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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).
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.