PINMRF Checkout Quiz - Bruker/TopSpin Version

Transcription

1 PINMRF Checkout Quiz - Bruker/TopSpin Version Please carefully read every question and select the best answer(s). Some questions may have more than one correct answer. To receive full credit you must mark all correct answers. You must answer at least 27 questions correctly to pass (ca. 80 %). This is an open-book quiz. You may use any training materials and notes that you have. You have 30 minutes to complete this exam. Name: Group: Date: Trained by: Signature: By signing above you certify that you will abide by the PINMRF rules and regulations, and that you have understood the safetyrelated material that has been presented to you : Revised for TopSpin - JSH : Updated - KOC : Updated - JSH : Created - JSH

2 1. Which of the following lock functions need to be optimized before locking your sample? A. Field and lock gain. B. Sweep rate, lock gain and lock power. C. Shims, lock gain and lock phase. D. Field, lock gain, and lock phase. E. None of them relevant lock functions are set by using the correct lock command. 2. Which of the following lock functions may need to be optimized after locking your sample? A. Spin rate and lock gain. B. Lock gain and lock power. C. Lock gain and lock phase. D. Field and lock gain. E. None of them you should never adjust any lock function. 3. When should you adjust the lock phase? A. Never. B. When the lock level is too low. C. When the lock level is too high. D. When the shimming is poor. E. When you are bored. 4. The new AV-III-400-HD NMR at Purdue is equipped with a BBO probe. If your sample is dissolved in deuterated water, which command should you use to set up a proton experiment? A. rpar h1.qnp.d2o B. rpar c13.tbi.d2o C. rpar h1.bbo.cdcl D. rpar h1.bbo E. rpar h1.prob.solv 5. Any user-specific parameters can be changed (such as changing the number of scans) A before the standard parameters have been read. B. after the standard parameters have been read. C. never parameters should not be changed. D. none of the above. 6. If your sample will not spin properly, what can/should you do? A. Increase the spin rate setting. B. Eject and re-insert the sample several times to clean out the system. C. Run your experiment without spinning if the locking and shimming are OK. D. Remove your sample and transfer the solution to another NMR tube. E. Turn up the air pressure using the regulator close to the spectrometer. F. Check the spinning using the lock standard sample if it is still not good, notify PINMRF staff.

3 7. If your sample tube breaks with all or part of the tube in the NMR magnet, what should you do? A. Pick up any glass outside the magnet, hide the spinner, and leave the lab as quickly as possible. B. Remove the probe from the magnet, and then clean out the glass from the probe. C. Put a note on the spectrometer that a sample is broken in the magnet. D. Notify PINMRF staff that a sample has broken, giving details of the sample composition. E. Turn up the air pressure, using the regulator close to the spectrometer, to blow out any glass. 8. When using the sample temperature controls, which of the following apply? A. Do not cool your sample below 10 C above the freezing point of your solvent. B. Do not heat your sample above 10 C below the boiling point of your solvent. C. Do not heat your sample above 100 C. D. Cooling your sample below ambient temperature may require further training. 9. After acquiring a proton spectrum of a sample, which steps need to be taken to acquire a carbon spectrum of the same sample? A. Change EXPNO number in edc (edit current dataset) window. B. Set the standard parameters for carbon (i.e., rpar c13.prob). C. Lock your sample. D. Shim your sample. E. Set the receiver gain. 10. Which PINMRF Bruker/TopSpin NMR spectrometer combination listed below has the highest sensitivity for both 1 H and 13 C? A. AV-III-400-HD B. AV-III-500-HD C. AV-III-800 D. Avance-DRX The signal-to-noise ratio of a spectrum is proportional to the square root of the number of scans acquired (!! α ns ). Therefore, if you have run a 13 C experiment for four hours, and would like to increase the existing signal-to-noise ratio by a factor of two, how much longer will you need to acquire data for? A. Four hours. B. Eight hours. C. Twelve hours. D. Sixteen hours. 12. When naming NMR datasets, which of the following statements is correct? A. You can use any characters in the dataset name, up to 80 characters. B. You can use letters and numbers and the space bar. C. You can use letters and numbers and the dash and the underscore. D. You must not use capital letters.

4 13. Safety regulations prohibit persons with pacemakers or magnetic objects inside the line of a superconducting magnet. A. 50 Gauss B. 10 Gauss C. 5 Gauss D. 2 Gauss E. 1 Gauss 14. In order to autophase your spectrum, type A. apk B. aph C. phase D. you must always manually phase your spectrum. 15. If the volume of your sample is ca. 700ul (standard volume) which of the following figures below represents the correct sample position in the sample depth gauge?

