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Organisationseinheit der BAM
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.
Humidity-Sensing Materials
(1999)
A silicon MIS-structure prepared with thin layers of the super-ionic conductor LaF3 and Pd is used to detect hydrogen. The sensor is able to detect hydrogen in a concentration range from below one ppm to the lower flammable limit in air which is 4 vol.-%. The chip operates at room temperature which results in an extremely low energy consumption compared to other hydrogen sensors. Only once per day a short heating pulse is necessary to reactivate the sensor chip. In cooperation with the BAM, a long-term experiment was carried out. The duration of the measurement was about three months, with a hydrogen exposure every two weeks. The sensor signal remained stable over the measured period.
A series of Mg₁₋ₓZnₓTiO₃, x = 0–0.5 (MZT0–MZT0.5) ceramics was synthesised and characterised. The dielectric properties of the samples in the frequency range of
1 Hz – 7.7 GHz were explored using three different methods:
a contacting electrode method, a parallel-plate method and a perturbed resonator method. The electrical properties in the space charge and dipolar polarisation frequency ranges are discussed in relation to the phase composition and microstructure data. Differences in the zinc Substitution divided the dielectrics into two groups, namely MZT0-MZT0.2 and MZT0.3–MZT0.5, each with different amount of a main Mg₁₋ₓZnₓTiO₃ solid solution phase and a secondary solid solution phase. Zinc substitution promoted the density of the ceramics, improved the purity of the main phase and increased the permittivity for frequencies up to 10⁸ Hz, but reduced the permittivity in the microwave range. In the MZT0.3–MZT0.5 samples, for frequencies less than 1 MHz the quality (Q x ƒ) factors were lower and log σ ₐ.c, the AC conductivity, was higher than for the MZT0–MZT0.2 samples. Above 10 MHz, the (Q x ƒ) factors and log σ ₐ.c of the two groups were similar.
This work reported the investigation on the effect of relaxation to the permittivity (epsilon' r ) characteristic of Mg1-x Zn x TiO3 ceramics for x = 0 – 0.5 (MZT0 – MZT0.5) measured from 1 Hz to 330 MHz. Within that frequency range, the relaxation effect that consists of the space charge (SC) and the dipolar (D) polarization mechanisms were identified. The contribution of the D relaxation in MZT0 – MZT0.2 systems extents overall from about 100 Hz to 330 MHz, while that in MZT0.3 – MZT0.5 systems is from 50 kHz to 330 MHz. The remaining frequencies, i.e. from 1 to 90 Hz for MZT0 – MZT0.2 and from 1 Hz to 50 kHz for MZT0.3 – MZT0.5, are attributed to the SC relaxation. The D polarization mechanism provides constant epsilon' r values which vary from (15.4 – 17.0) ± 0.3 throughout the samples. Contribution of the SC polarization mechanism to the characteristic is supported by the simultaneous presence of different content and level of resistivity of the secondary phase of (Mg1-αZnα)2TiO4 in MZT0 – MZT0.2 systems and of (Zn1-αMgα)2TiO4 in MZT0.3 – MZT0.5, along with the presence of the main Mg1-x Zn x TiO3 phase, as a result of the variation of zinc content in the systems.
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.
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).
A market survey has been performed of commercially available hydrogen safety sensors, resulting in a total sample size of 53 sensors from 21 manufacturers. The technical specifications, as provided by the manufacturer, have been collated and are displayed herein as a function of sensor working principle. These specifications comprise measuring range, response and recovery times, ambient temperature, pressure and relative humidity, power consumption and lifetime. These are then compared against known performance targets for both automotive and stationary applications in order to establish in how far current technology satisfies current requirements of sensor end users. Gaps in the performance of hydrogen sensing technologies are thus identified and areas recommended for future research and development.
Spices have an important impact on daily aliment. Changes of their quality resulting in far reaching consequences in different foodstuffs and imply financial losing and even health hazard. In this study it is demonstrated that application of two different portable multi gas sensors (electronic nose and ion mobility spectrometer) supported by multivariate data analysis can contribute to ensure quality control of spice mixtures and to find out product adulteration. Headspace above spice mixtures for sausages and saveloy and product counterfeitings was investigated by a metal oxide based electronic nose (e-nose of KAMINA-type). Linear discriminant analysis (LDA) of sensor resistivity data was performed for differentiation. Simultaneously an ion mobility spectrometer (IMS) was coupled to the emission chamber for detection of gaseous components above spice mixtures. The measured spectra show differences between the two spice mixtures and were discussed using a principal component analysis (PCA). The two multigas sensors permit discrimination between the types of spice mixtures and can indicate product adulteration. Additionally, a headspace gas analysis by gas chromatography was performed to identify the main volatile components and to prove the chemical basis for the observed differences of the multi gas sensors.