Preparation of reference materials for the determination of RoHS-relevant flame retardants in styrenic polymers

AbstractReference materials for the analysis of polybrominated diphenyl ethers, polybrominated biphenyls and other common brominated flame retardants (FR) in styrenic polymers were prepared to suit the demands of actual restriction of the use of certain hazardous substances in electrical and electronic equipment analytics. Three methods of preparation were employed, viz. pellet forming, dissolution/vaporisation and extrusion, whereby extrusion proved to be the most suitable method. For extrusion, three procedures of pre-mixing were investigated: the polymers were either mixed with FR powder, FR solutions or FR concentrates that were taken from waste industrial polymers. The latter procedure proved to be most appropriate in terms of analyte concentration, predictability and recovery. The homogeneity of the samples, as well as the chemical and thermal long-term stabilities, was investigated. The result was an optimised method to prepare a suitable reference material for laboratory use. Figure 

[1]  D. Barceló,et al.  Optimization of congener-specific analysis of 40 polybrominated diphenyl ethers by gas chromatography/mass spectrometry. , 2002, Journal of mass spectrometry : JMS.

[2]  Rudi van Eldik,et al.  Identification of brominated flame retardants in polymeric materials by reversed-phase liquid chromatography with ultraviolet detection , 1998 .

[3]  A. Gelbin,et al.  Retention-time database of 126 polybrominated diphenyl ether congeners and two bromkal technical mixtures on seven capillary gas chromatographic columns. , 2005, Journal of chromatography. A.

[4]  Rudi van Eldik,et al.  Rapid identification of RoHS-relevant flame retardants from polymer housings by ultrasonic extraction and RP-HPLC/UV. , 2005, Journal of chromatography. A.

[5]  M. Riess,et al.  Identification of flame retardants in polymers using curie point pyrolysis-gas chromatography/mass spectrometry , 2000 .

[6]  R. van Eldik,et al.  Versatile and fast gas chromatographic determination of frequently used brominated flame retardants in styrenic polymers. , 2008, Journal of chromatography. A.

[7]  J. Björklund,et al.  Gas chromatography and mass spectrometry of polybrominated diphenyl ethers , 2003 .

[8]  H. Ortner,et al.  Influence of particle size on XRF wear analysis in plastics processing , 2005 .

[9]  Eva Jakobsson,et al.  Gas chromatographic identification and quantification of polybrominated diphenyl ethers in a commercial product, Bromkal 70-5DE , 1998 .

[10]  J. Pauwels,et al.  Uncertainty calculations in the certification of reference materials. 2. Homogeneity study , 2001 .

[11]  K. Weber Eine vereinfachte Formulierung des Korngrößeneinflusses , 1976 .

[12]  Martin Schlummer,et al.  Analysis of flame retardant additives in polymer fractions of waste of electric and electronic equipment (WEEE) by means of HPLC-UV/MS and GPC-HPLC-UV. , 2005, Journal of chromatography. A.

[13]  R. Hale,et al.  Detailed polybrominated diphenyl ether (PBDE) congener composition of the widely used penta-, octa-, and deca-PBDE technical flame-retardant mixtures. , 2006, Environmental science & technology.

[14]  E. Dyremark,et al.  Automated rotary valve injection for polybrominated diphenyl ethers in gas chromatography , 2003 .

[15]  E. Dyremark,et al.  Influence of the injection technique and the column system on gas chromatographic determination of polybrominated diphenyl ethers. , 2004, Journal of chromatography. A.