NMR & Structure Analysis
Prof. dr. J. Martins

 

 

Equipment
300 MHz
500 MHz
700 MHz
Work in progress
Bruker Avance 300
description | installation
Bruker DRX500
description
Bruker Avance II 700
description

 

300 MHz AVANCE (since 2002) Ultrashield

responsible operator: R. De Vierman

Technical Description

    • Three-channel spectrometer
    • 5mm BBO probe with ATM
    • BACS-60 Sample changer for 60 samples
    • z-Pulsed Field Gradients
    • 2H gradient shimming
    • Operator Access and Open Acces
    • Running XWINNMR 3.6 and ICONNMR
    • Involved in last year elective course ‘Advanced NMR'

Mission

To provide usual and advanced NMR techniques to support the organic and polymer synthesis activities of the Department.

Typical measurements include :
1D 1H and 1D 13C (regular, APT, DEPT,…)
2D 1H-1H (mainly gCOSY and TOCSY with others available upon request)
2D 1H-13C (HSQC, HMBC, HSQC-TOCSY)

occassional measurements include:
1D 1H with diffusion filter, of interest to have ‘polymer only' 1H spectrum
1D 1H with 31P decoupling
          simplification of multiplicity patterns in 1H NMR of organophosphorous compounds
1D 11B usefull in hydroboration chemistry
1D 19F
1D 29Si usefull in silicon based protecting groups and silicone polymers
1D 31P usefull in organophosporous chemistry
2D 1H-29Si HSQC/HMBC
          allows to localise Siliconether groups on the hydrocarbon skeleton
1D version available for single silicon containing compounds

All of these are available within ICONNMR within operator and open acces modes.

 

500 MHz AVANCE (since 2000)

responsible operator: George Verhegge (4496)

Technical Description

    • Fully equipped three-channel spectrometer
    • 5mm probes : all with Z-gradient (50 G/cm)
      • 5 mm TBI ( 1H, 31P, BB) inverse type
      • 5 mm DUAL ( 1H, 13C) direct type, high s/n for 13C
      • 5 mm SEI ( 1H, 13C) inverse type
      • 5mm TXI ( 1H, 13C, 15N) inverse type on loan from HNMR-VUB
    • NMRCASE sample changer for 24 samples
    • 2H gradient shimming
    • BVT-2000 Eurotherm controller
    • BCU-05 precooler for stable temperature operation
    • Operator Access Only
    • Running XWINNMR 3.6 and ICONNMR
    • Upgraded from an AM500 (1987) with reuse of the Oxford magnet

Mission

To provide usual and advanced NMR techniques in support of the organic and polymer synthesis activities of the Department

Typical measurements include:
1D 1H and 1D 13C (regular, APT, DEPT,…)
2D 1H-1H (mainly gCOSY and TOCSY with others available upon request)
2D 1H- 13C (HSQC, HMBC)

Main research instrument of the NMR and Structure Analysis research unit.

  • Structure Analysis of organic molecules
    Typical measumerents include
    1D 1H and 1D 13C (regular, APT, DEPT,…)
    2D 1H-1H gCOSY, DQF-COSY, E.COSY, TOCSY, NOESY, off-resonance ROESY
    2D 1H-n X HSQC, HMBC, HSQC-TOCSY, HSQC-NOESY
    nX is either 13C, 15N, 31P
  • Diffusion NMR spectroscopy for in organic chemistry and the material sciences
    Typical measumerents include
    1D 1H diffusion filtered
    2D DOSY
  • Biomolecular NMR spectroscopy
    Typical measumerents include
    1D 1H presat, watergate, excitation sculpting
    All of the above techniques with water suppression included (either presat or watergate)
    2D 1H-15N HSQC (flip-back, sensitivity-enhanced)
    2D 1H-15N Cleanex-HSQC
    3D 1H-15N HSQC-TOCSY, HSQC-NOESY
    3D triple resonance techniques (HNCA, HncoCA, HNCO, HncaCO, HNCACB, CBCAcoNH)
    R1 , R2 and Heternonuclear 1H-{15N} NOE experiments for dynamics

 

700 MHz AVANCE (fall 2005)

responsible operator: dr. Bernd Fritzinger

Technical Description

    • AVANCE II : Newest generation of Bruker spectrometers
    • Fully equipped three-channel spectrometer
    • Liquid state probes
      • 5 mm TXI ( 1H, 13C, 15N) inverse type
      • 5 mm TBI (1H, 119Sn, BB) inverse type
    • high resolution Magic Angle Spinning probe
      • 4 mm 1H, 13C, 119Sn single coil with gradient at magic angle
    • probe for limited quantities and/or volumes
      • 1 mm TXI ( 1H, 13C, 15N) inverse type, 5 mL active coil volume
    • all probes are equipped with Z-gradient
    • Sample changer for 60 samples
    • 2H gradient shimming
    • BCU-05 precooler for stable temperature operation
    • Liquid N2 cooling system for measuremtns till -150°C
    • Operator Access Only
    • Running TOPSPIN 1.3

Mission

The 700 MHz is the ‘crown jewel' of the Interuniversitary NMR Facility which has been created to support fundamental, basic and applied research in the chemical, material and biomolecular sciences.