Characterisation of polymeric materials as passivation layer for calorimetric H2O2 gas sensors
(2012)
Calorimetric gas sensors for monitoring the H₂O₂ concentration at elevated temperatures in industrial sterilisation processes have been presented in previous works. These sensors are built up in form of a differential set-up of a catalytically active and passive temperature-sensitive structure. Although, various types of catalytically active dispersions have been studied, the passivation layer has to be established and therefore, chemically as well as physically characterised. In the present work, fluorinated ethylene propylene (FEP), perfluoralkoxy (PFA) and epoxy-based SU-8 photoresist as temperature-stable polymeric materials have been investigated for sensor passivation in terms of their chemical inertness against H₂O₂, their hygroscopic properties as well as their morphology. The polymeric materials were deposited via spin-coating on the temperature-sensitive structure, wherein spin-coated FEP and PFA show slight agglomerates. However, they possess a low absorption of humidity due to their hydrophobic surface, whereas the SU-8 layer has a closed surface but shows a slightly higher absorption of water. All of them were inert against gaseous H₂O₂ during the characterisation in H₂O₂ atmosphere that demonstrates their suitability as passivation layer for calorimetric H₂O₂ gas sensors.
The present work describes a novel multiple sensor-type system for the real-time analysis of aseptic sterilisation processes employing gaseous hydrogen peroxide (H2O2) as a sterilant. The inactivation kinetics of Bacillus atrophaeus by gaseous H2O2 have been investigated by means of a methodical calibration experiment, taking into account the process variables H2O2 concentration, humidity and gas temperature. It has been found that the microbicidal effectiveness at H2O2 concentrations above 2% v/v is largely determined by the concentration itself, while at lower H2O2 concentrations, the gas temperature and humidity play a leading role. Furthermore, the responses of different types of gas sensors towards the influencing factors of the sterilisation process have been analysed within the same experiment. Based on a correlation established between the inactivation kinetics and the sensor responses, a calorimetric H2O2 sensor and a metal-oxide semiconductor (MOX) sensor have been identified as possible candidates for monitoring the microbicidal effectiveness of aseptic sterilisation processes employing gaseous H2O2. Therefore, two linear models that describe the relationship between sensor response and microbicidal effectiveness have been proposed.
For the sterilisation of aseptic food packages it is taken advantage of the microbicidal properties of hydrogen peroxide (H2O2). Especially, when applied in vapour phase, it has shown high potential of microbial inactivation. In addition, it offers a high environmental compatibility compared to other chemical sterilisation agents, as it decomposes into oxygen and water, respectively. Due to a lack in sensory detection possibilities, a continuous monitoring of the H2O2 concentration was recently not available. Instead, the sterilisation efficacy is validated using microbiological tests. However, progresses in the development of calorimetric gas sensors during the last 7 years have made it possible to monitor the H2O2 concentration during operation. This chapter deals with the fundamentals of calorimetric gas sensing with special focus on the detection of gaseous hydrogen peroxide. A sensor principle based on a calorimetric differential set-up is described. Special emphasis is given to the sensor design with respect to the operational requirements under field conditions. The state-of-the-art regarding a sensor set-up for the on-line monitoring and secondly, a miniaturised sensor for in-line monitoring are summarised. Furthermore, alternative detection methods and a novel multi-sensor system for the characterisation of aseptic sterilisation processes are described.