THE HEBREW UNIVERSITY CENTER FOR NANOSCIENCE AND NANOTECHNOLOGY

Simultaneous Thermogravimetry - Differential Scanning Calorimetry coupled with Mass Spectrometry (STA TG-DSC MS)


Overview of Technique

The simultaneous application of Thermogravimetry (TG) and Differential Scanning Calorimetry (DSC) to a single sample in an STA instrument yields more information than separate application TG and DSC in two different instruments. STA enables simultaneous quantitative monitoring of mass- and thermodynamical changes which occur in the tested material under heating. Coupling of MS to the instrument for thermal analysis allows identification of materials/components being evolved during the heating experiment. Therefore combination of STA TG-DSC with MS provides a unique straightforward tool for distinct experimental characterization of chemical reactions and phase transformation in a wide range of materials.
Our STA-MS instrument is manufactured by NETZSCH-Geratebau GmbH (http://www.netzsch-thermal-analysis.com/en/products-solutions/simultaneous-thermogravimetry-differential-scanning-calorimetry.html?tx_solr%5Bfilter%5D%5B0%5D=productAutomaticSamplerChanger%253AYes&tx_solr%5Bfilter%5D%5B1%5D=productCategory%253ASimultaneous%2BThermogravimetry%2B-%2BDifferential%2BScanning%2BCalorimetry&tx_solr%5Bfilter%5D%5B2%5D=productPurpose%253AHigh%2BTemperature ).

Basics and Tutorials

Please, read about basics of thermal analysis in the following web resources:

Equipment Specifications

STA TG-DSC 449 F3 Jupiter®
Furnace Silicon Carbide
Temperature range -150°C to 1550°C
Heating rates 0.001 K/min to 50 K/min
Cooling rate(free cooling) 1540 to 100°C : 60 min
Weighing range 35 g
Max. initial weight 35 g
Atmospheres inert (N2, Ar), oxidizing (dry air), reducing (Ar+5% H2su ), vacuum
Integrated mass flow controller for 2 purge gases and 1 protective gas
High vacuum-tight assembly up to 10-4 mbar (10-2 Pa)
Automatic sample changer (ASC) for up to 20 samples and references (optional)
Coupling to Mass Spectrometer over a heatable adapter

The STA 449 F3 Jupiter® runs under Proteus® Software on Windows® XP and Windows7®. The Proteus® Software includes everything needed to carry out a measurement and evaluate the resulting data. The Proteus® software is licensed with the instrument and can be installed on other computer systems.

QMS 403 D Aeolos®
Mass range 1 u to 300 u
Analog scan scan rates> 0.2 s/amu
Scan Bargraph scan rates > 200 ms/amu
Ion source electron impact, energy 100 eV
Detector Faraday and SEV (Channeltron)
Multi Ion Detection (MID)Vacuum system turbomolecular pumps and diaphragm pumps (oil-free vacuum)
Quartz-glass capillary 5 µm diameter, in metal tube, with supply coil, easily exchangeable
Adjustable heating of adapter head, capillary and QMS inlet system to a maximum of 300°C
  • 2 Y2O3coated iridium cathodes
  • Bypass system for extraction of gas at the furnace
  • Optimized ion source (response time, sensitivity, service life)
  • Coupling with DSC, TG, STA, DIL via heated adapters
  • Characteristic temperatures (Onset, Peak and End)
  • Peak areas for quantitative evaluation and calibration
  • Spectra subtraction
The QMS 403 D Aeolos® runs in couplings with NETZSCH thermal analysis instruments under Proteus® Software on Windows®.