It has been a busy couple of weeks.

SMASH 2012 (http://www.smashnmr.org/) was great.  Good to see old friends and make new ones.  Providence was a delight and the talks were smashing (pun intended).  Some highlights include an fascinating comparison of sigma calculation methods to assess diastereomers by Michael Lodewyk, absolute configuration by chiroptics and RDC by Griesinger and FHU qNMR (fuck you, NMR!) by Jonas Buser.  I also enjoyed the entire JBCA sesssion.  I learned more useful things in Chuck Ross's 1 & 1/2 hour "Teaching Mass Spectrometry to NMR Spectroscopists" tutorial than an entire semester course. 

When I returned it was my turn to give a talk at our "What's Hot" symposium.  So overall it was a hot week.

I also returned to find my Haskris peeing pink fluid all over the floor due to a cracked fitting.  That was messy to fix and clean up.
 
Finally, many congratulations to SCC assistant director and KU NMR lab customer extraordinaire Dr. Jennifer Golden for her NCI grant. 

http://www.news.ku.edu/2012/september/18/golden.shtml

Cryoprobe maintenance and HVAC

Yesterday afternoon our Bruker engineer completed the annual cryoprobe maintenance.  The cryoprobe has cooled to operating temperature and is available for use.  Please submit your samples for Siena to the in-rack in Malott B042 or SBC 1004.

Unfortunately, as is the trend this summer, there is an HVAC problem in Malott B042.  The room temperature is creeping up to 85 F, which is the maximum recommended room temperature.  I have shut off the console to Paris to cool the room and will continue to monitor the situation closely.  If the temperature in the NMR room goes above 85 F, I'll have to shut down Siena, as well.  Obviously, I'd like to avoid shutting down this instrument because of the backlog of samples due to annual maintenance. 

I apologize for the inconvenience.

Justin

Too hot to handle

On Saturday afternoon the air conditioning unit on the east side of SBC stopped functioning.  As you can imagine the temperature in all labs and offices on increased rapidly without AC.  The NMR consoles produce a lot of heat and there are several components that are susceptible to damage if this heat is not dissipated.  Hence, I had to shut down both Yosemite and BigSur consoles.  The problem was still not fixed on Sunday afternoon and the temperature in the room had reached 96 F, so I shut down workstations to minimize heat in the room.

Hence there is no access to BigSur or Yosemite at the present time, nor can you get data off of these instruments.  If you need access to data, please check the backup server.  I do not know when these instruments will be available, as the repair of the building AC is beyond my control.

Kudos to Warren for calling me when the temperature of the room started to rise or there could have been catastrophic damage to the consoles of both 400s, the 800 and maybe even a mass spec.

500 w/cryoprobe in Malott

Siena (500 w/cryoprobe in Malott) will be unavailable on Monday August 6th until the morning of Wednesday August 8th because of annual service to the cryoprobe.  We apologize for the interruption in service, however, in order to continue to acquire top quality spectra on this instrument, we must clean, replace, repair and/or service the many vital working parts of this instrument.

You can continue to submit samples for the cryoprobe both at Malott and SBC.  Sarah and I will run them once the instrument is back up on Wednesday.

Please let me know if you have any questions or concerns.

Regards,

Justin

Solid State NMR lab

We are trying to get the word out about a relatively new and unique service here at KU - a regional solid state NMR lab. 

The KU Solid State NMR facility specializes in the analysis of solid materials. Projects come from a wide variety of fields including soils, pharmaceutics, biomass, catalysts, biological materials, organometallics, and inorganics. The lab is equipped with a Bruker Avance III three-channel spectrometer and two probes.

The primary probe is a Multiple Sample Solids probe from Revolution, NMR (Ft. Collins, CO). This probe has four independent circuits in it that can be operated simultaneously. Two of those circuits are equipped with 7 mm spinning modules, one has a 2.5 mm spinning module, and one has a 4 mm spinning system. The 4 mm system has HXY triple resonance capability. The other three circuits are HX circuits. The X and Y channels of all four circuits can work with nuclei ranging from 15N to 31P.

The second probe is a Bruker (Billerica, MA) 4mm two channel (HX) probe. It has variable temperature capabilities from -50 C to + 80 C.

Inquiries regarding use of the facility should be directed to:
Dewey Barich, Solid State NMR Facility
dhbarich@ku.edu
785-864-4719
2095 Constant Ave.
Lawrence, KS 66047

 Also see the website at ...

http://kunmr-suse.msg.ku.edu/ssnmr.html

Yosemite RF issues solved

Late in the afternoon of Thursday April 12th we experienced catastrophic instrument failure on Yosemite, the walk-up 400 MHz NMR in SBC. Without going into too much detail, the problem was that the instrument was not producing the proper frequency radio frequency (RF). As you can imagine incorrect frequencies lead to a myriad of problems with NMR spectroscopy.

