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Eingeladener Vortrag
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Especially trace amounts of water vapour in gases can be reliably determined by coulometric trace humidity sensors. The principle of these sensors is based on water vapour absorption in a hygroscopic layer and its subsequent electrolytic decomposition. The calibration of sensors was performed in the humidity range, expressed as frost point temperature, from −30°C to −80°C . This range is equivalent to volume fractions smaller than 376 µL·L−1. Generated humidity was measured with coulometric sensors and a chilled dew point hygrometer that was used as reference. An empirical non-linear function was found between sensor signal and measured reference humidity. This function consists of two parameters with a measurement uncertainty. Both calibration parameters were checked by means of one-way analysis of variance. It showed that gas specific function can be used for humidity measurement in nitrogen, hydrogen, dinitrogen monoxide, compressed and synthetic air. It is possible to determine trace humidity in all tested gases with an expanded uncertainty less than 2.1 K (coverage factor k=2 ) regarding frost point temperature.
Pollution through emission of toxic gases is an increasing problem for the environment. It affects similarly agricultural, industrial and urban areas. In future, environmental emissions in ambient air must be monitored at even lower concentrations as nowadays. One environmental relevant compound is ammonia and its conversion product ammonium that have strong negative impact on human health and ecosystems. Most ammonia measurements in ambient air are performed in the range below 1000 nmol·mol-1 and thus there is a need for reliable traceable ammonia gas standards and in addition in situ analytical procedures for monitoring (in ambient air to avoid that thresholds are exceeded). Therefore, the use of reference materials is necessary for development accompanying test or for calibration, e. g. of structure-integrated sensors and mobile multi-gas sensors.
The developed gas standard generator produces gas mixtures that comply with the metrological traceability for ammonia gas standards in the desired environmentally relevant measurement range. The method is based on the permeation of ammonia through a membrane at constant temperature and pressure. The resulting ammonia penetrant gas flow is then mixed with a carrier gas flow to generate a gas standard flow of known concentration. The dynamic rage is enlarged by using a two dilution steps. Depending on the permeation rate, generable molar fractions are possible in the range nmol·mol-1 to a few µmol·mol-1. We present the design of an ammonia gas standard generator and first results of the characterisation of its individual components supporting the uncertainty assessment according to GUM for stable gas concentrations in this range. The relative uncertainty of the generated ammonia gas standard is smaller than 4 % (k = 2).
Technische Richtlinien enthalten Empfehlungen sowie Anforderungen zum Stand der Technik zur Aufstellung von Bewertungskriterien und Behandlung wissenschaftlich-technischer Fragen. Sie fördern den Erfahrungsaustausch und Technologietransfer zwischen Entwicklern und Anwendern.
In unserem Beitrag stellen wir die Richtlinie VDI/VDE 3518 vor. Diese Richtlinienreihe definiert Begriffe, beschreibt den Aufbau und klassifiziert Multigassensoren (Blatt 1), befasst sich mit den Anforderungen für das Unterscheiden, Erkennen und mengenmäßige Bestimmen von Gemischen gasförmiger Stoffe und die Prüfung von Multigassensoren (Blatt 2) und gibt Anleitung für geruchsbezogene Messungen mit „Elektronischen Nasen“ (Blatt 3). Multigassensoren können als elektronische Nasen in Anlehnung an den biologischen Geruchssinn zur Wahrnehmung und Charakterisierung von Gerüchen eingesetzt werden. Die Spezifik von Multigassensoren besteht darin, dass durch die Wahl und Betriebsweise der Sensoren eine Vielzahl von geeigneten Messsignalen erzeugt werden, aus denen mit mathematischen Verfahren die für die Anwendung gewünschten Informationen extrahiert werden. Dazu ist ein Training der Messeinrichtung mit Proben bekannter Eigenschaften notwendig.
