Sample Submission
Our five solution NMR instruments are available to trained users for walk-up use without the need for booking.
Only trained and registered users nominated by their supervisor and approved by the NMR manager are allowed to enter the NMR lab and place their samples in sample changers.
Before taking your tube(s) to the NMR lab, please wipe the bottom ~10 cm of your tube with acetone or isopropanol. If the surface of the NMR tube is not clean, your NMR tube will fail to spin, and the dirt from the NMR tube will transfer to the inner glass in the probehead inside the magnet.
On entering the NMR lab, leave your watch, wallet, bank/travel cards, keys and any other personal items, which can be affected by magnetic fields, on the filing cabinet near the entrance or on the table between the old fridge and the printer. You can now cross yellow/black 5 Gauss lines on the floor.
To choose a position for your sample in the sample changer, use the Windows workstation of the spectrometer selected by you. Log in by selecting your supervisor’s initials from the list and typing the correct password (case sensitive, check CAPS LOCK on the keyboard).
Please check the window with 60 or 24 (400MHz only) numbered circles coloured green (available, e.g. position 25 on the left), light green (reserved, e.g. position 26), yellow (finished) or red (currently running) on the screen. Select a position in green. In case there are no green positions, choose a position in yellow (finished samples) and press the “Delete” button, which is near the middle of the screen.
If there is a tube in the position reserved by you, remove it from the sample changer, release it from the blue spinner and place this tube in the beaker on the PC desk of the spectrometer. You could now use this spinner with your sample tube. If there is no tube in the position selected by you, look for a free spinner in the sample changer (400MHz), in the rack above the spectrometer console (500, 600 and 700 MHz NMRs) or on the PC desk (300MHz NMR).
Before inserting your NMR tube into the spinner, clean the outside surface of the tube from fingerprint residues with the medical wipes provided.
Use a depth gauge to set the NMR tube inside the spinner at the correct position. The NMR sample depth gauge can be found on the PC desk or above the console of every spectrometer. The cylindrical depth gauge, similar to those used on our spectrometers, and its schematic presentation are shown on the right.
Each spectrometer has its own gauge. Please check that there is no broken glass or liquid inside the gauge before using it!
The sample is inserted slightly into the blue spinner first, then placed in the gauge for the correct height adjustment by further insertion. The tube is positioned such that the bottom of the tube touches the white level at the bottom of the gauge. You may damage the equipment if you do not position the NMR tube correctly.
The sample can now be placed in the position you selected in the sample changer. Do not place an NMR tube in the sample changer if it is held loosely in the spinner. It will slip down inside the spinner when transported to and from the magnet. Please replace the tube or contact the NMR manager.
Once the sample tube is placed in the sample changer, return to the workstation and double-click on the position number on the screen to open an experiment line and fill in the details (position 20 in the example below):
(1) Name - use letters and numbers, no space, no special characters except “-” or “_”, e.g., ABC001 or XY-498 or AX_034. Initials of the person submitting the sample are used as the first two or three letters. Avoid using very long names.
(2) No. - the experiment number (e.g. 10) will be provided automatically and correctly by the program. You do not need to change it.
(3) Solvent - choose from the dropdown list.
(4) Experiment - choose from the dropdown list.
(5) Title/Orig - provided by you in a free format as a description of your sample with an additional e-mail option.
Should you wish to run more than one experiment, click “Add” and select another experiment from the dropdown menu. If you choose a 2D experiment, 2 or 3 experiments will appear in the list automatically. Avoid deleting additional lines or editing numbers in the “No.” column. See (5) in Common problems for more details.
Highlight the first line with the position number and click the “Submit” button in the left middle of the screen. This will submit all experiments for a given position without the need to submit each experiment separately. Click “Change User” to log out and disable access to your account.
If you are in the NMR lab to collect your samples, please check the sample changer first, then the beaker on the desk and then the old fridge opposite the 300MHz magnet. If your NMR tube is in the sample changer, remove it from the sample changer, release it from the blue spinner and place the spinner in the rack either on the spectrometer consoles (500, 600 and 700MHz NMRs) or on the PC desk (300MHz). On the 400MHz NMR, place the spinner back in the same position in the 24-position sample changer. Never place free spinners without samples back in the sample changer on spectrometers with BACS-60 (300MHz). Do not take away spinners from the NMR lab. These are expensive, over £100 each. If found anywhere else in the department, they must be returned to the NMR lab. Do not use the NMR lab for sample storage. Users must collect their NMR tubes from the NMR lab once all the NMR experiments have been run. The sample changers will be emptied from time to time. Samples removed can be found in beakers on PC desks or in the old fridge opposite the 300MHz magnet.