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Polymer Characterization Facility

Facility Director

hawker [at] mrl [dot] ucsb [dot] edu (Professor Craig Hawker)

Technical Director

Dr. Rachel Behrens, rachel [at] mrl [dot] ucsb [dot] edu

Training

Users of the MRL Synthesis and Characterization Laboratory are required to go through two levels of training before they are authorized to perform data collection independently. The training consists of

  1. General lab safety training, provided by the UCSB Environmental Health & Safety Department (EH&S).
  2. Instrument training, conducted by the manager Rachel (rachel [at] mrl [dot] ucsb [dot] edu) or an authorized user delegated by the laboratory manager.

Scheduling for Instruments

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Instruments

  1. DLS

    The DynaPro NanoStar™ from Wyatt Technology is Dynamic Light Scattering (DLS) instrument that is used for the analysis of protein solutions, aggregates, buffers, nanoparticles, polymers, or other products in solution. In a DLS measurement, the time-dependent fluctuations in the scattered light are measured by a fast photon counter. The fluctuations are directly related to the rate of diffusion of the molecule through the solvent. Therefore, the fluctuations can be analyzed to determine a hydrodynamic radius for the sample (0,5 nm to 1000 nm).

  2. DSC

    Differential Scanning Calorimeter (DSC) from TA Inst. Co., measures the difference in heat absorbed or released by sample, as compared to an inert refference (empty pan), as both are heated, cooled or held at constant temperature (isothermal). Exothermic transitions result in the release of heat: crystallization, curing, decomposition, etc. Endothermic transitions absorb heat: melting, glass transition, evaporation, etc. DSC Q-2000 using the Tzero technique provides significant improvements in baseline flatness, transition, resolution and sensitivity.

  3. Gas Chromatograph

    The Gas Chromatograph (GC) makes possible to separate the volatile components of a very small sample and to determine the amount of each component present. A GC consists of a flowing mobile phase, an injection port, a separation column containing stationary phase, a detector, and a data recording system. Typically samples of 1 µL or less are injected on the column. These volumes can be further reduced by using what is called a split injection system in which a controlled fraction of the injected sample is carried away by a gas stream entering the column.

  4. GPC - DMF

    Gel Permeation Chromatography (GPC) is a separation method for the determination of molecular weight averages (Mn) and molecular weight distribution (PDI=Mw/Mn). The testing report can include calibration plot, chromatogram, number average molecular weight and PDI of the polymer. GPC-DMF is using DMF as a solvent. Gel Permeation Chromatography (GPC) separates molecules on the basis of hydrodynamic size (not Mw).

  5. GPC - chloroform

    Gel Permeation Chromatography (GPC) is a separation method for the determination of molecular weight averages (Mn) and molecular weight distribution (PDI=Mw/Mn). The testing report can include calibration plot, chromatogram, number average molecular weight and PDI of the polymer. GPC-chloroform is using chloroform as a solvent. Gel Permeation Chromatography (GPC) separates molecules on the basis of hydrodynamic size (not Mw).

  6. GPC - MALS

    Multi-Angle Light Scattering Detection (MALS) results in the measurement of absolute molecular weight which is independent from the column calibration. The amount of light scattered (measured by MALS) is proportional to the molar mass of the polymer (M), the concentration (c) of the polymer, and the square of specific refractive index increment (dn/dc). Special procedures must be taken if the sample absorbs or if the sample fluoresces with exicitation at the wavelength of the laser (663.1 nm).

  7. GPC - Prep

    Preparative Gel Permeation Chromatography (GPC- Prep) is used for the fractionation of polymer samples on a preparative scale. The elution order is from high molar masses to low molar masses. Therefore, the method can be used for determination of oligomers content and purification of polymer sample (removal of low molecular weight impurities, e.g., residual initiator, additives). These low molecular weight components are eluted after the main fraction of the polymer and can be readily removed by “end-shaving”.

  8. Microwave Reactor (Biotage)

    Biotage Microwave Reactor is designed to enhance the ability to perform chemical reactions under controlled conditions on a laboratory scale. Microwave chemistry is based on the efficient heating of materials by “microwave dielectric heating” effects. This phenomenon is dependent on the ability of a specific material (solvent or reagent) to absorb microwave energy and convert it into heat. It accommodates 0.5 mL to 35 mL vessels with septa for reactions performed at elevated temperature and pressure.

  9. Microwave Reactor (CEM)

    The CEM Focused Microwave TM Synthesis System, Discover S is designed to enhance the ability to perform chemical reactions under controlled conditions on a laboratory scale. The system facilitates either homogenous or heterogeneous solution phase chemistry, solid phase chemistry or chemistry conducted on solid supports.

  10. Nano ITC

    Nano ITC (Isothermal Titration Calorimeter) directly measures heat evolved or absorbed in liquid samples as a result of mixing precise amounts of reactants. A spinning syringe is utilized for injecting and subsequent mixing of reactants. Spin rates are user selectable. It is also the only method capable of determining the enthalpy, entropy, and the Gibbs free energy of a reaction in a single titration experiment.

  11. Rheometer with oven

    Rheometer is a mechanical spectrometer that is capable of subjecting a sample to either a dynamic (sinusoidal) or steady (linear) shear strain (deformation). Then measuring the resultant torque expended by the sample in response to the shear strain (shear strain is applied by the motor- torque is measured by the transducer). In the dynamic mode, the motor begins all tests at the motor zero position, and drives symmetrically about motor zero to the strain commanded by the software.

  12. Rheometer with water bath

    Rheometer is a mechanical spectrometer that is capable of subjecting a sample to either a dynamic (sinusoidal) or steady (linear) shear strain (deformation). Then measuring the resultant torque expended by the sample in response to the shear strain (shear strain is applied by the motor- torque is measured by the transducer). In the dynamic mode, the motor begins all tests at the motor zero position, and drives symmetrically about motor zero to the strain commanded by the software.

  13. Viscolite 700HP Bench Viscometer

    The Visolite 700H  is a handheld or bench-mounted instrument for the measurement of viscosity of fluids by insertion. The actual sensor has a solid construction with no moving parts.  It is connected toa ench - top microprocessor (HP550) unit by a flexible cable, and the whole instrument is powered by a transformer/adaptor unit. The Viscolite can be used with any volume of fluid. Unlike conventional rotating cylinder viscometers there is no specific quantity of fluid, or size of vessel, required to ensure accuracy.