• NMR Submit Sample Form in HTML format or PDF format
• NMR Facility Usage Fees
• Scheduling Policies
• NMR Training
• Sample Preparation
• Safety Issues

• Backup tape(600Mb): $10/ea.
• Backup CD (1Gb): $10/ea.
• Low temperature Experiments: Cost of cryogens($50/N2(l) tank)

• A financial statement signed by a person responsible for the running costs of the samples must be submitted before time is scheduled or along with submitted samples.
• All other expenses related to the sample, solvents, NMR tubes, MAS rotors, etc. are to be provided by the users.
• There will be a charge for repair(including parts) of damage to the instrument caused by negligence of the user.
• The instrument time needed for training will be charged based on the prime-time assisted operation hourly rate.
• Additional charges may be assessed to cover staff time spent with exceptionally involved experiment setup or data work-up, including preparation of specialized sample holders.
• Each Faculty member will be given 100Mb of space on the data server at no charge.

Instrument scheduling varies depending on the instrument. Five instruments ( GN-300, Mercury 400, Mercury 300, Gemini 300, and Gemini 200) have short time blocks available for walk-up spectrometer use. Advanced scheduled overnight runs are also available on these instruments. Long time blocks are available on the Varian 600 , Bruker 500, Chemagnetics 200, and the (advanced scheduling required)

• An NMR Facility Account must be established by a person responsible for NMR Facility charges prior to the submission of samples or scheduling of instrument time.
• To use the spectrometers, certified users who have previously been trained and checked out by one of the Facility staff members can either sign up or ask the staff for spectrometer time. Non-certified users must submit their samples to the Facility.
• Prime time is 9:00am - 5:00pm Monday - Friday. This time period is mainly for short experiments, and for those who need assistance in setting-up experiments.
• Non-prime time refers to all other times. These time slots are for longer experiments. Assistance from the Facility staff will normally not be available during these times.
• The scheduling will be on a weekly or monthly basis depending on the instrument. For instruments scheduled weekly, the fixed schedule will be posted on the scheduling notebook inside of each spectrometer room (9 and 15 Dabney) by noon Friday. Once a schedule is set up, no change will be made, and the billing will be based on this fixed schedule. But a time switch by mutual agreement between users is possible. In this case, users must inform the pertinent Facility staff as soon as possible, preferably before the time they actually use the spectrometer. For instruments scheduled monthly, the schedule will be available in 12 Dabney on the FOURTH FRIDAY of the month.
• Highly labile samples may require special scheduling. Such requests should be made at least two weeks in advance.
• The NMR Facility will reserve a portion of the instrument time for instrument maintenance, instrument repair, instrument upgrades, and to run submitted samples. This time will vary from week to week as necessary. Magnets are normally filled with cryogens on Tuesday morning.
• Requests for time on the 600 MHz and 500 MHz spectrometer should include justification for the need for the higher field.
• Any time not previously allocated will be available on a first-come-first-served basis as long as the prime time and non-prime time rule is followed.
• If an experiment cannot be done due to the spectrometer problems, it will be scheduled on the next available scheduling cycle with priority over new requests. In this case, the person who wants to use the spectrometer does not need to submit Request for Spectrometer Time again unless there are any changes. Those reassigned will be notified by a staff member.
• Data should be removed from the spectrometer hard drive within a week of its acquisition. In an emergency, a master copy can be obtained from the Facility Staff. A two week notification is required.

• Mercury 400, Mercury 300, Gemini 300 and Gemini 200: Request for Spectrometer Time must be submitted to Dr. Sabapathy Sankar . The fixed schedule will be posted on the scheduling notebook inside of each spectrometer room. The Gemini spectrometers are self scheduled instruments. Please sign-up on the schedule sheet in the instrument room.
• Other spectrometers and/or times are available to certified users but must be scheduled by Facility staff members.
• Varian 600, Bruker 500 : Requests for spectrometer times must be submitted to Dr. Hanna Gracz by 10:00am on the LAST FRIDAY of the month for times in the next month. Please provide information as to the amount of NMR time desired, the desired start date, and the experiments that will be performed. Late requests will be given the lowest scheduling priority. Users are requested to notify the NMR Facility one week in advance if they are unable to use their scheduled NMR time. Users who fail to notify the NMR Facility at least 3 days in advance will be charged for the time scheduled. The schedule will be posted on the scheduling notebook inside room 12 Dabney by noon on the LAST FRIDAY of the month.
• Chemagnetics 200 MHz : Requests for spectrometer times must be submitted to Dr. Jeff White.

