NMR Facility Recent Notices

NMR Lab Remains Open Until Further Notice (03/17/2020)

The NMR Facility will remain open until further notice. Keep in mind that user operation shutdown is totally possible in the coming days in concert with plans around campus.

Please use the sanitizing wipes to clean hands and surfaces after you have used the instruments. The lab area is one of the common places that potentially may spread the virus around.

Bruker 400 MHz Instrument Installation Postponed (03/16/2020)

We have postponed the installation of the new Bruker 400 MHz spectrometer until the conv-19 virus crisis is under control. In the likelihood of campus lockdown, I'll post notices regarding the status and operation of the NMR lab.

This notice page will serve as the main notice area for the status and operation of the NMR lab.

Keep Workstation Areas in NMR Rooms Clean (03/06/2020)

Due to widespread coronavirus concerns and rapidly worsening situations, it is important that everyone takes precautions and make efforts to keep the common areas in the NMR rooms clean. Hand sanitizing wipes are provided on each table next to the workstations. Please use them and close the lids after use.

Night Run Mode on New Bruker 500 (03/02/2020)

Night mode (off-peak hours) has been turned on the new Bruker 500 under IconNMR. Please watch the light status, with steady yellow indicating experiments are queued to run or are runnig. DO NOT remove any samples from the autosample changer from this point on. Currently, night mode starts at 9PM and ends at 9AM on the next day.

Please try not to leave samples for night mode early during the day in order not to block the use of the sample slots. We'll set up more strict rules for the instrument soon.

Electrical Work in NMR Rooms (03/02/2020)

Emergency power outlets are being installed in the NMR rooms. If ongoing work interferes with your work in the area, please yield to the utility work. The work is expected to last a few hours.

New Bruker 400 Is Here (02/27/2020)

The new Bruker 400 MHz NMR spectrometer has arrived today. There are a few large crate boxes in the NMR room. Please use caution when walking around. Installation will be scheduled soon. Operation is expected after mid April.

Sample Pickup from Bruker 500 (02/26/2020)

A lot of samples have been left with spinners in the SampleJet on the new instrument after the experiments are done. Please come back and pick up your samples as soon as possible. The samples will be left in a beaker on the table. There is no guarantee that the samples will not be misplaced or lost.

New 500 Open for Trained Users (02/19/2020)

We have gone through a lot of things in two days with the Bruker engineer. The instrument is now open for trained users to use with IconNMR. Please use the booking page to roughly book your time. Any queued or currently running experiment should not be interrupted, but you may set up and submit new experiments to run.

We are working on the rules of operation. I'll update what changes we will make or will consider in the coming days.

Bruker Engineer Visit. New 500 Offline (02/18/2020)

A Bruker application engineer will be here today to help set up the new 500. The instrument will be unavailable for use until we finish the work.

Brief Shutdown Tomorrow of All Instruments for Utility Work (02/11/2020)

To finish installation of the air purifier for the new 400 MHz instrument, we'll have to shutdown all instruments for up to 2 hours from 7:30AM-9:30AM on Wednesday, Feb 12. Once work is done, we'll bring the instruments back up immeduiately.

New Bruker 500 Training and Use (02/05/2020)

We have started to open the 500 for general use. This will be a gradual process with priority given to projects that need the enhanced sensitivity and auto-sample loading capability. I'll try to train one or two people from each group to get started. If you have prior experience with a Bruker instrument running IconNMR under Topspin and will use the instrument immediately, please let me know. We will try to off-load heavy traffic on the Varian 400 and 500.

Some long-term procedures such as booking, rules and charging are still being worked out. But none should hold off general use. All common nuclei can be detected. The instrument is most useful for all X nuclei and 19F with a gain of 4X in sensitivity or 10-16 times reduction in data collection time (see sample data below). 1D 1H and 2D NMR sensitivity is similar to that on the 600.

Ideal use is that data collection is quened for multiple samples each set to run multiple experiments with the autosampler. Please note the sample tube height limit below. Any long experiment set from one user exceeding an hour or two during the day should be set up to run later at night. We will work out the rules.

Parameters haven't been calibrated for some non-common nuclei. We'll do the calibration as the needs come up. 2D NMR will be tested soon.

*Sample data from Julie Yu in the Lipshutz group

Sample Tube Height Limit with Bruker's Auto Sample Lift (01/27/2020)

The Bruker auto- sample lifting case has a safety lever that limits the sample length to slightly longer than ~ 7 inches. The NMR tubes in the chem store meet this requirement and are 7 inch long. To be compatible with the Bruker autosampler, please don't order new NMR tubes longer than 7 inches unless this is really necessary. Manual tube insert and eject (bypassing the autosampler) can be done, but it appears confusing to the system as it goes back and forth bewteen auto- and manual sample loading, causing significant delay.

New Bruker 500: Taking Samples to Run for X Nuclei (01/16/2020)

The new Bruker 500 equipped with a Prodigy cold probe is up running. However, it is not ready for open access which needs a few computer setup steps to be done. But, we'll run some samples for low sensitivity nuclei under a different mode. If you have samples that normally need hours of runtime on the other instruments for good signal-to-noise, please let me know and we'll run them on the new 500. The nuclei involved may be 13C, 15N, 29Si, etc.

Sample Insert Issues on 400 (01/13/2020)

The sample insert barrel on the 400 has been cleaned. Hopefully this will prevent the occasional problem with sample getting stuck and not sitting all the way down. Please pay attention to a distinct click sound when the sample settles and sits at the bottom of the barrel. If the sound is absent, the sample is likely not in the detection area, causing the lock signal to be extremely weak or absent. However, you should still see noise in the lock curve (Lock→Scan). If this happens, try to re-eject and re-insert the sample from the command line.

This issue is separate from the total loss of lock signal due to another unidentified hardware issue which requires a power cycle of the console. In this case, the lock curve is completely flat without any noise.

Adding Separately Collected Data (01/06/2020)

Sometimes it is necessary to accumulate data in separate data collections off the same sample or separate samples of the same molecules. Please follow this instruction to add up the spectra from such separate data accumulations.

NMR500: 30 mins max 9AM-4PM, 60 mins 4PM-9PM on Weekdays (01/06/2020)

We have revised the reservation limitation back to normal operation mode. However, the maximum block is relaxed to 30 mins from 9AM-4PM and 60 mins from 4PM-9PM on weekdays, instead of 20 mins between 9AM-4PM and 30 mins between 4PM-9PM as in the past. This should allow some 13C experiments to be done within the 30 min or 60 min block. For a single 1H experiment, 10 mins is sufficient for most samples. Please be on time and avoid overbooking and instrument time waste. Once the new instruments are running, we'll revise the rules accordingly.

NMR500: 60 Mins Max Block From 9AM-4PM on Weekdays (12/31/2019)

Update: Over the holiday period, the max block reservation on nmr500 has been further relaxed to 60 mins from 9AM-4PM on any weekday; there is no restriction during all other times. Please only reserve what you need. There is no change to the rules for the 400 and 600.

Enjoy the holiday break and look forward to a brand new decade!

Update: New 500 MHz Instrument Installation (12/20/2019)

Update (12/20/19): The loaner autotuning module is not working for X-nucleus tuning. All tests have been halted until we receive new parts from Europe after the new year.

Earler: Specification tests are ongoing, mostly quite well. The Prodigy cryoprobe is running. However, the variable temperature cooling unit (BCU II) was dead on arrival. Additionally, the autotuning module wasn't included in the box. Both new ones will be shipped from Europe, but they won't arrive before the end of the holidays. In the meantime, a loaner autotuning module has been sent to us from Bruker US center so that we may use the instrument and operate it at room temperature or above.

An application scientist will visit the site and assist setting up open-access operation and the software. The priority right now is to make sure the instrument meets all expected specifications before acceptance. We expect gradual open access along with user training to start early next year. Any urgent needs will be considered before that.

Enjoy the holiday season and stay tuned!

Bruker's User Height Sample Lift in Action (12/12/2019)

The magnet has been energized. Specification tests on the room temperature probe are in progress. The cooling unit isn't working; a new one has been requested and will be shipped from Europe but it may take some time to get here if it's available. We'll be focusing on room-temperature operation for now. The Prodigy cryoprobe will be assembled and tested next.

Here is a video clip of the 24-slot user height sample lift in action. It is a well designed, very useful, and user-friendly feature. The rest is real science we'll be doing.

VIDEO: Bruker's User Height Sample Lift

Mnova 14.1.1 Has Been Released (12/12/19)

There are some bug fixes. See release notes and instructions on how to obtain and activate new licenses.

New Bruker 500 MHz Spectrometer Being Installed (12/2/2019)

Please watch out for electric cables on the floor.

Update, 12/09/19: We'll energize the new magnet this week. There is a small chance of quenching during the process. We will not block access to the NMR rooms, but if a large amount of helium gas is released, please leave the rooms immediately. We do not foresee other safety issues.

Update, 12/05/19: The first engineer has finished the initial part of the installation. It'll take at least another week for the magnet to be energized early next week and up running later that week. The magnet has been pumped to reach low vacuum, then cooled and filled with cryogen. Another Bruker engineer will be here next week to energize the magnet to the targeted field of ~ 500 MHz (or ~ 11.764 Tesla). Following this, we'll be focusing on meeting various specifications.

We'll get routine experiments all configured ready for open access as soon as possible, but the instrument is unlikely to be ready for major open access until after the holidays. In the meantime, please enjoy a relaxing holiday season and get ready for much improved access and new capabilities.

Earlier: Please say hi to Bruker engineer Chris who came to install the new Bruker 500 MHz spectrometer this week. The NMR rooms are very crowded right now. Please use caution and watch out for gas and power lines on the floor.

Possible Power Outage Due to Fire and Rainstorm (11/26/2019)

Due to ongoing Cave fire and upcoming rainstorms, unexpected power outage will likely occur over the next week or two. If regular power is lost, please finish your work ASAP. The UPS will last ~ 10-20 mins, but building compressed air will be lost; it'll have to be turned back on by campus Facility. Do not continue to use the instruments after the loss of regular power.

Lock Issue on NMR400 Remains. See Instruction for Fix (11/22/2019)

If you enounter locking or loss of signal problem on the 400, please follow the instruction posted on the side of the console or contact me to fix it.

New Bruker 500 MHz Spectrometer Has Arrived (11/22/2019)

The first of the two spectrometers has arrived early today. All the crate boxes have been moved into the NMR rooms. Kudos to Adrian and Trevor for doing the heavy lifting. Please use caution when walking around in the NMR rooms and keep the doors locked at all times.

Energizing the magnet and installation has been scheduled to start in the first week of December, starting on Monday, Dec 2. After the magnet is energized and brought up to field, the engineers will spend time testing and meeting specifications. Any user work will wait untill the process is complete. We don't expect any significant open access before year end.

