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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.
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).
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.