@incollection{KirchnerReisertSchoening2014, author = {Kirchner, Patrick and Reisert, Steffen and Sch{\"o}ning, Michael Josef}, title = {Calorimetric gas sensors for hydrogen peroxide monitoring in aseptic food processes}, series = {Gas sensing fundamentals. (Springer Series on Chemical Sensors and Biosensors ; 15)}, booktitle = {Gas sensing fundamentals. (Springer Series on Chemical Sensors and Biosensors ; 15)}, publisher = {Springer}, address = {Heidelberg}, isbn = {978-3-642-54518-4 (Print) ; 978-3-642-54519-1 (Online)}, doi = {10.1007/5346_2013_51}, pages = {279 -- 309}, year = {2014}, abstract = {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.}, language = {en} } @article{KirchnerReisertPuetzetal.2012, author = {Kirchner, Patrick and Reisert, Steffen and P{\"u}tz, Patrick and Keusgen, Michael and Sch{\"o}ning, Michael Josef}, title = {Characterisation of polymeric materials as passivation layer for calorimetric H2O2 gas sensors}, series = {Physica Status Solidi (a)}, volume = {209}, journal = {Physica Status Solidi (a)}, number = {5}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {1862-6319}, doi = {10.1002/pssa.201100773}, pages = {859 -- 863}, year = {2012}, abstract = {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.}, language = {en} } @article{HennemannKohlReisertetal.2013, author = {Hennemann, J{\"o}rg and Kohl, Claus-Dieter and Reisert, Steffen and Kirchner, Patrick and Sch{\"o}ning, Michael Josef}, title = {Copper oxide nanofibres for detection of hydrogen peroxide vapour at high concentrations}, series = {physica status solidi (a)}, volume = {210}, journal = {physica status solidi (a)}, number = {5}, publisher = {Wiley}, address = {Weinheim}, issn = {1862-6319}, doi = {10.1002/pssa.201200775}, pages = {859 -- 863}, year = {2013}, abstract = {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.}, language = {en} } @article{OberlaenderKirchnerBoyenetal.2014, author = {Oberl{\"a}nder, Jan and Kirchner, Patrick and Boyen, Hans-Gerd and Sch{\"o}ning, Michael Josef}, title = {Detection of hydrogen peroxide vapor by use of manganese(IV) oxide as catalyst for calorimetric gas sensors}, series = {Physica status solidi A: Applications and materials science}, volume = {211}, journal = {Physica status solidi A: Applications and materials science}, number = {6}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {1521-396X (E-Journal); 1862-6319 (E-Journal); 0031-8965 (Print); 1862-6300 (Print)}, doi = {10.1002/pssa.201330359}, pages = {1372 -- 1376}, year = {2014}, abstract = {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.}, language = {en} } @article{JildehKirchnerOberlaenderetal.2020, author = {Jildeh, Zaid B. and Kirchner, Patrick and Oberl{\"a}nder, Jan and Vahidpour, Farnoosh and Wagner, Patrick H. and Sch{\"o}ning, Michael Josef}, title = {Development of a package-sterilization process for aseptic filling machines: A numerical approach and validation for surface treatment with hydrogen peroxide}, series = {Sensor and Actuators A: Physical}, volume = {303}, journal = {Sensor and Actuators A: Physical}, number = {111691}, publisher = {Elsevier}, address = {Amsterdam}, issn = {0924-4247}, doi = {10.1016/j.sna.2019.111691}, year = {2020}, abstract = {Within the present work a sterilization process by a heated gas mixture that contains hydrogen peroxide (H₂O₂) is validated by experiments and numerical modeling techniques. The operational parameters that affect the sterilization efficacy are described alongside the two modes of sterilization: gaseous and condensed H₂O₂. Measurements with a previously developed H₂O₂ gas sensor are carried out to validate the applied H₂O₂ gas concentration during sterilization. We performed microbiological tests at different H₂O₂ gas concentrations by applying an end-point method to carrier strips, which contain different inoculation loads of Geobacillus stearothermophilus spores. The analysis of the sterilization process of a pharmaceutical glass vial is performed by numerical modeling. The numerical model combines heat- and advection-diffusion mass transfer with vapor-pressure equations to predict the location of condensate formation and the concentration of H₂O₂ at the packaging surfaces by changing the gas temperature. For a sterilization process of 0.7 s, a H₂O₂ gas concentration above 4\% v/v is required to reach a log-count reduction above six. The numerical results showed the location of H₂O₂ condensate formation, which decreases with increasing sterilant-gas temperature. The model can be transferred to different gas nozzle- and packaging geometries to assure the absence of H₂O₂ residues.}, language = {en} } @article{JildehKirchnerBaltesetal.2019, author = {Jildeh, Zaid B. and Kirchner, Patrick and Baltes, Klaus and Wagner, Patrick H. and Sch{\"o}ning, Michael Josef}, title = {Development of an in-line evaporation unit for the production of gas mixtures containing hydrogen peroxide - numerical modeling and experimental results}, series = {International Journal of Heat and Mass Transfer}, volume = {143}, journal = {International Journal of Heat and Mass Transfer}, publisher = {Elsevier}, address = {Amsterdam}, issn = {0017-9310}, doi = {10.1016/j.ijheatmasstransfer.2019.118519}, pages = {Article number 118519}, year = {2019}, abstract = {Hydrogen peroxide (H2O2) is a typical surface sterilization agent for packaging materials used in the pharmaceutical, food and beverage industries. We use the finite-elements method to analyze the conceptual design of an in-line thermal evaporation unit to produce a heated gas mixture of air and evaporated H2O2 