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Thermal Analysis and Soft Materials Characterization

Thermal analysis covers a range of techniques used to determine the physical or chemical properties of a substance as it is heated, cooled, or held at constant temperature. MRL’s Thermal Analysis and Soft Materials Characterization suite hosts a wide range of instruments for your research.

Techniques

Center for Excellence in Soft Materials

Techniques for evaluating materials' properties include particle size analysis, Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), Dynamic Mechanical Analysis (DMA), and Differential Thermal Analysis (DTA).



Equipment in this Core

Equipment Name Contact Location Techniques
Equipment Name Contact Location Techniques
Metrohm 915 KF Ti-Touch (Volumetric Method) raremy 133 MRL
  • Center for Excellence in Soft Materials

Karl Fischer (KF) Titration is a widely used technique for the quantification of water content in materials. The water content is identified through a chemical reaction that directly consumes water. The fundamental chemical process is called the Bunsen Reaction and is given below:

2H2O + SO2 + I2 à H2SO4 + 2HI

From the reaction equation it is clear that the amount of water in the reaction is directly proportional to the amount of iodine required to consume it. Water content in samples can therefore be directly and accurately obtained by measuring the amount of iodine used in the reaction. The MRL has two compact instruments available for KF Titration experiments. This combination enables water content analysis from 100% water down to parts-per-million (ppm) levels.

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Metrohm 917 Coulometer (Coulometric method) raremy 133 MRL
  • Center for Excellence in Soft Materials

Karl Fischer (KF) Titration is a widely used technique for the quantification of water content in materials. The water content is identified through a chemical reaction that directly consumes water. The fundamental chemical process is called the Bunsen Reaction and is given below:

2H2O + SO2 + I2 à  H2SO4 + 2HI

From the reaction equation it is clear that the amount of water in the reaction is directly proportional to the amount of iodine required to consume it. Water content in samples can therefore be directly and accurately obtained by measuring the amount of iodine used in the reaction. The MRL has two compact instruments available for KF Titration experiments. This combination enables water content analysis from 100% water down to parts-per-million (ppm) levels.

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Novocontrol Concept 47 Analyzer raremy 133 MRL
  • Center for Excellence in Soft Materials

The Novocontrol Analyzer is designed for the electric/dielectric characterization of materials. Frequency response analysis, dielectric/impedance spectroscopy and conductivity spectroscopy can be performed with this instrument. This modular system features the Novocontrol Alpha-A frequency response analyzer combined with PHECOS Lite temperature control system. Samples are sandwiched between two circular, gold plated electrodes, then placed into the instrument for testing. Results can be analyzed as measured or re-plot to fit various equations such as Arrhenius or Cole-Cole plots. Parameters for the Concept 47 system are listed below.

Frequency range – 3 µHz – 20 MHz

Temperature range – -35 °C – 150 °C

Sample diameter options – 40 mm, 30 mm, 20 mm

Electrode configurations – 2-wire modes available

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TA Instruments Affinity ITC raremy 133 MRL
  • Center for Excellence in Soft Materials

Isothermal Titration Calorimetry (ITC) measures the heat evolved or absorbed during a binding reaction occurring in a liquid medium – typically water. Microliter amounts of titrant are incrementally added to the analyte solution in the reaction cell and the heat of reaction is measured at each step until saturation. Software is then implemented to fit the reaction curve to known or developed chemical reaction models in order to calculate parameters such as binding constant (Ka), stoichiometry (n), enthalpy (ΔH) and entropy (ΔS). Features of the Affinity ITC are listed below.

 

Cell – Cylindrical, 24k Gold, 1mL volume

Syringe – AccuShot™ injection syringe, 0.01 µL minimum injection volume, up to 250 µL total volume

Mixer – FlexSpin™ stirrer, 0 – 200 rpm

Temperature range – 2 °C – 80 °C

Detectable energy range – 0.1 µJ – 5000 µJ

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TA DHR-3 Rheometer raremy 133 MRL
  • Center for Excellence in Soft Materials
Tosoh EcoSEC 8320 GPC System raremy 133 MRL
  • Center for Excellence in Soft Materials
Shimadzu DTA-50 Differential Thermal Analyzer (DTA) raremy mali85 133 MRL
  • Center for Excellence in Soft Materials

Differential Thermal Analyzer (DTA) uses a two-pan system to measure the heat flux difference between an empty pan (or one with a reference material) against the temperature of a sample of specific weight. The DTA-50 system uses temperatures in the range between room temperature and around 1400 oC to determine thermal transitions such as glass transitions, crystallization, phase changes, melting, stability, cure kinetics, etc. While it is not as sensitive as a differential scanning calorimetry (DSC), it is more versatile for harder materials, as our DSC system cannot operate above 400oC. The DTA-50 instrument is calibrated to 1100oC for accuracy.

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Malvern Zetasizer raremy mali85 133 MRL
  • Center for Excellence in Soft Materials

The Malvern Zetasizer Nano ZS is a multipurpose light scattering instrument. It is outfitted with a 633nm red laser and is designed to analyze nanoparticles, small molecules and polymers in liquid media. The instrument has a temperature range of 0 °C – 90 °C. Results are laid out in both table and report format; both of which can be exported at the end of the experiment. Available techniques and instrument accessories are detailed below.

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Q800 Dynamic Mechanical Analysis (DMA) raremy mali85 133 MRL
  • Center for Excellence in Soft Materials

Dynamic Mechanical Analysis (DMA) measures mechanical properties of samples. Its principal uses include measurement of a material's Young's modulus or viscoelastic properties as a function of temperature (or time). Testing can be performed in either tensile or cantilever bending geometries.

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Q50 Thermogravimetric Analysis (TGA) raremy mali85 133 MRL
  • Center for Excellence in Soft Materials

Thermogravimetric Analysis (TGA) measures weight changes in a material as a function of temperature (or time) under a controlled atmosphere. Its principal uses include measurement of a material's thermal stability and composition. The Q50 features a vertical beam balance design (sample capacity: 1000 mg) that supports precise TGA (balance sensitivity: 0.1 µg) measurements.

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Discovery 2500 Differential Scanning Calorimeter (DSC) raremy mali85 133 MRL
  • Center for Excellence in Soft Materials

Differential Scanning Calorimetry (DSC) measures heat effects associated with phase transitions and chemical reactions as a function of temperature.

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