In addition to the instrumentation available in the shared core facilities at the UTD campus, numerous analytical instruments are housed in the Center for Engineering Innovation and Advanced Polymer Research Laboratory. A brief listing of these instruments, their capabilities, and the types of information received from them are provided below. This instrumentation is available for academic and industrial partners, along with individual entities to use. There are two routes of utilizing the equipment: Sponsor Cost is designated for the service center director to perform the analysis, while the User cost is designated for the trained customer to perform the analysis.
If you are interested in using any of the instrumentation found in the Center for Engineering Innovation and Advanced Polymer Research Laboratory, please contact Dr. Ben Batchelor, the director of the CEI/APRL Service Center.
Dr. Ben Batchelor, CEI/APRL Service Center Director
Phone: 972-883-7257
Email: ben.batchelor@utdallas.edu
With the Mettler Toledo DMA861e Dynamic Mechanical Analyzer (DMA), a series of tension, shear, three-point bend, single or dual cantilever, and compression tests can be performed on a material between two grips or platens in a furnace accurate to less than 0.5°C between -150°C and 500°C. Under a steady temperature ramp (or complex temperature profile), the 40 Newton (N) load cell applies a sinusoidal mechanical force on the material as the temperature changes. To calculate the material properties, the DMA requires a host of inputs: a desired maximum applied strain (0.2 % is standard), a preload force (.01 N for instance), a Force Track (150%) and the specific dimensions of the sample to be tested. The testing equipment applies an oscillatory stress at the same frequency as the strain, but out of phase with the strain, to reach the specified input maximum. Back-calculating the force required to meet the given strain criterion through iteration, the DMA can output the elastic modulus of the tested materials as a function of temperature. This elastic modulus is determined through computation using the user-measured and inputted cross-sectional area of the material and the machine-calculated applied force to calculate the instantaneous modulus as a function of temperature as measured by the sample thermocouple positioned within the furnace. The dynamic linear response of materials is measured.
The Mettler Toledo DSC1 Differential Scanning Calorimeter (DSC) is a thermo-analytical device that measures the relative heat flow through a material relative to the heat flow though air (or any other substance placed into the reference pan) and tracks the difference in temperature needed to heat the sample as a function of temperature. The DSC consists of two sealed pans: a sample pan and the reference pan that is usually empty. The materials to be tested are either polymerized directly into the sample pan, or are placed into the pan after small samples are cut to sizes weighing usually between 1 and 100 mg. The final plot is a graph of differential heat flow as a function of temperature. This result, known as a heating or cooling curve for the given acrylate system, can be used to calculate the enthalpies of transitions. The DSC contains an attached Intracooler which extends the temperature range from -85°C to 700°C. A computerized robotic arm facilitates loading and unloading of up to 32 samples for rapid testing across material parameters.
The Lloyd Instruments LR5KPlus Universal Testing Machine (UTM) is a thermo-analytical device used to measure an array of mechanical properties. The UTM has swappable 5 kN, 1 kN and 100 N load cells to stretch or compress material samples. The UTM is coupled with the TC540 Heating and Cooling Thermal Cabinet allowing tensile and compression tests from between -70°C and 300°C with a temperature accuracy of 0.5°C. The UTM is also outfitted with a LASERSCAN 200 Non-Contacting Laser Extensometer than can accurately measure strains up to 2000 mm (limited to 600mm of viewable space at non-ambient temperatures in the TC540). The UTM is outfitted with a variety of grips and fixtures to test a range of materials. This includes wedge-action grips, self-tightening grips and compression platens. The data generated is usually a stress strain curve at a specific temperature, but specific tests can be customized for unique situations.
