Table 1: Shim Matrix and Job Parameter
files for various solvents:
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Settings on the Shim Panel |
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5 mm Dual Probe for 1H and 13C:
1. 13C - Transmitter: 90
degree = 5.2 msec
2. 1H - Transmitter:
90 degree = 12.5 msec
(used as P1 for COSY, NOESYand
as PW for Inversion Recovery,
not
for XHCORR and DEPT !)
3. 1H - Decoupler:
normal and reverse mode:
DP | 90 degree pulse | Remarks: |
0H | 10.4 msec | used as P1 in DEPTand XHCORR experiments |
4H | 22.0 msec | |
8H | 34.0 msec | used as P1 in TOCSY and ROESY experiments |
16H | 78.0 msec | used as P9 for CPD decoupling (only if DP = 16H!!!) |
180 degree DANTE pulse:
100 pulses à 1.75
msec (P8)
D8 = 100 msec
DP = 8H
A : continue
a phase correction in EP after using APK.
Ctrl-A : release knob A inside EP mode.
B : biggest
peak mode (the tallest peak will be used for any action.)
Ctrl-B : release knobs A and B inside EP mode.
C : cursor mode
(the cursor position will be used for any action.)
Ctrl-C : invert orientation of knob C in phase correction routine.
D : dual display
(in EP). Enter the filename of the 2nd spectrum.
Ctrl-D : a) invert orientation of knob D in phase correction
routine.
b) turn on/off the grid.
E : toggle the
spectrum information (in EP).
F : define plotting
limits (in EP).
Ctrl-F : show the spectrum within the plotting limits
(in EP).
G : calibrate
the chemical shift scale
Ctrl-H or 'Bs' : stop the acquisition (careful! this
works everywhere!)
J : calculate
the line width of a single peak in EP. (Answer "LORE" and .001)
Ctrl-K : stop all processes on the spectrometer (careful! all
data will be lost!)
L : Load previously
saved integral file (integration routine)
Ctrl-L : turn Lock signal and spectrum on and off
M : a) define the
minimum intensity for peak picking (in EP).
b) start baseline correction of the integral (integration routine)
Ctrl-N : eject plotter paper (from inside EP)
N : define a
Hertz/cm or ppm/cm expansion for plotting
Ctrl-O : delete the current command line
Ctrl-PT : terminate plot
Ctrl-Q : quit the process in the current job, does not halt
a running acquisition
R : enlarge
a region of the spectrum in EP (R, move cursor, R)
Ctrl-R : show the complete spectrum (in EP)
U : update the
displayed region as new plotting region. (in EP)
X : plot the
currently displayed screen (in EP)
Ctrl-X : toggle between the NMR program and a background process.
Y : define the
tallest peak to be plotted with ......cm height (in EP)
Ctrl-Y : show/ hide imaginary part of the spectrum.
Z : mark begin
and end of an integral (integration routine)
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To prevent damage to the spectrometers during a severe thunderstorm,
the following shutdown procedure has to be executed exactly in this
order:
1. Terminate any NMR experiment: Press Ctrl-H
2. Save the present FID to the disk: Enter WR filename.extn
!
3. Type: MO!
4. Turn off the printer, the plotter, the floppy disk drive, the display
and the temperature unit.
5. Press the "STOP" button at the ASPECT 3000 computer (right,
front of console).
6. Switch off the hard disks (2) by turning their keys (left side of
console, behind the metal door).
7. Switch off the Disk Interface (box on top of the console).
8. Switch off the ASPECT computer by turning its key.
9. Pull the red "EMERGENCY" button as the last step( middle,
front of console).
Don't forget to turn off the other spectrometer and the PC in the lab! Now it is safe to leave.
To restart the spectrometers, please execute:
1. Push the red "EMERGENCY" button back in.
2. Go behind the console and switch the gray "MAIN POWERRESET"
button (on the bottom
metal bar of the console) into the left position.
If the spectrometer starts beeping continuously, the SCM under the
keyboard has to be reset.
3. Turn on the ASPECT computer with its key and press the "STOP"
button.
4. Switch on all other devices (printer, plotter, display, VT unit,
disk interface)
5. Turn on the hard disk drives (keys) and wait, until their green
"READY" lights are on.
6. Press "STOP CLEAR DISK" on the front panel of the ASPECT
computer
7. Confirm the date and time, which appear on the screen by pressing
"!"
on the keyboard.
Notes:
- After turning on the spectrometer, it takes 30 minutes for the lock
to stabilize.
- NEVER turn off the ASPECT computer before the hard disk. This might
damage files.