solution. For the numerical model, the required phase-transition variables of pure H2O2 solution and of the aerosol mixture are acquired from vapor-liquid equilibrium (VLE) diagrams derived from vapor-pressure formulations. This work combines homogeneous single-phase turbulent flow with heat-transfer physics to describe the operation of the evaporation unit. We introduce the apparent heat-capacity concept to approximate the non-isothermal phase-transition process of the H2O2-containing aerosol. Empirical and analytical functions are defined to represent the temperature- and pressure-dependent material properties of the aqueous H2O2 solution, the aerosol and the gas mixture. To validate the numerical model, the simulation results are compared to experimental data on the heating power required to produce the gas mixture. This shows good agreement with the deviations below 10\%. Experimental observations on the formation of deposits due to the evaporation of stabilized H2O2 solution fits the prediction made from simulation results.}, language = {en} } @article{JildehOberlaenderKirchneretal.2018, author = {Jildeh, Zaid B. and Oberl{\"a}nder, Jan and Kirchner, Patrick and Keusgen, Michael and Wagner, Patrick H. and Sch{\"o}ning, Michael Josef}, title = {Experimental and Numerical Analyzes of a Sensor Based on Interdigitated Electrodes for Studying Microbiological Alterations}, series = {physica status solidi (a): applications and materials science}, volume = {215}, journal = {physica status solidi (a): applications and materials science}, number = {15}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {1862-6319}, doi = {10.1002/pssa.201700920}, pages = {Artikel 1700920}, year = {2018}, abstract = {In this work, a cell-based biosensor to evaluate the sterilization efficacy of hydrogen peroxide vapor sterilization processes is characterized. The transducer of the biosensor is based on interdigitated gold electrodes fabricated on an inert glass substrate. Impedance spectroscopy is applied to evaluate the sensor behavior and the alteration of test microorganisms due to the sterilization process. These alterations are related to changes in relative permittivity and electrical conductivity of the bacterial spores. Sensor measurements are conducted with and without bacterial spores (Bacillus atrophaeus), as well as after an industrial sterilization protocol. Equivalent two-dimensional numerical models based on finite element method of the periodic finger structures of the interdigitated gold electrodes are designed and validated using COMSOL® Multiphysics software by the application of known dielectric properties. The validated models are used to compute the electrical properties at different sensor states (blank, loaded with spores, and after sterilization). As a final result, we will derive and tabulate the frequency-dependent electrical parameters of the spore layer using a novel model that combines experimental data with numerical optimization techniques.}, language = {en} } @inproceedings{OberlaenderJildehKirchneretal.2015, author = {Oberl{\"a}nder, Jan and Jildeh, Zaid B. and Kirchner, Patrick and Wendeler, Luisa and Bromm, Alexander and Iken, Heiko and Wagner, Patrick and Keusgen, Michael and Sch{\"o}ning, Michael Josef}, title = {Experimental and numerical evaluation of interdigitated electrode array for monitoring gaseous sterilization processes}, series = {12. Dresdner Sensor-Symposium 2015}, booktitle = {12. Dresdner Sensor-Symposium 2015}, doi = {10.5162/12dss2015/P3.11}, pages = {163 -- 168}, year = {2015}, language = {en} } @article{JildehKirchnerOberlaenderetal.2017, author = {Jildeh, Zaid B. and Kirchner, Patrick and Oberl{\"a}nder, Jan and Kremers, Alexander and Wagner, Torsten and Wagner, Patrick H. and Sch{\"o}ning, Michael Josef}, title = {FEM-based modeling of a calorimetric gas sensor for hydrogen peroxide monitoring}, series = {physica status solidi a : applications and materials sciences}, journal = {physica status solidi a : applications and materials sciences}, number = {Early View}, publisher = {Wiley-VCH}, address = {Weinheim}, issn = {1862-6319}, doi = {10.1002/pssa.201600912}, year = {2017}, abstract = {A physically coupled finite element method (FEM) model is developed to study the response behavior of a calorimetric gas sensor. The modeled sensor serves as a monitoring device of the concentration of gaseous hydrogen peroxide (H2 O2) in a high temperature mixture stream in aseptic sterilization processes. The principle of operation of a calorimetric H2 O2 sensor is analyzed and the results of the numerical model have been validated by using previously published sensor experiments. The deviation in the results between the FEM model and experimental data are presented and discussed.}, language = {en} } @inproceedings{OberlaenderKirchnerKeusgenetal.2014, author = {Oberl{\"a}nder, Jan and Kirchner, Patrick and Keusgen, M. and Sch{\"o}ning, Michael Josef}, title = {Flexible polyimide-based calorimetric gas sensors for monitoring hy-drogen peroxide in sterilisation processes of aseptic filling machines}, series = {Sensoren und Messsysteme 2014 ; Beitr{\"a}ge der 17. GMA/ITG-Fachtagung vom 3. bis 4. Juni 2014 in N{\"u}rnberg. (ITG-Fachbericht ; 250)}, booktitle = {Sensoren und Messsysteme 2014 ; Beitr{\"a}ge der 17. GMA/ITG-Fachtagung vom 3. bis 4. Juni 2014 in N{\"u}rnberg. (ITG-Fachbericht ; 250)}, publisher = {VDE-Verl.}, address = {D{\"u}sseldorf}, organization = {VDI/VDE-Gesellschaft Mess- und Automatisierungstechnik}, isbn = {978-3-8007-3622-5}, pages = {1 -- 4}, year = {2014}, language = {en} }