The NMR instruments operate 24 hours a day, seven days a week. Gemini 200 spectrometer is mainly used for teaching during the Spring and Fall semesters. All Gemini 300 spectrometer time and the rest of Gemini 200 spectrometer time are devoted to the users certified by the Department of Chemistry at NCSU. Instrument sign-up is divided into 20 minute blocks and overnight runs.One may sign up for multiple blocks not to exceed 2 during daytime hours.

For Mercury 400, Mercury 300, GN Omega 300, time slots of 9:00am -9:00pm on Monday, Tuesday, and Thursday, and those of 9:00am - 5:00pm on Wednesday and Friday are set aside for sign up for short term usage. Other times on the GN300 will be scheduled for long term usage. Occassionally, the entire time from noon Friday to noon Monday can be scheduled on the GN 300.

Normally, training on the Mercury 400, Mercury 300, GN 300 or Gemini 300 requires a minimum of 6 hours (3 x 2h classes). The time for training may take less time if an individual has previous experience on these spectrometers. The training classes will be arranged according to an individual's schedule. We do not encourage you to bring your own samples to the training session. Once an individual has completed the instrument training they are authorized to use the spectrometer.

To schedule training:
Training on the Mercury 400, Mercury 300, Gemini 200, Gemini 300, and the GN 300 may be scheduled with Dr. Sabapathy Sankar. Training on the Varian 600, Bruker 500 may be scheduled with Dr. Hanna Gracz. Training on Bruker DSX 300 and Chemagnetics 200 MHz may be scheduled with Dr. Jeff White. Other inquiries my be directed to Dr. Ken Hanck.

• Always use a clean and dry sample tube
• Always use the same sample volume or solution height.
• Recommended values for 5mm tubes is 0.6ml of solution
• Use the depth gauge to position the sample correctly in the spinner.
• Check that the sample tube is held tightly in the spinner so that it does not spin during an experiment.

• For Mercury 400, Mercury 300, GN 300, Gemini 300, and Gemini 200 NMR Spectrometers: For proton spectra, dissolve 5 - 10mg of sample in ~0.7mL of deuterated solvent. The NMR tube should have a minimum of 5cm of liquid from the bottom of the tube. For carbon spectra, make the sample as concentrated as possible(~50mg or more in 0.7mL of deuterated solvent). This will reduce the spectrometer time to get a quality spectrum.
• For the Varian 600, and Bruker 500 NMR Spectrometer: Prepare the sample using a volume of solvent so that the NMR tube has 3cm of liquid measured from the base of the tube. Typically this is approximately 0.6mL with most 5mm NMR tubes. The amount of solvent required will vary with the probe. For example, the NALORAC probes absolutely require sample volumes corresponding to 3cm in the NMR tube.
• Solvent Purity: Many solvents absorb water which can reduce the spectrum quality. Water absorption can be reduced by storing the solvents over dehydrating agents (molecular sieves) and/or in desicators.
  Deuterated chloroform contains a trace of acid. This can lead to the decomposition of acid-labile molecules.
  For low sample quantities or obstructed resonances solvents with higher deutrium incorporation than is available in the stockroom are available for purchase through a variety of vendors (ie. CIL). Typically the '100% Deuterated' solvents are expensive and are sold in small vials.
• Floating Particles: Best results are obtained on samples that are fully dissolved in the solvent. Filter out particles using a pipette that has a small piece of clean cotton in it.

Pacemakers may misfunction in the presence of the magnetic field. It is advised that persons with pacemakers do not go near NMR spectrometers. Please make arrangements with the NMR staff or other co-workers to acquire NMR data. Remember, the magnetic fields of the spectrometers are reasonably strong a considerable distance from the magnet.

Credit cards will be erased by the magnetic field. Watches may be damaged by the magnetic field. Do not bring credit cards and watches in the NMR labs.

Quenches
Magnet quenches occur very rarely but can have very serious consequences. A 'quench' is the spontaneous loss of the superconducting quality of the magnet. This causes the inner core of the magnet to become very hot and results in a rapid boil-off of the liquid nitrogen and liquid helium in the dewars surrounding the magnet. Typically, a quench produces a very loud constant noise and a large white plume from the top of the magnet. During the quench, oxygen is frozen out of the air and the room becomes filled with helium and nitrogen gas. Therefore, it is absolutely necessary to evacuate the room when a quench occurs. Quenches can not be predicted and, sometimes, not prevented.