TY - RPRT A1 - Kemmlein, Sabine A1 - Bergmann, Meike A1 - Jann, Oliver T1 - Standard measurement method for the determination of polybrominated flame retardants (pentabromo diphenylether, octabromo diphenylether) in products (Research Report 202 67 300 / UBA-FB 000839/e) T2 - UBA-Texte N2 - In accordance with the Directive 2003/11/EC amending the Council Directive 76/769/EEC for the 24th time, pentabromo and octabromo diphenylethers may not be used or put on the market in concentrations higher than 0.1 % by mass. To verify this threshold value a standard measurement method for the determination of selected pentabromo diphenylethers (pentaBDE-isomers) and octabromo diphenylethers (octaBDE-isomers) in polymers based on gas chromatography mass spectrometry (GC/MS) was developed. The following target compounds were selected for the investigations: BDE85 (2,2’,3,4,4’-pentaBDE), BDE99 (2,2’,4,4’,5- pentaBDE), BDE100 (2,2’,4,4’,6-pentaBDE), BDE203 (2,2’,3,4,4’,5,5’,6-octaBDE), BDE196 (2,2’,3,3’,4,4’,5,6’-octaBDE), BDE197 (2,2’,3,3’,4,4’,6,6’-OctaBDE). The following reference materials were prepared: polyurethane (PUR-H) and epoxy resin (EP) containing 0.1 % by mass of sum of pentaBDE isomers, polystyrene (PS) and acrylnitril-butadiene-styrenecopolymer (ABS) containing 0.1 % by weight of sum of octaBDE isomers. For quality assurance of the standard measurement method an interlaboratory comparison was conducted between 1 June and 30 November 2004 where 18 participants were involved. Data assessment was performed in accordance with DIN ISO 5725-2:2002-12 “Accuracy (trueness and precision) of measurement methods and results – Part 2: Basic methods for the determination of repeatability and reproducibility of a standard measurement method”. The following general mean values and standard deviations were obtained: 1.09 ± 0.16 mg g-1 (15 %) (sum pentaBDE isomers/EP), 1.3 ± 0.19 mg g-1 (15 %) (sum pentaBDE isomers/PUR-H), 0.99 ± 0.27 mg g-1 (27 %) (sum octaBDE isomers/PS), 0.42 ± 0.11 mg g-1 (26 %) (sum octaBDE isomers/ABS). The reproducibility standard deviation sRj and repeatability standard deviation srj were calculated as statistical parameters. The repeatability of the sum of pentaBDE isomers in EP was srj= 0.044 mg g-1 (4.0 %) and the reproducibility was sRj = 0.167 mg g-1 (15 %). srj and the sRj were 0.038 mg g-1 (2.9 %) and 0.195 mg g-1 (15 %), respectively, for the sum of pentaBDE isomers in PUR-H. For the sum of octaBDE isomers in ABS srj and sRj were determined to 0.029 mg g-1 (6.9 %) and 0.114 mg g-1 (27 %), respectively. For the sum of octaBDE isomers in PS the srj = 0.043 mg g-1 (4.3 %) and sRj = 0.255 mg g-1 (26 %) were obtained. KW - Pentabromo Diphenylether (pentaBDE) KW - Octabromo Diphenylether (octaBDE) KW - Polymer KW - Reproducibility KW - Repeatability KW - Directive 2003/11/EC KW - Directive 76/769/EEC KW - GC/MS KW - Polybrominated flame retardants PY - 2005 UR - http://www.umweltbundesamt.de/publikationen/standard-measurement-method-for-determination-of SN - 1862-4804 SN - 0722-186X IS - 31 SP - 1 EP - 151 PB - Umweltbundesamt CY - Dessau-Roßlau AN - OPUS4-12129 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -