Instrument Issues

It is imperative that samples are submitted to the SampleJet properly – this will help us avoid numerous system failures!

• Caps MUST be completely engaged on the NMR tube.  After quick inspection of the rack daily – we’re finding lots of caps that are barely holding on.  Please see the picture below.  If you tube is almost touching the bottom of the rack – your cap is not on far enough!!  If too long – the system will fail.
• Caps cannot be split!  Again, looking through the rack – there are usually several split caps.
• NMR tubes cannot be broken/cracked.  The caps must be on exactly straight.

With variations of tube lengths, caps on/off/split – the system can never fulling be calibrated.  Our errors will continue if these steps are not followed.   If this continues – we may have to start requiring only one brand of NMR tubes – which may increase your cost/sample.  You will still need to follow the direction above!

-TLW, NMR manager

The AVIII 400 NMR-Saffron is down due to a hardware failure.  Because there is a chance of sample breakage – the system will be unavailable until the issue is resolved.  Please plan on the system being down for a few days.  The 400 MHz in Evans is available (quick walk in the cold weather) or have a labmate run samples on the 600 MHz.

Problem details:  The SampleJet ‘arm’ falls after the sample is inserted.  When the sample is ejected, the NMR tube gets pushed down into the spinner.  At this point, the system fails to pick up the sample and stops the run.  So far, this has not broken an NMR tube, but it perhaps might.  Bruker has been contacted to determine the source of the problem.

Update 1.5.2018:  The system is now available.

The AVIII 400 MHz (in CBEC) is experiencing an occasional error. The instrument will fail to complete an ‘ATM’ or ‘rga’ during the experiments and the instrument then sits until we reboot. This appears to be a hardware problem in the console. I’m in communication with Bruker to pinpoint the issue and make repairs as quickly as possible. In the meantime, we’ll be checking the system as much as possible to keep the queue moving along. If the system has a failure on your sample, you will need to resubmit.

Thanks for your patience as we troubleshoot the problem.

UPDATE 7.5.2017

Topspin 3.5pl7 is currently being installed on the system to alleviate these intermittent atma issues.  Please be patient as there are a few issues with the upgrade.  Hopefully, the system will be back up and running today or tomorrow!!  Very sorry about this interruption!!

UPDATE 7.7.2017

Great news – the software upgrade has been completed successfully! Thanks so much for your patience having the system down for 1.5 days! Please keep me informed if you run into any problem – no matter how insignificant it seems. I’ll be monitoring the system carefully.

Continue to be diligent with sample handling:
No damaged/split caps
No damaged/chipped NMR tubes
Caps must be on completely
Double-check that your sample position # isn’t currently being used

Hopefully, we’ll have less issues from both software glitches and user error. We’d all like to less downtime on our workhorse NMR instrument!

UPDATE 8.1.2016:  ISSUE RESOLVED

The 600 MHz (NMR-Sage) is still experiencing ‘atma’ failures after a probe repair and a software upgrade.  The ‘atma’ command fails intermittently when tuning on the proton channel (any proton experiment or X-nuclei using proton decoupling).  Your experiments can still run; however, the signal intensity will be reduced (the pulse lengths will not be optimized with a de-tuned probe). Until this issue is resolved you’ll want to avoid multi-pulse (T1, T2 measurements), quantitative protons, water suppression, and 2D experiments, especially those which are phase-sensitive (NOESY, HSQC) as they will not acquire properly.

Bruker is aware of the issue and working with me to resolve the problem as quickly as possible.  Please watch for updates.

CLEAN/WIPE YOUR NMR TUBES and SPINNER every time! The probe coil and glass insert are terribly dirty and may be damaged.  It only takes one dirty sample to cause shimming/tuning issues, background signals, and/or costly damage.

As you may have noticed, the probe on the 600 MHz (NMR-Sage) has been experiencing an intermittent tuning issue. The ‘atma’ fails occasionally when using different solvents. In order to fix this issue, the probe will be shipped to Bruker next week for warranty repair. The repair should only take 1-2 days plus shipping time. Rather than re-train everyone on our back-up probe, the instrument will not be available for usage.

I’ve marked the instrument down next week Tues – Mon (June 21-27). Please check the FOM calendar and/or u.osu.edu/cbcnmr for updates.

The AVIII 400 is experiencing a hardware issue on the SampleJet.  Your samples are occasionally getting stuck in the system, which stops the runs.  If this issue continues to repeat at its current rate, we will be forced to shut the system down.  The sample shuttle (a fancy version of the spinner) is getting lodged in the BST (the top of the magnet).  There is a possibility of sample breakage, so we cannot continue to use the system.

Bruker – Zurich is working on figuring out what the issue might be.  The SampleJet keeps detailed logs of each sample insertion, including lift parameters and even a picture of each sample.  Since its probably nighttime in Europe, we’ll likely not hear back until tomorrow.

Thanks for your patience as we work through the issue.

Tanya

UPDATE:  This situation has been resolved by supplying more compressed air pressure to the system.