Logbook -- The first step for each user is to sign-in on the instrument logbook. Approved users must indicate their initials and full name and the name of their instructor/professor on the inside cover pages. Each user must use a single line to sign-in and indicate date, type of solvent and experiment, and comment on any problems encountered. Enter ok if no problems are encountered, during the NMR analysis. Make certain there is proper identification for the NMR sample tube which is keyed to a notebook, and the NMR spectral file or printed spectrum.
Switch on the Air Pump -- The air pump should be running. If not, turn on the switch located on the power cord. The air pressure gauge should read approximately 20 psig. There are several electrical outlets one for the air pump and one for the magnet plus computer and accessories. Never unplug the magnet.
Placing the Sample in the Magnet --Do Not Force Any Of The Following Steps, Do not rush be careful. The availability of sample spinners (yellow plastic tube holder with fins have been replaced) is limited for this instrument, and they can be easily cracked, broken or worn out by misuse. Additionally, NMR sample tubes can be easily broken and present a safety hazard.
2. Position NMR Tube -- Hold the yellow plastic spinner with the fins pointing up and press the sample tube gently down through the spinner about two-thirds of the way up the tube. Twisting the tube a little helps. Then lower the tube into the depth gauge on the front of the magnet. Now gently press the sample tube down until it stops (or push down on the spinner until it stops). Adjustment of the spinner depth is now correct. Lift the sample tube out of the depth gauge by the top and gently wipe off the lower portion of the tube using a Kim-Wipe.
3. Put the Sample into the Magnet -- Lift the smoked plastic dust cover on top of the magnet and lower the sample tube into the probe (the large hole under the dust cover). If a slight resistance is felt, gently move the tube around a little until it drops down into the center of the probe. Listen for a whirring sound as the sample begins to spin. If the sample tube drops into the probe and doesn't begin to spin, even though the air pressure is OK, press a finger over the lift air vent tube (a 3-mm tube immediately to the left of the probe hole). This should lift the sample tube out of the probe. The normal spin rate is about 50 rpm, i. e. two turns from the off position. The off position is all the way clockwise. 4. Removing the Sample from the Magnet -- Lift the smoked plastic dust cover on top of the magnet. Press a finger over the lift air vent tube (3-mm tube immediately to the left of the probe hole) and the sample will float on the lift air. Grasp the NMR tube and gently remove it from the probe and put the water tube back into the magnet at the end of an experiment. Close the plastic dust cover.