The Mettler Toledo TGA/DSC-1 Thermograviemetric Analyzer (TGA) is a thermos-analytical device that mesasures the weight changes of the material through the series of temperature changes. The TGA consists of a alumina crucible that is filled with the desired material and subjected to a ramping temperature change. When the sample is heated, there will be potential mass loss that will be recorded by a highly sensitive balance. This will give the user results on the temperature of degradation (Td), temperature of depolymerization, or the temperature that the material sublimates. The samples that are used are weighed between 2 and 50 mg, depending on sample geometry. The final plot is a graph of the percentage weight change over the desired range of temperatures. The TGA contains a furnace that extends the temperature range from 25 °C to 1000 °C and has two method gases that can be utilized: N2 for inert atmosphere or air for effects of oxidation. A computerized robotic arm facilitates loading and unloading of up to 32 samples for rapid testing across material parameters.
With the GCMS or Gas Chromatography Mass Spectrometer from Shimadzu (GCMS QP2010), the determination of small molecular masses can be performed. It can take pure substances along with mixtures to determine the purity and concentrations of multiple samples. The GCMS first analyzes the number of substances through chromatography then each individual peak can be analyzed for their specific masses. The GCMS QP2010 has a temperature range from room temperature to as high as 300 °C and can analyze masses from 2 amu to 1000 amu. Along with the GCMS program is a selected library containing 10,000 different references.
The Shimadzu IRAffinity-1 is an instrument for Fourier Transform Infrared Spectroscopy (FTIR). This instrument determines the infrared spectrum of liquids, powders, and films. This is an important analytical tool to determine the correct composition of materials and synthesized molecules with a wide application while remaining reliable. The IRAfffinity-1 can be performed in transmission mode for transparent films, powers in a KBR pellet, or liquids on a salt plate. It can also be coupled with a modular Atenuated Total Reflectance (ATR) for surface characterization of liquids, films, or other solids.
Gel Permeation Chromatography (GPC) is necessary for the characterization of polymers for their molecular weight. The molecular weight gives information for the potential properties of the materials such as strength, transition temperatures, and many others. The GPC that is utilized in this laboratory is the Shimadzu HPLC. The GPC has a temperature range from room temperature to as high as 80 °C, though is set on single temperature for the duration of the experiments and not a dynamic temperature range. The typical speeds of the GPC is at 1 mL/min with an autosampler to push through as many as 50 samples in one batch. The samples are pushed through a dual column system that is filled with polystyrene stable phase of varying pore sizes. The mobile phases that can be used are either chloroform or dimethylformamide (DMF). The dector of the GPC is a refrective index detector (RID) which is an all incompassing detector for any linear polymeric materials. The results will showcase a chromatography with values such as number average molecular weight and weight average molecular weight, both based off of a polystyrene calibration curve.
The Malvern RH-7 capillary rheometer is a large stand alone dual barrel rheometer to determine the melt viscosity of any meltable sample. It will show the resitance to flow or visocity of polymers for the use in development of melt processable materials. This information can be used as a starting point for development of methods for melt extrusion, injection molding, and melt blowing. The barrels are a tungsten carbide material which creates a frictionless environment in the barrel itself, then the samples are pushed through a variety of L/D dies. The information is correlated through a Bagley Correction to determine the melt visocity, flow, and shear stress curves.
Rates for external customers of the CEI/APRL service center.
| Equipment | Sample Size | Temp Range | Sponsor Cost | User Cost |
|---|---|---|---|---|
| DMA | 1 sample | -50 to 200C | $350/sample | $50/hour |
| DSC | 1 sample | -50 to 500 C | $200/sample | $35/sample |
| UTM | 5 identical samples | Single temp (-50 to 200C) | $400/sample | $75/hour |
| TGA | 1 sample | 30 to 300C | $225/sample | $40/sample |
| GCMS | 1 sample | 30 to 300C | $100/sample | $35/sample |
| FTIP | 1 sample | N/A | $75/sample | $25/sample |
| GPC | 1 sample | N/A | $150/sample | $35/sample |
| Capillary Rheometer | 1 sample | Single temp (30 to 300C) | $350/sample | $50/hour |