Filtern
Dokumenttyp
- Beitrag zu einem Tagungsband (6)
- Zeitschriftenartikel (3)
- Vortrag (2)
Schlagworte
- Coulometric sensors (4)
- Trace humidity measurement (3)
- ANOVA (2)
- Measurement uncertainty (2)
- Messunsicherheit (2)
- Chemical reaction (1)
- Chemical sensors (1)
- Coulometric humidity sensor (1)
- Coulometric sensor (1)
- Elektrolyseverfahren (1)
Organisationseinheit der BAM
Eingeladener Vortrag
- nein (2)
Die Spurenfeuchte von technischen Gasen kann zuverlässig mit coulometrischen Feuchtesensoren bestimmt werden. Das Prinzip dieser Sensoren basiert auf der Absorption von Wasser in einer hygroskopischen Schicht und anschließenderelektrolytischer Zersetzung. Die Kalibrierung der Sensoren erfolgte mit einem Spurenfeuchtegenerator bei Frostpunkttemperaturen kleiner als -30 °C bzw. einem Volumenanteil kleiner als 376 µL·L-1. Die generierte Feuchte wurde zusätzlich zu den coulometrischen Sensoren mit einem Taupunktspiegelhygrometer, welches als Referenz diente, gemessen. Zwischen dem coulometrischen Sensorsignal und der gemessenen Referenzfeuchte wurde eine empirische nichtlinare Funktion gefunden. Die resultierende Kalibrierungsfunktion, die aus zwei Parametern besteht, wurde hinsichtlich ihrer Messunsicherheit bewertet.
Zusätzlich erfolgt die Überprüfung der Kalibrierparameter mittels einfaktorieller Varianzanalyse (ANOVA). Die ANOVA zeigte, dass eine gemittelte Funktion für die Feuchtigkeitbestimmung in Stickstoff, Helium und synthetischer Luft für mehrere Sensoren angewendet werden kann.
Mit coulmetrischen Sensoren ist es möglich, die Spurenfeuchte in technischen Gasen mit einer erweitereten Unsicherheit hinsichtlich der Frostpunkttemperatur kleiner als 2,1 K zu ermitteln.
Planar coulometric sensors were tested in humidified synthetic air at various gas temperatures. Generated frost point temperature in the gas ranged from -30 °C to -60 °C and were measured by coulometric sensors and in addition by a calibrated dew point hygrometer. The gas temperatures, which were measured by a calibrated Pt100 sensor, were set to -20 °C, 0 °C, 23 °C, 40 °C, 50 °C, and 60 °C during the experiments. Empiric nonlinear functions were calculated between the generated humidity and the sensor signals. In comparison to the measured signals at 23 °C, the sensor signals were lower at the other gas temperatures. The measurements at 60 °C showed indistinct results due to a great signal noise. The response behavior of the sensors was similar at 23 °C, 40 °C and 50 °C. In contrast to that, the sensors reacted slowly at a gas temperature of -20 °C and 0 °C. In summary, with coulometric sensors it was possible to measure continuously trace humidity with an expanded uncertainty below 2 K.
This work presents a first attempt to use ionic liquids as a new coating for planar coulometric sensors. These sensors are used for the measurement of trace humidity in various gases. Usually, the coating of the sensors is tetraphosphorus decaoxide and its hydrolysis products. Instead, a hygroscopic ionic liquid was used as sensor coating in this work. Generated frost point temperatures tf in the gas ranged from -80 °C to -30 °C, which is equivalent to vapour mole fractions xv from 0.5 μmol·mol-1 to 376 μmol·mol-1. In addition to the coulometric sensors, the generated humidity is determined by a precision dew point hygrometer as reference. First results show that it is possible to measure humidity with ionic liquid based coulometric sensors.
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.
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.
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).
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.
A portable device for calibration of trace humidity sensors and an adopted calibration procedure have been developed. The calibration device is based on humidity generation by permeating water through polymeric membrane tubes. Water vapour transmission rates for various polymers were experimentally determined in order to select the most suitable polymeric material. The developed trace humidity generator consists of a gas-flow polymeric hose immersed in a water reservoir thermostated by a sensorcontrolled heater. Mole fractions of water vapour between 1 µmol/ molˉ¹ and 350 µmol/molˉ¹ (equivalent to frost-point temperatures from -76 °C to -31 °C) were generated by varying either the operating temperature or gas flow. The operating temperature can be varied from 20 °C to 60 °C and kept stable within 0.1 K. Uncertainty analysis indicated that the trace humidity generator produces gas flows of constant humidity amounts with a relative expanded uncertainty less than 3.4% (k = 2) of the generated value.