Open the folder for the NMR you want data from ( e.g. If an "Unknown Fingerprint" dialog appears, select Always then click Allow. Enter the Server, Username, and Password, then click Connect. From the dropdown at the top, select SFTP (SSH File Transfer Protocol). Click the Open Connection button in the top left. One such client is Cyberduck, a free program available for Windows, and Mac. Please note, this is different from a regular FTP file server, and you will need to use an SFTP-capable client to download your data. The data is available on the facility's SFTP file server (the server name, username, and password can be found in any of the NMR labs). If, after the third try, ii still produces errors, please eject your sample, leave a note on the spectrometer, and send an e-mail describing what happened. If it does, run ii a second (or third) time, until no errors pop up. This command can take a minute and may produce some error messages. If the above does not work, you can try to re-initialize the spectrometer hardware by typing ii in the Topspin commandline. This 'pages' the instrumentation specialist, and you will hopefully get a response in five minutes. This is often necessary when tuning to different nuclei such as 19F or 31P.įirst, call 9-3163 and leave a message. If wobb shows a featureless (but not noisy) line near the top of the display, try changing the tuning width ( wbsw) to 60 and re-tuning. If it does, run ii again until no errors pop up. If wobb shows a flat noisy line at the bottom instead of a tuning curve, type stop to stop tuning, then ii to re-initialize the spectrometer hardware. Broken tuning rods cost thousands to repair. 
If you have not been trained, or feel uncomfortable, do not tune the probe. If Topshim fails, the usual cause is a sample volume of less than 0.6 mL. Topshim often takes a long time with CDCl 3 - this is normal. If your sample is cloudy, or has a volume less than 0.6 mL, you may have no choice but to correct those issues prior to being able to lock. Be sure to select the correct solvent from the list! If you did not do so already, load a standard shimset ( rsh), then try locking once again. Leave a note on the spectrometer saying "BROKEN TUBE INSIDE PROBE, DO NOT USE THE NMR". Do not try to eject the tube or do anything else - that runs the risk of causing (more) damage. Inside the magnet: if you were spinning the sample, stop the spinning to avoid further damage. Leave the glass in the dustpan and notify the facility manager. Outside the magnet: please use the broom and dustpan to sweep up any broken glass and chemicals. No! If your tube slips in the spinner, even by a few millimeters, it will hit the thermocouple at the bottom of the probe and possibly shatter. Next, transfer the sample to a clean 5 mm NMR tube (you cannot use an EPR tube). If your sample does not dissolve in the solvent, you will not see an NMR signal from it.
What are the current user fees? NMR Answersĭissolve your sample in at least 0.6 mL of a deuterated solvent. How do I get the PDF spectrum off the MALDI computer?. Should I use the "pep CCA" or "prot SA" calibrant spot?. My spots are taking a long time to dry. How are the stock matrix solutions prepared?. 
What are the current user fees? MALDI Questions. How do I get my data from the NMR computers?. I'm having another hardware problem not listed here. Topshim is taking a long time or not working. The NMR won't lock onto my deuterated solvent. What should I do if an NMR tube breaks?.
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