Water quality - Determination of selected polybrominated diphenly ether (PBDE) in whole water samples - Method using solid phase extraction (SPE) with SPE-disks combined with gas chromatography - mass spectrometry (GC-MS)

This European Standard specifies a method for the determination of six selected polybrominated diphenyl ethers (PBDEs) listed in Table 1, representative for technical BDEs in water samples in mass concentrations ≥ 0,025 ng/l (for each individual congener). (The limit of quantification (LOQ) should be determined according to ISO 13530, on the basis of replicate determinations of the procedural blank, carried out under reproducibility conditions.) The method uses solid-phase disk extraction (SPE-disk) in combination with gas chromatography-mass spectrometry (GC-MS). It is applicable to the analysis of PBDEs in surface water containing suspended particulate matter (SPM) up to 500 mg/l (whole water samples), drinking water and groundwater.
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.
(...)

Wasserbeschaffenheit - Bestimmung von ausgewählten polybromierten Diphenylethern (PBDE) in Gesamtwasserproben - Verfahren mittels Festphasenextraktion (SPE) mit SPE-Disks in Verbindung mit Gaschromatographie-Massenspektrometrie (GC-MS)

Diese Europäische Norm legt ein Verfahren für die Bestimmung von sechs ausgewählten polybromierten Diphenylethern (PBDE), repräsentativ für technisches pentaPBDE, in Wasserproben fest, wie in Tabelle 1 angegeben. Die Mindest-Bestimmungsgrenze für jedes einzelne Kongener in Gesamtwasserproben liegt bei Massenkonzentrationen von  0,025 ng/l. Die Bestimmungsgrenze (BG) sollte nach ISO/TS 13530 auf Grundlage von Mehrfachbestimmungen von Blindwertproben unter wiederholbaren Bedingungen bestimmt werden.) Das Verfahren nutzt die diskbasierte Festphasenextraktion SPE-Disk) in Kombination mit Gaschromatographie-Massenspektroskopie (GC MS). Die Norm gilt für die Analyse von PBDE in Oberflächenwasser mit einem Schwebstoffanteil bis zu 500 mg/l (Gesamtwasserproben), Trinkwasser und Grundwasser.
Dieses Verfahren kann für die Analyse weiterer BDE-Kongenere, die nicht in Tabelle 1 angegeben sind, oder andere Arten von Wasser angewendet werden, dies muss jedoch vorher verifiziert werden.
(...)

Qualité de l'eau - Dosage du pentabromodiphényléther (PBDE) dans des échantillons d'eau totale - Méthode par extraction en phase solide (SPE) avec disques SPE, avec couplage chromatographie en phase gazeuse-spectrométrie de masse (CG-SM)

La présente Norme européenne spécifie une méthode pour le dosage des concentrations massiques  0,025 ng/l (pour chaque congénère individuel) d'une sélection de six éthers diphényliques polybromés (PBDE, voir Tableau 1) représentatifs des BDE dans des échantillons d'eau. (Il convient de déterminer la limite de quantification (LQ) conformément à la norme ISO 13530, sur la base de déterminations répétées du blanc d'analyse effectuées dans des conditions de reproductibilité.) Cette méthode utilise une extraction en phase solide avec disques (disques SPE) combinée à une chromatographie en phase gazeuse-spectrométrie de masse (CG-SM). Elle s'applique à l'analyse des PBDE dans les eaux de surface qui contiennent jusqu'à 500 mg/l (échantillons d'eau dans leur intégralité) de matières en suspension (MES), dans l'eau potable et dans les eaux souterraines.
Cette méthode peut être utilisée pour analyser d'autres congénères BDE non mentionnés dans le Tableau 1, ou d'autres types d'eau ; cependant, il est important de vérifier son applicabilité avant de l'employer.
(...)

Kakovost vode - Določevanje pentabromodifeniletra (PBDE) v celotnem vzorcu vode z ekstrakcijo na trdni fazi (SPE) s SPE-diski v kombinaciji s plinsko kromatografijo/masno spektrometrijo (GC/MS)

Razvoj metode za kvantitativno določevanje analogov pentabromodifeniletra, ki predstavljajo tehnično formulacijo pentabromodifeniletra v celotnih vzorcih vode z uporabo plinske kromatografije/masne spektrometrije (GC-MS).
V skladu z Direktivo 2008/105/ES se upoštevajo naslednji analogi:
– BDE28
– BDE47
– BDE99
– BDE100
– BDE153
– BDE154
Ta analitska metoda določa določevanje pentabromodifeniletrov, ki izpolnjujejo naslednje zahteve:
– analiza celotnih vzorcev vode, ki vsebujejo do 0,5 g/l trdnih delcev;
– meja določljivosti (LOQ) mora biti enaka ali manjša od 30 % EQS;
– merilna negotovost mora biti enaka ali manjša od 50 %;
– pred medlaboratorijskim potrjevanjem morajo biti metode v celoti preverjene interno in testirane glede robustnosti;
– evropska medlaboratorijska študijska primerjava bo potekala v skladu s standardom ISO 5725.