Unfortunately, I could not get parts to repair before my trip to ENC (my flight left Saturday morning) so I tried to patch together a work-around, which did not seem to work for anyone. Hence we had no walk-up NMR in SBC the week of 4/15/12. Yikes! My top two priorities upon returning were #1) get a work-around and #2) fix Yosemite. With the gracious help of Frank and Conrad of the SCC and CMLD, respectively, I was able to provide access to displaced Yosemite users on BigSur. To fix Yosemite, I spent a lot of time with the oscilloscope troubleshooting (aka scratching my head saying - "is that the way that output is supposed to look?"). Once I thought I'd isolated the problem I contacted Bruker center but they told me (in essence) "you have to replace your 10 year old fans before we'll send you any board so that you don't burn up our boards!" Then they gave me a quote for the fans ($30/fan) and mounting screws ($1/each) with 2-4 delivery time! Realistically, they probably could have delivered faster, but the price along with the delivery time and a delay in response prompted me to find the fans from a third party. The fans (NMB 4710KL-04W-B50-E00) were easy to find (I got them from newark.com). The mounting screws were tougher. Thanks to the resourceful Geoff Akien from CEBC I found them on Xoxide.com.

An ordering and delivery delay set me back a couple of days, but when I received and installed the fans, I was stunned to see my signal generation unit behaving. I borrowed thermocouples from HotRod Todd Williams in the MS lab and compared the temperature of Yosemite and BigSur. Holy cow, these console produce a lot of heat. It seems that microbay consoles are engineered on the edge (with regards to heat dissipation) and any diminishing cooling power can lead to terrible consequences. Moreover - and I put this as a warning to fellow managers - the fans Bruker will try to sell you are not perfect replacement in terms of air flow. Get the exact same fans or (if your fans are no longer sold) call NMB and make sure you get equivalent fans.

I have the hunch this story is not finished yet, but I've opened Yosemite back up to all trained users. I'll have to keep a close eye on this. Also, I replaced the fans in BigSur in 2009 with fans I bought from Bruker. I'm concerned they have a lesser airflow, which explains my strange problems with the GCU earlier in the spring and last fall.

Keep on precessing.

Justin

Recruitment

The NMR lab welcomes all prospective graduate students for the Departments of Medicinal Chemistry and Chemistry. We hope you enjoy your tour of the lab and please let us know if you have any questions.

Justin

Liquid Helium

This post may sound like me being a curmudgeon, but I'm 100% serious ....

All of the users of KU NMR facility know that NMRs use big magnets. What you may not know is how we get so many tesla from that big thing in the middle of the room. Well, the principle is similar to the electromagnet you played with in 8th grade science. The big difference is that the coil of wire inside the NMR is cooled to ~4 Kelvin (that is -452 F or -269 C, for our Canadian friends). How do we get it so cold? We used liquid helium.

Interestingly enough, terrestrial sources of helium were discovered by chemists at the University of Kansas.

http://www2.ljworld.com/news/2000/apr/16/kansas_celebrates_its/


And the state of Kansas has long been one of the biggest producers of helium. However the supply is running out.

http://www2.ljworld.com/news/2011/oct/29/state-helium-fields-nearly-exhausted/

Simple economics teach us that when supply decreases (or demand increases) price goes up. It is no surprise that helium prices continue to climb.

More distressingly, suppliers can't deliver helium in a timely manner. We ordered 100 L of helium to do fill three magnets this week. Like any volatile liquid, helium evaporates and we have to "refill" the magnets with new helium. I just got word today that we won't have helium until next week. Fortunately, I am aware of these issues and I planned ahead to give myself a cushion.

So, you might ask - why not just turn off the magnet if you don't get helium? Unfortunately, it doesn't work that way. There is no on-or-off button. The magnet is always "on". The only way to turn it "off" is "quench" the magnet. Once you quench a magnet it costs a lot of money (~$20,000) to turn it back "on".

So why am I so cranky? Well our lovely supplier can get plenty of tanks of gaseous helium to the Hyvee grocery store in Lawrence for Valentines Day, but can't get me 100L of liquid helium for my scientific instruments.

http://www2.ljworld.com/news/2012/feb/13/short-supply-helium-not-expected-deflate-valentine/

I hate Valentine's Day.

News for the week and K-INBRE conference

Hello loyal readers. As you might know there was a 4 hour power outage in Malott on Friday morning from ~4 AM to 8 AM. No word on the cause. The consequence is that the cryoprobe warmed up. It is cooling now and should be ready later this afternoon.

Sarah and I will be presenting posters at the K-INBRE symposium (http://www.kumc.edu/kinbre/symposium_info.html) on Saturday in KCMo. Sarah's poster is an update of our "LesFest" and CMLD EAB poster regarding qNMR. My poster summarizes some of the dynamics measurements I recorded for the Rivera group (http://www.chem.ku.edu/groups/rivera_grp/index.shtml). Should be a good time. I'll have to stop by the Classic Cup while I'm in the Plaza (http://www.classiccup.com/).

Justin