Those not following the policies of the NMR facility will have their access to the facility revoked.
-Only authorized users may operate the instruments in the NMR facility. Using someone else’s account is strictly forbidden.
-Only registered users are allowed to enter the NMR facility. Please contact the lab manager for an induction before entering.
-If there are any faults or software issues do not attempt to solve the problem.
– For any problems phone the lab manager using the the speed dial button on the the phone in the lab.
– Take extreme care when doing variable temperature studies as the probe can be damaged beyond repair. Do not exceed above 100°C and stay at least 10°C below the solvent boiling temperature. Cooling down VT experiments are not allowed without the presence of the lab manager.
-Do not bring or wear lab coats and gloves when you enter the NMR lab. You must not wear lab gloves when operating a NMR instrument.
Please remove your samples from the auto sampler within 24 hours after completion of your analyses.
- NMR times on the walkup 500MHz.
- Day queue: 09:00 to 18:00 . 10 hours.
- Night queue: 18:00 to 09:00 . 14 hours. Maximum 4 hours per user.
- Weekend queue: 09:00 Saturday to 09:00 Monday . 48 hours. 8 hours per user per day/night. Try not to use long analyses during the day.
- For the 600MHz and top load 500MHz use the booking sheet.
Please take care regarding the following:
- NMR tubes: Use only full length NMR tubes.
- Exit of NMR software: Don’t shutdown or close the software.
- Do not use a USB on the NMR controlled computers.
- Manual Re tuning: Not necessary or allowed.
- Your sample will be ejected automatically when finish and be replaced by sample in holder #1.
- Auto sampler: Do not re locate your sample after it was submitted to an assigned slot.
Label the samples appropriate as discussed in the Sample prep section.
Every week excess unnecessary samples will be cleared and discarded.
NMR times is always limited. Please book the NMR at least 12 hours prior to usage when special experiments are needed.
The following should represent best practice for the analysis of the majority of samples:
- Obtain proton spectrum.
- If the proton is clean and shows sufficient concentration then obtain COSY and/or HSQC.
- An HSQC will provide the chemical shifts of C-H, CH2 and CH3 carbons and this is usually fast using the NUS (Non Uniform Sampling) option.
- If the structure still cannot be confirmed then obtain a HMBC spectra.
- In most cases the structure can be resolved without a carbon analysis. Due to a carbon spectra being very lengthy, specially in dilute samples, use slightly longer HMBC or HSQC analysis.
- If the structure still cannot be confirmed consider specialist experiments (TOCSY, NOESY etc).