General Information

Status
Published
Publication Date
22-Sep-2015
Withdrawal Date
30-Mar-2016
ICS
13.060.50 - Examination of water for chemical substances
Technical Committee
CEN/TC 230 - Water analysis
Drafting Committee
CEN/TC 230 - Water analysis
Current Stage
9093 - Decision to confirm - Review Enquiry
Start Date
09-Feb-2022
Completion Date
14-Apr-2025
Directive
2000/60/EC - Directive 2000/60/EC of the European Parliament and of the Council of 23 October 2000 establishing a framework for Community action in the field of water policy (substitutes Directive Reference 01/991 - Common Position on WFD)
Mandate
M/424 - Mandate for standardisation addressed to CEN for the development or improvement standards in support of the water framework directive
Ref Project
SIST EN 16694:2015 - Water quality - Determination of pentabromodiphenyl ether (PBDE) in whole water samples using solid phase extraction (SPE) with SPE-disks combined with gas chromatography - mass spectrometry (GC-MS)

Overview

EN 16694:2015 - Water quality: Determination of selected polybrominated diphenyl ethers (PBDEs) in whole water samples - describes a validated analytical method combining solid-phase extraction (SPE) with SPE‑disks and gas chromatography–mass spectrometry (GC‑MS). The standard targets six PBDE congeners representative of technical pentabromodiphenyl ether mixtures (BDE‑28, BDE‑47, BDE‑99, BDE‑100, BDE‑153, BDE‑154) at mass concentrations ≥ 0.025 ng/L per congener. It is designed to extract both dissolved and particle‑bound fractions from whole water (including suspended particulate matter up to 500 mg/L), and is applicable to surface water, drinking water and groundwater.

Key Topics and Requirements

  • Scope and analytes: Defines six target PBDE congeners; allows extension to other congeners after verification of applicability.
  • Sample preparation: Addition of 13C‑labelled or analogous internal standards to a 1 L water sample, followed by extraction on SPE‑disks to capture dissolved and particulate fractions in one step.
  • Instrumentation: Primary detection by GC‑HRMS (EI); alternative detection modes include low‑resolution NCI‑MS or MS/MS - note that alternatives may require additional clean‑up (multilayer silica, GPC, sulfur removal).
  • Performance characteristics: Limit of quantification (LOQ) established per ISO 13530 using procedural blanks under reproducibility conditions; calibration and quantification procedures described (internal standards, linear range checks).
  • Quality control: Emphasis on blank control, batch‑to‑batch SPE disk consistency, system checks, and recovery assessment for internal standards.
  • Interferences & clean‑up: Guidance on avoiding extraction and chromatographic interferences and on when to apply additional clean‑up steps (Annex D).

Applications and Users

  • Regulatory monitoring: Designed to support monitoring under the EU Water Framework Directive (WFD) and associated EQS for PBDEs (whole water).
  • Environmental laboratories: Accredited and contract labs performing trace organic analysis of water for PBDEs.
  • Water utilities & authorities: Screening and compliance testing for surface water, groundwater and drinking water.
  • Research: Investigations of PBDE fate, partitioning between dissolved and particulate phases, and long‑term trend monitoring.

Related Standards

  • EN ISO 3696 - Water for analytical laboratory use
  • EN ISO 5667‑1 / EN ISO 5667‑3 - Water sampling guidance and preservation
  • ISO 8466‑1 - Calibration and evaluation of analytical methods

Keywords: EN 16694:2015, PBDE, pentabromodiphenyl ether, SPE‑disk, solid phase extraction, GC‑MS, water quality, whole water samples, LOQ, Water Framework Directive, environmental monitoring.

Frequently Asked Questions

EN 16694:2015 is a standard published by the European Committee for Standardization (CEN). Its full title is "Water quality - Determination of selected polybrominated diphenly ether (PBDE) in whole water samples - Method using solid phase extraction (SPE) with SPE-disks combined with gas chromatography - mass spectrometry (GC-MS)". This standard covers: This European Standard specifies a method for the determination of six selected polybrominated diphenyl ethers (PBDEs) listed in Table 1, representative for technical BDEs in water samples in mass concentrations ≥ 0,025 ng/l (for each individual congener). (The limit of quantification (LOQ) should be determined according to ISO 13530, on the basis of replicate determinations of the procedural blank, carried out under reproducibility conditions.) The method uses solid-phase disk extraction (SPE-disk) in combination with gas chromatography-mass spectrometry (GC-MS). It is applicable to the analysis of PBDEs in surface water containing suspended particulate matter (SPM) up to 500 mg/l (whole water samples), drinking water and groundwater. 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 European Standard specifies a method for the determination of six selected polybrominated diphenyl ethers (PBDEs) listed in Table 1, representative for technical BDEs in water samples in mass concentrations ≥ 0,025 ng/l (for each individual congener). (The limit of quantification (LOQ) should be determined according to ISO 13530, on the basis of replicate determinations of the procedural blank, carried out under reproducibility conditions.) The method uses solid-phase disk extraction (SPE-disk) in combination with gas chromatography-mass spectrometry (GC-MS). It is applicable to the analysis of PBDEs in surface water containing suspended particulate matter (SPM) up to 500 mg/l (whole water samples), drinking water and groundwater. 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. (...)

