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. Dont 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 dont 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 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 Dont 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 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