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Self-ignition Behaviour of Bulk Materials: How Reliable is the Extrapolation of Laboratory Tests?
(2022)
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 selfignition 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 highprecision 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.
Self-ignition Behaviour of Bulk Materials: How Reliable is the Extrapolation of Laboratory Tests?
(2022)
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 selfignition 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 highprecision 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.
The thermal decomposition of dicumyl peroxide dissolved in ethylbenzene has been studied in our laboratories using differential scanning calorimetry (DSC), calvet calorimetry (C80), adiabatic calorimetry, reaction calorimetry and micro calorimetry.
Based on the DSC and C80 experiments a formal kinetics model has been derived, which was compared to the other applied techniques. Finally we used our model to predict the thermal response of 216.5 L steel drums to exposure to constant elevated temperatures, both using the stationary Semenov approach as well as time-resolved CFD simulations. The prediction was compared to one-to-one testing using the UN-Test H.1. The observed level of consistency between model and experiments is remarkably good. The comparison with the 216.5 L testing clearly demonstrates that reliable and conservative predictions for technically relevant scales are possible as long as a validated model is used.
Estimation of self-heating temperatures for large volumes - application of heat flux measurement
(2019)
Model free estimation of activation energy from DSC can show strong deviation from other methods (complex mechanism).
First results show good agreement between heat flux from adiabatic and isothermal microcalorimeter.
Due to high sensitivity of microcalorimeters the extrapolation can be checked at relevant storage temperatures.
Higher reliability for extrapolations (check of applied model).
Heat flux measurements provide an alternative test method.