Please watch the notice area closely in the coming weeks for prompt status update.

~~~ Cheers, Hongjun

Decommissioning Idled 400 MHz Magnet (11/21/2019)

Here is a short video clip I took as the magnet is being quenched by the Bruker engineer Tony. Quenching started at ~ 30 sec mark with sudden intense liquid helium boil-off from the loss of superconductivity. You can see it was quite "uneventful" ....

VIDEO: Quenching/De-energizing an Unshielded 400 MHz Oxford Magnet

I wrote about helium and the helium shortage crisis in ~ 2014. The situation has not improved, unfortunately.

Farewell to an old magnet that has served many students and researchers for over 24 years!

Vacuum was broken during quenching. Ice condensation started to form outside the magnet.

Poor man's approach to testing whether the magnetic field is gone ... smooth transaction for a cup of coffee afterwards proved it :-)

12:50PM: All done! All instruments are open for use.
update (12:10PM): DO NOT ENTER NMR ROOMS UNTIL FURTHER NOTICE.
Update (8:00AM, 11/21): We will start the de-energizing process after 12PM. A short notice will be given before we initiate the steps.
Update (2:30PM, 11/20): It has been confirmed that de-energizing the old 400 will take place on Thursday. Exact timing is unknown. Expect short notice. See caution below for access restriction during the process.
Update (11/20): The engineer is unlikely to make it today. We are rescheduling the de-energizing work for tomorrow, Thursday.
Earlier (11/19): Tomorrow, Wednesday, there will likely be an engineer visit to de-energize the old 400 MHz NMR spectrometer. Exact time is unknown yet. When the vacuum is broken and the magnet starts to lose superconductivity, a large amount of helium gas will evaporate off the dewar. For safety reasons, we'll block off access to the NMR rooms for an hour or so during the process, although all doors and windows in the rooms will be openned. Once it's done, the status will be updated.

New Bruker 500 MHz Spectrometer to Arrive This Week (11/18/2019)

We will have delivery of a new Bruker 500 MHz spectrometer system likely by the end of this week, much earlier than expected. Due to a large number of boxes and several crates, extra space is needed in the NMR room for storage. Please use caution in the NMR room for your safety and also not to damage any equipment in a tight space.

Decommissioning the old, idled 400 and installing the new instrument has been scheduled to take place in the first week of December. Any changes will be updated as soon as we receive them. If things go smoothly as planned, we expect the new spectrometer to be open for use by the end of the year, likely partially after mid December. With the Prodigy cryoprobe, we expect a dramatic boost (3 to 4 folds relative to existing broadband probes) to signal-to-noise ratio across all nuclei, translating into an equivalent 10X reduction in data collection time for most samples. This is most useful for insensitive X-nucleus detection bewteen 15N and 31P frequencies.

Heating Problem in PSBN (11/13/2019)

We have no heating in the NMR rooms. The building boiler is still being repaired, installed. We expect return of heating and room temperature to ~ 22C within a week.

Additional Mnova Licenses Acquired (11/08/2019)

Update: New licenses have been added. The new licenses extend all updates up to 12/03/2020. Please follow this instruction for the new license required for future software updates.

Earlier: We are running out of floating Mnova licenses. Additional licenses have been acquired. Once the new additions are received, we are able to accommodate more users. Right now for the users who are at the required 90-day automatic renewing, you may see an error when opening Mnova. You may try another network connection (especially chemBiochemSecure) if it's a network connection issue. If it is due to the running out of the floating licenses, the problem will go away once we receive the additional licenses within days.

Lock Problem on NMR400B (11/05/2019)

Update: A board that was sent for checkup appears to be Ok. We continue to look for the source of the intermittent, sporadic signal loss problem. The instrument works fine except for this occasional, persistent problem. Please read the following instruction.

If you encounter an error that indicates lock failure with a message "S/N too small ..." after autolocking and/or the lock scan (in Lock panel) curve appears totally flat, please let me know. This problem also causes no signal in any spectrum. It can be fixed for the time being.

An instruction sheet to power cycle the console is left by the computer so that a user can fix it when I'm not available. Please only use this instruction for this particular problem for the time being. Repeated power cycling isn't good to the electronics in general.

If you have encountered this issue, please e-mail or let me know the time and the command or experiment you are using immediately before the problem.

Don't Use 600 for Direct 13C Detection (10/30/2019)

A change in the 600 configuration was made recently to give the maximum 13C excitation bandwidth. This change disabled 13C direct detection ability. Redgardless of the change, the probe is an inverse probe that has very low 13C sensitivity. The 600 should be used only for 1D 1H and 2D NMR (with indirect 13C detection).

Possible Electric Power Problem This weekend (10/18/19)

Depending on where you live, we have received alert notices for possible power shutoff this weekend due to high wind in the Santa Barbara area. Presently, no alert is given to UCSB, but power glitch is possible over the weekend. If we lose regular power, please finish off your work, save data ASAP and stay off the instruments. Building compressed air will be off in 20-30 mins once regular power is gone.

Promptly Cancel Reserved Time If Not To Be Used (10/21/19)

We continue to see many reserved block time slots are not being used and the reservation is left as is, blocking others from using the instruments. Please make sure to cancel leftover time slots after you are done and cancel ahead of time any reservation that is not going to be used. Any user can use the instrument if the booking user doesn't show up after 10 mins past the reserved time. But please consider reasonable circumstances and unforseen delays.

Lock Problem on NMR400B (10/10/2019)

Update (10/15/19): The lock still behaves erratically. As different boards are being swapped, you may see different issues. So far however, we are able to keep the instrument running for the most part. Gradient shimming isn't affected. If lock isn't stable, you should still do autoshim. Before data collcetion, you may turn off lock in the Lock panel and also enter alock=n at the command line. This allows you to run a brief experiment (<30 mins) unlocked. We'll continue to talk with Agilent engineers to have the problem fixed.

Earlier: The sporadic, inconsistent lock problem persists on the 400. We have been talking with Agilent engineers and support about the issue, have swapped multiple lock boards but still haven't traced down the exact cause yet. Over the last few days, it occurred a few times when autolock failed with an error message "S/N too small ..." among others. We were able to bring it back to working condition quickly each time. But this situation will continue until we track down the exact problem.

Update: New Instrument Proposal Funded by NSF (09/27/2019)

I'm pleased to announce that after a few months' research and negotiation, we have made our final decision to purchase two Bruker NMR spectrometers with this NSF instrumentation award. The package includes a Bruker 500 MHz and a 400 MHz spectrometer. The 500 MHz spectrometer will be equipped with a nitrogen cooled cryoprobe and a backup SmartProbe while the 400 MHz instrument will be equipped with a room-temperature SmartProbe. The delivery and installation will likely occur in February or March next year. Both instruments will be housed in PSBN 3608 next to the existing Varian 500 MHz spectrometer. The old Varian 400 MHz magnet will be decommissioned and removed during new instrument installation.

Earlier (06/24/19): I'm excited to share with you the news that our proposal to acquire a new state-of-the-art, 500 MHz NMR spectrometer equipped with a cryoprobe has been awarded by NSF through its highly competitive Major Research Instrumentation (MRI) program. This has been a multi-year effort with match-funding support from UCSB Office of Research, to acquire new solution NMR capabilities, improve instrument accessibility, and mitigate the danger of diminishing vendor support for existing instruments. This success cannot be attained without the hard ground-breaking research work and outstanding progress from many user groups across campus and our commitment to diversity, undergrad and graduate education, community outreach and support of regional industrial partners.

The cryoprobe will benefit all users, especially for X-nucleus detection by cutting data collection time by 10 folds. Proton sensitivity will also get a huge boost compared to existing broadband probes, allowing high-quality 2D NMR on the same probe. Additionally, with a separate room-temperature probe we will gain the new ability to pulse 1H/19F simultaneously, allowing observing one nucleus while decoupling the other or conducting 2D 1H-19F NMR experiments. Data quality, automation and ease of use will improve across the board.

We will immediately start the procurement process. The expected delivery and installation date is towards the end of this year or early next year. Once the new instrument is in place, current severe congestion on existing instruments will ease substantially, and an array of new experiments will open the door to exploring new opportunities in ongoing and proposed projects.

Extensive efforts in putting together this proposal were led by the NMR Facility (Dr. Hongjun Zhou) and Prof. Liming Zhang (PI). We thank additional support in contributing research and activity materials from other user groups led by Professors Trevor Hayton (co-PI), Bruce Lipshutz (co-PI), Javier Read de Alaniz (co-PI), Craig Hawker, Armen Zakarian, Alison Butler, Mahdi Abu-Omar, Gabriel Menard, and Gui Bazan. Additional support was provided by undergrad education led by Dr. Kalju Kahn and Dr. Morgan Gainer, and chemistry outreach programs led by Dr. Darby Feldwinn. We also thank regional user support from Dr. Raeanne Napoleon on behalf of SBCC Chemistry Department, and industrial users Next Energy Technolgies, Inc., Apeel Sciences, and Spero Energy, Inc.

Congratulations to all!

-- Hongjun Zhou, Director, NMR Facility, Chem and Biochem, UCSB

Sample Spilled on NMR400. System Down Until Tomorrow (09/23/2019)

Update (09/25/19): The residual peak appears much smaller. The probe has been re-shimmed. Make sure to enter init1h to load the new shim map and default shims.

While taking the sample out of the upper barrel, make sure to pull it STRAIGHT UP then out. It is important to keep focus and look at the position of the glass tube relative to the barrel. There is more danger involved when standing on the floor, not on the ladder, to take out the sample.

Update (09/24/19): A resonance peak is still visible after 24 hours of drying and blowing air following washing with a solvent. The probe has been re-washed. The instrument will remain down until the residual signal is gone, hopefully sometime tomorrow.

Earlier: A sample tube was broken at the top of the upper barrel. Some sample was spilled into the RF detection area. The probe will be washed, dried overnight. Most likely it'll be ready for use tomorrow.

When replacing a broken "idle"/dummy sample normally sitting in the probe, please use an empty tube to minimize the chance of sample spill.

Power Outage Over. All Instruments Up Running (09/15/2019)

Power has returned to campus. All instruments have been turned back on and are up running as of 1:30PM Sunday.

Lock Problem on NMR400 (09/12/2019)

Update (09/12/19): Our original board was put back in while we talk to Agilent and trace down the problem. The lock problem with the original board is also envolving. There appears to be occasional sudden jump in lock level. If lock isn't engaged after shimming, try another autolock. Then, you may adjust the gain and power in the lock panel.

Update (09/12/19): After an overnight, another check shows the lock level oscillates drastically with a ~ 10 sec cycle. This wasn't happening right after installation. Further test is being made. If the problem persists, we'll have to put back the original board again and look for a solution. Until then, you may use autolock and autoshim as usual.

Earlier (09/11/19): A different lock transceiver we just received fixed the lock issue on NMR400b. Autolocking should be more stable and robust now. However, the new lock transceiver appears to require much less power/gain to achieve the same lock level as the original board. Please pay attention to lock level after autolocking. If it exceeds or at 100%, please go to the Lock panel and drop the gain or power by a few units until the lock level is 70-90%.

Cooling, Heating in NMR Rooms (09/12/2019)

The Facility has done extensive work in the NMR rooms in the past week to fix long-standing issues with cooling and heating which is important for NMR. Cooling, repeated water dripping from the ceiling and flooding near the air condtioners have been fixed. Due to ongoing work with the building boilers, the NMR rooms will remain very cold (~16-19C) for another week until heating is turned back on.

All Instruments Down From 9PM Sat Till 2PM Sun (09/10/2019)

As noted in the campus wide notice, a planned power outage will take place from ~10PM Saturday Sep 14 to early afternoon Sunday, Sep 15. Although emergency power is available, not all parts of the instrument needs are guaranteed to be in place, especially compressed air supply. For instrument safety, we'll power down all instruments from ~9PM Sat till ~2PM Sunday.

Please plan ahead with your experiments and check the notice area for updates and changes.

NMR400 Lock Transceiver Changed (09/09/2019)

Update: Unfortunately, the newly received used board has a broken connector that rendered it useless. We are in touch with Agilent to get this resolved as soon as we can. The original board was put back in again. Please follow the instruction dated 08/29.

Earlier:A new lock transceiver board has finally made it way here. It'll be tested shortly. Chcek the latest status here later.

NMR400 Lock Transceiver Changed (08/29/2019)

Agilent has shipped us a new lock transceiver board from overseas but it has taken much longer time than expected to get here. The first replacement was defective as noted earlier. After waiting a week, I have requested the old board back. This board was put back in while we continue to wait or look for a replacement.

The existing lock problem with the original board is still there. You should use autolock and autoshim, redo autolock after gradient shimming if the lock doesn't come back by itself.

For some solvents, manually adjusting the lock through Lock Scan is needed. To manually adjust lock, go to Start->Lock, click Scan, then turn lock OFF to adjust Z0 with left or right button click inside Z0 button until the flat lines (red and blue) are observed. You may temporarily increase lock power to help locate the lock curve, but make sure to drop the lock power to 10-15 units below gain value before exiting lock panel. Once the "step-function" flat signals are located, check the Lock checkbox. Now it should show lock "Regulated".

NMR500 Returns to Normal Operation After Shim Stack Replacement (08/20/2019)

Great news: A used shim stack acquired from a 3rd party replaced the broken one. This fixed the broken Z4 in the old shim stack. Luckily, the new shim values are close to the old ones leading to a quick reshim with the new shim stack to achieve optimal values.

All operations on NMR500 return to normal, including restriction of 20 mins max block reservation between 9AM-4PM during weekdays. Now you can use autolock and gradient autoshim as usual. As always, enter init1h at the beginning of your session to load updated parameters.

The shim stack, sitting in the central bottom half inside the magnet, provides the shimming currents. Apparently, water in the compressed air line shorted one of the shims as reported earlier. This was the most serious damage in years, and is more so given the expense and difficulty of finding a replacement part.

Update: New Lock Transceiver for 400 to Arrive Next Week (08/20/2019)

Due to dwindling part supply, Agilent cannot locate the part in the US. A new replacement lock transceiver for NMR400 will be shipped from an Asian Facility and hopefully arrive next week. An Agilent engineer will then install it. With luck, that will fix the lock problem.

Shim Stack Replacement on NMR500 (08/19/2019)

The broken shim stack will be replaced on NMR500 these few days with a refurbished part. This may take unknown number of hours mostly due to the work involved to get the shims right after replacement. Please be advised the schedule may change on short notice.

New Lock Problem on NMR400. New Board Likely Faulty (08/16/2019)

The lock worked well for some hours yesterday after the transceiver board was replaced. But this morning it was found that lock jumps between on and off rapidly. It appears the new board is faulty. Agilent has been informed of the issue. The engineer will return and fix it as soon as posisble.

Lock and shim as usual, but data must be collected with lock OFF. As long as lock is OFF, brief <20-30 mins experiments should work fine. Please follow this instruction to keep lock off.

Follow all normal steps, including init1h, lock, shim, autune, etc
Before data acquisition, make sure to turn lock OFF: uncheck Lock in Lock panel. Also, enter alock=n to turn off autolock
Because lock has to be OFF, long experiments more than 20-30 mins are not recommended.

Issues on NMR400B Have Been Fxed (08/15/2019)

Lock instability on NMR400B has been fixed by replacing the broken lock transceiver board. Much lower lock power and gain are needed now than before for the same lock level. Normally, lock power should be limited to ~15 units lower than gain. A separate issue involving vibration sideband peaks has also been fixed. Please enter init1h to load new shims which have changed substantially from previous values.

NMR400B Will Be Interrupted on Thursday for Repair (08/14/2019)

An Agilent engineer will be here Thursday afternoon to replace a faulty part that will likely fix the lock issue. If things go well, the interruption will be an hour or so. All blocked time slots will be relieved as soon as the timing and situation becomes clear, but expect possible interruption to any booked time in the afternoon.

All Systems Down Tue Morning for Air Safety Work (08/12/2019)

Update (08/13/19): Utility work has been completed. All instruments are back to operation.

Earlier (08/12/19): Tomorrow, Tuesday morning, from 8 to ~12, campus Facility personnel will install water trapping safety features along all compressed air lines in the NMR room. All instruments will be shut down until the work is finished. The safety features have to be put in place to minimize the chances of water leaking into compressed air which has done serious damages to the instruments in the past.

Update: NMR500 Still Requires Manual Shimming (08/1/2019)

We are still looking for a replacement shim stack. This has been the most difficult part to replace in years. After talk with multiple vendors, there is still no concrete lead at this point. See notice posted around 06/14/2019 for events leading to this situation.

Manual shimming Z1 and Z2 is required on NMR500 until the shim stack is replaced. Data quality is acceptable for most purposes after shimming. Please make sure the sample volume is ~ 700uL. The volume is especially important due to the broken Z4.

Gradient Shimming on Strong H1 Signal (07/26/2019)

