29Si, 13C, 31P 1D NMR

Bruker Avance AV 300 / QNP probe

  1. Preliminaries
    1. Sign the logbook (name and phone number)
    2. Login to the computer
      • user name
      • password
    3. Open Topspin (double-click the icon)
        topspin icon
  2. Acquire a 1H spectrum
    1. Is the shimming okay?
    2. Does the sample appear as expected?
    3. Calibrate the 1D spectrum
    4. If you'll use proton decoupling, check the optimal SFO1

  3. Create a new experiment number
    new window
  4. Tune and match
    type: w
    shows a wobble curve for the nucleus defined in ased
    the woble curve is displayed in the acquisition window
    if you do not see the "dip", check the qnp position on the probe!
    1 = 29Si, 2 = 13C, 3 = 31P
    To end the wobble routine: stop

  5. Modify parameters
    1. Set the region(s) of interest
      (sw = ppm range; o1p = center of range)
      If your using 1H decoupling,the parameter o2p is for the 1H's

    2. Set nsand check the experimental time (expt)

  6. Acquisition
    1. type: rga
    2. or type: zg

  7. Processing
    Type: ef

  8. Plotting
    For a simple printout of the screen, type: prnt
    To export pdf files of your plot, or have control of colors, fonts, sizes
    enter the topspin plot editor by typing: plot
    In brief, a description of the plotting elements:
    “Data” contains the list of expno's listed in the plot editor's portfolio
    The green squares icon allows data window selection
    “Edit” to change colors, fonts, displayed regions, etc.
    “1D/2D Edit” to interactively change intensity and plot region
    File, Print to get a hardcopy (control p)
    File, Export to save a picture (formats include: pdf, jpg, emf, and bmp)
    DO NOT SAVE (this changes the file called by “layout” in topspin)

  9. Save your data onto another computer
    1. Open the my computer file icon on the desktop (double-click nmr200)
    2. Click the “start” icon to get to the nmrlab4 network shortcut
    3. Drag and drop files to nmrlab4.
      Preserve the hierarchy:
      directory/data/user/nmr/name/ expno

  10. Remove your sample
    1. on the BSMS keyboard:
    2. TURN OFF: spin and lock (no light = off)
    3. press “lift on/off” (green = on)
    4. gently remove your sample from the magnet – lift it up to clear the magnet
    5. press “lift on/off” (no light = off)

  11. Log off

  12. Open your files on another computer
    Topspin icon
    1. Open the program Topspin
    2. Navigate to your data using the Browser
    3. Drag you data file into the display window

  13. Report problems and bugs to Yael or Shifi - 3748