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Nuclear Magnetic Resonance Facility

Instructions For Operating The Bruker Avance 300 MHz NMR Spectrometer

1. Click on ICON-NMR
2. Choose Routine Spectroscopy
3. Click on identify User, scroll down to select your ID, enter your password and press Enter
4. Click inject/insert
5. Click insert new sample
Use the sample depth gauge to adjust the sample depth (2.0cm) in spinner, clean your sample tube with a Khimwipe
After you hear air escaping from the top of the magnet, place sample in top of magnet
Click OK in the pup up window in center of screen
6. Use mouse to highligh the define name and type file name via keyboard (sample_expt_date_name, i.e. ethanol_h_012505_rl) , change experiment number to 1
7. Choose the solvent of your sample from the list and click OK
8. Choose the experiment you wish to execute from the list
9. Type text in the window then click set title
10. Click options at top of grey window, activate manual lock/shim
11. Click Start, a new window appear
12. Click lock to open lock window. A continuous wave signal should be observed in the lock display window.
13. Click automatic lock in manual lock routine window
After the computer locks on the deuterium signal the lock display will exhibit a flat line in the upper position of the display window and the lock on/off button on BSMS board will be illuminated (green light on)
14. When manual shim routine window appears, don’t click on anything yet
Check BSMS display to make sure on axis and fine buttons are on (green light on).
Press Z1 button and turn round knob to increase position of lock signal
If signal goes out of window then press lock gain button and turn round knob counterclockwise to get signal back on scale.
Press Z1 again and continue shimming to maximize intensity of lock signal
Press Z2 and maximize intensity of lock signal by turn round knob
Repeat with Z1 and Z2 until the lock signal will no longer increase, press STANDBY button
When shimming is completed click shim ok button on manual shim routine window
15. The software now will begin to do an automatic determination of the receiver gain then start the data collection, processing, and plotting. You can get printed spectrum from the printer. (You may process and change plot parameters manually, see manual processing and plotting procedure)
16. When done with data collection and plotting, click continue routine flow chart window
17. Click eject and terminate, remove sample from the top of magnet, click OK, If you want to run additional experiments on the same sample, click use same/continue, choose new experiment, then start new experiment. If you want to collect data on a different sample, click insert new sample, repeat step 5.

Instructions For Manual Data Processing And Plotting

1. After data collection click on spectrum on routine flow chart window
2. To expand a region:
Click on left mouse button on left side of region of interest then click on the middle button move mouse to right side of region then click on middle then left mouse button
3. To calibrate the spectrum:
Expand around region containing reference peak and click on calibrate button
Move the mouse to the top of the reference peak then click on middle mouse button
Enter correct reference value in CPR window and hit enter key when done
4. The buttons on the left side of the screen allow for increasing or decreasing intensity,
expanding or compressing spectrum, moving the spectrum position vertically etc.
5. To set the peak-picking threshold:
Press YU button to change spectrum vertical scale to cm
Type pscal choose global, click on utilities button then choose mi
Drag the mouse to set the threshold line at desired position then click on the left mouse button to set the position (any peaks above threshold line will be included)
Click on return button when finished
6. To integrate the spectrum:
Expand around the farthest left region of peaks to be integrated
Click on integrate button
Click on left mouse button to the side of the farthest left peak to be integrated then click on the middle mouse button
Move the mouse to the right side of the peak to be integrated then click on the middle then
left mouse buttons, use the left arrow key to move the spectrum to the next region of peaks
Repeat the above sequence to integrate the remaining peaks in the spectrum, click return then choose Save as intrng and return
7. Type edg to set some plotting parameters
Change plabels to yes (to plot peak frequencies on spectrum)
Click on edplabl then change plunit to ppm or Hz and plcolor to black
integr and ilabels should be set to yes to plot integral curves on spectrum
title should be set to yes if you want a text written on the top of the spectrum. this can be entered from the text box in ICON-NMR or by typing setti and entering title param should be set to yes to plot parameters
click edspect
set cy = 0; this will allow for manual adjustment of spectrum intensity otherwise with cy = 12.5 the computer scales all peaks relative to largest peak
dhei = 11.0 if integrals are to be plotted on spectrum otherwise set to dhei = 13.5
if you aren’t plotting integral curves
click save when you have made changes
8. To define the plot region:
expand or display region to be plotted on screen, click on dp1 button to define plot region at small CPR window hit enter key 3 times to set plot region (you can also enter a value) every time the horizontal or vertical scale is changed the plot region has to be redefined
9. Type view then click quit. Type plot or click on plot button to plot spectrum.