In cases where the sample is free of deuterons, locking and shimming on H2 signal are not possible. The experiment must be run UNLOCKED. It is critical to turn lock OFF in the lock panel and also make sure autolock doesn't kick in at the start of the experiment by entering alock='n'.

To retain decent lineshape, you may use an identical but deuterated solvent to shim with H2 shimming before loading the non-deuterated sample. But, ideally with a strong H1 signal, you may shim on the H1 signal by following the steps outlined here. When reasonably strong H2 signal is present, don't use H1 gradient shimming.

Compressed Air Leak Near 600 (07/18/2019)

Update (07/19/19): A leaking air filter has been changed. But a faulty pressure meter next to it started to leak air as well. A replacement has been ordered but can only be installed early next week. The instrument works fine.

Earlier: There is a leak in the compresesd air line near the 600 instrument. The hissing noise gets louder when the sample is inserted. We have called campus Facility. A faulty filter will be replaced, hopefully in the next few days, to fix the problem.

Compressed Air Gone. Instruments Down. (07/16/2019)

Update (4:40PM): Air is coming back on. Okay to use instruments.

Earlier: Building compressed air is gone. Don't use the instruments until air is back on. You can check the air pressure from the gauge on the wall. Normal pressure should be 90-100 PSI.

Please leave any sample stuck inside the magnet in a safe place for users to pick up later.

Instrument Reservation Issues (07/15/2019)

Over the summer period, our already busy instrument schedules often get busier with more visiting scholars and research interns joining various summer programs. It appears that we still find a good number of occasions, some reported by users, when an instrument is booked but not used, or used very late by the user while others have to wait for access.

Again, please do not overbook more than what you need, show up on time, and cancel all unused slots as soon as possible.

Any booking that a user fails to show up to use after 10 mins past the booked time is open for other users on a first-come-first-served basis. However, please do take into account unexpected situations and emergencies and yield to others' booked time if warranted.

New 500 MHz Instrument Proposal Funded by NSF (06/24/2019)

I'm excited to share with you the news that our proposal to acquire a new state-of-the-art, 500 MHz NMR spectrometer equipped with a cryoprobe has been awarded by NSF through its highly competitive Major Research Instrumentation (MRI) program. This has been a multi-year effort with match-funding support from UCSB Office of Research, to acquire new solution NMR capabilities, improve instrument accessibility, and mitigate the danger of diminishing vendor support for existing instruments. This success cannot be attained without the hard ground-breaking research work and outstanding progress from many user groups across campus and our commitment to diversity, undergrad and graduate education, community outreach and support of regional industrial partners.

The cryoprobe will benefit all users, especially for X-nucleus detection by cutting data collection time by 10 folds. Proton sensitivity will also get a huge boost compared to existing broadband probes, allowing high-quality 2D NMR on the same probe. Additionally, with a separate room-temperature probe we will gain the new ability to pulse 1H/19F simultaneously, allowing observing one nucleus while decoupling the other or conducting 2D 1H-19F NMR experiments. Data quality, automation and ease of use will improve across the board.

We will immediately start the procurement process. The expected delivery and installation date is towards the end of this year or early next year. Once the new instrument is in place, current severe congestion on existing instruments will ease substantially, and an array of new experiments will open the door to exploring new opportunities in ongoing and proposed projects.

Extensive efforts in putting together this proposal were led by the NMR Facility (Dr. Hongjun Zhou) and Prof. Liming Zhang (PI). We thank additional support in contributing research and activity materials from other user groups led by Professors Trevor Hayton (co-PI), Bruce Lipshutz (co-PI), Javier Read de Alaniz (co-PI), Craig Hawker, Armen Zakarian, Alison Butler, Mahdi Abu-Omar, Gabriel Menard, and Gui Bazan. Additional support was provided by undegrad education led by Dr. Kalju Kahn and Dr. Morgan Gainer, and chemistry outreach programs led by Dr. Darby Feldwinn. We also thank regional user support from Dr. Raeanne Napoleon on behalf of SBCC Chemistry Department, and industrial users Next Energy Technolgies, Inc., Apeel Sciences, and Spero Energy, Inc.

Congratulations to all!

-- Hongjun Zhou, Director, NMR Facility, Chem and Biochem, UCSB

NMR500 Still Requires Manual Shimming (06/21/2019)

The 500 still requires manual shimming as we look for a replacement part. Unfortunately, Agilent Technologies has not located a part yet. We are exploring other options. See notes below for steps of manual shimming Z1 & Z2.

Latest Instrument Status (06/14/2019)

Update (11:00AM, 06/14/19): There is some humming noise coming from an inline air filter on the wall that gets louder when ejecting/inserting a sample. We have requested a check by Facility. The instrument is fine.

Separately, some personnel issues at Facility have caused an unpredictable delay to planned work on the air supply line.

Update (3:00PM, 06/11/19): Unfortunately planned work with the air supply lines didn't happen today. We are rescheduling the work. New dates will be announced once they are set.

Update (8:30AM, 06/10/19): Water trapping saftety loops will be installed in the compressed air supply lines in both NMR rooms. NMR500 will be offline on Tuesday (06/11) morning; 600 and 400 will be offline on Wed (06/12) morning. The instruments will be open as soon as the work is done.

Update (3:00PM, 06/07/19): All instruments are open now. 500 still requires manual shimming (after init1h) due to damaged Z4 shim. See instruction posted below on 05/31/19 for Z1 and Z2 shimming method.

Update (11:30AM, 06/07/19): New air filters were installed this morning. The lines were flushed. The 400 and 600 are now back on with building compressed air. The 500 may be up running later, but it is uncertain.

Next week more safety hardware will be installed in the air supply lines. We expect interruptions to instrument access of two mornings.

Update (2:30PM, 06/06/19): We have received new air filters. They will be installed early tomorrow morning. Hopefully we'll have all instruments on building compressed air by the end of this Friday.

Update (8:30AM, 06/06/19): NMR500 has been taken off the reservation page until we have the compressed air lines fixed and the instrument tested. The damaged shim stack will be fixed by an on-site engineer visit, hopefully soon.

Update (4:00PM, 06/05/19): A new gas cylinder will be hooked up around 5PM which should allow the 400 to run for up to 6 hours. If the sample doesn't eject, insert the sample, don't leave gas blowing, and come back to pick up the sample tomorrow. The 600 will run normally. NMR500 will remain off until the compressed air filters are replaced and the instrument is tested in the coming days.

Update (10AM, 06/05/19): The broken building compressor has been located and switched off. However, the flooded filters on several air lines have to be replaced, possibly tomorrow once order comes in. For now, the 600 is made open using building air. The 400 is working with nitrogen gas but expect disruptions when gas runs out and has to be replaced. The 500 will stay down for most of the day.

If things go well, we may have all instruments running by end of the week. But we must make sure air is clean enough and the probes and shim stacks where air flows through are safe.

Update (8AM, 06/05/19): A full gas cylinder is used up likely within 6 hours. We'll conitune to push to have the gas problem fixed at the root ASAP. For now, the temporary solution with nitrogen gas will continue, but unfortunately this will greatly limit access. Please read all updates and check the schedule before coming over to use the instruments.

NMR500 still requires manual shimming if it is up running. An engineer visit is being scheduled.

Update (5PM, 06/04/19): A nitrogen gas cylinder has been connected to the 400 MHz instrument. Please use caution in the instrument area and keep the cylinder against the wall, away from the magnet. The gas may not last more than a day. We'll have to see. Nitrogen gas use is kept to bare minimal, for cooling the probe coil and shims. DO NOT regulate VT and change the temperature. DO NOT run long experiments for more than an hour or two at a time. You must make sure eject air is shut off before walking away. If the sample doesn't eject, do not use the instrument.

There is no answer yet as to the problem source of the building compressed air. Tomorrow we'll try to connect the 600 MHz instrument to a cylinder as well. Given the unknown circumstances and time to clean up the gas line, please postpone any overnight or experiment longer than two hours.

Earlier: Emergency: All Systems Shut Down Immediately (06/04/2019)
The building air line has been flooded and contaminated with large amount of water and vapor and possibly some oil. All instruments have been shut down immediately until further notice. The water present in compressed air line is likely what caused the shim (shorting) problem on the 500 earlier.

How long the instruments will be down is not clear at this point. The root cause of the water/oil contamination has to be identified and fixed. Then the compressed air lines have to be flushed to remove the moisture and oil. The building manager (Cabe) is working on this with high priority. In the meantime we are working on temporary solutions.

Hardware Problem on NMR500 Requires Manual Shimming (05/31/2019)

NOTE: Due to these unexpected changes below, we'll temporarily relieve the block reservation restriction on the 500. Now you may reserve up to one-hour block each time on the 500 from 9:00AM to 9:00PM during any weekday until further notice.

Update, 06/03/19: Please check the schedule before work even though you have reserved time. Due to ongoing diagnostic work, sporadic instrument shutdown is expected. Once the faulty part is confirmed, we'll send it for repair or acquire a new replacement board.

Earlier, 05/31/19: Z4 shimming hardware on the 500 appears to have broken in the last day or two. The shimming board has to be replaced which may take a week or two. The shims have been adjusted with a large change in Z6 to partly compensate the effect from missing Z4 but the result isn't ideal. Lines are broader, but for quick check of 1H spectrum, it should be Ok. 13C is less impacted. Make sure your sample volume is close to 700 uL in order to have good results starting with the default shims loaded with init1h.

Manual Shimming

Auto-locking (Find Z0) works fine. However, auto-shimming failed to work well with other shims; manual shimming Z1 and Z2 is required.

To manually shim, first adjust the lock level to ~ 60-70%. Go to Start->Lock panel to adjust lock power and gain. Make sure not to saturate the lock with too much power. Typically power should be lower than gain by 10-20 units. If the lock is jumpy and swings a lot, it is a sign the lock is saturated with too much power.

To shim, go to Start->Shim panel, left or right mouse button click inside Z1 (and Z2 later) to adjust the shim toward where the lock level is higher. Middle mouse button click inside a shim to change the stepsize of each click. You may start with a stepzie of 100, then drop it down to 10 as the shim approaches an ideal value. After Z1 is adjusted, move on to adjust Z2 and then back to Z1, iteratively until the lock level is the highest at set power and gain. If the lock level reaches >90%, reduce the gain or power to drop the level down to ~70-80% then go back to adjust Z1 and Z2 again.

Once shimmed, data quality for 13C should be fairly good.

Large Changes in Shims on NMR500 (05/13/2019)

Large changes in X,Y shims have been made to obtain optimal lineshape. Please always enter init1h to load up-to-date default parameters at the start of your session.

Promptly Cancel Unused or Leftover Reservation (05/02/2019)

As all instruments are getting fully booked, please keep track of your reservations and cancel leftover booking or slots not going to be used as soon as possible so that others can use the instrument.

If a user doesn't show up to use the reserved time after 5-10 mins passing the start of the reserved time, other users may use the booked slots until the user comes. I may cancel any open, unused bookings as well when a user fails to come to use the instrument. But please take into consideration unexpected delays when using others' booked time slots.

Lock Problem on NMR400 (04/29/2019)

There appears to be a problem with locking on NMR400. This will be checked very soon, tomorrow morning at the latest.

Double Check Reservation Time (04/26/2019)

It was noted that occasionally a user might have booked time on the wrong day, especially involving overnight and early morning hours, leaving open slots when the experiment is running. If this happens, the next user who has reserved this time may have to stop the running experiment.

For all reservations, please check the actual date and slots after reserving time online. Booking instruction can be found here.

Campus-wide Network Disruption (04/24/2019)

Today in the afternoon there have been repeated campus-wide network disruptions. Chemistry buidling local network and all NMR instruments remain functional. If you need to reserve time or view reservations, you may try a computer located in the chemistry building including all NMR workstations. If the reservation page isn't accessible, please use the instruments on a first-come-first-served basis if the instrumnet hasn't been booked.

Lost keys Near NMR500 (04/24/2019)

A user left a set of keys near the 500. Please contact me if you have taken them. Thanks.

NMR600 Receiver Fixed and Replaced (04/16/2019)

The receiver on the 600 has been replaced with an exchange board. The above-normal amount of quadrature images seen earlier with nt=1 has disappeared. Regardless of its presence, for all NMR experiments, multiple of 4 or 8 scans (that is nt=4*n or 8*n where n is an integer) should be used. For 1D experiment, the setting is the default. For 2D NMR, an additional need for proper multiple scans has to do with full phase cycling for artifact removal or coherence selection. The proper number depends on the experiment. If you have any doubt, please ask.

NMR500 Probe Replaced (04/11/2019)

Luckily we have located and acquired a used broadband probe of the same model to replace the broken one on the 500. The probe has been tested and shimmed. It gives roughly the same specs as the old one. Please enter init1h at the start of your session to load new hardware parameters. All procedures remain the same.

Note that spin remains disabled until further notice. If you encounter an error after starting the experiment regarding being unable to spin, go to Spin/Temp panel, set spin rate to zero, then click Spin Regulation OFF.

Again, please use care to measure the depth of the tube before inserting it into the probe and also minimize all other dangers that may damage the probe. Replacement parts have become hard to find and repair is costly.

NMR500 Probe Problem. Spinning Turned Off (03/22/2019)

The glass insert in the NMR500 probe is broken. This is the glass lining with a diameter slightly larger than the 5mm tube that shields other parts of the probe from the sample tube area. Once we get back the repair cost estimate, the probe will be sent out to have the insert replaced.

Before inserting a tube into the probe, make sure the depth of the NMR tube is measured with the gauge so that it is not deeper than the maximum length specified. Any longer than the maximum depth may cause the tube to hit the bottom of the glass lining in the probe.

Because of this, spinning on the 500 has been disabled to minimize further damage. A large change in shims was found and corrected. Please always enter init1h at the start of the session to load the newest settings.

NMR600 Receiver Replaced (03/22/2019)

The receiver on the 600 was sent for repair. It came back and was put back in. Quadrature images are much smaller now but are still larger than normally expected. This shouldn't affect data quality if the scans are set to multiple of 4's. We'll be in touch with Agilent to have it completely fixed.

Spurious Peaks on NMR600 (03/06/2019)

It appears and was confirmed that there are some spurious quadrature image peaks and a center glitch peak on NMR600. A spare receiver has been put in. One of the receivers will be sent out for repair soon once the issue is confirmed. The lock phase has changed and has been updated. Please always enter init1h at the start of your session to load updated parameters.

Please always collect data with multiple of 4 or 8 scans. This is the default setting with parameter bs=4. The spurious peaks are much weaker, barely noticable with 4n scans.

Additionally, due to heavy instrument use, starting on Monday, March 11, long overnight experiments on the 400 will start from 9PM instead of 7PM till 9AM next day. We'll adjust the restriction as needed once more instrument time is available.

Promptly Cancel Unused or Leftover Reservation (03/05/2019)

In the past few weeks we've seen extremely busy reservations almost at full capacity across all instruments, especially the 400 and 500. It is noted some bookings aren't used fully or a user fails to show up to use the instrument. While there are always unexpected situations, please promptly cancel reservations that are not going to be used and cancel any leftover booking slots as soon as possible.

If a user doesn't show up to use the reserved time after 5-10 mins passing the start of the reserved time, other users may use the booked slots until the user comes. I may cancel any open, unused bookings as well when a user fails to come to use the instrument. But please take into consideration unexpected delays when using others' booked time slots.

We have submitted a NSF instrument grant application for a new 500 MHz instrument early this year. If it is approved in the summer, the situation will ease substantially. However, a new instrument will only be available in about one year from now in our best estimate.

Quantitative C13 NMR on NMR500 (03/02/2019)

To do quantitative C13 NMR on NMR500, enter setexp('qC13') at the command line. This script will load the default setup. A similar script will also be available on the 400 in the coming week. The T1 relaxation times of small molecules vary widely from a few secs to 30-40 secs. T1 limits the recycle delay for accurate integrals. Degassing the sample under oxygen-free environment significantly prolongs the T1 vlaues. If possible, for quantitative C13 NMR (and similarly other quantitative NMR), do not degas the sample to remove oxygen unless that is really necessary for this particular NMR experiment. Oxygen with its weak paramagnetism helps relax the spins. See this note and test by the NMR facility at the University of Ottawa. Adding O2 or other paramagnetic doping agents helps shorten T1. For polymers or macromolecules, this is less a concern due to their much reduced T1's. I'll post more details on quantitative C13 NMR and a few F19 related notes soon.

Quartz NMR Tubes for B11 NMR Available in Storeroom (02/22/2019)

The chemistry storeroom now has 5 mm quartz NMR tubes for cleaner B11 NMR. It's Wilmad brand 528-PP-7QTZ. See message below for other details on B11 NMR.

SNR and Uncertainty Estimate in vnmrJ and Mnova (02/17/29)

To estimate signal-to-noise ratio (SNR) of the peaks, please follow this instruction. It is helpful for uncertainty estimate if you are quantifying the measurements.

NMR Tubes for B11 NMR, Broad Background Signal Removal (02/08/2019)

If you need a cleaner and better-looking B11 spectrum, please order a 5 mm quartz NMR tube from Wilmad, either 507-PP-7QTZ or 528-PP-7QTZ. These tubes don't give a broad background B11 signal from the normal Pyrex tube.

