Abstract
The self-ignition behaviour of bulks is usually determined with the aid of isoperibolic or adiabatic hot storage tests; the sample volumes here are typically in the range of approx. 100 cm³ to several litres. The extrapolation to technically relevant volumes holds, however, considerable uncertainties. To reduce these uncertainties, a test stand was set up that allows to investigation sample sizes of up to 1000 dm³. These allow the study of self-ignition behavior closer to the conditions that prevail in practice. The suitability (or unsuitability) of the established methods (including dangerous goods classification tests) were to be demonstrated and influencing variables that cannot be measured on a laboratory scale were to be determined.
In addition, various analytical methods were used for the determination of reaction kinetic data of solid bulk materials and to predict the self-ignition behaviour of large storages. These are thermal analyses such as differential scanning calorimetry DSC, simultaneous thermal analysis STA as well as microcalorimetry for high-precision measurement of heat flows.
Complete test series using all mentioned test methods will be presented for crosslinked polyvinyl-pyrrolidone (PVP) and conclusions regarding the applicability of the extrapolation methods will be discussed. Hot storage tests up to semi-industrial scale and their combination with various thermoanalytical methods allow a much more precise prediction of the self-ignition behaviour of large bulks. A further promising approach to estimate their heat release rates, and hence, the risk of self-ignition under technical conditions, is the use of microcalorimetric methods.
