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Thermal analysis (TGA, TG-MS, ATD-GCMS)

thermal analysis

Simultaneous Thermal Analysis - Mass Spectrometry (STA-MS)

This equipment comprises a NETZSCH STA (Simultaneous Thermal Analysis) 409PG Luxx® coupled to an Aëolos mass spectrometer via a new heated capillary system. Essentially TG and DTA information can be determined simultaneously alongside real-time evolved gas analysis by mass spectrometry (EGA-MS).

Thermogravimetric – Differential Thermal Analysis (TG-DTA)

TG is a technique by which the mass of a sample is monitored as a function of temperature or time, whereas DTA is a technique by which the heat flow to or from a sample when compared to a reference is monitored. In both instances the sample is subjected to a controlled temperature program. Varied information can be gleaned from the analysis, which includes that detailed in the table below.

 TG

DTA 

Mass changes 

Glass transitions 

Temperature stability

Melting temperatures 

Composition content = moisture,
solvent, additives, polymer, filler.

Phase formations/transitions 

Oxidation/Reduction studies 

Reaction kinetics 

Decomposition temperatures/Kinetics

 

Dehydration

 

Solvent loss 

 

The STA equipment allows high accuracy and resolution in the sub-μg range as well as excellent stability. The furnace allows temperatures from room temperature to 1500 °C to be studied with heating rates from 0.1 to 50 °C/min. Samples weighing up to 5 grams can be tested. Thermal events under both reactive (e.g. air) and inert gases (e.g. nitrogen, helium and argon) can be investigated.

Evolved Gas Analysis - Mass Spectrometry (EGA-MS)

During real-time EGA, the mass spectrometer ionises the evolved gases, which are identified by their characteristic fragments. The spectrometer can either scan over a range of 0-300 amu or monitor individual ions of interest. In addition to real-time analysis the evolved gasses can be trapped on to activated carbon and subsequently analysed by Gas Chromatography-Mass Spectrometry. This can aid the identification of multiple evolved gases when complex samples are analysed.

ATD – Gas Chromatography – Mass Spectrometry (ATD-GC-MS)

ATD-GCMS

This equipment comprises a Perkin Elmer Automated Thermal Desorber (Turbomatrix 350) linked to a Perkin Elmer Clarus 500 Gas Chromatograph and Mass Spectrometer. Any gases of interest that are trapped on activated carbon can be desorbed using the ATD, individually separated by the gas chromatograph and then identified using mass spectrometry. This is a very powerful and sensitive technique when complex mixtures of evolved gases are produced.

Projects and Consultancy

The combination of Thermal Analysis and Evolved Gas Analysis (EGA) delivers extremely valuable information for material characterisation in research, development, and production areas such as polymers, composites, ceramics, catalysts, metals, pharmaceuticals, etc.

Within the thermal analysis suite at MERI, TGA, Differential Scanning Calorimetry (DSC) and Thermo-mechanical Analysis (TMA) equipment (Mettler Toledo) are also available. These are used for more 'routine analysis' and also allow samples to be prioritised and selected for further detailed analysis by STA-MS.

All the equipment is used for research in academic, industrial and consultancy projects.

Who to Contact

For more information about thermal analysis, please contact us at MERI@shu.ac.uk or 0114 225 3500.

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