Research Instrumentation Facility Instruments

The Bruker Avance III-HD 700 MHz spectrometer features a quadrupole resonance QCI-P cryoprobe (¹H, ¹³C, ¹⁵N, ³¹P with ²H lock and decoupling) and a SampleJet automated sample changer.

This spectrometer, installed in December 2013, greatly increases sensitivity for metabolomics research and supports fundamental studies in such broad areas as chemical synthesis, molecular evolution, signaling pathways, metabolism and other cellular processes.

The 700 MHz Avance III-HD NMR runs Topspin 3.6.2, which allows for non-uniform data sampling (NUS) with improvements in sensitivity in 2D and 3D data sets. NUS dramatically decreases experimental time for multidimensional NMR experiments. A complete set of standard triple-resonance NMR experiments used to assign a protein structure that would normally require weeks of dedicated NMR instrument time is reduced to a single day with the new instrument. NOAH experiments are also available for faster acquisition of data.

The SampleJet automated sample changer can accommodate over 500 NMR samples for HTS (high throughput screening). Additionally, an internal NMR thermometer that directly and continuously measures the actual sample temperature in real time is available.

Location: 836 Hamilton Hall

References:

Poudel, R., Bhinderwala, F., Morton, M., Powers, R., Rose, D. J. “Metabolic profiling of historical and modern wheat cultivars using proton nuclear magnetic resonance spectroscopy” Scientific Reports, 2021, 11, 3080

Lingjun, Y., Du, F., Chen, X., Zheng, Y., Morton, M., Liu, F., Du, L. “Identification of the Biosynthetic Gene Cluster for the anti-{MRSA} Lysocins through Gene Cluster Activation Using Strong Promoters of Housekeeping Genes and Production of New Analogs in Lysobacter sp. 3655.” Synthetic Biology, 2020, 9(8), 1989-1997, DOI 10.1021/acssynbio.0c00067.

Bhinderwala, F., Evans, P., Jones, K., Laws, B.R., Smith, T.G., Morton, M., Power, R., ”Phosphorus NMR and Its Application to Metabolomics,” Analytical Chemistry, 2020, DOI: 10.1021/acs.analchem.0c00591.

The 600 MHz NMR system was upgraded to a new Bruker NEO console with a 5 mm triple resonance TCI-H/F cryoprobe and a 3.2 mm solid state H/X probe (September 2020). The addition of this cryoprobe (¹H/¹⁹F, ¹³C, ¹⁵N with ²H lock and decoupling) greatly increases the sensitivity of this system, giving it sensitivity comparable to that of the 700 MHz NMR system.

The 24-place SampleCase can be cooled to accommodate automated analysis of temperature sensitive samples. In addition, the SampleCase can be used with practically any tube that will fit into a spinner—no special caps required. It works with Shigemi tubes, too!

This instrument also has a 3.2 mm H/X Solid State NMR probe to serve the solid-state needs of users.

Location: 32 Hamilton Hall

References

Patel, S.M., Smith, T.G., Morton, M, Stiers, K.M., Seravalli, J., Mayclin, S.J., Edwards, T.E., Tanner, J.J., Becker, D.F. “Cautionary Tale of Using Tris(alkyl)phosphine Reducing Agents with NAD+-Dependent Enzymes.” Biochemistry, 2020,.59(36), 3285-3289, DOI 10.1021/acs.biochem.0c00490. PubMed PMID: 32841567.

The 400 MHz NMR is our most active walk-up system meeting the sample analysis needs of many of the synthetic organic research groups. The console was replaced in December 2012. It has a BBOF probe with an ATM (automated Tuning and Matching Accessory). This upgrade automated many routine commands and makes acquiring 2D and variable temperature NMR easy.

Location: 836 Hamilton Hall

References

Chakrabarty, S. Palencia, H., Morton, M. D., Carr, R. O., Takacs*, J. M. “Facile access to functionalized chiral secondary benzylic boronic esters via catalytic asymmetric hydroboration,” Chemical Science, 2019, 10:18, 4854-4861, DOI 10.1039/c8sc05613g

The 300 MHz NMR is a walk-up system meeting the sample analysis needs of many of the undergraduates and synthetic organic research groups. The console was replaced in May 2014. It has a BBOF probe with an ATM (automated Tuning and Matching Accessory). This makes acquiring 2D and variable temperature NMR easy. The system has a SampleExpress sample changer with 60 places. Undergrads can submit samples to the sample changer for NMR data for many undergraduate laboratory classes. Other users can use ICONNMR to automate acquisition. The instrument is jointly shared between the Research Instrumentation Facility and the UIC. Reservations for the system can be made online.

Location: 313 Hamilton Hall

References

Haghshenas, H., Kim, Y.-R.. Morton, M., Smith, T., Khedmati, M., Haghshenas, D., “Effects of Softening Additives on the Moisture Susceptibility of Recycled Bituminous Materials Using Chemical-Mechanical-Imaging Methods”, Journal of Materials in Civil Engineering, 2018, 30(9), 04018207.

This GC-MS is shared between the undergraduate and graduate research facilities. It has an autosampler that can hold up to 108 samples for automated acquisitions. The observable mass range is up to 1050, with unit mass resolution. It can be operated in either the EI or CI mode. An EI-only NIST library is available on the computer. This system is web enabled and can load the data to UNL's Blackboard site.

This GC-MS is located in 414 Hamilton Hall.

The STA is a simultaneous thermal analyzer which allows users to obtain TGA and DSC data. The temperature range is from 20°C through 1000°C. The system is operated under computer control to allow for programming of temperature profiles. Samples can be heated under nitrogen or air. Other purge gases are possible upon request. Approximately 10 to 20 mg of sample is the standard size for analysis.

This Zeiss EVO MA10 Scanning Electron Microscope allows students to looks at materials and detect elements on the surface of the samples by XRay Dispersion Spectroscopy.

The NMR acquisition software is installed on several workstations as well for offline data analysis. Each workstation is equipped with the full Microsoft Office suite for data processing and document editing and Adobe Acrobat for saving documents as PDF files.

• Two Dell Windows based workstations with Bruker TOPSPIN software for offline data processing
• Additional Windows based computers for literature searching and text editing
• Black and white and color printing
• FTP host for facilities data storage and back up