Thermal desorption GC-MS as a tool to provide PAH certified standard reference material on particulate matter quartz filters.

Reference materials for particulate matter (PM) on filter media are not available for the quantification of polycyclic aromatic hydrocarbons (PAHs) in ambient air. This is due to the difficulty of obtaining reference material that has a homogeneous distribution on a filter surface that is large enough for characterization and distribution. High volume sample filters from different locations and seasons were considered to validate the feasibility of the use of quartz filters as reference material for PAH concentrations. A rapid thermal desorption (TD) technique coupled with gas chromatography/mass spectroscopy was applied to characterise the material for the content of fifteen different PAHs. TD technique allowed for rapid and accurate analysis of small sections of filter (5mm diameter), leaving enough material for the production of twenty sub-filter cuts (42 mm diameter) that could be used for distribution and control. Stability and homogeneity tests required for material certification were performed as indicated by the ISO guide 34:2009 and ISO 35:2006. The contribution of the heterogeneous distribution of PAHs on the filter surface resulted generally lower than 10% and higher for more volatile PAHs. One year of storage at -18°C indicated no significant variation in PAH concentrations. Nevertheless, a methodology for shipping and storing of the filter material at ambient temperature in especially designed plastic envelopes, was also shown to allow for stabile concentrations within twenty days. The method accuracy was confirmed by the analysis of NIST SRM 1649a (urban dust) and PAH concentrations were validated against the reference values obtained from an inter-laboratory exercise. In the case of benzo[a]pyrene for masses quantified between 100 pg and 10 ng the TD method provided expanded uncertainties of circa 10%, while the inter-laboratory reference value uncertainties ranged between 15 and 20%. The evaluation of these results supports the use of the presented methodology as a valid approach for the certification of PAH concentrations in PM10 quartz filters. The methodology allows for the production of a certificate of analysis for a single high volume filter, the concentration of which can easily be adjusted by selecting an appropriate sampling location.
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