TY - CONF A1 - Iznaguen, Hassan A1 - Ostermann, Markus A1 - Traub, Heike A1 - Piechotta, Christian T1 - Homogeneity of dispersed brominated flame retardants (HBCD) in polystyrene by LA-ICP-MS and XRF N2 - Polybrominated Flame retardants (PBFR) are of concern as emerging pollutants resulting from plastic waste, which set them free because these additives are not chemically bonded to the polymer. For this reason we fortunately use the laser ablation inductive coupled mass spectrometry (LA-ICP-MS) to verify the amount of 1,2,5,6,9,10-Hexabromocyclododecane (HBCD) in polystyrene (PS) resp polybrominated diphenylether (BDE-209) in polypropylene (PP). Results from X-ray fluorescence spectroscopy (RFA) are compared with those from LA-ICP-MS for studying the homogeneity of PBFR such as BDE-209 (0.1% wt. in PP) or HBCD (1% wt. in PS). RFA is well suited for the reason that it is a rapid, non-destructive and sensitive method. We also use the LA-ICP-MS as reference method for quantification of the content of PBFR herein and by measurement of ABS (acrylonitrile–butadiene–styrene, ABS) and correlate these data with RFA measurements. The necessity for the proof of homogeneity of BFR additives resulting from the use of these samples for weathering studies we perform to discover unknown transformation process and to get a certified reference method. For studying the homogeneity partition of BFR in PS or PP, we need to estimate the relation V/N (V=ablated volume, N=molar amount) for any studied area, which is in case of a homogenous partition for every area identical. To measure the ablated volume we applied the white light interference microscopy from which we derived the theoretical amount of ablated flame retardant. In correlation to an ablated CRM we get the molar amount of ablated BFR. From the counts (RFA) resp. the ratio of peak area of the bromine isotope we derive the concentration of BFR in ablated PS resp. PP. Another approach uses the applied external standard addition using RFA scanning. A cylindrical probe of defined geometry, corresponding to a defined amount of BFR, was removed from PS. Into this hole was added a solution of BFR of defined concentration and letting dried. RFA scanning of background and the hole gives a direct confirmation of the included amount of BFR herein. According to ISO 13528 samples for proficiency tests were acknowledged as homogenous if the criteria for homogeneity ss<0.3sigma were fulfilled. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - LA-ICP-MS KW - RFA KW - PBFR PY - 2017 AN - OPUS4-40248 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Iznaguen, Hassan A1 - Piechotta, Christian A1 - Ostermann, Markus A1 - Traub, Heike T1 - Homogeneity of dispersed brominated flame retardants (HBCD) in polystyrene by LA-ICP-MS and XRF N2 - To investigate the release or migration of flame retardants from polypropylene (PP) and polysytrene (PS) samples with a defined content of flame retardants as additives were prepared and used. Therefore a distinct 1,2,5,6,9,10-hexabromocyclododecane HBCD concentration of 1 wt.% in PS resp. a specified bromodiphenylether (BDE-209) of 0.1 wt.% in PP is defined. For the preparation of the samples granular PP or PS are extruded together with the BFR additives. Even the result of this process may lead to homogenous partitions of the BFR additives. So, the distribution of these additives must be proven before using the samples in an experimental setup for weathering studies. In accordance to the regulation of RoHS (2011/65/EU) , where the use of XRF is recommended for the proof of flame retardants in electronic consumer products, we use this method as a reference to the laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Therefore we present the correlation of these experiments. The experimental setup for the XRF experiment is like a standard addition: in cavities, which are introduced in the sample plates subsequently, solutions of defined concentration of flame retardants are put in there. According to the idea of standard addition, we get an information of the originating mass fraction of flame retardant in each sample and we can monitor the release and migration of these additives during/after the weathering experiments with high precision. An internal standard of HBCD is added as a marker and can be analyzed after the weathering experiment. T2 - 8th European Weathering Symposium EWS CY - Wien, Austria DA - 20.09.2017 KW - LA-ICP-MS KW - XRF KW - BFR PY - 2017 AN - OPUS4-43313 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -