Happy Holidays

Hi All,

It has been a while since my last blog post, so apologies to our many loyal readers :).

The fall semester was productive and fun. I hope the spring semester will be fruitful, as well. In the interim the K-INBRE symposium (http://www.kumc.edu/kinbre/) will be held in the Plaza in KCMO on 1/14/12. Sarah and I will both be presenting posters. It is a fun event for biomedical researchers from all over the state of Kansas. It is especially nice to interact with colleagues from Pittsburg, Hayes, Emporia and Topeka. The undergraduate researchers at these institutions always present some great work. I recommend it if you are in the area.

Finally, just a reminder that the NMR lab IS open for business through the "break". We'll even load samples on Siena every day EXCEPT December 24th through 26th and December 31st through January 2nd.

Have a happy holiday and enjoy your break.

Justin

500s in Malott B042

Hi all,

Two quick notes.

#1) Paris, the walk-up 500 MHz NMR in Malott B042, is back in service and ready for everyday use. The standard broadband probe is installed, so this instrument should give good results for 1H and 13C. With special training, you can retune this instrument for practically any other nuclei. Also, this probe is capable of high and low T NMR. If you have any questions please see me or Sarah.

#2) Siena, the 500 MHz NMR in Malott B042 with a cryoprobe, is down for the next couple of days for annual maintenance. This is necessary to change the pumps and filters that keep this instrument running. We hope that it will be available on Monday.

Regards,

Justin

TXI probe still in Paris

Hi All,

A couple of points:

I understand that losing access to Paris (the 500 MHz NMR in Malott B042) inconveniences the post-docs and students in Malott and we will get the BBO probe back into the instrument as soon as possible. In the meantime, please use the reserve software to book time on Florence (the 400 in 3002). There is amble time available on this instrument and we should all be able to acquire whatever data we need to progress in our research.

In additional news, it is "EAB" season at KU. COBRE and CMLD both have EABs this month. Although our lab is not reviewed during these processes, I believe that now is a good time to take stock of what we do well and what we could improve on. So Sarah and I will conduct a "self-EAB" assessment. I'm not sure that we'll ever present the results publicly, but if you are interested in knowing what we decide please contact me. Also if you'd like to add any feedback, please let me or Sarah know.

Finally, there was an interesting op-ed piece on NPR this week saying "Thank You" to our represented leaders (and our citizens) for continuing to fund science (http://www.npr.org/blogs/13.7/2011/09/08/140284902/a-scientist-s-gratitude).

J

TXI probe in Paris

Since most of the synthetic chemists are gallivanting around Denver for the ACS meeting, I decided to put the TXI probe in Paris. This probe gets much better sensitivity for 1H detected experiments (like the HSQC) at the expense of less sensitivity for 13C (or other heteronuclei) detected experiments. So Friday afternoon I swapped the probes. I've noticed that I always have a trickier time getting Paris shimmed back into spec than any other instrument. Fortunately, I took advantage of some computer aided shimming and was acquiring data by Saturday night. So far it looks good. I'll probably leave this probe in the instrument for a couple of weeks so that I can collect some spectra on a sample in 90% H2O/10% D2O for a client. Turns out I get better water suppression with the TXI probe than the BBO probe.

With the start of the semester, the ACS meeting and a holiday next Monday, this week seemed like a perfect time to play these games.

J

EPR Lab processing station

EPR Users -

I wanted to take a moment and inform everyone about our new EPR processing station in Malott 1002. The computer is adjacent to the EPR workstation (which controls the spectrometer). Both computers share a keyboard, mouse and monitor via a KVM switch, which is just a little black button next to the keyboard. To switch back and forth between the computers, just push the button!

Presently there is generic user "EPR User". If you choose this user from the list, the account should open automatically. I have installed EasySpin (http://www.easyspin.org/), a popular, robust and powerful spectral simulation tool. EasySpin requires MATLAB. Currently we have a 1 month (now 27 day) trial of MATLAB installed.

I would request that everyone who has recorded data on the EPR, please try out the processing station as much as possible over the next 27 days. Before we purchase a license for MATLAB, we would like to assess a) if EasySpin will suit the needs of the KU EPR community; b) if the current computer is powerful enough for our purposes.

I'm working on some documentation to help get started with EasySpin, so stay tuned.

J

Now witness the firepower of this fully ARMED and OPERATIONAL NMR Spectrometer.

