Facilities

Facilities

The Department maintains an impressive collection of Mass Spectrometry, NMR Spectroscopy, Optical Characterization and X-Ray facilities.

 

Mass Spectrometry Facility

The Department of Chemistry and Biochemistry operates an in-house Mass Spectrometry facility to support research and teaching activities. Mass Spectrometry is a primary tool for structure elucidation, molecular weight determination and molecular formula confirmation for organic and biological materials. This family of techniques measures the masses of organic and biological molecules by creating gas phase ions from the analytes and manipulating those ions in electric and magnetic fields. Chemical structure may be probed by fragmenting molecular ions and mass measuring the resulting product ions. 

A wide range of ionization techniques and capabilities are available. Services are available by sample submission to the facility staff or by direct instrument access for trained users on a 24/7 basis. Facility staff is available for operator training as well as consultation on experimental design and data interpretation.

Instrumentation Available

A Bruker Microflex LRF MALDI TOF mass spectrometer is used for the analysis of a broad range of compounds including small molecules, peptides, proteins, nucleic acids, and synthetic polymers. The Microflex LRF has a mass range of up to 20,000 Da in reflectron mode or up to 500,000 in linear mode. Additionally the instrument is capable of mass spectral imaging and post source decay analysis. Software is available for the analysis of polymer data.

A Waters GCT Premier Time-of-Flight MS is equipped with electron ionization (EI), chemical ionization (CI), and field ionization/field desorption (FI/FD) ion sources.  EI, CI, and FI techniques are suitable for volatile and semi-volatile organic compounds with sample introduction via an Agilent capillary GC or by direct insertion probe for thermally labile compounds.  FD is a powerful tool for the analysis of small polymers and other non-polar materials (<4000 Da). Full scan analyses and accurate mass measurement are available.

An HP GC/MSD is a dedicated GC-EI MS low resolution instrument for routine GC/MS analyses of volatile and semi-volatile organic compounds including reaction mixtures.

 
Ionization Techniques Available:
Electron Ionization (EI)
Chemical Ionization (CI)
Field Ionization/Field Desorption (FI/FD)
Matrix Assisted Laser Desorption Ionization (MALDI)
 
Services Available:
Full Scan MS
Accurate Mass Measurement (HRMS)
GC MS
Target Loaded MALDI TOF
Direct Insertion Probe EI, CI, FI/FD
Data Interpretation
Instrument Training

 

Facility Technician and Spectrometrist: Dr. Dmitriy Uchenik, uchenik@chem.ucsb.edu 
Location: Physical Sciences Building North (PSBN), Room 4624W
Phone: 805-893-4252
Webpage: Mass Spectrometry Facility

 

MALDI-TOF Tandem Mass Spectrometer

GCT Premier TOF Mass Spectrometer

 

Nuclear Magnetic Resonance (NMR) Facility

NMR spectroscopy is a highly sensitive technique in probing molecular structure and dynamics of chemical compounds, polymers and biomolecules. The in-house NMR Facility is currently home to five solution-state NMR spectrometers at 400, 500, and 600 MHz fields. Among them is a newly installed, state-of-the-art 500 MHz Bruker spectrometer equipped with a cryoprobe and an automatic sample lift. All spectrometers are equipped with multiple solution-state NMR probes for direct or indirect detection of 1H/19F and low frequency nuclei such as 13C, 31P, and 15N.  These spectrometers are dedicated to the needs of chemistry and materials research with the 600 MHz instrument also used for biomolecular NMR research.  Experiments conducted at the Facility range from routine 1D and 2D experiments for small molecule and polymer analysis at natural abundance to complex 3D and 4D multinuclear correlated experiments for proteins using isotope-labeled samples. All instruments are user-operated and are open to researchers with 24/7 access after proper training. User training is offered throughout the year in mostly hands-on individual sessions. Technical assistance is readily available for data collection and analysis.

The NMR lab of the Department of Chemistry and Biochemistry collaborates with the Spectroscopy Facility of the Materials Research Laboratory (MRL). The MRL-supported NMR facility is also available to all users on campus, and offers complementary capabilities, including solid state NMR instrumentation from 400 to 800 MHz, a CW Electron Paramagnetic Resonance (EPR) spectrometer and NMR imaging and diffusometry instrumentation. The laboratory of Professor Han offers other dedicated capabilities, including pulsed EPR and dynamic nuclear polarization NMR at 10 and 200 GHz.


