Hello all -

"Paris", the walkup 500 MHz NMR in the basement of Malott, is now operational.  We have replaced the high band amplifier and the instrument is meeting or exceeding performance specifications.  

Because there is a new amplifier the pulse widths and powers have changed.  In some cases, the powers have changed by a large amount.  It is very important the user do not "clone" old experiments and rerun with the same parameters.  Instead please be sure to load the experiment from the list of approved experiments and type 'getprosol' at the command line to read in new acquisition parameters.

If you have any questions, please contact me or Sarah.

Justin

NMRs in Malott B042 down until further notice ...

NMR lab users,

Presently, there is a lot of water in the compressed air lines in Malott Hall.  Since the NMRs use compressed air for VT, eject and spin air, as well as to drive the autosampler, I have to shut down the instruments until this issue can be addressed.  I have no estimate when these instrument will be available again. 

I will look into a work around for Siena (500 MHz NMR with cryoprobe) if it looks like it will take more than a day or so.

Sorry for the inconvenience,

Justin

Winter 2014

Hello all,

It has been a while since my last post.  A lot has happened in the last couple of months. 

#1) The great flood of 2014

On Sunday May 2, 2014 there was a great snowstorm in Lawrence, KS.  It was so cold I kept my faucets dripping in the house to avoid frozen pipes.  It wasn't the first time this winter, nor was it the coldest night of the winter.  It was icy and snowy, though.   For reasons that I do not understand, two pipe burst in SBC. 

Below is a picture taken by me of the office of my friend.  His office was the epicenter of the 2nd pipe bursting around 1 PM that day.  (By the way, I did not rush in to help, because by this time ServPro was on the scene.  I was trying to batten down the hatches in the NMR lab and stay out of the way).  ServPro and FO guys were right there, so the water got shut off mighty quick.  I show you this picture first so that you can imagine how several HOURS of water leak would appear. 

Apparently, the first pipe burst sometime in the early morning and ~1 inch of water filled up the floor of almost all of the instrument labs in SBC.  The building manager was first on the scene and immediately called a high-ranking University official, who was there in a flash to help out.  Kudos to him for being so hands-on.  I don't know who called the Mass Spec facility director, but he then called me and I got there as soon as possible. 

In the meantime, the building manager, high-ranking University official, Mass Spec facility director and two FO technicians triaged the whole building.  The turned off all instruments and tried to move water towards floor drains.  I was very impressed.  ServPro was there when I arrived with industrial strength suction and big bad fans to dry everything.  Things were looking good before we discovered the 2nd leak (see picture above).

With the NMRs already off there wasn't much I could do.  The floor in the lab were mostly dry by the time I go in.  I brought in some wood to prop all cables off the ground and moved everything to the center of the lab.  I feared maintenance guys near the magnet more than anything, so I put up big signs.   Anyways, we were without NMR for a couple of days.  Big fans dried the sheet rock to prevent mold.  Both NMRs fired up and we felt like we dodged a bullet.  I guess there is an important lesson about clearance on the floor in case of water. 

#2) Mysterious shim troubles

On March 12, 2014, the shims on Florence went for excellent to lousy.  This instrument is usually very robust and the shims do not need to be adjusted that much from day-to-day or month-to-month.  Suddenly and without warning the shims were so bad that I could not get close to line shape specification.  I don't know why.  I had to shut down the instrument for a couple of days.

We don't have a hypothesis why the shims got all drifty after years of stability.  One observation, and I don't know if it is relevant, is that over the winter we had a few days where the temperature in the NMR room went higher than we'd like (~27 C).  It has to do with balance the AC and heat in the winter months, particularly on warm weekends.  Good users altered me to the heat and I got in to shut down the system and/or open windows to cool the room.

Anyways, a couple of days of diligent shimming and we can make line shape spec again.

****


A hard winter.  Let's hope spring is easier.

New Probe

Twas the day after the day after Christmas and all through the lab,
Justin's cheer could be heard and they were not drab.
Our new probe had arrived so shiny and bright,
too bad the flush gas valve was busted, out of sight.

Yosemite back up ...

Hello all,

This message is critical for West Campus NMR users (Malott users can probably ignore it) ....
As some of you may know, "Yosemite", the open access 400 MHz NMR in SBC 1004, has been unavailable since mid-November due to a fried motherboard on the workstation (computer) operating the instrument.  A new computer has been purchased, configured and deployed. Yosemite is now available for all trained users.  (See http://nmrlab.ku.edu/user-training if you need training for this instrument.)

Unfortunately, there are a few hoops to jump through.

#1) Log in with your username and password.  The password should be the exact same password you use on other instruments in the NMR lab and the old workstation for Yosemite.

WARNING – I had to enter all the passwords by hand, so it is possible that I typed your password incorrectly.  If you cannot get access to your account, please let me or Sarah know and we can check the password.

#2) When you log in for the first time you’ll see a pop-up window.  Click the “Ignore” button on the bottom left.  You’ll have to do this two or three times.

 

#3) Follow the normal checklist to acquire NMR data.  When you type “edc” be sure to enter YOUR USERNAME (the same one with which you logged onto the workstation) in the box that says USER. 

Attached is a PDF of these instructions with pictures.  Also see http://nmrlab.ku.edu/ - there is a link on the home page and in the Documents tab under Resources.  There is also a copy attached to the monitor of the new workstation.

Please see Sarah or myself if you have any questions regarding access.

Two more issues:

#1) Data access. 

The new workstation should be configured as a SAMBA server, allowing access to any computer with a KU IP address (or on the KU VPN).  See http://nmrlab.ku.edu/how-access-data for instructions.  I was able to synchronize the data drive between the new and old workstation, hence there should be zero data loss.  Nevertheless, this computer failure is an excellent opportunity for groups to review their data backup plans!

#2) SCC NMR access

Jeff Aube and his group were kind enough to offer access to the SCC 400 MHz NMR in SBC 1004 ("BigSur") while Yosemite was down.  Since Yosemite is now available, access to BigSur will now be limited to the group of Professor Aube.  I'll leave the temporary user accounts open for a couple of days as people transition back to Yosemite, but expect them gone by next week.

In conclusion, Sarah and I thank you for your patience and understanding while Yosemite was down.  Obviously, we'd hoped to have the instrument available sooner, but the configuration and data transfer steps were a bit more complicated than expected.

Let us know if you have any questions.

Justin

NMR Users,

This message is critical for West Campus NMR users (Malott users can probably ignore it) ....

As some of you have noticed and reported there have been errors on Yosemite (the open access 400 MHz NMR in SBC 1004).  The motherboard of the workstation (computer) operating this instrument is fried, meaning that we will have to purchase a new computer and configure it to work with the instrument.  This task will be a priority for us, but it will take time.  Fortunately, Jeff Aube has agreed to allow 1D 1H on his instrument ("BigSur2") which shares the room with Yosemite. 

SO - If you are a trained Yosemite user who needs access to BigSur2, there is mandatory training/account set up.  Rather than trying to make appointment I will be in SBC 1004 on Thursday 11/14 from 10-11:30 AM and 2:30-4 PM and Monday 11/18 from 10-11:30 AM and 2:30-4 PM.  I will meet with any trained Yosemite users, either individually or in small groups of 2-4.  I'll make accounts on BigSur for you and show you how to collect 1D 1Hs.  I'll also explain the access rules for non-CMLD/SCC users and encourage you to use our sample courier service to the cryoprobe in Malott for your 13C NMR.  It should take less than 15 minutes. 

The other major issue is access to old data.  I sent an email on listproc with detailed instructions regarding our work-around to get access to old data.  Contact me if you did not get that email or have questions.


In conclusion, Sarah and I appreciate your patience and understanding as we work through this issue.  Hopefully our work-around will suffice for the time being and not inconvenience you too much.

As always, let me know if you have questions, concerns or comments.

Justin

People may have notice that Paris, the walk up 500 MHz NMR in Malott B042, has been out of commission for a couple of days.  I have been working on the shims.  There were several problems.  First of all, the temperature of the sample in the probe was higher than room temperature even when the VT heater is off.  Setting all the shims to zero and letting the instrument sit overnight results in the temperature falling to 22 C.  Ah ha.  The shims, which are just electromagnets, are heating up the sample.  If you are wondering why the shims are producing so much heat, my only guess is that I (or more correctly, we) have slowly and steadily over many years configured our shims with too much current.  Since we can make lineshape (or at least get pretty close) I can only guess that we must be really lucky and able to compensate for one high order shim being too high with another high order shim.

At any rate, I set all the shims to zero and shimmed the magnet from scratch.  I also made an adjustment to the shim stack.  (There was a loose nut and we moved it a couple of years ago.  I was able to correct for this movement, but I wanted to make sure the nuts were tight and would not move again.  Mission accomplished!).  I have melted my brain shimming - fortunately I can get baseball gameday audio on my phone.  Shims look good.  Temperature looks good.  Temperature calibration looks good.  I just need to make new 2H shim maps and check pulse calibrations.  Instrument should be available to all tomorrow.

J