Additionally, please follow this instruction to remove the broad background during processing.

Power Outage Possible from Weekend Rainstorm (02/01/2019)

Heavy rain and strong wind are expected over the weekend. Please see earlier notice below for precautions after a power outage.

NMR500 Workstation Crashed, Works Now (01/28/2019)

The 500 computer crashed late last night with file system errors. The computer has been fixed now. There may be a small amount of file damage. If you encounter corrupted old files and need them, please contact me. The files can be retrieved from backup copies.

Power Outage Likely from Series of storms (01/11/2019)

A series of rainstorms are coming to town in the next two weeks starting later tonight which are likely to cause power outages. As in the past, the outage will likely lead to loss of building compressed air and in turn loss of eject air. If you hear a sudden change of air hissing noise when ejecting a sample or the sample fails to come out, re-insert the sample. If the air compressor is down during the weekdays, you may contact Cabe directly (or call campus Physical Facilities) to have it turned back on. It may take several hours. DO NOT use the instrument after the air loss. For any emergency, please follow the instruction posted on the magnet.

Once regular power is lost, you should finish off your NMR work as soon as possible. The UPS backup power only lasts ~10 mins then the console will shut down. If the computer server is down due to a power glitch, it may prevent login at the NMR workstation.

Back to Normal Reservation Rules (01/07/2019)

Welcome back! Reservation rules have been reverted back to the regular ones.

Longer Block Reservation During Holidays (12/28/2018)

To ease use and allow longer daytime reservation over the holidays, the 400 and 600 are now unrestricted for all reservations. Block time reservation on 500 is eased to 2 hours max during 9AM-4PM Monday-Friday, unresticted over other times. As usual, please don't waste instrument access time. We'll have to revert back to prior rules once more users are back to work, likely later next week.

Before that, enjoy the freedom and the holidays!

Instrument Reservation and Waste (12/06/2018)

It has been noted that a good number of reservations are made but the users don't show up to use them or leftover unused time slots aren't canceled after the work is done. This is more serious on the new heavily used 400 MHz instrument.

While it is understandable there is an uncertain window of time when a sample or the user may be ready, please do not repeatedly reserve time slots without showing up to use the instruments. All wasted instrument time will be charged if noted. Other users may use discretion and are free to use the instrument if the reservation user fails to show up within 5-10 mins for any 10-30 mins reservation.

Thank you for your cooperation.

Mnova Software Update and License Renewal (12/03/2018)

We have just updated our site licenses to cover any software update in the next year up to release date 12/03/2019. Along with the change, the license server has been moved to a more permanet computer. All older versions of Mnova should continue to work under the new licenses. Howerver, regardless whether you update the software or not, you must download and re-activate (install) the licenses contained in this .zip file. The existsing ones will expire in a few days.

Please do the sofware license activation from a UCSB network. Any computer connected from outside campus may be blocked from activation. Once activated, the software remains activated for 90 days without required network connection. See this page for additional instruction.

Mnova License Expiration Warning (11/30/2018)

If you see a warnining about pending Mnova license expiration, ignore it for now. It has to do with a temporary solution for the license server. We'll get it resolved very soon.

Compressed Air Gone in PSBN. Instruments Down. (11/15/2018)

Update: Compressed air is back. All instrumnets are open for use.

Compressed air in PSBN is gone. Campus Physical Facility has been contacted. But it may take up to a few hours to get the compressor at the roof top checked and turned back on. Do not use the instruments until further notice.

NMR Tubes for Boron NMR (11/15/2018)

If you need a cleaner and better-looking B11 spectrum, please order a quartz NMR tube from Wilmad, either 507-PP-7QTZ or 528-PP-7QTZ. These tubes don't give a broad background B11 signal from the normal Pyrex tube.

Further information on removing or reducing background signal in B11 and Si29 NMR can be found here.

NMR500 Down. Sample Tube Broke in Probe (10/15/2018)

Update, 10/16/2018: It appears all residual signals are disappearing fast. The instrument will be open for use after ~4PM today.
Update, 10/16/2018: There is a broad residual peak in the spectrum collected with an empty probe, indicating some sample spill. The probe has been washed, broken glass removed. Now it is the being dried. The drying process may take 10-24 hours to remove all residual peaks including those from the cleaning solvent. DO NOT use the instrument until further notice.

Note that if a tube breaks inside the probe, please follow the procedure posted on the side of the magnet for steps and contact information. Most importantly, you must post a clearly written notice to block any other users from continuing to use the instrument.

Earlier: A sample tube broke inside the probe late Monday night. The probe will be checked in the morning. If the sample hasn't spilled, it should be up running in the morning. Otherwise, the spill has to be washed off and dry over Tuesday till Wednesday morning.

Spin Control on NMR500 (10/03/2018)

Note that correct spin operation involves automatic turning off sample spinning during gradient shimming and kickstarting spinning at the beginnng of the experiment. Please do NOT check-mark "Control Spin from this panel only" under Spin/Temp panel. Doing so prevents automatic spin control. If one user makes the wrong setting, this setting remains for all subsequent users.

If sample spinning doesn't kickstart when a typical 1D experiment starts after gradient shimming, go to Spin/Temp panel, make sure the Control Spin from this panel only box is NOT checked and the spin rate is 20, then click Regulate Spin. "Ignore spinner error" box should be checked.

Note sample spinnng is NOT engaged on NMR400 and NMR600.

See images below for correct setting on NMR500.

Spin under Start panel should be at 20 and checked.

Steps to Correct Mnova License Failure (09/12/2018)

Update, 09/27/2018: Make sure you only use Mnova version 12.0.1 or older. Newer versons of the software are NOT supported.

Earlier, 09/12/2018: After talking to the software vendor, we have a temporary solution for the loss of the license server. There is no need to update your license file unless you see the message that indicates a failure to connect to the server. If the error is displayed, follow the instruction at the top of this page.

Note the license above is the main NMR plugin that covers essentially what you need for NMR. If you have a need for other plugins and modules, please let me know.

Please note some users reported an error message about failing to connect to the license server, particularly when using the department wireless network. ChemBiochemSecure works, but ChemBIochemGadget doesn't. Please try another type of network or login with your computer, such as wired or network at home if you have trouble with connecting to the server. Once a connection is made, the license is good for 90 days.

Mnova Software License Server Down (09/10/2018)

Some users have experienced license errors in the last few days. This has been noted and affects everyone. Unfortunately, there is no immediate fix yet. Please use other processing tools for the time being. We'll try to get the issue resolved as soon as possible.

Separately, building compressed air was gone since late Friday. It was back as of 10AM this morning. Without air, the sample won't eject. DO NOT insert another sample. If this happens again and I'm not around, please contact building manager Cabe Fletcher. If he isn't around, contact campus Facility Services directly.

Avoid Simultaneous Overnight Booking on All 3 Instruments Before Midnight (09/06/2018)

All three instruments are still very busy. Please don't book any instrument by the same user during the same time period. Additionally, please avoid simultaneous overnight booking on all three instruments before midnight to allow other users to access at least one instrument. If you have questions, please let me know.

NMR400b Down from Broken Tube Inside Magnet (08/25/2018)

Update, Sunday 08/26/18: The probe is clean, mostly free of residual peaks after overnight air flusing and drying. It's open for use after 2PM today. Plesae focus and use care when ejecting or inserting a sample. Unless a sample is taken out, always assume there is a sample inside the probe before inserting another one.

Earlier, Saturday: It is disappointing to see this happens again. A user inserted another tube with sample inside on top of an existing tube inside the magnet. The top one broke and contaminated the probe. The probe has been washed and will dry over many hours to remove the bulk washing solvent and contaminants. Once it is clean enough, it'll be open for use.

Promptly Cancel Leftover Reservation (08/16/2018)

Given the very busy schedules of the instruments, everyone please reserve instrument time conservatively, come to use the instrument on time, and cancel unused time promptly to allow others to use the instrument in time. We continue to see significant reserved time left unused or a user not showing up to use the booked instrument.

NMR600 Up Running (07/30/2018)

Update, 07/30/18: Alex has just fixed the original 600 receiver by replacing a broken transistor on the board. The 600 is now fully functional to spec; the quad image issue below has been resolved.

Earlier: NMR600 is up running again. It turned out the receiver is the source of the problem which shorted the power supply circuit. Kowtows to Dr. Alexander Mikhailovsky, the Optical lab manager, who helped diagnose and trace down the problem linked to the power supply.

A spare receiver from the old 400 was put in. When collecting data, the scans should be done with multiple of 4 scans. This is typically the default setting. Quad images are visible when scans are not multiples of 4, but the spectra are acceptable with scans of multiple of 4. We'll have this problem fixed very soon.

NMR600 Malfunctions, Down (07/15/2018)

Update, 07/27/18: Significant progress has been made in fixing the instrument. We may have the instrument up running again early next week. Stay tuned.

Update, 07/25/18: Still waiting for a quote from Agilent after they located a spare part. In the mean time and separately, several new modules inside the power supply have been ordered. I'm hoping that replacing the modules may fix the power supply.

With luck, fixing the issue is still a week or two away.

Update, 07/20/18: Due to scarcity of spare parts, we are still waiting for Agilents' words on a replacement part & quote. In the meantime, we are also exploring other options. Better clarity will be in early next week.

Thank you for your patience. Please use the other two instruments very gently so that we don't add more disruptions to the existing one.

Update, 07/17/18: It appears the power supply module has a problem with one of its output. We'll get a quote for repair or replacement. Either way, this process will take days, a week or two, easily. The 600 has been taken off the reservation list for now.

Update, 07/17/18: The 600 is still down. It looks like we may have a longer period of downtime until the problem is found and fixed. Please prepare your work accordingly.

It happened suddenly today that NMR600 malfunctions and the computer is unable to communicate with the console. Rebooting the computer and resetting the console failed to get it to work. At this point, it is possible this may be a software issue, but it may also be due to a serious hardware problem in the console. Hopefully the 600 won't be down for more than a day or two. For now, the 600 is down until further notice.

NMR600 Software Update on Wed, Jul 11 (07/09/2018)

Update, 07/11/18: We'll have to reschedule another day for the software update due to complications of the update path.

We'll update the system and NMR software on NMR600 on Wednesday, Jul 11. The instrument will be down from 9AM to 4PM or until we complete the work. If the update is successful, we'll move to update the software on NMR500 as well.

Computer Login Problem Fixed (07/04/2018)

Earlier problems loggin onto all workstations have been fixed. All instruments are open for use.

Possible Power Outage Due to Heat Wave (07/03/2018)

Over the next few days, especially Friday to Sunday, an expected temperature rise will stress the power supply in the area, possibly leading to power outage. The building air compressor will go off once regular power is cut. If a sample doesn't get ejected, don't drop another sample in there. Take a look of air pressure from the meter on the wall in the air supply line. Normally reading is ~100-110PSI. It may take ~20 mins for the air pressure to come down to zero reading and ~20 mins to refill the line.

If a power outage occurs, please finish your experiment ASAP and eject the sample. Please wait until regular power comes back on before conducting additional work.

For emergency, please call the number posted on the magnet.

NMR400B Software Upgrade Complete (06/21/2018)

Thanks to our IT, both the system software and VNMRJ have been updated to the latest compatible versions on the 400. We'll schedule a day's work in the coming weeks to upgrade the software on the other instruments.

The operation of the instrument has been tested fine. Firefox browser should work fine now with the NMR website and other sites. If you encounter any problem from this change, please let us know.

VNMRJ Software Update & Web Browser on NMR400B (06/13/2018)

After our department web server switched to secure connection, the old version of Firefox on NMR400b stopped working. To make this feature available and enhance system security, we'll upgrade the system software along with the NMR software VNMRJ. The date for this work is set for Jun 21, Thursday from 9AM-5PM. If more time is needed, we'll post a separate notice.

All data on the instruments won't be affected. The software at the user level has few changes. But please plan ahead for your experiments on NMR400b as needed.

Please Keep Workstation Areas Clean (06/04/2018)

All users should make efforts to properly clean and dispose of broken tubes and sample spills while doing NMR experiments. It is irresponsible to leave the broken glasses and sample spill in the area without proper cleanup as it was reported in the 400 area over the weekend. The broken glass and chemical spill pose a health risks to every user.

If the Idle/dummy sample is broken, please replace it with an empty tube. Don't use a tube with any sample inside for this purpose. If a tube is broken on top of or inside the magnet and some liquid is spilled, please report it immediately to the manager and also leave a handwritten note to prevent any user from using the instrument.

Cancel Unused, Leftover Reservation (05/025/2018)

We continue to see some instrument reservations where the users don't come to use them, or leftover time slots wasted after a user finishes work early than expected.

Again a reminder to all users: with the instruments having a packed schedule, it is important that everyone reserves only what you need, notes the reserved time, arrives on time, and cancels the reservation if you cannot make it. After you finish your experiments, immediately cancel the rest of reserved slots left so that others can use the instrument.

Notes and Updated Reservation Rules on NMR400b (05/03/2018)

Update: Effective immediately, the reservation rules on NMR400b have been updated to better manage the busy booking situation on the 400. A maximum of 60 consecutive mins are allowed for a single user on the 400 from 9:00AM to 7:00PM on all weekdays. Longer reservation will be blocked by the booking software during these hours. At present, there is no restriction on reservation by consecutive group members. We'll see how this goes and revise the rules as needed.

The rules for all instruments are listed here.

If you only need 1H spectrum, please choose the 600 or 500. For 13C, you may use the 500 or the 400. Please leave the 400 as much as possible for other nuclei, including 19F and X nuclei, when tuning is required. For 2D experiments, use the 600 for best 1H sensitivity.

Earlier: Recently, the 400 has been busy with daily long, consecutive reservations. This has caused concerns to other users, delaying their work. We'll consider updating the rules to reflect a more balanced use of the instruments by all users and groups.

In most cases, however, occasional, extended use of the instrument is well justified. If you have any concerns, please let me know. Usually I'll talk to the user and make sure there is a genuine need for the time and if it is possible to do some off the peak hours.

For all users, please try your best to do any long experiment(s) after the daytime hours, and try to avoid booking too much time consecutively for a few days.

Class use of NMR500 this week (04/11/2018)

Chembio class will use the 500 a few hours each day for a few days this week. Instrument access to others will be reduced but only for a few days.

Loss of Compressed Air (03/23/2018)

Update: Compresesd air is back. All instruments are open.
04/02/18: Compressed air is lost again. Do not use instruments until air is back.

Recently there have been a few instances of losing compressed air. If compressed air is lost, the sample won't eject. Please DO NOT insert any sample unless the sample inside is taken out. If the building air compressor is down, it takes about 10-20 mins for air to totally escape from the air lines. You may still hear air hissing but the pressure won't be enough to operate the instrument. Check the air gauges behind the computers for pressure reading. Normal pressure is ~100 PSI.

For the loss of compressed air, if I'm not available, please notify our building manager Cabe Fletcher or campus Facility (EX 8300) directly to have the compressor checked and turned back on.

Storm may disrupt power and compresesd air supply (03/20/2018)

Due to the expected strong rain storm, we may experience electric power disruption and loss of compressed air. All instruments are connected to a UPS backup power which is on the building E-power line. The UPS has only ~10 mins power supply to support the instrument by itself until E-power kicks in, normally within ~30 secs after a power loss. But, as a safe precaution, once regular power is gone, please DO NOT use the instruments if you haven't started any operation even though the instrument is still running with backup power. The right thing to do is to finish off your work ASAP, eject the sample and wait until normal power is back before doing more NMR work.

If compressed air is lost, the sample won't eject. Please DO NOT insert any sample unless the sample inside is taken out. If the building air compressor is down, it takes about 10-20 mins for air to totally escape from the air lines. You may still hear air hissing but the pressure won't be enough to operate the instrument. Check the air gauges behind the computers for pressure reading. Normal pressure is ~100 PSI.

For the loss of compressed air, please notify our building manager Cabe Fletcher or campus Facility (EX 8300) directly to have the compressor checked and turned back on.

Possible Web Reservation Disruption (03/09/2018)

