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400 MHz FT-NMR (Bruker) | 400 MHz 핵자기 공명 분광기 (Bruker)

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보유장비 관련 정보
Laboratory/Field
  • Materials Characterization Lab
  • Spectroscopic Analysis
Model AVANCE III HD
Maker Bruker
Technician Sun-Phil Han
Contact 052-217-4174 / okno1234@unist.ac.kr
Status for Reservation 가능
Reservation Unit 10min Maximum Time (per day) 12hr
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/
    Varian 600 MHz FT-NMR / DOSY NMR Manual / 2D NMR Manual / SOP of Bruker 400 MHz FT-NMR

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

  • Specifications

    • 9.4 T magnet (100 MHz = 2.35T)

    • 2 channel console

    - Channel 1 : 1H(100%), 19F(94%)

    - Channel 2 : 31P (40%) ~ 15N (10%)

    • Channel 1 = 100 Watt / Channel 2 = 500 Watt

    • Gradient strength = 0.05 T/m (<3*10^-11 m^2/s), DOSY

    • Auto Tune & Match

    • 5 mm BBO NMR Probe

    • 24 Auto-sampler

    • Topspin 3.5 pl7 (Windows 7)

    • Temperature: RT (21 ~ 150 ˚C)

    • BBO probe Tune & Match range = 31P (40%) ~ 15N (10%)

    31P(40%): O

    13C (25%): O

    15N(10%): O

    35Cl(9.7%): O

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

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

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

    • None NMR solvent condition -> No Lock, Autoshim -> Poor or not easy measurement!!

    • 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 < Highest concentration

    Ex)

    Sample A (MW=200), 1 mg / 500 ul = 1*2 (mg/ml) / 200 (mg/mmol) = 10 mM

    Sample B (MW=500), 25 mg / 500 ul = 25*2 (mg/ml) / 500 (mg/mmol) = 100 mM

    • Degassing

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

    • Sample tube

    Wilmad(Thin wall): 527-PP-7 (Temp: O)

    Wilmad(Economy): WG-1228-7 (Temp: X, only RT)

    Wilmad(Cheap): WG-1000-7 (Temp: X, only RT)

    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

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