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Eingeladener Vortrag
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Der Beitrag präsentiert die erarbeiteten technischen Richtlinien zur Anwendung und Prüfung von Multigassensoren innerhalb der Richtlinienreihe VDI/VDE 3518 sowie in diesem Zusammenhang die Möglichkeiten der Sensorprüfung im akkreditierten Prüflabor des Fachbereichs 8.1 der BAM. Im Speziellen wird das in Kürze veröffentlichte Blatt 3 der Richtlinienreihe vorgestellt, das Bezug auf Multigassensoren für geruchsbezogene Messungen mit elektronischen Nasen nimmt.
Ammoniakemissionen in die Umwelt erfolgen insbesondere durch die Landwirtschaft (93,6 %), aber auch durch Verbrennungsprozesse in der die Abfallwirtschaft (2,3 %) und den Straßenverkehr (1,8 %). Dieser Stoff ist selbst in geringen Konzentrationen nicht nur eine Geruchsbelästigung, sondern auch eine Substanz mit ökologischer und klimatischer Relevanz.
Die Bestimmung von Ammoniak in relevanten Konzentrationen von kleiner 25 μg m-3 erfolgt im Allgemeinen über NH4+ als Analyten, spektralfotometrisch oder mit der Ionenchromatographie nach Überführung in die flüssige Phase. Wegen der niedrigen Konzentrationen an Ammoniak in der Außenluft wird meist eine gesammelte Probe verwendet oder die Bestimmung erfolgt nach einer aktiven, anreichernden Probenahme.
Die eigenen Arbeiten sollen dazu beitragen, die Ammoniak-Bestimmung in der Außenluft präziser, sowie schneller und kostengünstiger zu machen.
Die BAM prüfte daher kommerzielle elektrochemische und Metalloxid-basierte Sensoren, die für diesen Konzentrationsbereich aber nur bedingt geeignet sind. Deshalb wurden alternativ eigene Entwicklungen zum Nachweis von Ammoniak im Spurenbereich aufgenommen, wobei der Analyt über die Änderung der Fluoreszenz eines BODIPY-Farbstoffs bei 550 nm mittels eines portablen Fluoreszenz-Sensors direkt aus der Gasphase gemessen wird.
Zur Kalibrierung von Ammoniak-Sensoren und -Messgeräten steht ein stationäres System basierend auf der Mischung von zertifizierten Prüfgasen aus Druckflaschen mit kalibrierten Massendurchfluss-regler (MFC) zur Verfügung. Darüber hinaus erfolgt eine chemische Analyse der verwendeten Gasgemische mittels eines Massenspektrometers.
Für die Kalibrierung und Prüfung von Sensoren und Messgeräten vor Ort wurde ein mobiles Prüfsystem entwickelt. Die Generierung von Ammoniak-haltigen Gasen im Spurenbereich von 0,5 nmol/mol bis 500 nmol/mol erfolgt durch das Permeationsverfahren nach ISO 6145-10.
Für die Realisierung der Rückführbarkeit der Ammoniakbestimmung werden von den Nationalen Metrologischen Instituten sowie designierten Instituten Standards bereitgestellt und auch weiterentwickelt. Die primären metrologischen Standards beruhen auf SI-Einheiten und sind die Basis für eine Rückführbarkeit der Sensoren bzw. Analysengeräte.
Der Beitrag präsentiert die erarbeiteten technischen Richtlinien zur Anwendung und Prüfung von Multigassensoren innerhalb der Richtlinienreihe VDI/VDE 3518 sowie in diesem Zusammenhang die Möglichkeiten der Sensorprüfung im akkreditierten Prüflabor des Fachbereichs 8.1 der BAM. Im Speziellen wird das in Kürze veröffentlichte Blatt 3 der Richtlinienreihe vorgestellt, das Bezug auf Multigassensoren für geruchsbezogene Messungen mit elektronischen Nasen nimmt.
Moisture content and water activity are important parameters for quality characterization of products like bulk materials, powders, granules. Thus, an exact determination is necessarily required in a wide range of industrial applications. Moisture of materials is the content of non-chemically bound water in a solid or liquid. Water activity (aW) is a characteristic/parameter of the non-chemically bound ("free") water in materials and is measured as humidity over a solid/liquid surface at constant temperature (equilibrium moisture content). It is an important parameter to characterize the quality of e. g. pharmaceutical and food products. In our contribution, we present the developed MOISHUM device for staged determination of water activity and moisture content of liquid and solid materials.
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.
