Department of Chemistry · The University of Arizona
P.O. Box 210041 · 1306 E. University Blvd. · Tucson, Arizona · 85721-0041
phone (520) 621-6354 · fax (520) 621-8407
Nuclear Magnetic Resonance Spectroscopy
The facility is staffed by two Ph.D. Chemists and two graduate student research assistants. The laboratory is equipped with Bruker Avance DRX 600 MHz and 500 MHz spectrometers with the latest technology and capabilities for elucidation of structure and conformation of complex molecules in solution. Both instruments have 3-axis gradients, shaped pulses, 3 RF channels and digital oversampling and filtering. An SGI satellite workstation equipped with Felix and Insight software for processing and analysis of 2D and 3D NMR data is available and can be accessed from any networked PC. For multinuclear and variable-temperature work the Varian Unity 300 MHz is available, and the Bruker AM 250 MHz and Varian Gemini 200 MHz instruments are used for routine samples as well as undergraduate courses. All of the instruments are hands-on, with training provided in the form of intensive workshops and individual instruction as well as a formal graduate-level NMR course. In July, 2003 a new Varian Inova 600 will be installed, equipped for biological NMR and with an ultra-sensitive cryogenic probe. We are currently applying for funds to replace our Bruker AM-250 instrument with a new 400 MHz or used 500 MHz instrument.
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Electron Paramagnetic Resonance Spectroscopy
The Electron Paramagnetic Resonance Spectroscopy (EPR) Facility is equipped with a Bruker ESP-300E continuous wave X-band EPR spectrometer and three homebuilt broadband pulsed EPR spectrometers continuously covering the microwave frequency ranges from 2 to 18 GHz and from 26 to 40 GHz. The pulsed spectrometers represent unique high-power instruments suitable for all kinds of pulsed EPR applications, including fast reaction kinetics measurements and investigations of electronic and chemical structure of paramagnetic centers by electron spin echo envelope modulation (ESEEM), electron-nuclear double resonance (ENDOR) and electron-electron double resonance (ELDOR) techniques. The pulsed ENDOR accessory operates within the radiofrequency range from 0 to 220 MHz and has an output power of up to 800 W. The cryogenic setup based on Oxford Instruments flow cryostats and temperature controllers allows one to perform experiments at the temperatures as low as 4.2 K (liquid helium). A variety of spectral simulation and data manipulation software packages have been developed for analysis of the data. The facility provides services not only to the Department of Chemistry, but to all users throughout The University of Arizona or from other universities or businesses.
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X-Ray Crystallography
The X-ray diffraction facility is part of the Department of Chemistry at The University of Arizona, and provides diffraction service facilities to both the Department of Chemistry and the whole university, as well as collaborations with other users both in the USA and overseas. It is a shared multi-user instrumentation facility capable of carrying out experimental work on single-crystal and powder samples of chemical compounds for the purpose of determining molecular structure in the solid-state.
We currently have two instruments. For single-crystal work we have a Bruker SMART 1000 CCD detector, and for powder diffraction and thin-film studies we have a Philips X'Pert MPD diffractometer. Single-crystal work is routinely carried out at low temperature using an Oxford Cryosystems Cryostream low temperature device. Air, temperature and light-sensitive structures can be handled quite easily.
We offer both full structure and data collection-only services. In addition, trained users may carry out their own crystal mounting, data collection and subsequent structural analysis; hands-on use of the facility is strongly encouraged. Although housed within, and primarily serving. the Department of Chemistry we are open to users from throughout the university. Access to the Cambridge Structural Database is also available and full training can be given in searching the CSD effectively.
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Electron Spectroscopy and Surface Analysis
The Laboratory for Electron Spectroscopy and Surface Analysis (LESSA) offers a unique multi-technique surface analysis spectrometer for the study of solid surfaces using X-ray photoelectron spectroscopy, Auger electron spectroscopy and ultraviolet photoelectron spectroscopy, all under ultra-high vacuum conditions. The spectrometer is coupled with several different custom-designed vacuum systems used for the study of catalytical, electrochemical systems and materials fabrication.
The facility is open to all students for the study of thin films in such applications as solar energy, conversion chemical sensors, optical logic, and chemical reactions inducing corrosion and catalysis. Managed by a Staff Scientist in Surface Science, this is a facility unique to most chemistry departments in the country.
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Gas Phase Photoelectron Spectroscopy Laboratory
The Gas-phase Photoelectron Spectroscopy Laboratory (PES) is the country's only service facility for electronic structure studies by high-resolution, gas-phase photoelectron spectroscopy. Personnel include the facility manager, Dr. Nadine Gruhn, and a graduate research assistant. Spectra can be collected on a service basis, or students may perform their own data collection and analysis.
Photoelectron spectroscopy measures the ionization energies of molecules when electrons are ejected from different orbitals, and thus can be used to infer orbital energies. Experimental information can also be gathered on the geometry changes and reorganization energy that accompany ionization, as well as the bonding nature, atomic character, and delocalization of molecular orbitals. These measurements also serve as the principle benchmark for electronic structure calculations.
