DIN EN 16694:2015-12

Polybrominated diphenyl ethers (PBDE) are priority substances listed in Annex X of the EU Water Framework Directive (WFD, Directive 2000/60/EC) for which environmental quality standards (EQS) have been set at EU level for inland waters as well as other surface waters to protect the aquatic environment against chemical pollution (Directive 2008/105/EC). With the exception of metals, the EQS are expressed as total concentrations in the whole water sample. Furthermore, analytical methods used in WFD monitoring need to meet certain requirements as regards the minimum limit of quantification and the maximum tolerable measurement uncertainty (Directive 2009/90/EC). So far, there is no standardized method available for the determination of PBDE in whole water samples fulfilling those requirements. Hence, the European Commission mandated CEN to develop or improve standards in support of the implementation of the monitoring requirements of WFD. Directive 2008/105/EC has been amended by Directive 2013/39/EU; however, this standard has been developed for the analysis of PBDE as listed in Annex A of Directive 2008/105/EC. The priority substances list in Annex X of the WFD includes technical pentabromodiphenyl ether, which is regarded as a mixture of the congeners BDE-28, BDE-47, BDE-99, BDE-100, BDE-153 and BDE-154. The annual average environmental quality standard (AA-EQS) for pentabromodiphenyl ether in inland surface waters is 0,5 ng/l and is defined for the whole water sample including suspended particulate matter (SPM) present in the sample. Compounds such as PBDE strongly adsorb to environmental solids resulting in a fraction bound to particles, which may be substantial. The aim of the method is to extract whole water samples in one single step to determine the dissolved as well as the particle bound PBDE fraction. Identification and quantification of BDE congeners at trace level concentrations require both highly sensitive chromatographic equipment and effective enrichment steps and awareness of the potential impact of blanks. This European Standard specifies a method for the determination of six selected polybrominated diphenyl ethers (PBDE), representative for technical pentabromodiphenyl ethers (BDE) in water samples in mass concentrations ≥0,025 ng/l. The method uses solid-phase extraction with SPE-disks in combination with gas chromatography-mass spectrometry (GC-MS). It is applicable to the analysis of PBDE in surface water containing suspended particulate matter (SPM) up to 500 mg/l (whole water samples), drinking water and groundwater. The limit of quantification (LOQ) was determined according to ISO/TS 13530, on the basis of replicate determinations of the procedural blank, carried out under reproducibility conditions. This method may be used for the analysis of other BDE congeners not listed in Table 1 or other types of water. However, it is important to verify its applicability before use. This document (EN 16694:2015) has been prepared by Technical Committee CEN/TC 230 "Water analysis", the secretariat of which is held by DIN (Germany). The responsible German committee is Subcommittee NA 119-01-03-02 UA "Organische Verbindungen" ("Organic compounds") of Working Committee NA 119-01-03 AA "Wasseruntersuchung" ("Water examination") at DIN Standards Committee Water Practice (NAW).