Trace humidity was measured by using miniaturized planar coulometric sensors in technical gases such as hydrogen, nitrogen, helium, nitrous oxide, and synthetic air. Frost point temperatures tf in the gases ranged from −60 °C to −30 °C, which is equivalent to a vapour mole fraction xv from 10 μmol mol−1 to 376 μmol mol−1. In addition, the generated humidity was determined by using a precision dew point hygrometer as reference. Nonlinear calibration functions were calculated that correlated electric current (sensor signal) and reference humidity. Parameters of functions were tested with one-way analysis of variances (ANOVA) to prove if all used sensors had a similar behavior in the same gas during experiments. Results of ANOVA confirmed that averaged functions can be applied for trace humidity measurement in nitrogen, helium, nitrous oxide, and synthetic air. The calculated functions were negligibly different for nitrogen, helium, and synthetic air. In humidified nitrous oxide, a minor change of parameters was observed due to lower electrical currents. In total contrast to that, the measured sensor signals were significantly higher in humidified hydrogen and each sensor required its own calibration function. The reason was a recombination effect that favoured multiple measurements of water molecules. Nevertheless, it was possible to measure continuously trace humidity in all tested gases by using coulometric sensors with an expanded uncertainty below 2 K (k = 2).
Moisture content and water activity are important parameters of product characterization; thus, an exact determination is necessarily required in a wide range of industrial applications. Moisture content of materials is the content of non-chemically bound water in a solid or liquid. Water activity (aW) is a characteristic/parameter of the non-chemically bound ("free") water in materials and is measured as humidity over a solid/liquid surface at constant temperature (equilibrium moisture content). It is an important parameter to characterize the quality of pharmaceutical and food products. In our contribution, we present a developed device for staged determination of water activity and moisture content of liquid and solid materials.
Emissions of ammonia into the environment are mainly caused by agriculture, but also by combustion processes in waste and by road traffic. Even at low concentrations, this substance is not only an odour nuisance, but also a substance with ecological and climatic relevance. Therefore, BAM tested commercial electrochemical, and metal oxide based sensors, which have limited suitability for measuring in the environmental molar fraction range. Alternatively, own developments for the detection of ammonia in the trace range were implemented, wherein the analyte is measured by changing the fluorescence of a BODIPY dye at 550 nm by means of a portable fluorescence sensor directly from the gas phase. For the calibration of ammonia sensors and measuring instruments, a stationary system based on the mixture of certified test gases from pressure cylinders with calibrated mass flow controllers is available. A test gas generator was developed for on-site calibration and testing of sensors and measuring devices. The generation of ammonia-containing gases in the environmental relevant range of levels below 1000 nmol/mol is carried out by the permeation method according to ISO 6145-10. For the traceability of ammonia, standards are provided and further developed by the National Metrological Institutes and designated institutes. Metrological standards are based on SI units and are a basis for traceability of sensors or gas analysers.
Leaking methane from infrastructures, such as pipelines and landfills, is critical for the environment but can also pose a safety risk. To enable a fast detection and localization of these kind of leaks, BAM developed a novel robotic platform for aerial remote gas sensing. Spectroscopic measurement methods for remote sensing of selected gases lend themselves for use on mini-copters, which offer a number of advantages for inspection and surveillance over traditional methods. No direct contact with the target gas is needed and thus the influence of the copter downwash on the measured gas plume can be kept to a minimum. This allows to overcome one of the major issues with gas-sensitive mini-copters. On the other hand, remote gas sensors, most prominently Tunable Diode Laser Absorption Spectroscopy (TDLAS) sensors have been too bulky given the payload and energy restrictions of mini-copters. Here, we present the Unmanned Aerial Vehicle for Remote Gas Sensing (UAV-REGAS), which combines a novel lightweight TDLAS sensor with a 3-axis aerial stabilization gimbal for aiming on a versatile multicopter. The proposed system can be deployed in scenarios that cannot be addressed by currently available systems and thus constitutes a significant step forward for the field of Mobile Robot Olfaction (MRO). It enables tomographic reconstruction of gas plumes and a localization of gas sources. We also present first results showing its performance under realistic conditions.
Planar coulometric sensors were investigated in humidified synthetic air at various absolute gas pressures, i. e. 2 bar, 5, bar, 10 bar, and 15 bar. Humidified gas flow at adjusted gas pressure was split into two flows, one passed a coulometric sensor and the other one passed a reference hygrometer after decompression. Both signals were recorded and then compared after calculation of resulting frost point temperature. Calculation is based on a calibration function obtained at ambient pressure. Comparison showed that an increasing pressure resulted in a higher derivation between sensor signal (calculated frost point temperature) and reference frost point temperature. At an absolute pressure of 2 bar the differences were minor in consideration of the uncertainty, however at 15 bar the differences were 6.77 K. Nevertheless, it was possible to measure the gas humidity at higher pressure with coulometric trace humidity sensors.