Acquiring and processing a 1H
NMR spectrum on the Bruker ARX-300
Things
in bold should be typed on the command line
Things
underlined are buttons on the left-hand side panel of XwinNMR.
Things italicized are buttons on the BSMS
keyboard.
|
1. Insert sample |
If the lock is turned on
(LED lit or blinking) , press Lock On/Off to turn lock off If the spinner is on (LED
lit or blinking), press Spin On/Off to stop the spinner Press Lift On/Off
to eject the standard Put your sample in the
spinner, position it with the depth gauge, and place it in the bore Press Lift On/Off
to insert your sample Press Spin On/Off
to turn on the spinner |
|
2. Set up acquisition parameters |
edc Enter a NAME for the
experiment. Don’t use special characters (\$@#”^/ etc.). Use _ or – instead
of white space. Set the EXPNO (experiment
number) Click SAVE rpar 1h_std all reads standard 1H parameters |
|
3. Lock |
If the lock display window
is not open: lockdisp lopoi and select your solvent
from the list Press Lock On/Off
on BSMS Press Lock Gain and
set it at 120 ± 5 Press Lock Power
and adjust value to bring the lock level to the upper third of the lock
display window |
|
4. Shim |
Press Lock Phase
and adjust for maximum lock response Press Z and adjust
for maximum lock response Press Z2 and adjust
for maximum lock response Iterate between Z
and Z2 until the signal reaches maximum Press Standby |
|
5. Acquire FID |
rga automatic receiver gain adjustment ns to change number of scans, if desired zg zero file and go |
|
6. Window function & Fourier transform |
Wait
for acquisition to finish efp apply standard window function and FT |
|
7. Phase |
Click the |<>|
button to display the whole spectrum Click the PHASE
button to the left of the spectrum window (If you don’t see a PHASE
button click RETURN first) Click the *2 button
until details of the baseline are clear Click BIGGEST Click & Hold PH0 Drag the mouse up (or
down) to adjust the phase of the tallest peak Click & Hold PH1 Drag the mouse up (or
down) to adjust the phase of all other peaks Click RETURN à Save and Return |
|
8. Reference |
Zoom in on the reference
peak (Left click, middle click, middle click, left click) Click CALIBRATE Set the cursor on top of
the reference peak Middle click and enter the
reference value |
|
9. Peak Pick |
Click UTILITIES Click MI and click OK
if you get a pop-up window Move the mouse up or down
to position the blue line. Anything below the line will not be peak picked Click RETURN |
|
10. Baseline correct |
abs Don’t use abs after integration! |
|
11. Integrate |
Click the INTEGRATE
button to the left of the spectral window Click inside the spectral
display Middle click to start an integral
region Middle click to close an
integral region Move around the spectrum
using the < and > buttons Zoom in and out using the <>
and >< buttons Repeat until all peaks are
integrated Click RETURN à Save and Return |
|
12. Plot |
Click UTILITIES Click CY and set the blue line slightly above the tallest
peak you want plotted. Left click and enter 10 as
the height of the peak. Click RETURN Click DP1 Enter values for upper and
lower plot limits plot To print expansion plots: Zoom in on
the desired region Adjust CY as
above, if desired Click the PLOT
button |
|
13. Eject sample |
Press Lock On/Off
to turn lock off Press Spin On/Off
to stop the spinner Press Lift On/Off
to eject your sample Put the standard in the
spinner and place it in the bore of the magnet Press Lift On/Off
to insert the standard |