Reserach Support Services

Instrumentation

The NMR facility manages six superconducting pulsed Fourier-transform NMR instruments with proton frequencies of 600, 600, 500, 400, 300 and 200 MHz. For NMR satellite data processing and data storage we have a Quad-core Gateway 9515 Linux dataserver and compute engine running the Felix and XwinNMR software packages. We have a campus-wide site license for the MestReNova data processing package, and an SGI Octane workstation for molecular modeling and NMR-based structure calculation using the InsightII software package.

  1. Varian Inova 600 (installed in September, 2003) with cryogenic probe (installed in June, 2005)
  2. Bruker DRX-600 with triple-resonance, shaped pulse and 3-axis gradient capabilities (installed August, 1999)
  3. Bruker DRX-500 with triple-resonance, shaped pulse and 3-axis gradient capabilities (installed January, 1999)
  4. Varian Unity-300 (installed in 1993) with autosampler and two satellite Sun workstations "ernst" and "bloch"
  5. Bruker AVIII-400 (installed in 2009) with SampleJet automation
  6. Varian Gemini-200 with variable temperature capability (installed in 1993)
  7. Quad-core Gateway 9515 Linux dataserver and compute engine ("UANMR") running the Felix and XwinNMR software

1) Varian Inova 600 for Biological NMR The new Varian 600 was installed in September of 2003 and is fully equipped for biological NMR: Four RF channels, pulsed field gradients and cryogenically-cooled probe. This instrument was purchased with funds from BCMB (Biochemistry and Molecular Biophysics) and BIO5 Institute as part of the start-up funding for two new faculty hires in structural biochemistry: Megan McEvoy and Matt Cordes. The instrument is housed in Old Chemistry and operated by the Chemistry Department NMR Facility. Time is available to all researchers on campus, with priority for BCMB faculty.

Overhead Rail

Overhead rail system and stairs down into the NMR laboratory.

Cryogen tanks are raised with a sliding chain hoist, moved clear of the stairs and lowered to the floor.

 

 

 

 

 

Magnet

Inserting a sample into the actively-shielded 600 MHz Oxford magnet.

 

 

Inova 600 ConsoleThe two-bay console of the Varian Inova-600 with doors open. The RF transmitters (4 channels) are located in the upper right, with digital controllers and waveform generators below. Below this are the two pulse amplifiers and at the bottom is the power supply. On the left side, starting at the top, we have the frequency synthesizers, the acquisition computer, the gradient controller, and the shim and lock unit at the bottom. The air dryer (blue) is mounted on the wall in the background.

2) Bruker DRX-600 Purchased used (3 years old) in 1999 and installed in August of 1999, the Bruker DRX-600 has triple-resonance and triple-axis gradient capabilities.  It has been upgraded to include a fourth channel and 2H transmitter for 2H decoupling, as well as updated software to allow for 3-axis deuterium gradient shimming and easy setup of biological 3D experiments.  This instrument is currently used for small biological molecules such as glycopeptides, particularly in association with micelles.  It is also used for 2D experiments on complex natural products, and the 3 mm 13C probe permits 13C and DEPT on submilligram organic samples, as well as INADEQUATE on biosynthetically labelled samples.

Magnex Shielded 14.1 Telsa Magnet

 The actively-shielded 14.1 Tesla Magnex magnet is equipped with vibration-damping legs (grey).  The stability and resolution of this magnet are "sweet". Users have a choice of three probes: A Bruker TXI 5 mm triple-resonance (HCN) 3-axis gradient probe, a newer Nalorac 5 mm triple-resonance Z-axis gradient probe and a Nalorac 3 mm direct CH probe with Z-axis gradient.  Temperature control of the sample (7oC - 60oC) is provided by a Whatman air dryer, Bruker BCU 05 air chiller and a BVT 3000 controller.

DRX-600a

The Avance DRX console has a 3-axis gradient controller and amplifier, four full RF channels (each equipped with shaped pulse capability), and high power pulse amplifiers for H, X and Y with a 20 W 2H amplifier.   The gradient pre-emphasis unit allows users to balance the gradient amplifiers more conveniently.

3) Bruker DRX-500The Oxford 11.7 Tesla unshielded magnet began its life as part of a Bruker AM-500 spectrometer.  In January of 1999  the console, computer, upper bore tube, room temperature shims and probes were replaced to give the instrument triple-resonance, 3-axis gradient capability. The $330,000 for the upgrade came from an NSF Biological Multi-User Equipment grant, including a 50% match from the University. The DRX-500 has become the workhorse instrument for routine 1H and 13C spectra of organic samples, but is also used for selective 1D experiments (NOE, TOCSY) and 2D experiments (COSY, HSQC, HMBC, TOCSY, ROESY, NOESY). In 2009 the computer was replaced with a Linux workstation running Topspin 1.3 software, and a 2H transmitter board was added to allow automated 2H gradient shimming. A new probe (5 mm Bruker BBO Z-gradient) was added for direct-detect broadband (15N to 31P) applications.

 

Bruker DRX-500 MagnetThe unshielded Oxford 11.7 Tesla magnet is equipped with inflated-tire vibration dampers.  In addition to the new BBO probe, we have two 3-axis gradient probes:  Nalorac 5 mm inverse HCN and Nalorac 5 mm inverse broadband HX probe.   Temperature control of the sample (7oC - 60oC) is provided by a Whatman air dryer, Bruker BCU 05 air chiller and a BVT 2000 controller.  The magnet drifts down and requires lowering the 1H frequency by 100 kHz every 18 months.

