -80 ~ 130 °C

    Gradient strength: 0.06 T/m (<2.5*10^-11 m^2/s)

    - Automated triple resonance probe

    Ch1: 1H

    Ch2: 13C

    Ch3: 15N

    Sample amount: 400 ~ 700 µl

    Temperature: -20 ~ 80 °C

    - 5 mm double resonance MAS solid probe (Stator 파손으로 수리 중)

    Ch1: 1H, 19F

    Ch2: 15N ~ 31P

    Spinning rate: 5~10 kHz (Max: 12 kHz)

    Sample amount: ~ 100 mg (fine powder) or KBr mixture

    Temperature: RT

    - 1.6 mm HXY fast MAS triple resonance probe (수리완료)

    Ch1: 1H, 19F

    Ch2: 15N ~ 31P

    Sample amount: 10 ~ 20 mg (fine powder) or KBr mixture

    Spinning rate: 8~35 kHz (Max 40 kHz)

    Temperature: 0 ~ 60 C

    - Nano TM probe (Similar Bruker HR-MAS probe)

    Spinning rate: 2~2.5 kHz (Maximum 3 kHz)

    Sample amount: 40 µl (gel or para-magnetic sample)

    Temperature: 0 °C ~ 50 °C

    • XR - 401(temperature control unit)

    Temperature: -60 ~ 100 °C

    • 5mm DB auto-X probe Tune & Match range = 31P (40%) ~ 15N (10%)

    • Smart of i-Probe (Bruker) / Royal probe (Jeol) = 31P(40%) ~ 109Ag (4.65%)

    ex) 5mm DB auto-X probe

    31P(40%): O

    13C (25%): O

    15N(10%): O

    35Cl(9.7%): O

    33S (7.6%): X ->Find 31P(40%) ~ 109Ag(4.65%) Probe

    14N(7.2%): X ->Find 31P(40%) ~ 109Ag(4.65%) Probe

    25Mg(6.1%): X ->Find 31P(40%) ~ 109Ag(4.65%) Probe

    https://kodu.ut.ee/~laurit/AK2/NMR_tables_Bruker2012.pdf

    https://www.pascal-man.com/periodic-table/periodictable.shtml

    • NMR solvent and Referencing (+Quantitative NMR)

    1. Sample + NMR solvent (CDCl3, D2O, DMSO-D6, etc.) + reference compound

    2-1. Sample + NMR solvent (CDCl3, D2O, DMSO-D6, etc.)

    2-2. Reference sample

    3. Coaxial sample tube (Evans method) - Reference or NMR solvent in Inner tube / Sample in Outer tube

    -> Possible to measure Non mixture with NMR solvent

    • Sample volume = 500ul (400 ~ 700 ul)

    • Sample concentration

    1. 1H: 0.05 mM ~ 10 mM (Too high concentration cause line-broadening effect)

    2. 13C, 2D NMR(COSY, NOESY, TOCSY, etc.): 10 mM ~ 100 mM

    3. 15N, 17O, Hetero 2D NMR (HSQC, HMBC, HMQC, etc.): 100 mM <

    Ex)

    Sample A (MW=200), 0.05 mg / 500 ul = 0.5 mM (mmol/L) = 100 ppm (ug/ml)

    Sample A (MW=200), 1 mg / 500 ul = 10 mM = 2000 ppm

    Sample B (MW=500), 25 mg / 500 ul = 100 mM

    • Degassing

    Oxygen (Paramagnetic) -> Short T1&T2 relaxation-> Quench NMR signal -> Purge N2 or Ar gas

    • Doping agent (add Paramagnetic material)

    GdCl3 or CuSO4 (Polar) / Cr(acac)3 (Non-Polar) -> Short T1 & T2 relaxation -> Quench NMR signal -> Save time!

    1H (1mM)

    13C (25-50mM)

    • Sample tube

    Wilmad (Thin wall): 527-PP-7 Temp: O, MW> 1500 (Large or Polymer), To use Quantitative NMR or Coaxial tube (Non-mix NMR solvent)

    Wilmad (Economy): WG-1228-7 Temp: X (only RT), MW < 1500 (Medium)

    Wilmad (Cheap): WG-1000-7 Temp: X (only RT), MW < 250 (Small)

    https://www.bkinstruments.co.kr/Products/list.asp?page=1&s_type=&s_keyword=&p_cate=10&p_cate2=1018

  • Applications

    • Structural elucidation of chemicals

    • Structural determination of biomolecules (DNA, RNA, proteins, peptides, etc.)

    • Study of dynamic process

    • Drug design

    Dual broad band auto X probe

    Detectable nuclei: 1H, 7Li, 9Be, 11B, 13C 17O, 19F, 23Na, 27Al, 29Si, 31P, 35Cl, 119Sn etc

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