A disruption to the department web server that hosts NMR reservation pages is being resolved. There may still be sporadic disruptions. If this problem occurs over the weekend and you are unable to view and reserve time, please use the instruments on a first-come-first-served basis. Make sure to leave a hand-written note if you have to walk away from your experiment for a while.

Cancel Unused, Leftover Reservation (03/01/2018)

Tuning on NMR400B OK Now. Z0 for Locking on NMR500 Adjusted (02/20/2018)

A power loss to the 400 over the long weekend caused a loss to the tuning motor indexing positions. All motors have been re-indexed. Tuning works fine now.

Separately, the Z0 values on NMR500 used for locking have been adjusted to the central allowed range. All solvent Z0 values should shift to the right from the old values by roughly +23000 units. Make sure to enter init1h to load the updated parameters after login.

Lock on NMR600 Fixed (02/15/2018)

The lock problem on the 600 has been fixed with a new lock transceiver. Please follow regular steps of locking and shimming from now on. Disregard the steps below.

2D NMR on NMR600 (02/13/2018)

Except for the lock difficulty, the 600 performs well in 2D NMR (and 1D as well) if the sample stays locked during the experiment. However, due to the lock problem, additional power and gain are needed to keep the lock stable to overcome the brief lock drop (and possible lock loss) during gradient pulses. Gradient pulses, present in many pulse sequences, are used to to destroy certain coherences (transverse magnitizations) or to refocus others. During these pulses, field homogeneity is destroyed, making all resonances (including 2H lock signal) broad, lowering the lock level. The lock recovers during recycle delay.

Please contact me if you need assistance setting up 2D experiments. The lock issue is expected to be fixed in ~ one week.

Update: NMR600 Lock Problem & Workaround (02/09/2018)

A used part we just received didn't fix the lock problem. We'll proceed with a service order that has been placed with Agilent. There is no date scheduled yet for the repair, but presumably it'll be within one to two weeks.

In the meantime, the instrument is still useful if you can get the lock regulated by following the rough steps below.

NMR600 Lock Problem & Workaround (02/05/2018)

Update, 02/06/2018: A used part has been ordered and is expected to arrive in a few days. If this board doesn't fix the issue, we will proceed with a service order that has been placed with Agilent Technologies. We expect the lock problem will be fixed in about 1-3 weeks.

Note the lock has been changing over the past few days. The Lock Find Resonance procedure in step 3 below may not work anymore. After step 2, you may simply click Lock Scan in the Lock panel then wait for the scanning to establish the step-function lock curve (with a flat baseline and a rise to another flat line). You can also drag the Z0 value around the set value until the lock step-function curve shows.

If the lock is messed up when you adjust it, go back to Find Z0, bypass shimming, then manually adjust Z0 as shown below.

Earlier: The lock on the 600 doesn't work in the normal way anymore. A new replacement part is being discussed with Agilent Technologies but the order isn't finalized yet. Before the lock channel is fixed, please follow this workaround to get the lock regulated before your experiment. The key point here is to increase the Z0 value found by Find Z0 by roughly +6700 then re-establish the lock.

1: Follow the normal steps: enter init1h, select solvent, click Find Z0, then GradientShim.

2: Go to the Lock panel, add 6700 to the Z0 value you see in the value field and hit Enter or Return key to change the value. For CDCl3, the new Z0 value should be ~11079. You may also drag the Z0 value bar to the right to increase the value by ~6700. Then, click Lock Scan. You will see a wavy or flat line.

3: Go back to Start panel and click Lock Find Resonance with Simple selected as the scheme. This will likely get the lock regulated and stable. For 2D and long experiments, adjust power and gain to keep lock level at ~80%-90%.

For CDCl3 as solvent, the Z0 value after Find Z0 is ~4300. Following the steps above, add ~6700, we'll get the lock regulated with Z0 at ~11000.

The 6700 increase in Z0 seems consistent with all solvents. As usual, you may temporarily incresae the lock power or gain to boost the signal when adjusting lock, but make sure to drop the power down afterwards to below 40 for most solvents. The auto-locking method Lock Find Resonance auto-adjust the power and gain.

We'll try to the lock transceiver replaced as soon as possible.

Backup Power, Extension Cables in NMR Room (01/23/2018)

A new UPS backup power unit has been ordered. It'll soon be installed near the Agilent 400 MHz instrument to provide backup power to the instrument during power outage and protect the instrument. Once the instrument is switched to the new UPS, the extension power cables currently running from the adjacent room UPS will be removed.

Please use caution when walking over the power cables on the floor.

Cancel Unused, Leftover Reservation (01/17/2018)

Again a reminder to all users: with all instruments having a packed schedule, it is important that everyone reserves only what you need, notes the reserved time, arrives on time, and cancels the reservation if you cannot make it. After you finish your experiments, immediately cancel the rest of reserved time, if any, so that others can use the instrument.

Please Reserve Time before Using Instruments (01/03/2018)

Please try to reserve instrument time before using it unless the web site is down. The reservations allow usage statistics to be estimated in addition to avoiding use conflicts. Usage charge is based on actual computer login time.

NMR Lab Remains Open Over Holidays (12/21/2017)

Thanks to the brave firefighters, the massive Thomas fire is finally under control, but please observe all cautions related to power outage as discussed below. Please take a moment to visit this GoFundMe fund raising to support the family left behind by the fallen firefighter Cory Iverson.

The NMR lab remains open, and all instruments are operational over the Christmas and new year holidays. Staff support, however, is limited due to my travel schedeule. For urgent or emergent issues, please call the phone number posted on the side of the magnet. Please hold off all other requests and needs until the first week of the new year if I'm not available.

Have a fun holiday season!

Instrument & Computer Issues (12/11/2017)

Update: The server for the NMR workstations was down after extended power loss. If the server is down, login to the instrument workstation may be problematic. The server has been moved and connected to building e-power in addition to a UPS. All instruments are running.

Earlier: It appears a few workstations in the NMR lab are down or aren't accessible from the network. If the system works from the NMR room, you may continue to use it. All instruments will be checked in the early afternoon.

Major Power Disruption (12/05/2017)

Update (12/07/2017): With the ongoing fire situation, while all the classes are canceled, the NMR Facility remains operationl. However, staff support will be limited depending on multiple factors. I strongly urge everyone to keep travel & workload to the minimum until the peak risk days are over, possibly until early next week.

Because of the issues listed below, once regular power is gone, please DO NOT use the instruments if you haven't started any operation even though the instrument is still running with backup power. The right thing to do is to finish off your work ASAP, eject the sample and wait until normal power is back before doing more NMR work.

There is an ongoing major power disruption to a wide area due to the Ventura fire. The power is back right now but in the coming days and weeks, we still expect sporadic power instability.

Cautions for the NMR Instruments: All instruments are currently running. The instruments are all connected to their UPS backup units which are on the building emergency power circuit. The new 400 has just been connected to a UPS through an extension cable. The UPS systems should keep the instruments going for maximum 20-30 mins without the building emegency power. However, compressed air mayb be gone if regular power is down even briefly. Do not use the intrusments if air is gone because Eject/Insert and temperature regulation won't work.

In the past, the campus Facility is informed and a technician will come to turn the compressor back on once the power returns.

Lock Level after Power Cycle: Use init1h to load the latest starting parameters. The lock phase often changes by ~90 degree after each power cycle. If the console loses power and comes back, the lock level may be very low or not there at all. If you encounter very low lock level after auto-locking and shimming, you may go to the Lock panel, and change the lock phase (+ or -) by 90 degree, or 180 degree using 10 degree stepsize. The best phase would be where the lock level is the highest at given lock power and gain.

Problem with Lock/Key to PSBN 3608 (11/17/2017)

There appears to be some problem with the lock or key to PSBN 3608. A few keys have been stuck in recent days inside the lock and became hard to pull it out. If it is stuck, please wiggle the key gently left and right while pulling it gently. Don't force it which makes things worse or may break the key inside.

Air Conditioner Breakdown, Box of NMR Tubes Found (11/13/2017)

Update (11/14/2017): The air conditioner in the 600 room has been fixed now.
Earlier: The main air conditioner in the NMR rooms is broken. The door has been kept open during the day to allow cool air in. Please close the door if its still open after dusk and during the night.

A box of used NMR tubes were found in the men's bathroom. Please come to pick them up in the manager's office.

Reservation & Instrument Time Waste (10/27/2017)

Despite our effort to prevent instrument time from being wasted, there are still a good number of reserved time slots not actually used. Please keep track of your reserved time and cancel any 10-minute time slots that you won't use. If noted, all reserved but systematically wasted time slots will be billed.

Gradientshim on NMR500 Not Working (09/19/2017)

Update: The problem has been fixed. Make sure to use init1h to load updated shim & lock parameters.

Earlier: Gradient shimming on the 500 isn't working. It appears the gradient amplifier may be broken. An alternative amplifier has been put on the 500, tested with another probe. While shimming on 2H signal isn't working, gradient shimming on 1H signal is. This is still being looked at for pssible software or parameter issue.

If the problem cannot be fixed, the broadband probe will be put back in. You'd have to do manual shimming (Z1, Z2 back and forth to optimize lock level). Once shimmed, the data look fine.

Found USB Drive (09/07/2017)

If you have lost a USB flash drive with NMR data on it near the Chemistry building, please contact the manager.

NMR500 Up Running (09/05/2017)

It appears a power outage over the long weekend took down the 500. The 500 is up running now.

Tube Care & Breaking on All Instruments (09/01/2017)

Our standard practice is to have a dummy sample ("Idle" sample) in the magnet when the instrument isn't being used. These tubes are simply empty tubes. But they keep getting broken frequently due to improper practice of handling the tube and to a greater extent, other sample tubes as well.

Please pay attention to these basic steps while handling any NMR tube:

DO NOT leave the depth gauge with the sample inside standing freely on the table anywhere. It easily tips/flips and breaks. Please leave the dummy sample in the fixed holder on the 500 and 600 attached to the table, or leave it in the beaker on the 400.
DO NOT insert the glass tube into the spinner with the spinner and gauge sitting on the table, or with the spinner sitting in the fixed holder mounted on the table (available on the 500 and 600 table). ONLY insert the tube into the spinner with the spinner (or along with the gauge) held in your hand. With the spinner & gauge off your hand, the unknown amount of force and rigidity may cause the tube to snap easily.
If you break the dummy/idle sample tube, please replace it with a clean EMPTY tube. If there is any sample spill, please clean up the mess.
Any tube breaking accident that leaves the tube broken in the probe should be reported to the manager ASAP. A large hand-written, clearly visible note should be posted and stuck to the keyboard/monitor to warn others NOT to use the instrument. Serious damage may occur if additional samples are inserted into the probe without the broken tube and glasses removed.

NMR600 Receiver Improved (08/18/2017)

The 600 has been giving a larger than usual quadrature image & a center glitch peak. The issue isn't as obvious when the scans are done in multiple of 4s, but obvious when it ends in odd numbers. The receiver board is to blame for the problem. It has been fixed now.

The lock issue will be dealt with next. The problem is that lock is having trouble during initial locking to the H2 resonance. Right now, it can be easily fixed by clicking the "Lock Find Resonance" button after shimming or simply using the "autolock" process at the start of the experiment.

This is likley due to a problem with the lock transceiver. Unfortunately, the instrument has to be down for days to get the board repaired. We'll find a time to do so.

Autosampler on NMR400b Removed (08/15/2017)

The autosmapler on the 400 has been removed. If the need arises, it'll be put back on. The normal barrel insert should be easier in the operation mode we normally use.

NMR400b Ok to Use (08/14/2017)

A tube broke at the top of the barrel and stuck in the probe over the weekend. Luckily, the sample didn't spill. The barrel & probe have been taken out & cleaned. It's OK to use now. Make sure to load new shims with init1h.

Possible loss of compressed from 8-10AM Friday (07/27/2017)

Work is planned to fix an air leak in an area on the 3rd floor of PSBN. This likely won't affect the NMR rooms, but it is possible we may lose compressed air during the work.

Please use the instruments as usual. If there is difficulty ejecting/inserting a sample, stop using the instruments and retrieve your samples later.

Computer problem with 500 fixed (07/20/2017)

During trouble shooting of something else on the 600 with a part from the 500, the 500 was shut down but the computer was unable to come back up. It is most likely the power supply was bad. To keep the instrument running, the computer from the old 400 (currently not used) was used for the 500. The 500 is running fine. The old bad computer will be fixed.

In the coming days, there will be a few more sporadic short down periods for trouble shooting issues on the 600.

Use 500 for H1 only till later today (07/18/2017)

Update: The 500 is back to normal operatoin for H1 and C13.
A trouble shooting is being done involving both the 500 & 600. Please use the 500 for H1 only until further notice, likely later today.

Instruments Down for 2 Hrs. on Monday for Air Compressor Work (07/16/2017)

Update (11:10AM, 07/17): Compressed air is back. All instruments are open for use.

All instruments will be down for ~2 hours (9AM-11AM) due to building air compressor work. Reservation will be open once the work is finished.

Cancel Unused, Leftover Reservation (07/13/2017)

NMR500 Down for Computer Work (07/12/2017)

Update (2:00PM, 07/12): The drives have been replaced. The instrument is ready for use.

The 500 will be down for 2-3 hours to have two hard drives replaced. It'll be up running after the work is done. If you have reserved time after the blocked time period, those reservations may be removed if the work isn't finished. Please check the schedule as it goes.

Reservation Website Problem (07/10/2017)

It appears the reservation web site is sluggish and inaccessible at times. Please see note from a few days ago below. Use the instruments on a first-come-first-served basis if it is down.

Compressed air down from ~1-2PM on Friday (07/06/2017)

Campus Facility will do more maintenance & repair of the building air compressor. Compressed air will be off from ~1-2PM on Friday, Jul 7. All instruments will be down starting at 1PM until the work is done.

Reservation Web Site Up Running After Glitch (07/06/2017)

There was a glitch with the NMR website this morning. Our computer support has fixed the problem.

In case that the reservation site is down, please use the instruments on a first-come-first-served basis until it's back up again.

Brief loss of compressed air (06/30/2017)

Update: Compresesd air is back now. All instruments are ready for use.
There was a brief loss of compressed air around 2:00PM today. A valve in the building compressed is being replaced. The air loss should only last 20-30 mins.

Compressed air is gone in PSBN (06/23/2017)

4:10PM: Compressed air is back on. All instruments are running. Please use caution over the weekend for potential air problems.

3:00PM: Compressed air is gone in the building. Do not use any instrument until air is back. Physical Facility has been notified. It is unknown when air will be back.

If a sample is unable to eject, check the air pressure meter on the wall and stop using the instrument. Normal air pressure reading is ~ 100-110 psi.

Air Conditioner Still Under Repair (06/09/2017)

Update 06/13/2017: The air conditioner has been fixed now.

Campus facility replaced a broken compressor in the air conditioner in the room where the 600 and new 400 sit, but apparently that didn't fix the problem. It is still not cooling. They've been notified. Hopefully, it'll be fixed soon. In the meantime, during regular work hours, the front door may be left open to allow some cool air in. Please make sure all external doors are closed/locked during the evening.

Cancel Unused, Leftover Reservation (06/06/2017)

We continue to see that a number of reserved time slots are left unused each day. With all instruments having a packed schedule, it is important that everyone reserves only what you need, notes the reserved time, arrives on time, and cancel the reservation if you cannot make it. After you finish your experiments, immediately cancel the rest of reserved slots not to be used so that others can use the instrument.

Air conditioner in NMR room is broken, being repaired (06/01/2017)

The air conditioner in the NMR room where the 400/600 sit is broken. A new compressor was ordered. It is being repaired by campus Facility. Before it runs again, the room may be warm. During the daytime hours, the front door and back window may be kept open to allow some cooling. Please make sure the door and window are closed at night.

Spectrum Artifacts on NMR500 (05/08/2017)

There were some serious artifacts in the 1H and 13C spectra collected over the past day or two. There was a large, broad center glitch with rapid oscillations and many image peaks mirroring around the center. It appears this was due to a broken receiver. If you observed many unexpected peaks, some out of phase, this was the cause.

A working receiver from the old 400 has been put in the 500 while the broken one is being sent for repair. The quality of spectrum is normal now. You may use the instrument as usual. Please note and report spurious peaks and issues on the 500.

Possible Power Outage (05/06/2017)

There is a chance for power outage from the weather condition & possible thunderstorm over the weekend. If electric power is out, the eject air is most likely gone in ~30 mins once the building compressor turns off. If a sample is unable to eject, check the air pressure meter on the wall and stop using the instrument. Normal reading is ~ 100-110 psi. If this happens, in all likelihood, air won't be back until Monday.

Cancel Unused Reservation (03/30/2017)

There have been many unused time slots left in place after a user finishes the work early or doesn't show up. With all instruments having a packed schedule, it is important that everyone takes a look of your reserved time after you finish your experiments and cancel the rest of reserved slots not to be used ASAP so that others can use the instrument.

