Volume 1, Issue 1 | www.emory.edu/NMR 404-727-6621 | August 15, 1997 |
NMR Instrument Maintenance and Troubleshooting |
Probe Qs: One parameter affecting sensitivity is the probe Q. Q is defined as the frequency of the resonant circuit divided by the the half power bandwidth. Many of today's probe have unloaded Qs greater than 300. If all the other parameters are the same, the higher the probe Q, the greater the sensitivity. The Sample: One component which lmits probe Q is the sample. The sample increases loss in the resonant circuit by inducing eddy current in the solvent. The more conductive the samplethe more the losses and the lower the probe Q. This is often seen by the longer 90 degree pulses with water samples than with organic sovent samples.
The losses in the sample are induced by the electric field values inside the probe. The more distributed capacitance a probe has in its resonant circuit, the lower the electric field values. Therefore a probe with distributed capacitance is less affected by the sample. Unfortunately the capacitor usually has ahigh resistance than the coil. Therefore the use of distributed capacitors lowers the probe's unloaded Qs, but can raise the loaded Qs. This statement reduces to the probe designer's need to compromise probe design between organic and water samples.
Shimming Problems: You treat NMR instrument well, it will serve you better. You know more about NMR, you will be more productive. |
Raw Shimming If the instrument has a very poor homogenity, the following steps are recommended: 1. Spin sample at rate 15-20 hz. Adjust Z1 and Z2 to maximize the lock signal. Some instruments may allow you to observe an FID signal. 2.Turn off the spinner. Adjust X and Y to maximize the lock signal. 3. Adjust X and ZX to maximize the lock signal. 4. Adjust Y and ZYto maximize the lock signal. 5. Adjust XY and X2-Y2 to maximize the lock signal. 6. If a large signal intensity change observed, go back to step 1. After these adjustment, the instrument should be able to lock.
Spinning Shimming: A good shimming is the most important feature for the performance of an NMR spectrometer. The lineshape measurement: Use a 1% CHCl3 in CDCl3 standard sample. Measure the linewidth at 50%, 0.55% and 0.11% of the peak height. good NMR peak should be a Lorentzian line line shape.
50%: < 0.3Hz |
If you think you are computer illiterate, don't worry, you are not! The following people are even more illiterate. Check out the following excerpts from a Wall Street Journal article by Jim Carlton Compaq is considering changing the command "Press Any Key" to "Press Return Key" because of the flood of calls asking where the "Any" key is.
True story from a Novell NetWire SysOp.
The NMR Center has received several complaints about their boss's lastname. |