Thermoanalytical Methods in Vulcanizate Analysis II. Derivative Thermogravimetric Analysis

Abstract

Abstract We have shown in this and the preceding paper that fully compounded stocks can be analyzed for all main constituents by use of a combination of DSC, TG, and DTG. Further, this can be achieved on a time scale consistent with routine quality control. DSC gives information on cure characteristics, sulfur, and accelerator levels in approximately five minutes. Elastomer, elastomer ratio, carbon black, oil/plasticizer, and inorganic pigments are determined in about 35 minutes by TG/DTG, at a scan rate of 10°C/min. This time can be reduced by increasing the scan rate, but interference from highly exothermic reactions can be a limiting factor. Each compound must be treated individually to determine the maximum scan rate that can be used without impairing reproducibility. Clearly limitations exist for identification of unknown blends by DTG. The main problem is that many commercial elastomers have very similar thermal stabilities, which results in DTG peaks in the same temperature range. Further work is being undertaken with the DTG—gas chromatography interface to identify not only the pyrolysis products, but the temperature range over which they are evolved. In this manner, the DTG acts essentially as a thermal fraetionation unit and GC analysis of products from a given component in a blend can be achieved.