DRX-500 Console

The Avance DRX console has a 3-axis gradient controller and amplifier, a third (X nucleus) channel pulse amplifier and three full RF channels, each equipped with shaped pulse capability.  The Digital Quadrature Detection (DQD) capability eliminates F2 artifacts in fast 2D experiments on concentrated samples.

4) Bruker AVIII-400 The Bruker AVIII-400 was installed in November, 2009. It is equipped with a BBOF (Broadband 5mm Direct Z-Gradient) Probe and a BBI (Broadband 5mm Inverse Z-Gradient) Probe. The BBOF probe is tuneable to 19F on the broadband coil. The SampleJet autosampler is a revolutionary new concept: The NMR sample is picked up by its cap and inserted into a "shuttle" which grips the sample at the top of the bore and carries it into the magnet. Only a single shuttle is used, with capacity for 480 course samples (in 4 inch tubes in 5 racks of 96 tubes each) and an additional 96 research samples (in 7 inch tubes, hung on slots around the edge of the carrousel). Operation of the instrument is fully automated, using ICON-NMR software and automatic lock, tune/match and 2H gradient shimming. Fast experiments go into the day queue and longer experiments are deferred to nights and weekends. Data are deposited as zip files on a website, where they can be picked up by the users and processed using MestReNova software. We have a permanent campus-wide license for this user-friendly package running on Windows, Linux and Mac platforms.

Bruker AVIII-400

The AVIII-400 also has a solid-state capability, with basic CP-MAS and top-loading rotors. Solid-state experiments will be run at night or on weekends and should not interfere with the automation queue. The magnet is ultrashielded with a 1 meter radius 5 G limit. The instrument is installed in a large room with space for an "NMR classroom". This will include seating for 24 students, projector and screen, and webcam to show the operation of the autosampler.AVIII-400 NMR:

Bruker Ultrashield 9.4 Tesla magnet with TMC anti-vibration legs (background), SampleJet autosampler (top), microbay console (right) and Linux workstation (left), shown with (left to right) Dr. Guangxin Lin, Bryan Korth and Dr. Neil Jacobsen.

5) Varian Unity-300   The Varian Unity-300 was installed in 1993. It is equipped with a 4-nucleus (1H, 19F, 13C, 31P) direct probe and a broadband inverse probe. In 2002 we upgraded the Sun computers and the VNMR software for the Unity-300 and its satellite stations. The two satellite data processing stations (Bloch and Ernst) are SunBlade 100's with large monitors, and the spectrometer itself (Unity300) is operated by an Ultra-10 with a color LCD monitor. Variable-temperature work is very convenient, with both the standard heat-exchanger / bucket setup and a larger N2 (liq.) dewar with heat exchanger for overnight low temperature runs.  A 160 L N2(liq.) pressure-building tank in the adjacent room provides dry N2 gas for low temperature operation. Preferred applications include low temperature, fast multinuclear and routine 1H and 13C of organic samples.

 

Unity-300 Magnet

Oxford 7.05 Tesla magnet with "magnet leg" to the left, heat exchanger bucket underneath and large N2 dewar on the right behind\

Unity-300 ConsoleUnity-300 Console with two bays and variable temperature controller in the upper right. Two broadband channels make hardware changes unnecessary when changing from direct to inverse experiments

6) Varian Gemini-200  The Varian Gemini-200 was purchased in 1993 with funds earmarked for undergraduate education.  The instrument is used for demonstrations for each section of the organic chemistry course, and using the AVIII-400 SampleJet autosampler each student receives a 1H spectrum of his or her sample from the laboratory course for each experiment. Chemistry majors are all trained in hands-on use and receive a "driver's license" to operate the instrument independently in the Chemistry 412, 446 and 447 courses. The variable temperature unit is used to study dynamic behavior and paramagnetic shifts in the range of 20-100oC.

Gemini Console

The Gemini-200 console, with an oscilloscope and speakers on top, used for undergraduate demonstrations.

Gemini-200 MagnetThe "R2D2" magnet with the robot sample changer (now moved to the Unity-300) to its right.

7) UANMR - The Campus-Wide /k.uvcNMR Data Processing Server  The "nerve center" ofhe NMR Facility is the Quad-core Gateway 9515 Linux dataserver and compute engine ("uanmr") running the Felix and XwinNMR software packages. NMR users can also download the MestReNova data processing package using our perpetual campus-wide license. The Inova-600, DRX-600, DRX-500 and Unity-300 data disks are remotely mounted on UANMR so that data processing using either the Bruker software package XWinNMR or the third-party package Felix is no different from processing data on the instruments. UANMR can also be used remotely by any PC on campus using the eXcursion PC software, and spectra can be remotely printed.  The shell scripts "drx2felix1d", "drx2felix2d", "unity2felix1d", "unity2felix2d, "inova2felix1d and "inova2felix2d" allow simple conversion of Bruker or Varian data to Felix format and automatic construction of Felix macros for 1D and 2D data processing.  UANMR also operates the NMR reservation system, a text-based program for making and cancelling NMR reservations remotely using a secure shell login.  Data on UANMR and the remotely mounted disks are backed up on an array disk system on another server once a week. An older server ("samson") is an SGI Octane workstation with the Insight II software package for molecular modeling and NMR-based structure calculation.