TOP TOP

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:

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)

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 slots left so that others can use the instrument.

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)

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.

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)

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.

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: 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)