Basic Bruker C13 NMR Tutorial
Sample preparation and Spinner Loading.
Small mortar and pestle.
Small spatula.
NMR solid sample spinner with cap.
Sample spinner loading jig and ram.
Sample spinner cap removal device.
Small wooden splints.
Kim-Wipes.
Black permanent marker.
HOW TO PREPARE YOUR SAMPLE:
For proper spinning of the sample, the solid sample must be a dry, fine grain powder. If you
suspect that the sample may contain traces of a solvent, the sample should be dried in a 60 C
vacuum oven (~28 in. Hg) overnight. Any residual solvent in the sample will be centrifuged out
of the powder during spinning and will contaminate the solids probe (a $15000 investment, so
use care when preparing your sample!)
HOW TO PACK A SAMPLE SPINNER:
Use great care when handling the sample spinners and caps. They are precision instruments made from zirconium oxide and Kel-F and cost approximately $250 each!
DO NOT FORCE ANY OF THE FOLLOWING STEPS, BE SLOW AND GENTLE!!!
Place approximately 1 gram of the sample in a small mortar and grind to a fine consistency. Put
the sample spinner in the loading jig so that the funnel is up and place it on a pad (a folded Kim-Wipe) on the laboratory bench. Add a small amount of sample to the spinner and pack it in place
using the ram. Repeat this process until the spinner is nearly full. Remove the spinner from the
jig, invert the jig, and lower the spinner into it (funnel is down). Check the sample for proper
depth using the short end of the ram, it should touch the sample for a proper fill. Adjust the
sample as necessary. Place the spinner cap on top of the spinner, center it, and press down gently
until it snaps in place. When the cap is properly seated there will be no visible gap between the
spinner and cap.
HOW TO MARK THE SAMPLE SPINNER:
Remove the spinner from the jig and clean thoroughly using a Kim-Wipe. Then use the black
marker to color one-half of the bottom of the spinner. This marking is used to measure the
spinning rate. Let the marking dry thoroughly.