Compressed air gone in PSBN. All instruments down. (04/17/2017)

Update: Air is back. Ok to use.

Earlier: The building compressed air is gone. We are waiting for facility people to turn air back on. Eject/insert operation doesn't work. Do not use the instruments until air is back.

NIH SIG Acknowledgement (03/28/2017)

The NMR Facility has been supported by instrumentation grants from NIH and NSF. If you include NMR data collected on the new 400 in any publication, please acknowledge the recent NIH Shared Instrumentation Grant (SIG): 1S10OD012077

Please keep the common area clean (03/23/2017)

Please pay attention to keeping the computer desk areas for each spectrometer clean. There have been papers, gloves, pipettes, broken glasses, chemical spills ... accumulating on the desk area and the floor below. Please take away the items you bring into the NMR room unless it is a need for them to be there after each use. For everbody's saftety, a user is responsible for throrough cleanup of the area of chemical spill if a tube breaks in the desk area according to the Policies and Rules.

You may use the hand sanitizing wipes provided in the spectrometer area.

Protein NMR on the 600 (03/17/2016)

There will be a few nonstop experiments for protein NMR in the coming few weeks, each lasting ~ 4 days over a weekend. Once the data are collected, we don't expect extended protein NMR use on a regular basis.

Use white or tan colored spinner on nmr500 (03/10/2017)

It appears that recently some spinners may have deterioted over time making the tube easier to break as it settles too quickly in the barrel. This also explains recent problem of slow sample ejection with the other kind spinner. Please use the white or tan colored spinners only on nmr500 (see picture below).

Do not remove them from the 500 area. Do not use the other, lower-quality spinners on the 500. Those spinners are OK for the 400 & 600. In most cases of tube breaking in the barrel, the quality of the tube is still a factor. All tube and washing requirements still apply.

Please record which kind of spinner is assoiciated with tube breaking inside the magnet. We will have more of the high-quality spinners (white or tan ones) available soon. This problem may have to do with the sligtly larger air gap between the cheaper spinner & the barrel due to wearing over time from repeated use. The leaky air gap may have let the sample drop too fast. But, we need to watch how it goes over time to be certain.

It is critically important that in addition to other posted steps, if a tube breaks inside the magnet, a clearly written note in large font should be placed in front of the computer/keynoard to warn others not to use the instrument. The instrument should not be used until the broken glass is removed and the probe is checked.

Mnova License Update & NIH Support Acknowledgement (03/10/2017)

Please follow this instruction to update your Mnova software licenses and install the newest version of the software (optional). Older versions of the software should continue to work under the new licenses covering any versions available up to 02/27/2018.

The NMR Facility has been supported by instrumentation grants from NIH and NSF. If you include NMR data collected on the new 400 in any publication, please acknowledge the recent NIH Shared Instrumentation Grant (SIG): 1S10OD012077.

Eject Issue on NMR500 (03/03/2017)

It happened a few times recently that a sample was slow to eject. A user unknowingly inserted another sample to sit on top of the "idle" dummy sample. No harm was done except that the samples had to be extracted manually. The occasional problem may be due to fluctuation in air pressure and tempearture in the room.

As a precaution, always assume there is a sample in the magnet; it has to be taken out before a new one is inserted. The sign that a sample is stuck in the barrel is the lower hissing noise and muffled air out of the top of the insert barrel.

Please see notes below and read proper procedures for sample tube washing & drying (03/01/2017)

NMR500 down again due to broken tube (02/28/2017)

Update (03/01/2017): Ok to use now.
Earlier: A tube broke inside the probe later in the afternoon. The probe will be checked tomorrow. Hopefully it'll be OK to go after washing. While the cause of tube breaking inside the probe isn't always clear, bent, scratched, or low-quality tubes and tubes that have been washed or dried under very hash condition can break much easier than the rest. Sample spinning on NMR500 puts more strict requirement on tube quality.

Please carefully read the proper procedures for washing and drying NMR tubes in addition to getting quality tubes and trashing very old and scratched ones. Pay attention especially to how the tubes are dried. Prolonged high-temperature drying is strongly discouraged (see bottom section from Wilmad reference page. Copied below.).

From Wilmad:
"Drying tubes at elevated temperatures can reshape and ruin precision NMR tubes. For this reason, Wilmad does not recommend drying NMR tube under any circumstances. An alternative way is to use vacuum oven that will remove water at lower temperatures.

The preferred method of water removal is chemical, not physical, treatment. In most cases, it is the protic content of water that must be avoided. So WILMAD recommends exchanging the protons of chemisorbed water with a deuterated solvent such as D2O prior to a short drying period in the oven. A bottle of D2O that isn't being used any longer is perfect for this purpose. "

Mnova License File Updates (02/27/2017)

Tube broke inside probe. NMR500 down (02/25/2017)

Update (02/25/2017):The probe is clean now. Ok to use.

A tube broke inside the probe Friday night. The probe has been washed. It will dry over the next 24 hours or so. Once clean, the instrument will be up running again.

Mnova Software License Renewal (02/24/2017)

Due to increased users, we are running out of existing Mnova licenses. We are in the process of acquiring more licenses. Before new licenses are available in the next few days, you may see an error message when your computer contacts the license server automatically once every few months. Unless your license is able to be renewed, the software is not usable. We'll try to resolve the situation ASAP.

Possible Power Outage and Cautions (02/16/2017)

With heavy rain and strong wind expected over the next few days, we'll likely see sporadic electric power outages. Building power loss often leads to loss of compressed air even if emergency power comes back on shortly.

If power or compressed air is lost, stop using the instruments. If a sample cannot be ejected, please leave a note in front of the monitor and also enter the command "i" (or click Insert button) in VNMRJ to shut off eject air. You may notify campus physical facility at X8300 to have someone over to turn the PSBN compressor back on.

The compressed air pressure gauge on the wall that supplies instrument air normally indicates ~100 psi. It takes a good 10-20 mins for air to die down completely after the building compressor is down, and similar amount of time for it to fill the lines to 100 psi when it comes back up.

NIH Grant Support Acknowledgement (02/14/2017)

Web Reservation Problem Fix (02/07/2017)

After several unsuccessful attempts at fixing the software bug, I think I finally nailed down the codes where the problem originated. The problem was that sometimes even after a successful reservation, the slots were left unchecked and blank with a "SUCCESS" message, and all subsequent reservations for the day were left blank. I hope this fix did it and it won't happen again. But, please let me know if similar situation occurs again. -- HZ

Spin Control on NMR500 (01/18/2017)

Please do NOT check-mark "Control Spin from this panel only" under Spin/Temp panel. Doing so prevents automation control of spinning during and after gradient shimming. If the sample isn't spinning on the 500, go to Spin/Temp panel and make sure this box is NOT checked and the spin rate is 20, then click Regulate Spin. "Ignore spinner error" box should be checked. See images below for correct setting.

Spin under Start panel should be at 20 and checked.

Update on Web Reservation Problem (01/16/2017)

I may have managed a fix for the recurring problem where reservations are blank after submission with a "Success" message. This seems to only occur when multiple users try to reserve the same timeslot(s), leading to conflicts. Now, if this occurs, you may see a message asking for waiting a short period (~1 min) before another reservation attempt. I hope to do a realistic test later this week.

Web Reservation Problem (01/11/2017)

There is still a reservation problem that occurs when the schedule is busy. Usually the reserved slots don't show up and the page is unusable for the day. I use a temporary page change to fix it. This has to do with the program which seems to run into issues when multiple users try to book the same timeslots. If the problem stays much longer and cannot be fixed, we'll have to switch to other reservation software.

In the meantime, if the page is blank and unusable, please use the instrument on a first-come, first-serve basis until the reservation works again. Thank you for your patience!

Problem with C13 detection on NMR500 has been fixed (11/21/2016)

A hardware (PTS frequency synthesizer) failure in C13 detection has been repaired. You can use the 500 for 13C detection now. 1H detection hasn't been affected.

Problem with C13 Detection on NMR500 (11/04/2016)

It appears that C13 detection on NMR500 isn't working properly. There is only a good peak from the solvent. A suspect part is being sent for repair. The roundtrip will likely take a few weeks. During this time, for C13 detection, please use NMR400b (first choice) or NMR600.

H1 detection on NMR500 is fine.

NMR600 lock issue (10/21/2016)

There appears to be an issue with lock regulation after auto-locking (Find Z0) and shimming. The lock often is low and isn't regulated after autolocking. The first, quick manual solution is following:

(1): After Find Z0 and autoshimming, if the lock isn't regulated, click Start->Standard->Lock Find Resonance (select when->Simple if it is not selected already. See screenshot below). This will likely allow the lock to be regulated. Then you can collect your data.

(2): Alternatively, you may choose to leave the lock alone, simply submit the experiment afer shimming. There is an autolock adjustment period at the beginning of data collection. This seems to be working well to get the lock engaged and regulated. If not, however, stop the experiment, try (1) or another method.

For long running experiment (hours), adjust lock power/gain so that lock level is above 80%.

Compressed air gone (10/17/2016)

Update: Compressed air is coming back. It should be Ok to use the instruments after 10AM.

Compressed air in PSBN is at very low pressure. Campus Facility has been notified. Until the air is back on, please do not operate any instrument.

Compressed air likely gone (10/15/2016)

A user reported saturday night that the sample doesn't eject on all instruments. This indicates there is low compressed air pressue. DO NOT USE the instruments if the sample doesn't eject. It is likely the air will wait till Monday to be corrected and turned on by campus facility people.

Cancel reservation if it's not to be used (10/14/2016)

The instruments have been busy lately. If you reserve time but have a change with your plan or if you are unable to use the reservation, please do remember to cancel the time as early as possible so that other users can use it.

NMR500 Down (09/28/2016)

Update: The probe looks Ok after cleaning & overnight drying.

A tube broke inside the probe. The 500 is down until further notice.

A majority of the tube breaking accidents came from a few users from one or two labs. While user error cannot be ruled out, it is likely due to the age and existing damage to the tubes. Please discard very old tubes (if you can tell) and any tubes with visible damages. Do not wash or dry tubes under high-temperature conditions.

NMR500 Computer Overheat (09/28/2016)

The hot weather and broken air conditioner apparently caused the 500 computer to overheat, killing the power supply. I replaced the power. It's working now. But, please note any abnormality of the computer.

NIH Grant Support Acknowledgement (09/13/2016)

The NMR Facility has been supported by instrumentation grants from NIH and NSF. If you include NMR data collected here in any publication, please acknowledge a recent NIH Shared Instrumentation Grant (SIG): 1S10OD012077-01A1.

Flooding in NMR Room (08/30/2016)

There was a major flooding in the NMR room (3608/3614) from a broken water pipe in the upstairs X-ray lab. The NMR instruments are working OK. Please keep an eye on any water falling over the top of the magnets. That'd be very bad. Importantly, watch any signs of electrical shorts/sparks, any exposed electrical power strips/outlets on or close to the floor. It's been checked but there may be things unnoticed. Facility is working to clean up and stop the water accumulation. But, it will take some days for the water to dry out. We will look for a long-term fix of various issues in the building.

OneNMR Probe is back on NMR400b (08/08/2016)

The probe has been repaired and put back on NMR400b. New shims were made and auto-tuning was checked. It appears to be working fine as expected. Make sure to enter init1h to load new parameters.

Compared to the dual broadband probe, oneNMR probe has higher 1H/19F sensitivity but similar X-channel sensitivity.

Building Compressed Air Problem Again (07/28/2016)

Update, 4:00PM: Well, we lost air pressure again after 20-30 mins. Now, it is inching back up. But, clearly, the building compressors need to be replaced ASAP.
Update, 03:26PM: Air is back. But be cautious with air problems in the coming days and weeks until the compressor is totally fixed by PF.
Earlier (2:50PM): The building compressed air is gone again. Please don't use the instruments until air is back on. The campus Physical Facility has been notified.

Once air starts to come back, it may take 10-20 mins for the pressure to be fully back up (to ~ 100psi). There may be some air hissing for some time initially, but that may not be enough for the instruments.

Sporadic Compressed Air Problems (07/22/2016)

Update (01:17PM): Compressed air is back.
Update (12:48PM): Compressed air is gone again. With the repeated loss over the past day or two, expect more air troubles and be cautious when using the instruments.

Earlier: Apparently, the building compressed air was gone sometime last night, again. It is back now around 9AM.

This may have to do with the intense heat. We expect it may well happen again. If the sample doesn't eject or there is no air hissing or only muffled hissing, please stop operating the instrument. A clear indicator of lost compressed air is low or zero reading of the air line pressure gauge. Normally, the pressure should be ~100psi.

The campus Facility maintains the compressor(s) for the building. The best approach if air pressure is gone is to let me and/or Cabe Fletcher, our building manager know. If he isn't available, please call Physical Facility directly at extension 8300, and report the air loss to PSBN building. Note that chemistry and PSBN buildings have separate compressed airlines and compressors.

Compressed Air Gone (07/21/2016)

Update (4:45PM, 07/21/16): Compressed air is back. Proceed to use the instruments with caution.

Earlier: It appears building compressed air is down. All instrument operation should wait until air is back. If air comes back, you may hear air hissing from the top of the magnet. If there is a user sample held at the top (from an earlier Eject command), please remove the sample and leave it at the table.

Issues and Status of NMR400b (07/08/2016)

The power and pulses of some nuclei have been calibrated. These include H1, F19, C13, P31, Li7, V51, & B11. More to come. There are big changes to H1/F19 pulses and only small changes to X-nuclei. These changes have been made into the routine experiments.

Issues and Fixes:
(1): You may see error messages in the first few steps after the first login. It appears the error always goes away if you enter the following exact command (also posted in front of monitor):

psclipboard[1]='psstage:' su

Additionally, exiting vnmrJ and restarting it may help as well.

(2): Autoshim: New shim files have been generated following an auto-testing procedure. For solvents with weaker deuteron (H2) signal (such as CDCL3), it now takes longer time to finish shimming by using more scans. For samples with stronger H2 signal (such as benzene, D2O), it takes half of the time. The onscreen spectrum display is also off.

(3): Lock power & gain: The auto-calibration also led to different lock and gain power settings from those on the other probe. The power/gain adjustment is done automatically during autolock. The level appears to be around ~50% after locking. This is fine. But, for long experiments (hours), please increase the gain so that the lock reaches ~80-90% level.

New probe Installed on NMR400b (07/07/2016)

The OneNMR probe is broken with a stuck tuning stick. The probe needs to be sent to the vendor for repair. The process may take a few weeks. In the meantime, a different (dual broadband) probe has been installed. Some basic parameters and shims have been calibrated. But the entire process will take some days to get through.

The dual broadband probe has lower 1H/19F sensitivity, but the X-channel sensitivity is similar to that of OneNMR probe. The autotune features are tested briefly. It seems working. But, many X-nucleus pulse parameters have not been tested yet. We'll get through them over time.

Please proceed to use the instrument with caution. All notes for NMR400b still apply until further notice.

Autotune Problem on NMR400B (July 7, 2016)

There is a tuning problem developed over the past day or two. The X-channel often fails to tune with an error message. The 1H/F19 channel tunes fine.

This problem is being worked on.

NMR500 Sample Eject Issue (July 1, 2016)

Recently, the 500 occasionally has taken a long time to eject the sample or failed to eject the sample. You could hear the muffled hissing sound. In all circumstances, assume there is a sample in the probe. Don't insert a new one unless you are certain it's empty by noting the typical loud air hissing sound for an empty probe with eject air on.

NMR500 Down till Jul 1 (June 27, 2016)

Update, July 1: The probe has been checked and is ready for use.

A user broke a sample tube by bumping it at the top of the insert barrel. It appears a portion of the glass tube fell into the barrel, preventing safe operation of the instrument. This has to wait until I come back in town to get taken care of.

Such accidents are totally preventable. Please focus when inserting or removing the sample tube. All it takes is a few seconds of your complete attention!

Tube broken in probe. NMR500 down (June 14, 2016)

Update 06/15/206: A broad, weak, residual peak left after cleaning is gone now. It's clean and ready for use.

Tube Cleaning: (1) Prolonged drying of > 30 mins at high-temperature (>100C) should be avoided. Instead, use low-temperature (<50C) in a vacuum oven or under a hood with vacuum. (2) It is critically important to place tubes on a perfectly flat tray when drying at high temperature.

Update: The probe was contaminated from last night's spill. It's been cleaned and is being dried. Expect the probe ready for use in ~24 hours.

Earlier: A NMR tube broke inside the probe yesterday aftrnoon. The sample didn't spill. Again, early last night a tube broke inside the probe and the user walked away without giving any notice. It appears the next user managed to insert a sample but couldn't get it out. The earlier tube was still inside and was broken in pieces.

While the glass tube does break occasionally, it is totally unacceptable to walk away without giving notice to the users afterwards and notifying staff of the incident so that no serious damage happens.