400 MHz

500 MHz
600 MHz
600 MHz
 

Facility Manager and Spectroscopist: Dr. Hongjun Zhou; hzhou@chem.ucsb.edu

Location: Physical Sciences Building North (PSBN), Room 3614A
Phone: 805-893-2938
Wepage: NMR Facility

Hongjun Zhou

Dr. Hongjun Zhou

 

Changes in 1H spectrum in a variable temperature (VT) experiment indicates exchange among multiple conformers of a chemical compound

Changes in 1H spectrum in a variable temperature (VT) experiment indicates exchange among multiple conformers of a chemical compound

 

2D 1H-15N corelation spectrum shows perturbations to the protein amide resonances upon DNA binding

2D 1H-15N corelation spectrum shows perturbations to the protein amide resonances upon DNA binding

 

Optical Characterization Facility

In the Optical Characterization Facility, light is used to probe the intrinsic properties of materials prepared by chemists and serves as an analytical and quality control tool. We study energy and charge migration in materials for novel optoelectronic devices, test new biosensors and materials for data storage, zap bacteria with laser beams, and provide state of the art technical capabilities that are not commonly available to non-expert chemists in their own laboratory. The optical characterization facility gives students the ability to have hands-on experience in modern optical spectroscopy. The facility does not have dedicated instruments; rather experiments are designed to meet the need of the user. The facility manager assists its users in the design, assembly, and final analysis of experimental data. Custom optical experiments and support include photoconductive atomic force microscope, solar simulators for photovoltaics research or optical setups for characterization of organic semiconductors and many more chemical, materials and biological systems.

Major Capabilities and Areas of Expertise:

Time-resolved fluorescence measurements in the range 50 ps – 10 s (time-correlated single-photon counting etc.).
Transient absorption spectroscopy with sub-100 fs resolution
Custom luminescence spectroscopy (temperature-dependence, photoluminescence up-conversion, thermoluminescnce, electroluminescence, quantum-yield measurements)
Non-linear optical spectroscopy (multiphoton absorption and optical harmonics spectroscopy)
Raman spectroscopy and microscopy
High laser power processing of materials
Optical holography

Facility Instrumentation include 1 kHz repetition rate, 100 fs pulse Ti:Sapphire amplifier, Ti:Sapphire femtosecond oscillator laser, optical harmonics generator, high power Ar-ion laser with single-mode operation capability, various smaller semiconductor and gas lasers. We also have several monochromators equipped with spectroscopic CCD cameras, single channel detectors and a high-end Raman microscope.

Facility Manager and Spectroscopist: Dr. Alexander Mikhailovsky; mikhailovsky@chem.ucsb.edu
Location: Chemistry 3312
Phone: 805-893-2327
Webpage: Optical Characterization Facility

Alexander Mikhailovsky

Dr. Alexander Mikhailovsky assisting with lasers and optical spectrometers

 

X-Ray Facility

The in-house X-ray facility allows for single crystal x-ray structure determination for researchers in the Department of Chemistry and Biochemistry, as well as UCSB wide. There are three instruments currently housed in the facility. A fine focus sealed tube Mo source better for small molecule structure determination, a rotating anode Cu source used mainly for protein crystallography and other biologically relevant samples, and a sealed tube Cu source for 2-D powder diffraction. Three instrumentations are available:

The Kappa APEX II diffractometer has a fine focus sealed tube Mo x-ray source combined with a Bruker 4 axis diffractometer an APEX II detector and an Oxford Cryostream-Plus low temperature device

The Proteum diffractometer is equipped with a Microstar rotating Cu anode x-ray source and a 3 axis platform diffractometer, alongside a Proteum detector and an Oxford 700 Cryostream low temperature device

The Powder diffractometer is a Scintag X2 with a sealed Cu tube x-ray source and a solid-state point detector

Faculty and students also have access to the complementary MRL X-ray facility, located just a few steps from the chemsitry building (http://www.mrl.ucsb.edu/mrl/centralfacilities/xray/index.html) ).

Facility Manager and Crystallographer: Dr. Guang Wu; wu@chem.ucsb.edu

Location: Physical Sciences Building North (PSBN), Room 4608
Phone: 805-893-2399
Webpage: X-ray Facility

4 axis Apex II diffractometer

4 axis Apex II diffractometer with fine focus sealed tube source and cyro setup

Dr. Guang Wu

Dr. Guang Wu
 

Recharge Rate:

  • Low Temperature Single Crystal Data collection: $200.00/sample
  • Low Temperature Single Crystal Data collection and Structure Determination: $252.00/sample
  • Room Temperature Single Crystal Data collection: $150.00/sample
  • Room Temperature Single Crystal Data collection and Structure Determination: $202.00/sample
  • Single Crystal Cell Determination:$30.00/sample
  • Other Special Service: Rate depending on the nature of the experiment and measurement time