Instrumentation in the PES Facility includes two photoelectron spectrometers, each with a 36-cm hemispherical electron-kinetic-energy analyzer and custom-designed sample entry, ionization sources, and detection and control electronics. Experimental techniques have been developed that allow manipulation of samples that are extremely air, moisture, light, and thermally sensitive. Sample entry and sublimation areas have been customized so that samples with sublimation temperatures up to 500°C can be analyzed.
As the only site in the United States that currently has capabilities for gas-phase photoelectron spectroscopy of large neutral molecules, the Facility has a strong commitment to collaborative research efforts with external researchers. In recent years Facility staff has collaborated with over 50 domestic and international research groups.
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Proteomics
The Arizona Proteomics Consortium provides state of the art protein analysis for researchers at the University of Arizona. Officially organized in January 2006 from previously existing entities, it is supported by the Arizona Cancer Center, Arizona Research Laboratories, BIO5, the Department of Chemistry and Southwest Environmental Health Sciences Center (SWEHSC). Currently, the Proteomics Laboratories are housed in the College of Pharmacy, the Department of Biochemistry and Molecular Biophysics and in Chemistry; with the main Laboratory scheduled to move to the new BIO5 (Keating) Building in late Fall, 2006. Services provided by the Arizona Proteomics Consortium include analysis of whole proteins by MALDI/TOF, separation of protein mixtures by 1-D and 2-D gel electrophoresis followed by nano-HPLC-MS/MS, protein separation and analysis by nano-LC/LC-MS/MS (MUDPIT), albumin depletion of serum samples, and difference protein analysis by differential in-gel electrophoresis (DIGE). Assistance with experimental design and training of researchers in this growing technology are provided by the Director, George Tsaprailis and Associate Director, Linda Breci along with a staff of one post-doctoral associate, three Research Specialists, and one Senior Staff Engineer.
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Computing & Graphics Facility
The Computer and Graphics Facility (CGF) is available to students so that they may analyze chemical systems via semi-empirical and ab initio methods. Available hardware includes SGI workstations and IBM RS/6000 computational servers. Access to university supercomputers is provided via the departmental network. Main titles in the facility's software library include MacroModel, Jaguar, Spartan, Gaussian, ADF, Cerius2, and the Cambridge Structural Database.
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Mass Spectrometry
The Mass Spectrometry Facility The Mass Spectrometry Facility provides state-of-the-art support (teaching and research) in Mass Spectrometry campuswide and for the local community. The MS Facility is extensively involved in national and international research collaborations which helps to enhance national reputation of U of A in Analytical Chemistry. Three permanent staff scientists operate the facility. They are joined with 2 or 3 graduate students with a year by year appointment. The mass spectrometric and analytical services include molecular weight determinations, structure elucidations, and qualitative and quantitative analyses of organic and bio-organic compounds. Instrumentation includes a Hewlett-Packard GC/MS system, a Varian GC/MS instrument, a JEOL HX110A high resolution magnetic sector instrument equipped with a home made TOF analyzer for MS/MS (CID and SID) measurements, a Finnigan LCQ HPLC/MS system, a Bruker Reflex III MALDI-TOF instrument, and a recently installed IonSpec FT-MS 4.7 T instrument. Services provided include EI, CI, FAB, ESI and MALDI ionization techniques. Currently, the JEOL HX110A, the Bruker MALDI-TOF, and the IonSpec FT-MS instruments are the only high resolution instruments on campus and in Southern Arizona. They are mainly used for accurate mass measurements (elemental analysis). Molecular weight determination of relatively large biomolecules (e.g., proteins) and peptide/protein sequencing are performed mostly on the Finnigan LCQ HPLC/MS system. The Bruker MALDI-TOF instrument also provides the capabilities for the analysis of synthetic polymers and large biomolecules, as well as accurate mass (high resolution) measurements for compounds up to ca. 6,000-7,000 u. The IonSpec FT-MS instrument is used for delicated structural analyses, i.e., when ultrahigh resolution (e.g., 500,000) and mass accuracy (< 5 ppm) are required.
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Chemical Synthesis Facility
The Chemical Synthesis Facility is a research support facility established to provide chemical synthesis expertise to the Department and to the University community. This facility is equipped to prepare compounds for use as test articles or synthetic intermediates. The facility has the capabilities to perform multi-step organic synthesis, chromatographic separations and chemical purification for research groups lacking resources for these needs. The chemical synthesis facility is staffed by a Ph.D. chemist. This facility is located in CSML 538.
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Equipment Shops
The Electronics Shop is staffed by a full-time electrical engineer and a technician, experienced in the design and adaptation of electronic equipment for academic studies.
The Machine Shop's instrument maker is also at the service of faculty and students. A non-credit course is offered and a student machine shop is open 24 hours a day for work on individual projects.
The Glass Shop is staffed by a a master glassblower, the highest ranking obtainable. He is available for the design and production of special glassware for anyone in the Department.
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