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Polymer Characterization Lab

Established with partial support from TAML (Tennessee Advanced Materials Laboratory), the Polymer Characterization Laboratory (PCL) is housed at IAMM.  One of the premier academic laboratories in the world for characterizing polymers in terms of molecular weight, molecular weight distribution, conformation, size, and thermal properties, the lab serves a wide range of users from across the UT campus, as well as external users from industry and national laboratories.

Katrina D. Pangilinan Facility Manager kpangili@utk.edu 865-974-2087
Mark Dadmun Scientific Leader dad@utk.edu 865-974-6582

Malvern High Temp GPC

Viscotek High Temp GPC The Malvern Viscotek 350B GPC is a high temperature instrument that provides advanced triple detection to high-temperature applications. The triple detector array includes a differential refractive index (RI) detector, a right angle (90°) and low angle (7°) light scattering detector, and a viscometer detector that combine to deliver accurate and precise molecular characterization of a sample. The column set installed consists of three CLM6210 mixed-bed HT-GPC columns that can accommodate a wide molecular weight range of polyolefin samples. In addition to molecular weight moments and dispersity, advanced detection offers additional molecular characterization data such as intrinsic viscosity, hydrodynamic radius, branching content, and recovery, among others. The Viscotek 350B GPC is equipped with the Vortex auto-sampler which houses up to 29 samples, with heating and stirring, to be run according to the set sequence with each sample taking about an hour.

Nuclear Magnetic Resonance Spectrometer

The Jeol JNM-ECZS 400 MHz NMR allow users to probe many nuclei, such as 1H, 13C, 15N, 31P, and 19F. The response of the nuclei to the magnetic field provides details of the electronic structure of a molecule and its individual functional groups. NMR spectroscopy also provides detailed information about the dynamics, purity, reaction state, and chemical environment of molecules. The Spectrometer is equipped with a 24-seat autosampler to facilitate quick turnaround of data acquisition. It has a highly stable control system which allows analysis at low and high temperatures.

Small Angle X-Ray Scattering

The Xenocs Xeuss 3.0 SAXS instrument is a powerful technique that allows for the determination of size, distribution, shape, and order of nanoparticles and macromolecules. This instrument has 2 radiation sources, Cu and Mo, that can be switched and aligned automatically. It can operate over different configurations that spans a variety of q-ranges; WAXS, SAXS, MSAXS, and USAXS. Accessories include a low-noise flow cell for dilute or low scattering samples, BioCube for low volume samples, capillary holder for liquid samples, gel and powder sample holder, GISAXS sample holder for thin film and surface analysis, heating stage, and humidity stage.

Aqueous GPC System

The aqueous GPC system consists of a Waters 515 HPLC pump, a Rheodyne model 7725 manual injector with a 10 µL loop, and a Knauer RI detector K-2301. It uses 0.2M NaNO3 in water as eluent with a flow rate of at a flow rate of 0.35mL/min. Data is collected and analyzed using Polymer Labs Cirrus software. The column set installed in this instrument consists of two columns of Tosoh TSKgel Super AWM-H (6mm ID x 15cm, 9µm), along with a TSKgel AW-H guard column (4.6mm ID x 35mm, 23µm). The instrument is calibrated in the molecular weight range of ≈600 up to 1,000,000 Daltons using a set of PEO/PEG standards.

Tosoh EcoSEC GPC System

The EcoSEC GPC system is a semi-micro system with a low dead volume which allows for the use of semi-micro GPC columns. The EcoSEC is a self-contained system with temperature controlled pumps, column ovens, and detectors operating in the range of room temperature + 10°C up to 60°C. The instrument has both an RI detector and a UV detector which operates at a single wavelength between 195-350 nm. The RI detector has a flow reference cell rather than the conventional static reference cell. The operating flow rates are 0.35 ml/min for both the reference cell and the sample cell. The EcoSEC has a 100 sample capacity autosampler. The column set installed in this instrument consists of the following three columns: 2 Tosoh TSKgel SuperMultiporeHZ-M; 4.6×150 mm; 4 µm; and a TSKgel SuperMultiporeHZ-M guard. The calibration range is ≈600 to 7,500,000 daltons using either PS or PMMA standards.

TA Instruments Q-50 TGA

The Q-50 is a thermogravimetric analyzer capable of determining the properties of materials associated with weight change such as dehydration, gas evolution, oxidation, and degradation. Samples can be analyzed in the temperature range from room temperature up to 1000°C in an environment of either air or nitrogen. The following pans are available: 100 µl platinum pans, 100 µl ceramic pans, and 500 µl ceramic pans.

Multimode Scanning Probe Microscope (SPM)

The Digital Instruments scanning probe microscope is used to perform the full range of atomic force microscopy (AFM) techniques to measure surface topography. It is possible to see features less than 5 nm in size. In addition to tapping and contact modes, more advanced techniques such as fluid imaging, nanoindentation, and heating/cooling can be studied. A supply of tapping mode tips (Veeco, model TESP) along with silicon wafers (5 x 5 mm) are available.

