Abstract
An attempt has been made to review the development of thermoanalytical procedures as they have been applied to elastomers and elastomer systems over the past 10 years. For all rubber industry products, temperature and its effects, either alone or in conjunction with the chemical environment, play an important role from the production stage through to the final failure of the product in the field. It is thus not surprising that thermal analysis, in which temperature is the prime variable, has found such diverse applications in elastomer studies. The identification and quantitative analysis of rubber formulations have received most attention. Such formulations produce characteristic “fingerprints” when studied in DTA, DSC, TG, or TMA. In DSC, the determination of the glass transition characteristics, the observation and determination of crystallinity, the detection of cyclization reactions, and the monitoring of thermal and oxidative degradation characteristics can all be observed in a single experiment covering the temperature range from −150 to +600°C. At normal heating rates, e.g., 20°C/min, such information is available in 40 min. TG/DTG analysis can yield the elastomer or elastomers content, oil and plasticizer, carbon black (level and often type), and inorganic ash in less than 60 min. Processing and curing can also be studied. Blend compatibility can be assessed on the basis of both Tg and crystallinity measurements and the data used to determine optimum mixing times. Sulfur vulcanization and peroxide curing of elastomers is readily monitored by DSC and can be used for confirmation analysis of the presence of curatives. Limitations in such analysis exist, but as understanding and ability to interpret cure exotherms increase, valuable information about the mechanism and the nature of the cured network will be obtained. The testing of rubber compounds involves many hours of labor by current procedures. The rapidity of thermal analysis promises to offer some relief. In addition to DSC and TG, TMA, a relatively new technique, offers a rapid approach to low-temperature testing. Dynamic mechanical analysis (DMA) offers a rapid route to determining dynamic properties, but as yet, relatively little has been published on the application of this new technique to elastomers. As environmental concern increases, techniques such as evolved gas analysis (EGA) and combined techniques such as TG/gas chromatography are predicted to play an important role. As for the future, it is readily apparent that the principles of the methods have been established and, in several cases, it now remains to reduce them to a practical level. In some areas, such as vulcanization studies, much remains to be undertaken to improve our interpretive skills. Although there is some indication that certain industries have produced “in-house” standards for the analysis of rubber compounds by DSC and TG/DTG, it will only be when national and international standards organizations study and produce standard procedures, that the techniques will be generally adopted. Maurer's prediction in 1969 of increased applications of DTA and TG in elastomer studies has undoubtedly proved correct, and with the proliferation of reliable commercial instrumentation, significant developments can be anticipated in the next decade.
Assessment of Residual Solvent and Drug in PLGA Microspheres by Derivative Thermogravimetry