5 16. If the volume of your sample is ca. 400ul (not the standard ul) which of the following figures below represents the correct sample position in the sample depth gauge? 17. After passing this checkout exam, which NMR spectrometers are you allowed to operate (assuming you have not received any other PINMRF training)? A. Varian Inova-300 B. Bruker ARX-300 C. Bruker Avance DRX-500 D. Bruker AV-III-800 E. Chemagnetics Infinity-400WB F. All Bruker TopSpin spectrometers. G. All Bruker TopSpin spectrometers except for the Bruker Avance DRX with the TXI cryoprobe. 18. When running more than one sample on a Bruker/TopSpin NMR spectrometer, you must A. Tune, match, and shim every sample. B. Spin, calibrate the pulse width, and lock every sample. C. Lock and shim every sample. D. Use the depth gauge, lock, and shim every sample. E. You don't need to do anything. Parameters only need adjusting on the first sample.

6 19. NEVER place an empty spinner into the bore of the magnet! This statement is A. TRUE B. FALSE 20. NEVER lean against or push on the magnet! This statement is A. TRUE B. FALSE 21. On the PINMRF Bruker DRX-500 spectrometers, the ON AXIS and FINE functions on the keypad must be selected on prior to shimming. This statement is A. TRUE B. FALSE 22. When leaving the spectrometer, you ONLY need to A. Click on exit and log out. B. Click on exit. C. Click on eject and terminate and then insert and lock standard sample. D. Insert the lock sample, issue the standard command, wait for the standard command to complete, exit TopSpin, then log out. 23. When is it acceptable for you to take metal objects near the magnet? A. When there is no sample in the magnet. B. When there is no experiment running. C. When the metal objects are small, such as paper clips or staples. D. When no-one else is around. E. When you want to show your friends how powerful the magnet is. F. Never. 24. In case of an NMR related (non-medical) emergency, who should you contact first? A B. Your Principal Investigator. C. The highlighted name on the PINMRF emergency contact list near the computer. D. Your friend who knows a lot about NMR. 25. Which of the following is the correct entry for the dir variable in the edc menu on a PINMRF Bruker Avance DRX spectrometer? A. /u B. /nfs/pathfinder/d1/u C. /opt/topspin D. None of the above.

7 26. Which of the following is the correct entry for the dir variable in the edc menu on a PINMRF Bruker AV-III spectrometer? A. /home/userid where userid is your login ID B. /opt/topspin/data/userid/nmr where userid is your login ID C. /opt/topspin D. None of the above. 27. If you find that your NMR tube is very loose in the sample spinner, what should you do? A. Stick a piece of Kimwipe or other paper into the spinner to help hold the sample. B. Remove the rubber o-rings from the spinner. C. Step on the ears of the spinner with your foot to compress them more tightly. D. Put your NMR sample into a new tube that fits correctly. E. Check the fit of the standard sample if it is loose too, notify PINRMF staff. 28. If your lock signal is unstable (it fluctuates to higher and lower levels) what should you do to correct this? A. Stop your work immediately and notify PINMRF staff. B. Eject your sample and restart the process again. C. Decrease the lock gain. D. Decrease the lock power. E. Nothing can be done about it it s the nature of the specific sample. 29. Which 2D NMR experiment(s) are set up for you to run using standard parameter sets on a PINMRF Bruker/TopSpin NMR spectrometer? A. COSY. B. TOCSY. C. ROESY. D. Phase-sensitive DQF-COSY. E. HMQC / HMBC. F. HETCOR / COLOC. 30. If an NMR magnet quenches while you are running an experiment, what should you do? A. Run out of the lab as fast as you can and then set off the nearest fire alarm. B. Stop your experiment, remove your sample from the magnet, then notify PINMRF staff. C. Open the lab windows and doors, cover the magnet, then notify PINMRF staff. D. Leave the lab immediately, crawling close to the floor if necessary, then notify PINMRF staff. E. Notify PINMRF staff, then wait until the vapor clears to continue your experiment. 31. Which NMR experiments in the list below require additional training from PINMRF staff before you are allowed to run them on the PINMRF Bruker spectrometers? A. Some low-temperature VT experiments. B. The 13 C DEPT experiment. C. Any experiment with nuclei for which we do not have a PINMRF parameter set. D. Any multi-dimensional experiment for which we do not have a PINMRF parameter set.

8 32. You are running a 1 H NMR experiment and you notice that the peaks in your spectrum are broad and have an extra splitting on the upfield side. Which of the following are possible source(s) of the problem? A. The shims are not optimized. B. The probe tuning is poor. C. You loaded the wrong parameter set. D. The sample is not spinning. E. The sample volume is too small. 33. You are trying to print out your spectrum but the printer is not responding. Which of the following activities are reasonable for you to attempt regarding the problem? A. Check that the printer has paper if not, you may reload the printer. B. Execute the plot command approximately 20 times to force the printout to appear. C. Turn off the printer s power, wait one minute, then power up the printer again. D. Turn off the power to the spectrometer computer. E. Notify PINMRF staff. 34. If you have a PINMRF related problem, and need to ask Donna Bertram who to contact about it, where could you find her during normal business hours? A. RHPH G43 B. WTHR 365B C. WTHR 361 D. She works from home. You would have to her your questions. 35. On the PINMRF Bruker/TopSpin NMR spectrometers, what do these commands mean? ns ef zg print rpar rsh standard apk exit edte