Diese Richtlinie soll Herstellern, Anbietern und Nutzern als ein Leitfaden Informationen und Erläuterungen für die korrekte und sichere Arbeit mit Multigassensoren liefern. Sie soll Prüflaboratorien und Anwendern helfen, bei der Beurteilung von Qualitätsmerkmalen einheitlich vorzugehen und dafür gemeinsame Randbedingungen anzugeben
A hydrogen sensor based on a silicon Metal/Solid Electrolyte/Insulator/Semiconductor (MEIS) structure with thin layers of the super-ionic conductor LaF3 and Pd gate metal was investigated in a hybrid structure on a resistance heater mounted on a ceramic substrate. The sensor was operated at room temperature, however, a short heating impulse once a day ensures a fast and reproducible dynamic behavior. The sensor was characterized in the concentration range typical for alarm levels up to 40% of the lower flammability limit and shows a logarithmic dependency of the sensor signal from the hydrogen concentration and a mean sensitivity of about 140 mV/decade. The response time (t90) is about 8 s. In a long term test for a period of three month, the sensor was exposed to hydrogen every two weeks. The sensor signal was shown to be stable in dynamic behavior, sensitivity and signal difference.
The chapter describes the application of electronic noses (multigas sensors) for the quality control of spices and spice mixtures. Electronic noses were successfully applied for headspace analysis of spices. It was demonstrated in many investigations that electronic noses can contribute to the characterization of spices and spice mixtures in order to distinguish spices and spice mixtures, differentiate by origin, growth seasons,and processing,indicate adulteration from original, detect mold infestation. Electronic noses can be used as a fast screening method to provide information about the product quality. However, it needs samples and methods for reference, careful training, and complex calibration to consider influencing and disturbing effects as well as the possible limitations of the instrumentation. The correlation to classical chemical analysis methods is always advisable. Machined olfaction methods are capable to support the sensory analysis; however, they cannot yet substitute them.
The efficiency of gas sensor application for facilitating the safe use of hydrogen depends considerably on the sensor response to a change in hydrogen concentration. Therefore, the response time has been measured for five different-type commercially available hydrogen sensors. Experiments showed that all these sensors surpass the ISO 26142 standard; for the response times t90 values of 2 s to 16 s were estimated. Results can be fitted with an exponential or sigmoidal function. It can be demonstrated that the results on transient behaviour depend on both the operating parameters of sensors and Investigation methods, as well as on the experimental conditions: gas change rate and concentration jump.
Hydrogen sensors - A review
(2011)
Hydrogen sensors are of increasing importance in connection with the development and expanded use of hydrogen gas as an energy carrier and as a chemical reactant. There are an immense number of sensors reported in the literature for hydrogen detection and in this work these sensors are classified into eight different operating principles. Characteristic performance parameters of these sensor types, such as measuring range, sensitivity, selectivity and response time are reviewed and the latest technology developments are reported. Testing and validation of sensor performance are described in relation to standardisation and use in potentially explosive atmospheres so as to identify the requirements on hydrogen sensors for practical applications.
Five miniaturized sensors based on dew-point,
capacitance or resistance measurement were tested for the
detection of humidity in compressed gases.
The dew-point sensors with optical or dielectric detection of
condensation were used at gas pressures up to 3 MPa in
dew-point range of -20 to 70°C and show no systematic
deviation and an uncertainty of dew-point temperature
mostly less than 1 K. The LiCl sensor has also a low
uncertainty but exhibit a systematic deviation to higher
values of dew-point. Capacitive polymer sensors can
indicate also a dew-point, even down to -70 °C and have an
uncertainty of about 1 to 2 K. The oxide sensor works in the
dew-point range of -10 to 20°C and has a signal what
exponential decreases with increasing gas pressure up to 10
MPa.
All types of sensor can be applied in compressed gases at
least up to 3 MPa, but their different change of sensor signal
due to the gas pressure has to be considered.
The efficiency of gas sensor application for facilitating the safe use of hydrogen depends to a considerable extent on the response time of the sensor to change in hydrogen concentration. The response and recovery times have been measured for five different hydrogen sensors, three commercially available and two promising prototypes which operate at room temperature.
Experiments according to ISO 26142 show that most of the sensors surpass much for a concentration change from clean to hydrogen containing air the demands of the Standard for the response times t(90) and values of 2 to lös were estimated. For an opposite shift to clean air, the recovery times t(10) are from 7 to 70 s. Results of transient behaviour can be fitted with an exponential approach. It can be demonstrated that results on transient behaviour depend not only from investigation method, and the experimental conditions, like gas changing rate and concentration jump, as well as from operating
Parameters of sensors. In comparison to commercial MOS and MIS-FET hydrogen sensors new sensor prototypes operating at room temperature possesses in particular longer recovery times.