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Lab/Instrumentation

Owens Laboratory Facilities

The 1100 square foot Owens Group laboratory is well-equipped for MALDI research. Most MALDI experiments are conducted on a donated commercial Bruker Reflex III reflectron TOFMS system. The standard nitrogen laser on the system has been supplemented with a Continuum, Inc. Minilite I Nd:YAG laser equipped with both 2nd and 3rd harmonic generation crystals. The lab is also home to two custom-built, single-sample at a time linear MALDI TOFMS instruments. Everyday method development as well as routine samples are now run on the Reflex III instrument. Additional laser equipment in the Owens laboratory includes a Lambda Physik LPX105i excimer laser coupled with a Lambda Physik LPD3002 dye laser (with second harmonic generation crystals to cover the wavelength range of 220-900nm), and two Laser Science, Inc. 337ND near-diffraction limited nitrogen lasers. One of the custom-built TOF instruments was designed to allow a single sample to be simultaneously interrogated with both a nitrogen laser and excimer/dye laser beam. Routine laser diagnostic equipment, including fast photodiodes, power meters and beam profilers are also available. Routine MALDI sample storage and preparation equipment such as freezers, micro-centrifuges, speed-vacs, and several electrospray deposition setups, are also available within the laboratory.

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Departmental Facilities

The department maintains a professionally staffed Mass Spectrometry Facility (in Stratton 406) available to all members of the university community. Currently operating instrumentation consists of a Bruker Autoflex III matrix-assisted laser desorption ionization (MALDI) time-of-flight mass spectrometer (TOFMS) (NSF CRIF-MU #0840273), a Thermo-Electron LTQ-FT 7T Fourier-transform ion cyclotron resonance (FT-ICR) spectrometer with both atmospheric pressure chemical ionization (APCI) and electrospray ionization (ESI) sources (due to the He shortage only the LTQ portion of the instrument is operating), and a Waters ZQ single-quadrupole mass spectrometer interfaced with a Waters 2695 high-performance liquid chromatograph (HPLC) with both ESI and APCI capability. Samples may be submitted for analysis or users may be trained in operation of the instruments for use in long-term projects.  The professionally staffed Chemistry Department NMR facility (in Disque 112) is equipped with a 500MHz Varian Unity Inova NMR system with multi-nuclear capability. The probe on the 500 MHz instrument is a cryogenically cooled triple resonance model (1H {13C/15N}) suitable for protein analysis. The Chemistry Department Analytical Instrumentation Laboratories are equipped with the usual array of open-access chemical analysis instrumentation, including: (in Disque 407) a Shimadzu UV-1900 UV/visible absorption spectrometer, a Shimadzu UV-2600 UV/visible absorption spectrometer equipped with a temperature controlled cells, a Shimadzu UV-3600 UV/visible/NIR absorption spectrometer with a 120mm diameter diffuse-reflectance integrating sphere, A Shimadzu Tracer-100 Fourier-transform infrared (FTIR) absorption spectrometer, a Shimadzu AIM-9000 FTIR Microscope system (with different beamsplitters for near- mid- and far-IR capability),a Shimadzu RF-6000 fluorescence spectrophotometer, a Shimadzu Prominence-i LC-2030C 3D Plus HPLC (with both UV-visible diode array and refractive index detectors), a Shimadzu Nexis GC-2030 capillary-column gas chromatograph (GC) equipped w/AOC-20i Plus Auto-injector/AOC-20s Plus Auto-sampler System, a Shimadzu GC-2010+ capillary-column GC Shimadzu GC-MS QP-2020 GC/MS system w/AOC-6000 Autosampler, and a Shimadzu AA7000 flame atomic absorption spectrometer equipped with a GFA-7000A graphite-furnace accessory and a ASC-7000 auto-sampler capable of either macro or micro-sampling (between 5-90 uL of sample required). In the Analytical/Inorganic Teaching Laboratory (in Disque 409), a Perkin-Elmer (PE) Spectrum One FTIR (equipped with a universal diamond ATR and transmission sampling accessories), a PE LS55B Luminescence spectrometer, a PE Lambda-2 UV/visible spectrometer, a BAS Epsilon system, and a UCT Inc., Positive Pressure Manifold (for performing solid phase extraction). The Department Vibrational Spectroscopy Laboratory (in Disque 113) is equipped with a PE Spectrum One FTIR (also  equipped with a universal diamond ATR and transmission sampling accessories) and a Renishaw 1000 Raman Microscope system (equipped with three laser wavelengths: 514.5nm, 632.8nm and 785nm). The Department Microscopy Laboratory (in Stratton 416) is equipped with a Bruker (formerly Veeco Metrology, Inc.), Multimode NanoScope IIId SPM System which performs all major SPM imaging techniques including contact and non-contact atomic force, lateral force, TappingMode (air), magnetic force and electric force microscopy, and a PE Lambda-950 UV/visible/NIR spectrometer equipped with a Labsphere, Inc., 60mm diameter diffuse-reflectance integrating sphere. The Department Polymer Analysis Laboratory (in Disque 210) is equipped with . The Department Organic Instrumentation Laboratory (in PISB 502) is equipped with two PE Clarus 500 capillary-column GCs (one with dual flame ionization detectors (FIDs), the other with one FID and a thermal conductivity detector (TCD)), two PE Spectrum 2 FTIRs, each equipped with a diamond ATR, a PE model 343 polarimeter, a CEM model X microwave synthesis system, and an Anasazi, Inc. EFT-90 90MHz NMR with C and H capability.

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Data Conversion Software:

I've recently made available (in open source format through SourceForge fidtojcamp.sourceforge.net) a small utility program I wrote to convert data from the native Bruker FID format (collected using either XACQ or FlexControl) to a standard JCAMP format file. Note that the utility allows the data to be written with the x-axis in either TOF or mass, which is particularly handy for viewing the data in TOF format (as the newer FlexAnalysis software cannot display the data in this manner). Once the data is in JCAMP format it can be viewed using JSpecView; this allows for the easy on-line sharing of data as well.

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