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Sterilisation processes are compulsory in medicine, pharmacy, and food industries to prevent infections of consumers and microbiological contaminations of products. Monitoring the sterilisation by conventional microbiological methods is time- and lab-consuming. To overcome this problem, in this work a novel biosensor has been proposed. The sensor enables a fast method to evaluate sterilisation processes. By means of thin-film technology the sensor's transducer structures in form of IDEs (interdigitated electrodes) have been fabricated on a silicon substrate. Physical characterisation of the developed sensor was done by AFM, SEM, and profilometry. Impedance analyses were conducted for the electrical characterisation. As microbiological layer spores of B. atrophaeus have been immobilised on the sensing structure; spores of this type are a well-known sterilisation test organism. Impedance measurements at a fixed frequency over time were performed to monitor the immobilisation process. A sterilisation process according to aseptic filling machines was applied to demonstrate the sensor functionality. After both, immobilisation and sterilisation, a change in impedance could successfully be detected.
The sterilization of packages in aseptic food processes is highly significant to maintain a consumer-safe product with extended shelf-life. Today, the sterilization of food packages is predominantly accomplished by gaseous hydrogen peroxide (H2O2) in combination with heat. In order to monitor this sterilization process, calorimetric gas sensors as differential set-up of two platinum temperature sensors representing a catalytically active (additionally deposition of MnO2) and a passive segment have been recently developed. The temperature rise of the exothermic decomposition serves as an indicator of the present H2O2 concentration. In the present work, a theoretical approach considering the sensor’s thermochemistry and physical transport phenomena was formulated to evaluate the temperature rise based on the energy content of gaseous H2O2. In a further part of this work, three polymers have been analyzed with respect to their application as passivation materials. The examined polymers are photoresist SU-8, perfluoroalkoxy (PFA) and fluorinated ethylene propylene (FEP). Thermal analyses by means of differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA) have been conducted to determine the operation limits of the polymers. The overall chemical resistance and stability of the polymers against the harsh environmental conditions during the sterilization process have been examined by attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR).
In this work, the catalyst manganese(IV) oxide (MnO2), of calorimetric gas sensors (to monitor the sterilization agent vaporized hydrogen peroxide) has been investigated in more detail. Chemical analyses by means of X-ray-induced photoelectron spectroscopy have been performed to unravel the surface chemistry prior and after exposure to hydrogen peroxide vapor at elevated temperature, as applied in the sterilization processes of beverage cartons. The surface characterization reveals a change in oxidation states of the metal oxide catalyst after exposure to hydrogen peroxide. Additionally, a cleaning effect of the catalyst, which itself is attached to the sensor surface by means of a polymer interlayer, could be observed.
In the present work, a novel method for monitoring sterilisation processes with gaseous H2O2 in combination with heat activation by means of a specially designed calorimetric gas sensor was evaluated. Therefore, the sterilisation process was extensively studied by using test specimens inoculated with Bacillus atrophaeus spores in order to identify the most influencing process factors on its microbicidal effectiveness. Besides the contact time of the test specimens with gaseous H2O2 varied between 0.2 and 0.5 s, the present H2O2 concentration in a range from 0 to 8% v/v (volume percent) had a strong influence on the microbicidal effectiveness, whereas the change of the vaporiser temperature, gas flow and humidity were almost negligible. Furthermore, a calorimetric H2O2 gas sensor was characterised in the sterilisation process with gaseous H2O2 in a wide range of parameter settings, wherein the measurement signal has shown a linear response against the H2O2 concentration with a sensitivity of 4.75 °C/(% v/v). In a final step, a correlation model by matching the measurement signal of the gas sensor with the microbial inactivation kinetics was established that demonstrates its suitability as an efficient method for validating the microbicidal effectiveness of sterilisation processes with gaseous H2O2.
A wireless sensor system based on the industrial ZigBee standard for low-rate wireless networking was developed that enables real-time monitoring of gaseous H2O2 during the package sterilization in aseptic food processes. The sensor system consists of a remote unit connected to a calorimetric gas sensor, which was already established in former works, and an external base unit connected to a laptop computer. The remote unit was built up by an XBee radio frequency (RF) module for data communication and a programmable system-on-chip controller to read out the sensor signal and process the sensor data, whereas the base unit is a second XBee RF module. For the rapid H2O2 detection on various locations inside the package that has to be sterilized, a novel read-out strategy of the calorimetric gas sensor was established, wherein the sensor response is measured within the short sterilization time and correlated with the present H2O2 concentration. In an exemplary measurement application in an aseptic filling machinery, the suitability of the new, wireless sensor system was demonstrated, wherein the influence of the gas velocity on the H2O2 distribution inside a package was determined and verified with microbiological tests.
We present a sensor concept based on copper(II)oxide (CuO) nanofibres for the detection of hydrogen peroxide (H2O2) vapour in the percent per volume (% v/v) range. The fibres were produced by using the electrospinning technique. To avoid water condensation in the pores, the fibres were initially modified by an exposure to H2S to get an enclosed surface. By a thermal treatment at 350 °C the fibres were oxidised back to CuO. Thereby, the visible pores disappear which was verified by SEM analysis. The fibres show a decrease of resistance with increasing H2O2 concentration which is due to the fact that hydrogen peroxide is an oxidising gas and CuO a p-type semiconductor. The sensor shows a change of resistance within the minute range to the exposure until the maximum concentration of 6.9% v/v H2O2. At operating temperatures below 450 °C the corresponding sensor response to a concentration of 4.1% v/v increases. The sensor shows a good reproducibility of the signal at different measurements. CuO seems to be a suitable candidate for the detection of H2O2 vapour at high concentrations.
Resistance behaviour of the sensor under exposure to H2O2 vapours between 2.3 and 6.9% v/v at an operating temperature of 450 °C.