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Analysis of Thermoset Materials, Precursors and Products

Smithers Information Ltd, Aug 2003, Pages: 160


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Thermosets comprise around 25% of world plastic consumption. The use of thermosets dates back over 100 years to the advent of phenolics. Today, a large range of different reactive chemicals is used in the synthesis of these resins. Common thermoset systems include phenol-formaldehyde, melamine-formaldehyde, urea-formaldehyde, resorcinol-formaldehyde, epoxy, polyurethane, polyalkyd , silicone, polyester, acrylic, furan and polyimide.

A variety of additives are found in thermosets. Plasticiser-type compounds are used to promote flow in high viscosity compounds such as epoxy resins. Particulate fillers are used to reduce cost or improve properties and fibrous materials for increased strength and rigidity. Other additives include antidegradants, curing agents (hardeners and accelerators), flame retardants and lubricants.

Thermosets are used in a wide range of applications from mouldings and composites to adhesives. Analysis of thermosets is carried out to determine the reasons for failure, for quality control, to measure residual monomer, to detect contaminants, to monitor the extent of cure and for deformulation. Materials based on thermosets present the analyst with considerable challenges due to their complexity and the wide range of polymer types and additives available. The author of this review has many years of experience in the Polymer Analysis division at Rapra Technology Limited. He has a practical understanding of the usefulness and feasibility of the many techniques on offer to the chemist.

Wet chemistry techniques were mainly used historically. One example is the spectrophotometric titration of epoxy groups using a halogen acid and 2,4-dinitrobenzene sulfonate as the chromophore.

Spectroscopic techniques include infrared spectroscopy, ultraviolet, nuclear magnetic resonance, atomic absorption, X-ray fluorescence and Raman spectroscopy.

Chromatographic techniques include gas chromatography- mass spectrometry, HPLC, liquid chromatography-mass spectrometry, gel permeation chromatography, thin layer chromatography and supercritical fluid chromatography.

Thermal techniques used to analyse thermosets include differential scanning calorimetry, dynamic mechanical thermal analysis, thermal mechanical analysis, thermogravimetric analysis and dielectric analysis.

There are many other analytical techniques covered in this review, which describes their specific uses and even set up details for some analytical techniques. The references at the end of the report describe many specific instances of the analysis of thermoset materials published over the last 10 years.

The review is accompanied by around 400 abstracts from papers and books in the Rapra Polymer Library database, to facilitate further reading on this subject. A subject index and a company index are included.


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