Quick Procedure for WM250:
1) Sample insert and setup:
- -insert sample in sample holder, measure correct position on drawing on magnet
- -remove cap from top of magnet
- -turn on the SAMPLE LIFT fast by approximate one turn, insert sample and turn sample
lift off to insert sample. Then put cap back on top.
- -Slowly turn up the SPINNING AIR until you reach a reading of ~100. If it doesn't spin,
try to adjust the screw on top of the red cap to control the air flow.
- -Turn the intensity on the oscilloscope up to see the lock signal. Adjust the H0 Fine
button to move the middle of the two signals to the center of the screen. If you use a
solvent different from CDCl3 or don't see a signal on the screen adjust the field with the
H0 Coarse knob first. Note that the value for CDCl3 is posted next to the knob, other
solvents require slightly lower numbers (counter clockwise turn).
- -Push the LOCK ON button to obtain field frequency lock. The oscillating signal turns
into a horizontal line in the upper half of the screen and the green light to the lower left
comes on. Sometimes it is necessary to re adjust H0 Fine and LOCK AMPLITUDE.
- -Adjust the Z and Z2 shims for maximum height of the lock signal. Reduce the LOCK
AMPLITUDE if necessary
2) Experiment setup and acquisition
- -Type rj h1.cdcl <ENTER> ( or call up the file apprpriate for the solvent you are using)
- -Type pj <ENTER> <ENTER> (after the first <ENTER> your parameter name from rj
shoulb be inserted automatically, otherwise rj was not executed correctly)
- -change ns or rd if necessary
- -Type rga, wait until the message rga finished is printed
- -Type zg and wait until all accumulations have been executed
- -Type ef for exponential multiplication and Fourier transform
- -Type apk for automatic phase correction
3) Spectrum manipulation and plotting
- -Type ep to enter the expanded display mode. In this mode, the knobs [A] and [B] now
allow you to horizontally move and zoom the spectrum, respectively.
- -The big black VERTICAL DISPLAY knob can be used to zoom the vertical display of
the spectrum.
- -In the basic ep window, knobs C and D move the cursor, but have special functions in
some of the subroutines.
- -<Ctrl>-R displays the entire spectrum, <Ctrl>-B resets to the last expansion. You can
also zoom in on a peak by moving the cursor to one side, type R, move to the other side
and type R again.
- -Manual phase correction: In the ep mode, hit p. The highes peak in your window will be
selected. Adjust the phase of that peak with knob [C] to pure absorption. If necessary hit
<Ctrl>-C to reverse the action of knob C. Then adjust the rest of the spectrum with
knob [D]. If finished, exit the phase mode with M to save the phasing.
- -Calibration: Move the cursor on top of the desired peak and hit G. Then type in the value
in ppm and hit M to save or <ENTER> to return.
- -Integration: Type I to enter the integration routine. Move the spectrum to the first peak
you want to integrate and move the cursor to the left of that peak. Tgype Z to zero the
integral. Then move to the right of the peak and hit Z again to finish the integral. Repeat
this for every peak you want to integrate. If you want to scale an integral, hit A before the
second "Z" and you will be prompted to enter a number. If you are finished, type E to
exit and confirm the suggested integration file name, int1.001, by hitting <ENTER>
- -Setting the plot width: Type F. Enter the downfield limit in ppm, followed by
<ENTER>, and then the upfield limit (in the main command mode, you can type F1 to
enter these values).
- -Exit to the command mod by hitting <ENTER>.:
Now you are back to the command mode.
- -Type DPO to set title, turn peak picking off or switch between ppm and Hz display
- -Type np to send a new page to the plotter
- -Type px to plot the spectrum only OR Type pxb to plot spectrum and integration. You
will be asked to enter the name of the integration range file, int1.001 from above.
Finishing
- -Turn off the spinning air.
- -Turn off LOCK
- -Turn down the intensity on the oscilloscope
- -Remove cap.
- -Turn up the SAMPLE LIFT quickly and immediately take out your sample.
- -Set the H0 COARSE back to the value for CDCl3
- -Sign the log book.