A) The basic features of our 6 open-access NMR instruments are listed below.
|
Automation |
Detect |
VT |
|||
|
Sampler |
Available experiments |
Not available experiments |
|||
|
A400a |
y |
All nuclei |
F1 Obs/H1 Dec |
n |
|
|
A400c |
y |
All nuclei |
F1 Obs/H1 Dec |
n |
|
|
A500a |
n |
All nuclei |
F1 Obs/H1 Dec |
minus 80 to plus 130 |
|
|
A500b |
n |
All nuclei |
F1 Obs/H1 Dec |
minus 10 to plus 130 |
|
|
A600a |
y |
C13 and H1 |
Any other nuclei |
n |
|
|
A400b |
n |
C13, H1 and F19 |
Any other nuclei |
minus 80 to plus 130 |
|
|
F19 Obs/H1 Dec |
|||||
|
Access |
Day Time |
Day time |
|||
|
Host name |
limitation |
Priority |
|||
|
A400a |
A400a.chem.yale.edu |
30 min/sample |
2 |
||
|
A400c |
A400c.chem.yale.edu |
10 min/sample |
2 |
||
|
A500a |
A500a.chem.yale.edu |
||||
|
A500b |
A500b.chem.yale.edu |
||||
|
A600a |
A600a.chem.yale.edu |
2 hours/sample |
1 |
||
|
A400b |
A400b.chem.yale.edu |
||||
How to get time:
A400a, A400c and A600a: Walk-in.
A500a, A500b and A400b: on-line booking. There are several rules. Only one booking is allowed. Only one day before can be booked.
B) Sample preparing:
1. D2 solvent: for field lock, gshmming, magnet homogeneity.
2. Sample length and position: the minimum sample length is 3.6 cm for 5 mm diameter tube and 2.8 cm for 3 mm diameter tube in the Agilent NMR machines. Sample should be symmetric to the center of the coil.
3. Sample should be well dissolved, including the temperature request.
C) For machines without an autosampler:
Login with Yale NetID/password.
“Start” -> “Eject”, remove the dummy sample and put your sample into the magnet. Do not put your sample into the magnet if the dummy sample is missing!
On the left side of VnmrJ, click “Protocol”.
Click “New Study” -> “Sample name” -> “Solvent” -> Select experiments.
Top: “Experiment selector”
“View” -> “Experiment selector” or “Experiment selector Tree”
“Liquids” -> “Std 1D” -> P31, F19 and (C13)Dept (for example)
“UserStudies” -> Other nuclei, such as B11, Si29 If an option you need is missing, contact CBIC staff.
To modify default parameters: double click the experiment -> modify the parameters -> “Show time” and “Save” to update.
(C13) Dept -> “XH Multiplicity editing” -> “XH/XH3 up & XH2 down” -> “Quaternary Carbon” -> “Suppress”.
“Day” or “Night” -> “Priority”
“submit”
Middle: “Study Queue”
“Sample”
“Spectrometer” displays the whole list: active, finished, queued.
D) For machines with an autosampler.
Before setting up your experiments, look at the sample position selection diagram on the screen and see what positions are available. The position diagram has seven different statuses for each position indicated by different colors: sample loading (light blue), running (purple), waiting in day queue (yellow), finished (green), waiting in night queue (dark blue), failed (red) and empty (gray). If the tray position screen is not visible, click “Open tray panel” button just below the command line, at the left top corner.
Press the footswitch to unlock the door of the automation unit, open the door and add your sample(s) to the tray(s). Make sure the door is fully closed and re-locked after you add your samples.
In VnmrJ: Click -> “New Study”, enter sample name, solvent and comment (=title). Select experiments you want to run, highlight the position of your first sample in the tray (by clicking on it), then click “submit”.
If you make a mistake, right-click on the position and select “delete”, “edit” or any other commands.
When taking samples out of the trays, press the footswitch to request unlocking of the door. Do not touch other people’s samples! Pick up your NMR sample as soon as possible after it has finished running even if you no longer need it – we do not want to deal with your lab waste!
Some tricks for setup of experiments in automation:
1. A400a and A400c are for short experiments: maximum time is 30 minutes or 10 minutes (respectively) for each sample during the day time. For A600a, the daytime limit is 2 hours per sample. If the experiment time requested is longer than the time limit, the experiment will automatically change to ‘night queue’.
2. Each user has a maximum two samples set/running as ‘priority’, each of which will run first before any non-priority experiment in the queue.
3. After selecting the experiment and double clicking it, the acquisition parameters can be modified. Click “save” button before exiting the modified mode.
4. For multiple samples with the same experimental parameters, the same ‘submit’ mode can be used. Only the sample name, solvent, comment and location need to be changed.
5. A600a has much higher sensitivity and should only be used when your sample has low quantities of material. Use A400a and A400c if possible.
E) Transferring data to your desk:
WinSCP -> “Host name” -> “User name” and password -> /home/Your_NetID
F) On-line support.
1. Training. click “CIC Homepage”, look at User guides -> NMR.
2. Troubleshooting. Look for solution: click “CIC Homepage” ->” Troubleshooting”. And see the possible solutions.
3. Report problem ASAP -> click “Report a Problem” on the booking web-site-> Or find staffs.
4. MNova installation and usage.
When you use the machine first time independently, you may ask us to monitor the process.