Step-Into and Step-Return: To debug a method, you need to use "Step-Into" to step into the first statement of the method. ("Step-Over" runs the function in a single step without stepping through the statements within the function.) You could use "Step-Return" to return back to the caller, anywhere within the method. Alternatively, you could set a breakpoint inside a method.
Washed Out - Within and Without (2011).zip
All data on the instruments won't be affected. The software at the user level has few changes. But please plan aheadfor 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 NMRexperiments. It is irresponsible to leave the broken glasses and sample spill in the area withoutproper 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 immediatelyto 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 wastedafter 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 blockedby the booking software during these hours. At present, there is no restriction on reservation byconsecutive 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 forother 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 onlyfor 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 stillhear air hissing but the pressure won't be enough to operate the instrument. Check the air gauges behind the computersfor 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. Allinstruments are connected to a UPS backup power which is on the building E-power line. The UPS has only 10 mins power supply tosupport 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 ifyou 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 stillhear air hissing but the pressure won't be enough to operate the instrument. Check the air gauges behind the computersfor 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, pleaseuse the instruments on a first-come-first-served basis. Make sure to leave a hand-written note ifyou have to walk away from your experiment for a while.Cancel Unused, Leftover Reservation (03/01/2018)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.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. Allmotors 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 valuesshould shift to the right from the old values by roughly +23000 units. Make sure to enter init1hto 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 homogeneityis destroyed, making all resonances (including 2H lock signal) broad, lowering the lock level. The lock recovers duringrecycle 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 withinone 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 beingdiscussed with Agilent Technologies but the order isn't finalized yet. Before the lock channel is fixed, please follow this workaroundto get the lock regulated before your experiment. The key point here is to increase the Z0 value found by Find Z0 by roughly +6700 thenre-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 instrumentto provide backup power to the instrument during power outage and protectthe instrument. Once the instrument is switched to the new UPS, the extension power cables currently runningfrom 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 onactual 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 thisGoFundMe fund raising to support thefamily 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, islimited 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 instrumentworkstation 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 multiplefactors. 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 ifyou 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 untilnormal 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 poweris 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 becauseEject/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 ononce 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 theconsole loses power and comes back, the lock level may be very low or not there at all. If youencounter 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 keygently left and right while pulling it gently. Don't force it which makes things worse ormay 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 toallow 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 cometo 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 ofreserved time slots not actually used. Please keep track of your reserved timeand cancel any 10-minute time slots that you won't use. If noted, all reserved but systematicallywasted 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 hasbeen 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 whenthe instrument isn't being used. These tubes are simply empty tubes. But they keep getting broken frequentlydue 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 withthe 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. Alarge 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 tubeand glasses removed.
NMR600 Receiver Improved (08/18/2017)The 600 has been giving a larger than usual quadrature image & a center glitch peak. The issueisn'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 duringinitial 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 normalbarrel 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'taffect 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 wasshut down but the computer was unable to come back up. It is most likelythe power supply was bad. To keep the instrument running, the computer from the old400 (currently not used) was used for the 500. The 500 is running fine. The old badcomputer will be fixed.In the coming days, there will be a few more sporadic short down periodsfor 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 beopen 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 bedown 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 untilit'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 buildingcompressed 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 forpotential air problems.3:00PM: Compressed air is gone in the building. Do not use any instrument until air is back. Physical Facility has beennotified. 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, butapparently that didn't fix the problem. It is still not cooling. They've been notified. Hopefully, it'll befixed 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 repairedby campus Facility. Before it runs again, the room may be warm. During the daytime hours, the front door andback 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 wasa 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 sentfor 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 reservedtime 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/insertoperation 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 areaaccording 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 dataare 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 settlestoo 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 willhave 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 placedin front of the computer/keynoard to warn others not to use the instrument. The instrument should not be useduntil 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 sampleto 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 beenwashed or dried under very hash condition can break much easier than the rest. Sample spinning on NMR500 puts more strict requirementon tube quality.Please carefully read the proper procedures forwashing and drying NMR tubes in addition to getting quality tubes and trashing very old and scratched ones. Pay attention especially tohow 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 morelicenses. Before new licenses are available in the next few days, you may see an error message when your computer contactsthe 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 notein 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 minsfor air to die down completely after the building compressor is down, and similar amount of time for it to fill the linesto 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 wherethe problem originated. The problem was that sometimes even after a successful reservation, the slots wereleft 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. -- HZSpin 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/Temppanel 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 shortperiod (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 slotsdon'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 seemsto run into issues when multiple users try to book the same timeslots. If the problem stays much longer and cannotbe 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 reservationworks 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'tregulated 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 ifit 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, pleasedo 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 indicatesthere 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 tubeswith 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 thepower. 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 wateraccumulation. But, it will take some days for the water to dry out. We will look for a long-term fix of various issuesin 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 appearsto 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-channelsensitivity.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, thebuilding 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 totallyfixed 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 airhissing 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 sampledoesn't eject or there is no air hissing or only muffled hissing, please stopoperating the instrument. A clear indicator of lost compressed air is low or zero readingof 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 topof 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:' suAdditionally, 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 displayis 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 reaches80-90% 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 processmay 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-nucleuspulse 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 untilfurther 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 bynoting 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 operationof 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 ( 2ff7e9595c
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