Netzsch Differential Scanning Calorimeter Precision and Mass Spectrometer

Two high vacuum Differential Scanning Calorimeter machines allow for determination of caloric effects of a sample by measurement of the difference in the heat flow rate between a sample and a reference. One is a platinum furnace allowing high precision measurement and the other is a silicon carbide furnace paired with a mass spectrometer.

Instrument Overview

The DSC instruments allow for the acquisition of quantitative and qualitative data on endothermic and exothermic processes of a sample as it undergoes chemical or physical changes induced by changing temperature. This is done by measuring the heat flow into, or out of, the sample as a function of temperature. This enables the characterization of the material’s thermal transitions. Due to the high precision of the system they can also be used to determine the Wigner energy, the energy trapped in a crystiline material caused by irradiation damage. A quadrapole mass spectrometer ionizes chemical species evolved from the samples in the DSC and is used to characterise and identify species based on the individual mass to charge ratio. These systems have been modified for use in a radioactive environment (MRF research room).

Applications:

  • For the analysis of solids or powder samples
  • Thermal transitions
    • Melting temperature and enthalpy
    • Glass transition temperature
    • Crystallisation temperature and enthalpy
    • Phase transformations and diagrams
    • Transition enthalpies
    • Reaction enthalpy and kinetics
    • Degree of crystallinity
    • Specific heat
    • Purity
  • Thermal history of a sample
  • Wigner Energy determination
  • Mass spectrometer
    • Specific heat capacity
    • Melting and crystallization
    • Phase transformations

Technical Specification:

Platinum Furnace:

  • 25-1500°C
  • 50 K/min maximum heating rate in the 1200°C temperature range
  • 20 K/min maximum heating rate above the 1200°C temperature range
  • Pt-Rh meander heater
  • Air-cooled double shell
  • Integrated protective tube for gas flow with stop valve
  • Noise resolution of<50 nV, and accuracy of 1.5°C or 0.25%.

Silicon Carbide Furnace:

  • 25-1600°C (with a mass spectrometer)
  • 50 K/min maximum heating rate in the 1200°C temperature range
  • 20 K/min maximum heating rate above the 1200°C temperature range
  • SiC heating element
  • Al2O3 protective tube for gas flow with stop valve
  • Noise resolution of<50 nV, and accuracy of 1.5°C or 0.25%.

Mass Spectrometer:

  • 1 u to 300 u mass range
  • 0.5 u to 1.5 u resolution
  • 25 eV to 150 eV electron energy
  • 0.1 mA to 2 mA emission current
  • > 100 u/s (scan bar graph) electronic scan rate
  • Single-step pressure reduction, no orifice
  • Crossbeam EI ion source
DSC undergoing integration into a Research Room

DSC undergoing integration into a Research Room

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