Now witness the firepower of this fully ARMED and OPERATIONAL NMR Spectrometer!

I wanted to thank everyone for their patience over the past few weeks while I tinkered with BigSur. This afternoon I put the BBO probe back into the instrument and recalibrated it. With this probe everyone should enjoy higher signal-to-noise on carbon-detected experiments like the 1D 13C, DEPT and APT (although I would be remiss in my duties if I didn't point out that Siena is more than 4x more sensitive than BigSur!)

The reason I had to perturb BigSur was a) replace the workstation; b) diagnose some unsettling problems with 1H sensitivity. The computer was swapped last month. Switching the probes help diagnose a problem with our receiver preamplifier that was introducing extra noise into 1H spectra. Although this noise was minor and I'm certain that no one noticed, we could see it in our standard tests and Sarah and I don't like it when our spectrometers misbehave!

As always let us know if you have any questions,

Justin

Care and Feeding of BigSur

Today is maintenance day on BigSur, the CMLD-SCC NMR. I made two major upgrades:

#1) BigSur has a new workstation. I swapped the old workstation (which had a bad fan) for a brand new computer. As far as I can discern the configurations are the same, however let me know if you notice any odd behavior. The only difference you should be aware of is that you'll need to remap your network drives in order to access your data remotely. I synced the data with the old computer, so if you remap the drive you should be able to continue as if nothing changed.

#2) I swapped the probe. The old (BBO) probe could not be tuned properly on the 1H channel, leading to large(r) pulse widths, low(er) 1H signal-to-noise and less 1H decoupling bandwidth. I put a different probe (called a BBI) in the magnet. This probe will have slightly better 1H sensitivity at the cost of less 13C sensitivity. Hence, I would recommend considering sending any 13C-detected experiments to the cryoprobe via our courier service.

Justin

Happy Birthday Les Mitscher

The KU NMR lab would like to wish a very happy 80th birthday to Professor Les Mitscher. Les is a University Distinguished Professor in the Medicinal Chemistry Department in the School of Pharmacy. Les's research focuses on spectroscopy, synthesis, screening and structure determination primarily of naturally occurring antimicrobial, anticancer and antimutagenic agents, and development of combinatorial methodologies.

To honor Les's contributions there is a symposium today (I call it "LesFest"). The KU NMR Core lab is presenting a poster entitled "qNMR: absolute and relative quantitative NMR," which covers recent work we have done to establish a qNMR protocol at KU.

I finally rearranged the 500 MHz NMR lab in Malott B042. I've wanted to do this since I started at KU, but I procrastinated and procrastinated. It always bugged me that the workstation was in the 5 gauss line. And it bugged me even more that users had to walk behind the console, stepping over all the power, RF and pneumatic cables, to get to the workstation. This new setup just seems more logical and efficient to me.

Let me know if you like it.

Justin

KU EPR lab

The KU NMR lab is excited to announce the addition of a new instrument. Yesterday we completed the installation of a brand new EMXplus Electron Paramagnetic Resonance (EPR) spectrometer. EPR Spectroscopy is used to characterize the structural and physical properties of paramagnetic molecules. Paramagnetic molecules are an important class of molecules of interest to scientists in the fields such as chemistry, physics, biology, materials science, pharmacology, toxicology and medicine. Hence, EPR spectroscopy is an important tool for many researchers across the KU campus and regionally.

Below is a picture of our fearless engineer Jesse Liu with Dominic Leto, a graduate student from the Jackson lab helping with the installation.



Initially we have set the rates at $5/hour for internal users and $8/hour for external users. Consumables such as EPR tubes, solvents, cryogens, etc. are not included and will be charged separately.

Please don't hesitate to let us know if you have any questions about how this new instrument can help your research!

J

Lab cleaning

Recently, I cleaned the lab in SBC. This task included sweeping all the sand and salt off the floors, dusting the countertops, organizing the bookshelves and properly discarding of some abandonded samples.

Please try to keep the lab clean and orderly. And pick up NMR tubes. Refer to NMR lab chemical hygeine plan (http://www.msg.ku.edu/nmr/Documents/ChemicalHygiene.pdf) for details.

Thanks,

Justin

Instruments on West Campus Down for 1.5 hours

Due to air compressor maintenance, the NMRs in SBC will be down from noon to 1:30 PM on Wednesday 2/9/11. We apologize for any inconvenience.

Justin