Schott Instruments ViscoSystems AVS 370 Dilute Solution Viscometer

The Schott Instruments AVS 370 is an automated dilute solution viscometer where the initial concentrated solution is placed in the viscometer and the dilutions are done automatically utilizing the Dilut 4.0 software which is computer controlled. The system will do up to 5 dilutions per experiment. The total capacity of the viscometer is 75 ml so the only limitation to the number of dilutions is the total volume. The following three viscometers are available: type 531-03 (0.47 mm capillary with K = 0.003); type 531-10 (0.64 mm capillary with K = 0.01); and type 531-13 (0.84 mm capillary with K = 0.03). The viscometer is equipped with optical sensors for starting and stopping the timer, a heater/cooler bath for temperature regulation, a built-in magnetic stirrer to assure homogeneity in the solution, and an automatic burette for accurately and uniformly dispensing solvent.

TA Instruments Q-2000 DSC

The Q-2000 is a differential scanning calorimeter capable of measuring the heat capacity, glass and melting transition temperatures, percent crystallinity, and heat of fusion using standard and temperature-modulated methods. The DSC is equipped with an autosampler capable of performing up to 50 consecutive analyses. An RCS (refrigerated cooling system) allows experiments to be conducted from -90°C to 550°C. Both standard aluminum pans and hermetic aluminum pans are available.

TA Discovery TGA-MS

The Discovery Series TGA/MS is a thermogravimetric analyzer coupled with a Mass Spectrometer, capable of determining the properties of materials associated with weight change such as dehydration, gas evolution, oxidation, and degradation. Samples can be analyzed in the temperature range from room temperature up to 1200°C in many different environments.  The Gas Delivery Module allows gas switching and blending of up to four different gases.  The IR furnace is capable of heating rates of 0.1 to 500°C/min. in linear control, or over 2,000°C/min. in ballistic heating.  Air sensitive samples can be analyzed by using sealed aluminum pans that the auto- sampler will ‘punch’ open before loading into the furnace.  The instrument also comes equipped with 25 position auto-sampler. The following pans are available: 100 µl platinum pans, 100 µl high temperature platinum pans , 250 µl ceramic pans, and 80 µl sealed aluminum pans.

ALV Light Scattering System

ALV/CGS-3 Compact Goniometer System The ALV / CGS-3 compact goniometer is a self-contained system with 22 mW HeNe laser, ALV-proprietary optical fiber based detector, APD-based single photon detector, ALV/LSE-5003 electronics and ALV-5000/EPP correlator. It offers identical overall performance for simultaneous measurement of DLS & SLS data and the optical detection was designed such that a significantly higher count rate per mW is obtained. The complete shielding of the unit ensures it is a class 1 laser product. The goniometer angular range is from 17° to 150° with a resolution of 0.025° and a travel speed of 20°/s.

DMF GPC

This GPC system is designed for applications using DMF or DMF with 0.1M LiBr. It consists of an Agilent model 1260 Infinity pump, a Rheodyne model 7725 manual injector with a 200 µ l loop, and a Varian 390 LC detector system consisting of an RI detector and a two angle light scattering detector. the following column set is used: four PSS (Polymer Standards Service) GRAM; 8×300 mm; 10µm; 100, 1000, and 3000 Å along with an 8×50, 10µm guard column. The columns are calibrated with a set of PS standards in the molecular weight range of ≈600 up to 7,500,000 daltons.

Thermo Scientific FT-IR Spectrometer

The Nicolet iS50 FT-IR Spectrometer measures the absorption spectrum in the mid-IR region (5000-400 cm-1). This is a powerful technique that provides chemical information of materials that absorb specific frequencies that are characteristic of their structure. The spectrometer has a deuterated triglycine sulfate (DTGS) detector with adequate sensitivity for routine analysis, and a mercury cadmium telluride (MCT) detector for applications requiring higher sensitivity and faster response. The instrument can be used in transmission and ATR modes.

Thermo Scientific Evolution 300 UV-Vis Spectrophotometer

UV-Vis Spectroscopy is an analytical technique for the quantitative determination of the absorption of analytes in the ultraviolet-visible spectral region. The Evolution 300 UV-Vis Spectrophotometer has a double beam optical design with a xenon flash lamp light source that has a spectral range of 190-1100 nm.

Other Accessories

The Polymer Characterization lab is also equipped witht he following additional accessories to aid in the experimentation process: a Cahn C-33 Microbalance (±0.001 mg), a Fisher Scientific model FS20H sonicator, a Denver Instruments model P-114 analytical balance (±0.1 mg), a Carver Laboratories model C heater/press, a Boekel Industries, Inc. model 107800 laboratory oven, a Labnet Spectrafuge 16M microcentrifuge, and a Thermo Scientific model 37600 vortex mixer.

  Internal Academic External Academic Commercial
Polymer Characterization Instrumentation Unassisted $20/hour $30/hour $100/hour
Polymer Characterization Instrumentation Assisted $40/hour $60/hour $200/hour
Sample Preparation Assisted $40/hour $60/hour $200/hour

User rates subject to change without notice.