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Quantitative chemical analysis of airborne particulate matter (PM) is vital for the understanding of health effects in indoor and outdoor environments, as well as for enforcing air quality regulations. Typically, airborne particles are sampled over long time periods on filters, followed by lab-based analysis, e.g., with inductively coupled plasma mass spectrometry (ICP-MS). Within the EURAMET EMPIR AEROMET project, cascade impactor aerosol sampling was combined for the first time with on-site total reflection X-ray fluorescence (TXRF) spectroscopy to develop a tool for quantifying particle element compositions within short time intervals and even on-site. This makes variations of aerosol chemistry observable with time resolution of only a few hours and with good size resolution in the PM10 range. A proof of principles of this methodological approach and the comparison to standard methods within the scope of a field campaign will be presented. Secondly, aerosol sampling and TXRF analysis seems suitable for the quantification of elements in indoor aerosols as well and may provide an important enhancement of existing methods for the analysis of organic species in aerosols (such as sampling and TD-GC/MS). As an example, the TXRF analysis of particles emitted from laser printers under controlled conditions in an environmental test chamber will be presented.
The development of traceable new methodologies to quantify elemental air pollutants in particulate matter (PM) supports modernization of methods used in air quality monitoring networks in Europe. In the framework of the EURAMET EMPIR AEROMET II project, the combination of cascade impactor aerosol sampling and total reflection X-ray fluorescence elemental spectroscopy (TXRF) was investigated. This technique requires a traceable calibration based on reference samples. This paper describes a new, simple and effective method to produce such reference samples using flexible, reusable, and low-cost parylene C shadow masks, fabricated by photolithographic steps. These shadow masks can be used to produce reference samples that mimic the Dekati cascade impactor’s deposition patterns by applying as-prepared micro stencils to 30 mm acrylic substrates and evaporating a reference material (Ti) in arrangements of thin circular dots. The highly flexible direct patterning of acrylic discs with reference material, otherwise impossible with conventional photolithography, allows multiple reusing of the same micro stencils. The aspect ratios of the dots could be repeated with an error less than 4 %. A first set of standard reference samples for the 13 stages of the Dekati cascade impactor was produced and preliminary TXRF measurements of the deposited Ti masses were performed. The centricity of the deposition patterns turned out to be an important parameter for the quality of the TXRF results. The parylene mask technology for the production of reference samples turns out to be a promising new approach for the traceable calibration of TXRF spectrometers for the quantification of element concentrations in environmental aerosol samples but, due to its great versatility, it could be used for several other micropatterning applications on conventional and unconventional substrates.
Quantitative chemical analysis of airborne particulate matter (PM) is vital for the understanding of health effects in indoor and outdoor environments and required by EU air quality regulations. Typically, airborne particles are sampled on filters, followed by lab-based analysis, e.g., with inductively coupled plasma mass spectrometry (ICP-MS). Within the EURAMET EMPIR AEROMET project, cascade impactor aerosol sampling was combined with on-site total reflection X-ray fluorescence (TXRF) spectroscopy. The study aimed at a proof of principles for this new mobile and on-size tool for the quantification of aerosol element compositions and element mass concentrations within short time intervals of less than 12 h. In a field campaign the method’s technical feasibility could be demonstrated. The TXRF results were traced back to a stationary, reference-free XRS setup in the laboratory of the German national metrology institute PTB at the BESSY II electron storage ring in Berlin, Germany. Simultaneous PM10-filter sampling, followed by standardized lab-based analysis, allowed for a comparison of the field campaign data of both methods. As Fig. 1 shows, the correspondence between PM10 filter sampling and ICP-MS, and on the other hand, cascade impactor sampling and TXRF is quite encouraging. However, for some of the analysed elements, e.g. V and Pb, the observed deviations are higher than expected and this highlights the fact, that spectral deconvolution strategies for TXRF on cascade impactor samples still need some improvement.
This work was supported by the EMPIR programme, co-financed by the Participating States and from the European Union’s Horizon 2020 research and innovation programme, through grant agreements 16ENV07 AEROMET and 19ENV08 AEROMET II
Quantitative chemical analysis of airborne particulate matter (PM) is vital for the understanding of health effects in indoor and outdoor environments, as well as for enforcing EU air quality regulations. Typically, airborne particles are sampled over long time periods on filters, followed by lab-based analysis, e.g., with inductively coupled plasma mass spectrometry (ICP-MS). During the EURAMET EMPIR AEROMET project, cascade impactor aerosol sampling is combined for the first time with on-site total reflection X-ray fluorescence (TXRF) spectroscopy to develop a tool for quantifying particle element compositions within short time intervals and even on-site. This makes variations of aerosol chemistry observable with time resolution only a few hours and with good size resolution in the PM10 range. The study investigates the proof of principles of this methodological approach. Acrylic discs and silicon wafers are shown to be suitable impactor carriers with sufficiently smooth and clean surfaces, and a non-destructive elemental mass concentration measurement with a lower limit of detection around 10 pg/m3 could be achieved. We demonstrate the traceability of field TXRF measurements to a radiometrically calibrated TXRF reference, and the results from both analytical methods correspond satisfactorily.