Calorimetry - patrick-shamberger/PHATE_Lab_Handbook GitHub Wiki

STA 449 F3 Jupiter & QMS 403 Quadro Aeolos

The simultaneous thermal analyzer NETZSCH STA 449 F3 Jupiter® allows the measurement of mass changes and thermal effects between 40°C and 1100°C.

  • Temperature range: 40 to 1650 °C
  • Furnace Types: Rh, SiC
  • Atmospheres: vacuum, inert (N2, He, Ar), static, dynamic, oxidizing, reducing
  • Crucile Types: Al2O3, Aluminum (coming soon!), PtRh10 w/ option for Al2O3 liner
  • Heating rate: 0.001 to 50 K/min
  • Sensor Thermocouple: Type S
  • Sensor Types: TGA, TGA-DTA, TGA-DSC (Cp)
  • Balance Resolution: 0.1 ug (over entire weighing range)
  • Sample Type: Ceramic, Glass, Metals, Melts / Liquids, Powders, Fibers and Multi-Layer Materials
  • Sample Volume: TGA - up to 10 ml, DSC - up to 85 ul
  • Evolved Gas Analysis: QMS (via capillary coupling)

The Aëolos QUADRO quadrupole mass spectrometer is a compact mass spectrometer with a heated capillary inlet system for routine analysis of gases and, in particular, volatile decomposition products of thermal analysis.

The system possesses the following features: • Single-step pressure reduction • Minimization of cold spots on the entire path of the gases due to an even temperature of maximum 300 °C • Heated chamber for easy handling and precise adjustment of the quartz glass capillary inlet to the QMS • Very robust and service-friendly while still maintaining high sensitivity (detectable mass loss in the μg-range) • TGA-MS measurements under humid atmospheres possible • Hyperbolic quadrupole system with pre-filter for improved transmission in the high mass range and improved sensitivity in the low mass range (e.g., H2, He) • SEM with discrete dynodes and integrated Faraday cup for high dynamic range and long lifetime STA & QMS

Setaram Microcalvet

The Setaram Microcalvet is a microcalorimeter our lab utilizes for a wide variety of materials and a wide variety of applications. As opposed to our Q2000, the Microcalvet can operate at extremely slow rates with very sensitive and accurate heat flow detection.

Microcalvet Capabilities

Capabilities of the Microcalvet include but are not limited to:

  • Determination of Thermophysical Properties

This includes: Latent Heat, Onset temperature, and Isobaric Specific Heat Capacity.

  • Investigation of Kinetically Limited Processes

The slow rates allow for direct investigation of a multitude of kinetically limited processes.

  • Investigation of Stability and Reversibility

A user-friendly, visual programming language interface that allows for extended cycling and data collection parameters.

Many more capabilities exist for this calorimeter, such as mixing and pressure-dependent measurements, but require external modules.

Microcalvet Specifications

  • Temperature range: -45 to 120 °C
  • Scanning Rates: 0.001 to 5 °C/min
  • Sample Sizes: 3-10 mg preferred, can measure up to 50 mg
  • Re-usable Hermetically Sealed Stainless Steel Vessel

Using the Setaram System

To schedule a sample run or inquire about using the system, please contact:

Chase Somodi

(216)-533-9942

[email protected]

Please see papers listed below for Setaram Writeup examples

C. B. Somodi, K. McCormick, D. P. Tabor, E. B. Pentzer, and P. J. Shamberger, "Kinetics of the plastic crystal transition in neopentyl glycol", Journal of Applied Physics, vol 135, no. 14, 2024, doi: 10.1063/5.0192791

S. Ahmed, D. Ibbotson, C. B. Somodi, and P. J. Shamberger, "Zinc nitrate hexahydrate pseudobinary eutectics for near-room-temperature thermal energy storage", ACS Applied Energy Materials, vol. 2, no. 3, 2023, doi: 10.1021/acsaenm.3c00444

TA Instruments Q2000

The TA Q2000 Differential Scanning Calorimeter is used for a wide variety of materials and applications. It measures the heat flow associated with changes in phase (phase transitions) as a function of time and temperature.

System Specifications

  • Autosampler

  • Liquid nitrogen cooling system

  • Controlled environment (Nitrogen gas)

  • Ambient pressure

  • Temperature range: -170°C to 725°C

  • Scanning rates: 0.1 to 40°C/min

  • Sample types: liquids, metals, powders

  • Sample size: 50 mg or less, 5-15 mg preferred

  • Sample holder: DSC pans/lids (aluminum, hermetic, non-hermetic, etc.)

Please see papers listed below for examples of DSC writeups:

S. Chakravarty, D. J. Sharar, and P. J. Shamberger, "Heterogeneous nucleation of gallium with lattice-matched cubic carbide and nitride phases," Journal of Applied Physics, vol. 130, no. 12, 2021, doi: 10.1063/5.0060207.

S. Ahmed, A. Hoe, F. Alamo, N. Turner, and P. J. Shamberger, "Experimental determination of high energy density lithium nitrate hydrate eutectics," Journal of Energy Storage, vol. 52, 2022, doi: 10.1016/j.est.2022.104754.

Simultaneous differential thermal analysis and thermal gravimetry (TA Q600)

The TA Q600 combines the capabilities of DSC and TGA, i.e, can give heat flow change and mass flow change as function of temperature and time.

Specification from Catalogue:

  • Sample Capacity 200 mg (350 mg including sample holder)
  • Balance Sensitivity 0.1 μg
  • Temperature Range Ambient to 1500 ˚C
  • Heating Rate – Ambient to 1000 ˚C 0.1 to 100 ˚C/min
  • Heating Rate – Ambient to 1500 ˚C 0.1 to 25 ˚C/min
  • Furnace Cooling Forced Air (1500 to 50 ˚C in < 30 min, 1000 ˚C in 50 ˚C in < 20 min)
  • DTA Sensitivity 0.001 ˚C
  • Calorimetric Accuracy/Precision ± 2% (based on metal standards)

* If you are using above 500°C please use ceramic pans.

This equipment is owned by Shamberger lab but is at the shared facility, i.e., is used by other groups on campus so please check the shared calendar to schedule equipment time.

To get trained on using theis equipment please contact : Dr. Anup Bandyopadhyay. Additionally, the primary user may be tasked with calibrating the equipment.

Please see papers listed below for examples of SDT writeups:

Overcoming Thermal Energy Storage Density Limits by Liquid Water Recharge in Zeolite-Polymer Composites