D.    Appendix

Table 1: Shim Matrix and Job Parameter files for various solvents:
 

Solvent
SHIM Matrix Files
JOB Parameter Files
acetone-d6
S05ACET
JH5ACET
JC5ACET
acetonitrile-d6
S05CD3CN
JH5CD3CN
JC5CD3CN
benzend6
S05C6D6
JH5C6D6
JC5C6D6
chloroform-d
S05CDCL3
JH5CDCL3
JC5CDCL3
DMSOd6
S05DMSO
JH5DMSO
JC5DMSO
D2O
S05D2O
JH5D2O
JC5D2O
methanol-d4
S05CD3OD
JH5CD3OD
JC5CD3OC
methylene chloride-d2
S05CD2CL
JH5CD2CL
JC5CD2CL
pyridine-d5
S05PYR
JH5PYR
JC5PYR
THF-d8
S05THF
JH5THF
JC5THF
toluene-d8
S05TOLU
JH5TOLU
JC5TOLU

 


Table 2: Startup Parameters for the AM-360 NMR Spectrometer
 
  Solvent 
Settings on the Shim Panel
1H NMR Parameters
13C NMR Parameters
  FIELD 
LOCK POWER
LOCK GAIN
  O1 
    SR 
  O1 
  O2 
SR
acetone-d6
4170
15
105
7478
5858.0
5217
7478
-3840.5
CD3CN
4150
25
105
7875
 
5217
7475
-3838.4
C6D6
4530
15
105
5624
4003.6
4786
5624
-4269.1
CDCl3
4530
35
105
5750
3986.6
521 7
5750
-4239.0
DMSO-d6
4210
20
105
7313
5692.7
5228
7313
-3827.3
CD3OD
4250
25
105
7200
5692.0
 
7200
 
CD2Cl2
4400
25
105
         
pyridine-d5
4650
25
105
5624
4003.6
4786
5624
-4431.6
TFA-d
4950
45
110
4663
2504
4223
4663
-4831.5
THF-d8
4120
35
105
6927
5305
5228
6927
-3989
toluene-d8
4650
25
105
5625
4004.4
4786
5625
 
D2O
4340
25
105
6529
4908.5
4975
6529
-4029.8

 



90 Degree Pulse Lengths - AM-360

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
 



Special Keystrokes:

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)
 


Tuning and Matching Settings for the AM 360 - 10 mm BB Probe

 
Nucleus
Frequency [MHz]
Tuning
Matching
 
2H
55.264
8494
823
7Li
139.903
8984
995
9Be
50.594
8374
803
11B
115.502
8945
992
13C
90.518
8865
966
14N
26.006
6947
755
15N
36.479
7654
822
17O
48.805
8326
800
23Na
95.227
8878
974
25Mg
22.028
6622
700
27Al
93.805
8876
975
29Si
71.515
8754
865
31P
145.731
8993
995
33S
27.611
7266
783
35Cl
35.274
7626
824
39K
16.799
5468
600
119Sn
134.180
8975
995
 
Limits:
min. Frequency: 9.8 MHz
 
max. Frequency: 155 MHz



Emergency Shutdown of the AM-360 spectrometer

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.
 
 

(C)1998    Jürgen Schulte