So far these incidents are mostly limited to a small group of users and labs. After talking with the user yesterday, it appears again the tube was likely the main cause (old tubes that may have been treated with high heat).

NMR500 running but use manual shimming only (June 8, 2016)

Update: Auto-locking and shimming works now. There was a bent pin in the probe gradient connector. That was straightened. All good to go.

Earlier: NMR500 is clean now. But, gradient auto-shimming isn't working. This may not be related to the tube breaking accident at all. While the problem is being checked, please use manual shimming after init1h. If you accidentally clicked "gradient shim", enter init1h and use manual shimming.

NMR500 Down from Tube Breaking (June 7, 2016)

A tube broke inside the probe last night. The sample was spilled. The probe has been washed and is being dried inside the magnet. It will likely take 24 hours for residual peaks from the washing solvent to go way.

The few tube breaking accidents mostly came from users from two labs. It is very likely in this case, the tube was damaged before use. Some of the NMR tubes being used are very old. At least one lab received many old tubes discarded by another lab. Some tubes don't meet specs we require. Please read notes below for tube requirement and discard any tubes with even slight damage.

Missing Spinner on NMR500 (June 1, 2016)

A spinner used for high- or low- temperature experiment is missing, likely since last night. Please return to the 500 ASAP if you accidentally took it with you.

Idle Sample & Temperature Regulation (May 10, 2016)

Only NMR600 should be set to regulate temperature at 25C, except during VT experiments. Temperature regulation should be left OFF on the 500 and 400 (with the VT green light off) except during VT experiments.

A dummy, "idle" sample is always in the magnet when it is not in use. If a user breaks this tube, please simply use a clean, empty tube. DO NOT use any tube with a sample inside.

NMR500 Still Down (Apr 9, 2016)

Update, 8:30PM, Apr 9: The probe is clean and is ready for use now.

Update, 10AM, Apr 9: The residual solvent peaks are still fairly strong. The probe is still being flushed with air to remove these peaks. Please plan to use the 400 and 600 for your experiments over the weekend until further notice.

Please read NMR tube requirement below. The sample on NMR500 spins and requires good-quality tubes. A Norell brand, empty tube found at the 500 (likely replaced by a user after the empty Idle sample was broken) and used for the "Idle" sample is noticeably thinner than the required Wilmad 5mm tube. This can be felt without a doubt as the tube is pushed through the same spinner.

EARLIER (Apr 8): A sample broke inside the probe during an VT experiment. The probe is being cleaned. It will likely be ready for use on Saturday.

Tune Probe Back for H1 After F19 Detection (Mar 31, 2016)

On NMR400b, after you tune the probe to F19 and finish detection, please make sure to load a H1 detection experiment and tune the probe back for H1 detection. The next user assumes the H1/F19 channel is tuned for H1 detection. This arrangement, without asking a user to tune the probe for H1 every time, is to prevent repeated probe tuning and long-term damage to the probe.

To set the probe for H1 tuning, simply enter setexp('H1') at the command line, or just load one of your saved, earlier H1 .fid file into the current experiment. Then, click autotune.

If you are done with the current sample, you can also enter init1h. But note this will also load default shims and lock parameters.

NOTE: Significant signal loss is expected if H1 is detected while the probe is left tuned for F19. If H1 signal strength is way off what you expect, follow the steps above, tune the probe to H1 and recollect the data.

NMR500 Down (March 10, 2016)

Update: OK to use now 03/11/2016

A sample tube broke inside the probe and the probe is contaminated. It's cleaned and is being flushed with air. Likely the probe will be free of the residual solvent and ready for use tomorrow morning.

NIH Grant Support Acknowledgement (March 2, 2016)

If the new Agilent 400 MHz instrument is used for any part of data collection included in a publication, please acknowledge and cite the following NIH Shared Instrumentation Grant (SIG): 1S10OD012077-01A1.

Please send me the full reference information including title, author list, journal, volume and page numbers. We are required to report results and progress provided by this NIH funded major instrument. The publication record is also needed to support future grant application for instrument purchase and upgrade.

NMR400b Issues and Status (02/19/2016)

We have been intermittently having issues with autolock, autoshim and data collection in general on the 400. Most often, when the instrument has this particular problem, there is a message in the top message area that says "Z0 too small ...", occasionally "Z0 too big ..." with a large negative or positive Z0 value below. Z0 value isn't changed, lock may be on, but the 1H spectrum is flat with noise. Fixing it needs a power cycle of the console.

We suspect that this specific problem is due to a broken board in the console. This board has been replaced today. Auto-locking, shimming and data collection is all normal.

Please write down the problem and time if the failure comes back again and send the manager an e-mail. We will continue to search for the origin of the problem and get it fixed.

Sample Tube Broke on NMR500 Again (02/08/2016)

Update: The probe looks OK now. Please read earlier notes for cautions.

Earlier, 02/06/2016: A sample tube broke into pieces and sample spilled inside the probe on nmr500. Not surprisingly, the tube was an unmarked tube, without any manufacture label, likely a low-grade disposable tube. Residual peaks are seen in empty probe. This requires the probe be washed and dried over the next day or two. If the peaks remain, the probe would be sent to the vendor for a costly clean-up.

It is disappointing to see old, unmarked, low-quality tubes continue to be used, leading to such accidents. All users should follow earlier instructions to discard all tubes with visible damages, tubes without manufacture labels, economy-grade and disposable tubes. Only tubes suggested below from Wilmad should be used.

Please read and follow the instructions on sample tubes below (01/25/2016)

Another tube broke inside the 500. This is the 3rd time by the same user in one month. However, it was not a user operation error. It is clear that this has to do with the sample tube quality. It was an unmarked tube which has a distinct blue tint in the glass, different from the Wilmad glass. It was from a batch of tubes given by another lab.

For instrument safety, all users should read the information below and check the sample tubes, discard the bad ones (and tubes without labels), and only buy quality tubes.

Required NMR Tubes (01/20/2016)

It appears that recent repeated sample breakups on NMR500 have to do with sample tube quality. From now on, only one type of NMR tubes will be available in Chem Store. Please only order Wilmad Labglass 500 MHz rated, precision tubes (5 mm Thin Wall Precision NMR Sample Tube, 7" Long, 500MHz rated, SKU: 528-PP-7). This is the minimal requirement. Note that this is also called & listed as "Standard Wall" tubes on Wilmad website. Higher MHz rated or longer Wilmad precision tubes are fine, but it is not necessary here and they are more expensive.

All economy grade NMR tubes (with a label starting with WG-... from Wilmad), tubes without any manufacturer labels/markings (likely disposal tubes), and all tubes with visible damages and scratches should be discarded. Disposable and economy grade tubes in particular are of much lower quality, designed to meet much lower standards, and not intended for prolonged repeat use under harsh conditions (VT, strong acid/base, etc.). Lower MHz-rated tubes also have much less degree of "concentricity" and "camber" (see below). All these also affect resolution and signal-to-noise in addition to the risk of damaging the instrument.

Main Differences between Economy and Precision Tubes, according to Wilmad:

Glass Quality: Precision tubes are made of ASTM Type 1 Class A glass, have 3 fold less paramagnetic contamination comparing to the Economy tube. The Economy glass is ASTM Type 1 Class B.
Temperature Tolerance: Precision tubes can be operated safely at temperature up to 230C, and within a temperature step of 120C. Economy tubes have much less thermal-shock resistance and are only intended for use under ambient temperature.

For the reasons why the tube quality is vastly different by design and understand the meanings of "Concentricity", "Camber", etc., please refer to this Wilmad reference page.

NMR500 Down (01/19/2016)

Update 01/20/2016: The broken tube with sample inside has been taken out. The probe looks OK and is ready for use.

The tube was an economy grade tube rated for 200 MHz instruments. The breakup is likely due to the low-quality of the tubes, the age of the tube, bending over time, or existing damage to the tubes.

Many of the tubes in circulation might be of low quality when bought new. They are cheaper for a reason and do not meet the strict requirement needed for the instruments and spinning. Please ONLY buy the 500 MHz rated NMR tubes from the Chem store or the same types of tubes from Wilmad Labglass. All other branded tubes, low MHz rated ones, economy grade, particularly old and over-used ones, tubes that have gone through high-heat cleaning, and any tubes with slight damages or visible scratches should be discarded immediately.

Earlier: A user reported a sample tube broke with the bottom section still inside the probe. Please do not use the instrument until the broken tube is taken out and the probe is cleaned, likely on Wed. morning.

Lab Coats and Other Items in the NMR Room (01/15/2016)

Some have concerns about wearing lab coats sitting at the workstation and operating the instruments. We had not set explicit rules until now. Following standard protocols at most other NMR facilities and similar laboratories, and in consultation with the department NMR Committee, we now ask that all users do not bring and wear lab coats in the NMR room. Use of pipettes and wearing surgical gloves are also not permitted. These new rules have been added into existing rules for the NMR Facility listed here. In cases where lab coats, pipettes or gloves have to be used, please notify the manager of such needs.

I am aware that these rules may cause inconvenience to many. But, it is the right thing to do for the safety and health of everyone. Even with these rules, I ask everybody to try your best not to break samples and spill chemicals in the NMR room. The room itself is similar to an office space and does not have a wet lab area or ability to deal with many unknown chemicals in the lab; some of them could be toxic or hazardous. We ask that everyone follows standard rules and protocols that apply in dealing with chemicals in your office space and help prevent the spread of toxic and hazardous materials.

Please let us know if you have questions and concerns about these additional rules.

Holidays and Instrument Issues (12/23/2015)

On Monday, there was a problem on the 500. It turned out that an unknown user broke a tube inside the probe (again), left the bottom section with the sample inside and didn't leave a note. The broken top section along with the spinner was apparently taken out. Subsequently, a few users had repeatedly tried to use the instrument but was unable to get data.

The computer does keep a record of login and out. Accidents do happen. However, walking away without notifying others and the manager is totally unacceptable. It may potentially lead to expensive repair and work delays for everybody else.

Happy Holidays: There will only be limited staff support over the holiday week (Dec 23 to Jan 3). Please use the instruments with care.

NMR500 ready for use (12/18/2015)

Following tube breaking and chemical spill inside the the probe, the probe was cleaned and flushed with air overnight. It appears clean now and is ready for use.

NOTE: A tube may accidentally break by hitting other surfaces as it travels down in the barrel. But, this is extremely rare. More often, this is caused by other reasons. Among them, the depth of the tube inside the spinner is not set properly (too deep) or the sample is dropped in the magnet without air support, or both.

Please do not clean the tubes under high temperature because the tube may bend in high heat. Any tubes with scratches or slight damages in the bottom 1/3 section of the tubes should be trashed immediately.

NMR500 Down (12/17/2015)

A sample tube broke inside the probe. The probe has been cleaned but it will take a number of hours to dry out the solvent and test for residual chemicals inside the probe. It is likely going to take today and overnight before we are able to know better of the probe status.

Power Outage during Holidays and El Nino (12/15/2015)

Last night under a very windy condition, apparently there was a power glitch which shut down NMR600 console but the other two instruments seemed OK.

The general electric power situation in the Santa Barbara area and on-campus is not good, to say the least. In fact, "Everyone between Goleta and Ventura is now designated the most vulnerable communities in California." Southern Cal Edison is working on putting together emergency power generation in preparation for El Nino (not exactly voluntarily), but it is clear that their efforts fall far behind what is needed for reliable power. This is a patch-up work, not a permanent solution (See video reporting of the serious power problem here). . The possibility of widespread and prolonged power outage (weeks) during El Nino and other major risks (i.e. earthquakes) in our area is very real.

Please note the the signs of the instrument shutdown due to power outage. Do not use the instruments if there is a power loss. Longer power glitches beyond a few mins will almost certainly shut down the instruments and turn off the building air compressor. Loss of compressed air occurs almost every time when there is a power outage or glitch, disabling sample insert/eject operation.

Login/Network Problem (12/11/2015)

It appeared the department network cable broke last night and in the early morning (see Ted Cabeen's message). This seemed to have been patched up for now. You can login normally now. But there may be further interruptions as the cable is being replaced more permanently.

Power Supply Problem on NMR600 (Dec 6, 2015)

Update: The blown fuses have been replaced by Facility in the afternoon. Power is restored to the 600.

It appears there is a power supply problem to nmr600. Please do not sign up or use the instrument until further notice, most likely Monday, after Facility checks the supply issue.

Spin Control on NMR500 (Nov 20, 2015)

Please do NOT check-mark "Control Spin from this panel only" under Spin/Temp panel. Doing so prevents automation control of spinning during gradient shimming. If the sample isn't spinning on the 500, go to Spin/Temp panel and make sure this box is NOT checked and the spin rate is 20, then click Regulate Spin.

NIH Grant Support Acknowledgement (July 15, 2015)

According to NIH grant guidelines, if the new Agilent 400 MHz instrument is used for any part of data collection included in the publication, please acknowledge the following NIH Shared Instrumentation Grant (SIG): 1S10OD012077-01A1.

Please send me the full reference information including title, author list, journal, volume and page numbers. We are required to report results and progress provided by the NIH funded major instrument. The publication record is also needed in future grant application. Thank you for your support and efforts!

Compressed air situation (Oct 15, 2015)

02:20PM: PSBN compressed air is now back. Hope it lasts! All instruments are open.

Earlier: Building compressed air was back on for a brief half an hour then it was off again. Facility has been contacted but it is not clear when the air will be fixed and remain stable. Please proceed with caution these few days even after air is back. There are pressure meters in the main air lines on the wall. Normally the needle is at ~100psi. If the reading is much lower, the instruments cannot be operated and the samples will not eject.

All instruments are down due to power outage (Oct 14, 2015)

Please do not use the instruments until further notice. Earlier power outage has knocked out building compressed air, making samples unable to eject.

Update of Mnova Software (Oct 12, 2015)

Please update your Mnova software to its newest version (v10.0.2) and re-do your license activation with new license files by following the instruction here. There is no need for re-sending your HostID if you have been using the older licenses.

Guide for Long-Running Experiment (Sept 10, 2015)

When forcing a prior user out or stopping a running experiment, check the web reservation first.

If you set up a long experiment (hours or overnight) and you don't plan to stay in the NMR room through the experiment, please leave a handwritten message that lists your name and rough starting and ending time of the experiment, and leave it in the keyboard area or over the monitor. The note should help prevent others from accidentally stopping the running experiment.

All experiment time should be reserved first on the web. Failure to do so may lead other users to stop any running experiment because some users forget to log out or forget to stop a running experiment before logout.

Please also cancel all unused time from the website if the experiment is finished earlier.

Chemical Shift Referencing Description (Aug 25, 2015)

Some users had questions and confusions about how to describe the chemical shift referencing method in a publication. Please read this summary.

Water Leak from AC (July 20, 2015)

There is some water on the floor and dripping from the pipe near the ceiling in the 500 instrument area. The campus facility is working to fix the AC unit that has iced up. The AC unit has to be warmed up overnight to let ice thaw. Please continue to use the instrument with caution.

Web Reservation Problem (06/23/2015)

Web reservation continues to encounter a problem where a successful reservation message is given but the reserved slots are blank. This is likely due to multiple users trying to reserve the same slots at the same time, a software bug. If this happens, please let me know and use the instruments on a first-come first-served basis until the page is fixed, often involving wiping out all existing reservations.

Compressed Air Is back

After a brief, ~ 10 mins problem of low air pressure, building compressed air is back now.

Web Reservation Is Back (June 1, 2015 1:30pm)

Our IT support has made good progress in migrating the site. Please use the web to reserve time for your experiments now. However, if the site has troubles, use the instruments on a first-come, first-served basis. Please report any problems to the manager.

NMR Reservation Page Down Monday afternoon June 1 (05/29/2015)

Department IT is migrating our servers. The NMR reservation system will be down for the afternoon of June 1 Monday, possibly till the next morning. Please use all instruments on a first come, first served basis starting 12:00PM Monday June 1. The web signup may not reflect current usage. Do not reply on it for your experiment during this time. Please write down your name and time duration in the log book for any longer experiment if you step out the NMR lab during the experiment.

New Recharge Rates Take Effect July 1, 2015 (05/15/2015)

The NMR committee and the department have approved updated recharge rates for the NMR instruments. Please see the new rate table here. The new rates take effect on July 1, 2015. The rates reflect continuing support from the department and the goal of recovery of maintenance, repair and staff support cost.

NMR400 Back Running After Probe Cleanup (04/30/2015)

The probe was cleaned after the broken tube was removed. Some liquid was spilled both by the initial breakup and by the following users' repeated sample insert/eject. The probe was washed, cleaned and was put back. Most residual peaks are gone now after blowing air through the probe overnight. Please use the instrument with care and follow the instructions below.

NMR400 Down (April 29, 2015)

The new NMR400 is down due to probe contamination from a broken NMR tube. Please make sure to follow these two minimal steps if an NMR tube (empty or with liquid) breaks inside the probe:

(1): Post a clearly written note in large font and stick it to the monitor to warn others NOT TO USE THE INSTRUMENT!
(2): Notify me ASAP by seeing me or calling my cell phone number posted on the side of several magnets.

Failure to do so causes the liquid sample to dry in the probe and other users to do more serious damage to the probe by using it further. It is entirely the user's responsibility to prevent others from using it further until clear instruction is obtained from Staff.

In this case, the liquid section of the tube broke off and remained inside the probe while the spinner with the rest of the tube was taken out. But several users continued to use the 400 with the broken tube inside over the following 20 hour period, unaware of the situation since late yesterday afternoon. The note left by the responsible user was too casual and uninformative to stop others from using it.

Mnova Upgrade to Version 10.0.0 (Apr 14, 2015)

Please follow these steps to upgrade your Mnova to v10.0.0. Note the exact version number. Versions newer than this one is NOT supported. The prior license that supports version up to 8.1 will not work anymore. However, the older versions of the software are covered with the new licenses if you choose to use them. At the minimum, you need to install the new licenses with existing Mnova or v10.0.0.

Note that only one version of the software can be installed on a computer. Uninstall the old one before installing a new one.

Data Station Is Ready for Use (Feb 12, 2015)

The data station is back running with a new operating system and vnmrJ 4.2. The new vnmrJ software is the same one on the new 400. Please follow the instructions in front of the monitor to change a few initial default settings.

Compressed Air Is Back (Feb 9, 2015)

The buidling compressed air is back now. Please report further problems. If I am not around, please report loss of compressed air to our building manager Cabe Fletcher or Facility Management directly.

Building Compressed Air Loss (Feb 7, 2015)

From a student's report, it is likely the Chem & PSBN buildings lost compressed air on Saturday. DO NOT use the instruments until air comes back on. To test, try to eject the sample. The sample spinner is unable to eject or insert without air support.

Data station repair (Jan 15, 2015)

The data station (rabi.chem.ucsb.edu) is still down due to a hard drive failure. Some data under your home directories have been recovered but vnmrJ remains inaccessible. We will reinstall a newer version of system software on a new drive during the week of Jan 26. This computer is only supposed to be used for data processing of existing data collected on the other instruments; it should not be used to store long-term data.

Please take steps to transfer any data you may want to keep under your home directory on the data station (i.e. /home/group_name/username, but NOT any data under /nmr400, /nmr500 ... etc.). The raw and other data on the NMR instruments are not affected. All existing home user folders and data on the data station will be removed after Jan 25. However, the home directories will be backed up before the removal.

Instruments Up Running (Jan 3, 2015)

NMR400b, NMR500 and NMR600 are back running after the planned, area power outage.

Holiday Schedule (Dec 12, 2014)

Please pay attention to posted and updated notices.

The instruments will stay open to regular access, except during the period of a scheduled power outage on Jan 3, 2015. Some of the components are on emergency power, but it is not certain it will survive the power switch. You are advised not to plan any time-sensitive experiments during the power outage. All instruments will be checked on Jan 4.

I will be out of town from Dec 27 to Jan 3. My emergency assistance number is posted on the magnet. Happy Holidays! -- H. Zhou

Instrument Shutdown (Nov 29, 2014)

All instruments were powered up around ~1:30PM, Nov 29 (Saturday). Please use caution and observe notices posted here and in the room for updated schedule. There is no official word whether this is the end of the power outage. There may never be one.

Building air is still OFF. Do not do any VT experiment until further notice. Also, the lack of magnet leg air support will cause some vibration noises to the spectrum.

Lock phase is likely off ~ 100 degree when a power cycling occurs. Lock and shim as usual. Then, Optimize lock phase to achieve highest lock level. Lock phase has been updated in init1h script. Please always enter this script at the beginning of the session to update parameters.

Instrument Shotdown (Nov 20, 2014)

Due to a planned area power outage, all instruments will be shutdown from 10PM, Nov 28 (Friday) to 2PM, Nov 29 (Saturday). Please observe notices posted for updated schedule.

Have Lock Regulated Before Experiment

Reservation Problem (Nov 5, 2014)

There have been sporadic web reservation problems. Reservation is not shown even the booking is said to be successful. If the site is not functioning, please e-mail me and use the instruments on a first-come-first-served basis until it's fixed. -- H. Zhou

Have Lock Regulated Before Experiment

On all instruments, please pay attention to the lock level & status. Lock must be regulated before data collection. The status is shown in the lock panel ("Regulated"). If the lock is toggled on but is not regulated, the resonances would shift bewteen scans and may lead to broad or multiple peaks.

On NMR400b (new 400), this is especially important beacuse of a slow locking process due to the new software issues. If lock cannot be regulated within a few seconds, first try to click "Lock Scan" button to force faster scanning. If lock is still not regulated, try toggle lock off and adjust Z0 manually, then toggle lock on again.

We'll look into the slow locking problem along with other issues.

Current Default Probes and Best Applications

Please follow this link to read the current probe configuration and best experiments to use for.

Web Reservation Problems

It looks like we still have on and off web reservation problems. When it happens, I switch the webpage to a backup page. That always wipes out all the previous reservations. If you cannot reserve time online, please use the instrument on a first-come-first-served basis.

Agilent Engineer Site Visit Today (August 27, 2014)

The engineers will be here to check out problems with the new 400. Exact time of the visit during the day is unknown. Interruptions to service may occur with short notice. You may continue to use the new 400 until further notice.

Training on New 400 (July 2, 2014)

See training schedule with Elizabeth Levy posted between 400 and 500.

Data Transfer and Networking (June 19,2014)

The changes made to the department networking setup will affect how off-campus data transfer and login in general is done. Please let me know if you have trouble getting essential data to off-campus computers. Otherwise, for the time-being, try to use campus network connections for data transfer.

Continuing Training on New 400 (June 13, 2014)

See training schedule posted between 400 and 500. Or, you can contact me directly for training outside these hours.

Continuing Training on New 400 (May 9, 2014)

We are still training experienced NMR users (>=2 years doing routine NMR here) to use the new 400 MHz spectrometer. Please sign up for time with our assistant Elizabeth Levy next week from 10 to 11AM each day (half hour slot) on a schecdule posted between the old 400 and 500. I'll also train users as needed. Once this group of users are trained, it'll open up to all users.

Reservation Problem (May 1, 2014)

There have been sporadic web reservation problems. Reservation are not shown even the booking is successful. This often is correctly by switching between a different spectrometer name which removes prior reservation. Please re-reserve the time on new page. If the site is not functioning, e-mail me and use the instruments on a first-come-first-served basis until it's fixed.

New NMR400 Online Reservation (Apr 25, 2014)

For the users who have been trained to use the new 400, please reserve time online under NMR400 (New). The users who have not been trained to use the new instrument should not sign up under the new 400 before training. The old NMR400 is offline for now (see below).

Sign up for training on new NMR400 (Apr 25, 2014)

A training signup sheet is posted between the old 400 and 500. This is the time when Elizabeth Levy, NMR Assistant, will be available to show existing users how to use the new instrument under the new vnmrJ. The new program has a good number of bugs but overall the instrument is convenient to use and the data quality is very good. We will stay with the existing procedures until the autosmapler be put into better use, if any.

As a start, only experienced NMR users (>=2 years doing routine NMR here) are allowed to use the nmr400. Once this group of people are trained, it'll open up to all users.

Old NMR400 Down and NMR Assistant (Apr 25, 2014)

The old nmr400 is down for now. The receiver has been having problems over the past few months and it has likely given up. This is only coincidental with the addition of autolocking and shimming features (which seem working). Once the problem is confirmed, it will take some time to get the receiver (or other problematic part) replaced. The old parts are not being made new anymore and it takes longer to get things replaced or repaired.

The new NMR400 is gradually opening up to new users. Over the next few weeks, we'll have users trained to use it, starting with more experienced users. Please do not attempt to use it unless your account is created by me on the instrument and you have gone through a brief training.

Elizabeth Levy is our new assistant at the NMR Facility. She will show existing users how to collect H1, C13, P31 and F19 spectra on the new 400 in the coming weeks.

Autlock and autoshimming on old nmr400

We have the auto-locking and auto-shimming hardware installed on the old 400 MHz spectrometer. Both features function the same way as on the 500 and 600.

New 400MHz Magnet Installed and Running (Apr 7, 2014)

The new 400 MHz instrument has been installed. Groups of users will be added this week. The new instrument has auto-locking, shimming and tuning capabilities. The probe (oneNMR probe) offers much better H1 sensitivity and normal sensitivity for broadband nucleus frequencies (N15 to P31 frequencies, including 13C).

New 400MHz Magnet Installation (Mar 18, 2014)

The new 400 MHz instrument is being installed this week and maybe next week. The new instrument will share the room with the 600 MHz instrument. Some noise and interruption may occur in the room. Please check all notices posted in the room and on this web site.

Computer Network Problems (Jan 3, 2014)

There have been department computer network connection problems during the holidays. Connections and access to the NMR workstations from external computers are still down, and likely sections of the networking in the building are also down, depending on your location; exactly what kinds of connections are affected are not clear. Department IT support is working on this issue.

If you have trouble transferring data with department wireless connections, please try a land-based, wired connection from your lab (or the other way around). If you cannot reserve time online from any of your computers, please walk to the NMR room and use any of the NMR workstations to reserve time.

Holiday Schedule (Dec 10, 2013)

I'll be on vacation from Dec 25 to Jan 2, in addition to time-off on normal school holidays. The NMR instruments will be open for use as usual. Please follow all instructions and rules, and use care. Happy holidays! - H. Zhou

Reservation System Problem (Sept 27, 2013)

There have been occasional problems with the online reservation system, likely due to problems in the DB. Please report the problems ASAP to me if you cannot make reservation.

Please follow reservation rules (August 16, 2013)

It's been reported that some users reserve a lot of instrument time but do not show up or only use a small portion of it. Please do not reserve more than what you need and always cancel unused time. Charges of doubling the amount of reservation will be applied if a large portion of unused time is not canceled in time.

If a user is late for more than 5 mins for the reserved time, the reserved time is forfeit and another user can use that time slot at his/her discretion. Please report all systematic abuse of instrument time to the Manager.

Project code problem update (July 22, 2013)

Latest: There is still a problem with the nightly DB update script that has made most codes disappear from the DB. This has been fixed manually for now. The script will be dealt with as soon as possible.

The current setup gives a user a few tries for entering a correct code, but does not force the user out of the system if the code is incorrect. However, the username and time used are logged.

Project Code Database Updates & Issues (July 19,2013)

As it's been just found out, the project code database that is used for login on the NMR instruments hasn't been updated for a long while although the time stamp appears current. Hopefully, the problem has been fixed.

Due to a few months' lagging in the update, many old codes that you may have been using have expired and cannot be used anymore. If this happens to you, please talk to your group leader about the new codes you should use and have you authorized to use these codes.

High-temp VT Issues (July 10,2013)

High-temperature VT operation on NMR500 has some issues both on the software and hardware sides. I have added an on-screen message which is displayed once vnmrJ window opens. It displays the current VT status (regulated or not) and temperature. The normal status is NOT regulated (simply taking input air) and the message is in green. If VT is regulated, sometimes left as is by the previous user, the message is displayed in red.

The issue is being examined. All users who do VT experiments must request training first.

NMR400 broadband probe contaminated (April 30, 2013)

Update: The probe has been cleaned up and the strong contaminant peak between 8-10ppm is removed. See earlier notice below.

Earlier: NMR400 is out of service due to probe contamination likely because liquid was spilled into the probe from unknown tube breaking accident or some liquid left on the side of an NMR tube was accidentally brought into the probe.

Please make sure to wipe clean the NMR glass tube, particularly the bottom section, before inserting the tube into the instrument.

Also, make sure after you load your sample into the tube, wipe clean the side of the tube and make sure there are no chemicals/liquid/dust on the outer surface.

License for Mnova NMR Sofware (March 27, 2013)

The latest version of Mnova NMR software that is covered by our license is version 8.1.0 (NOT 8.1.1 and any version after 8.1.1). Do not use any version after this one because it is not supported.

To download version 8.1.0, go to the Mnova website here.

Please follow this instruction to activate the licenses you need.

NMR500 Schedule Problem (Jan 10, 2013)

The database seems to be having a problem causing trouble to the 500 signup. For now, all records on the 500 are cleared. Please proceed to sign up online.

Room-temperature probe on NMR600 (Oct 19, 2012)

The cold probe system on NMR600 is broken. A room-temperature HCN probe is installed. The probe is best for 1H detectioin, including 1H-detected 2D NMR.

NMR500 should have better C13 sensitivity with the brodaband probe installed.

NMR600 is down due to sudden loss of cooling water. (Oct 18, 2012)

Compressed air is back. All instruments are OK now. (Aug 22, 2012)

NMR600 cryoprobe status (June 27, 2012)

Cryoprobe on NMR600 unexpectedly warmed up last night. It's cooled down now and is ready for use.

NMR600 is back running (April 20, 2012)

The cryoprobe has been cooled down. Please pay attention to the probe status displayed on the monitor behind the workstation. Do not use the instrument unless the status is "Ready".

EARLIER: NMR600 is down due to an unexpected cryoprobe warmup. The probe is being cooled down. In case that this accelerated cooldown fails, the probe will be fully warmed up and then cooled down again. This cycle takes ~24 hours.

Check the schedule page for the instrument status.

Mnova 7.1.2 update available (April 11, 2012)

Upon my request, the new version allows easier iterative phase correction after baseline correction. Previously, the phase button greys out after baseline correction in an inconsistent manner. Please stay with the normal flow of processing routines, that is, apply phase correction before baseline correction. Only to adjust small phase defects after baseline correction.

Please go to Mnova website here to download the newest software. The program will request to remove the old version from your computer. Simply click OK.

Mnova NMR Software License Activation (January 13, 2012)

We have acquired a perpetual site license for the main Mnova NMR data processing and analysis software. Please follow this instruction to activate the licenses you need. The best way is for each lab to discuss the number of licenses needed and computers to install it. A one-time $40/license charge applies to all new licenses. Existing license holders are offered a one-time free upgrade.

New Data Processing Workstation Available (December 7, 2011)

A new data processing station running Fedora version of Linux is available now. The computer is named rabi (full domain name: rabi.chem.ucsb.edu). The previous computer (nmrserver) has been relocated to my office.

The computer is named to honor the first scientist who discovered NMR phenomenon in 1938, Isidor Isaac Rabi. Rabi was awarded the Nobel Prize in Physics in 1944 for this discovery that also led to laser technology and atomic clock.

Please change the setting in your secure FTP program to connect to rabi.chem.ucsb.edu. FTP access to nmrserver is blocked. All your data on nmrserver have been saved under your home directory on the new computer.

Mnova NMR Software Introduction (December 1, 2011)

Dr. Chen Peng from Mestrenova Research will present an overview of their Mnova NMR software on Monday, Dec 5 from 10AM up to 12PM in PSBN 4606. All users (from both Chem and MRL) are welcome to attend his talk. Seats are limited.

NMR600 Down Due to Power Outage (December 1, 2011)

The cold probe warmed up due to power loss last night. The probe will be cooled down after full warm up completion. It should be available Thursday afternoon.

In the coming days (and the windy days in general), please watch out for power problems that likely will affect all instruments, particularly the cold probe on NMR600.

Detrimental effects of low sample volume on NMR signal (October 28, 2011)

I continue to see some users choose to use a small sample volume in a regular NMR tube. The wishful thinking is that packing more material in a small volume will always lead to better signal-to-noise. The opposite is often true with regular NMR tubes and very low sample volume.

See drastic loss of signal-to-noise and good lineshape as sample volume drops far from 700uL.

NMR600 is available now (October 27, 2011)

The cold probe has been cooled down. The instrument is open now.

Earlier: Due to unexpected cooling water shutdown, the cold probe has been warmed up overnight. It'll be cooled down again after the completion of the repair work. The typical warmup and cooling cycle takes about a day. I expect the instrument to be back online late Thursday afternoon.

Hongjun Zhou (hzhou@chem.ucsb.edu)