EN 16694:2015 is classified under the following ICS (International Classification for Standards) categories: 13.060.50 - Examination of water for chemical substances. The ICS classification helps identify the subject area and facilitates finding related standards.

EN 16694:2015 is associated with the following European legislation: EU Directives/Regulations: 2000/60/EC; Standardization Mandates: M/424. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.

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Standards Content (Sample)


2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Wasserbeschaffenheit - Bestimmung von Pentabromdiphenylether (PBDE) in Gesamtwasserproben mittels Festphasenextraktion (SPE) mit SPE-Disks in Verbindung mit Gaschromatographie - Massenspektrometrie (GC-MS)Qualité de l'eau - Dosage du pentabromodiphényléther (PBDE) dans la totalité de l'échantillon d'eau par extraction en phase solide (EPS) avec disques EPS, avec couplage chromatographie en phase gazeuse-spectrométrie de masse (CG-SM)Water quality - Determination of pentabromodiphenyl ether (PBDE) in whole water samples using solid phase extraction (SPE) with SPE-disks combined with gas chromatography - mass spectrometry (GC-MS)13.060.50VQRYLExamination of water for chemical substancesICS:Ta slovenski standard je istoveten z:EN 16694:2015SIST EN 16694:2015en,fr,de01-december-2015SIST EN 16694:2015SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16694
September
t r s w ICS
s uä r x rä w r English Version
Water quality æ Determination of selected polybrominated using solid phase extractiocombined with gas chromatography æ mass spectrometry Qualité de l 5eau æ Dosage du pentabromodiphényléther avec couplage chromatographie en phase gazeuseæ Wasserbeschaffenheitt æ Bestimmung von in Gesamtwasserproben æ Verfahren mittels Verbindung mit Gaschromatographie æ This European Standard was approved by CEN on
t y June
t r s wä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
t r s w CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x x { vã t r s w ESIST EN 16694:2015

Suitable gas chromatographic conditions and example chromatograms . 20 A.1 GC-HRMS conditions for the chromatograms in Figure A.1 . 20 A.2 GC-MS/MS conditions for the chromatograms in Figure A.2 . 23 A.3 GC-NCI-MS conditions for the chromatograms in Figure A.3 . 25 Annex B (informative)
Repeatability and reproducibility data . 26 Annex C (informative)
Examples of suitable solid phase extraction disks . 29 Annex D (informative)
Clean up procedure . 30 D.1 Reagents . 30 SIST EN 16694:2015

0,025 ng/l for each individual congener. 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. Table 1 — Polybrominated diphenyl ethers (PBDE) determined by this method Congener Abbreviationa Formula Molar mass CAS RNb
g/mol
2,4,4’-Tribromodiphenyl ether BDE-28 C12H7Br3O 406,8954 41318–75–6 2,2’,4,4’-Tetrabromodiphenyl ether BDE-47 C12H6Br4O 485,7950 5436–43–1 2,2’,4,4’,5-Pentabromodiphenyl ether BDE-99 C12H5Br5O 564,6911 60348–60–9 2,2’,4,4’,6-Pentabromodiphenyl ether BDE-100 C12H5Br5O 564,6911 189084–64–8 2,2’,4,4’,5,6’-Hexabromodiphenyl ether BDE-154 C12H4Br6O 643,5872 68631–49–2 2,2’,4,4’,5,5’-Hexabromodiphenyl ether BDE-153 C12H4Br6O 643,5872 207122–15–4 NOTE EC numbers are not applicable for PBDE congeners. a Numbering analog to IUPAC nomenclature for PCB b CAS RN: Chemical Abstracts Service Registry Number 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) EN ISO 5667-1, Water quality - Sampling - Part 1: Guidance on the design of sampling programmes and sampling techniques (ISO 5667-1) EN ISO 5667-3, Water quality - Sampling - Part 3: Preservation and handling of water samples (ISO 5667-3) ISO 8466-1, Water quality — Calibration and evaluation of analytical methods and estimation of performance characteristics — Part 1: Statistical evaluation of the linear calibration function 3 Principle A mixture of suitable internal standards (13C12-labelled BDE or fluorinated BDE) is added to a 1 l water sample, which is then extracted using a solid-phase extraction disk (SPE-disk). The disk is eluted with a SIST EN 16694:2015

The gas supplies shall be in accordance with the respective manufacturer's instructions. 6.5 Non-discriminating GC injector, e. g. splitless mode of a split/splitless injection system or programmable temperature vaporizer (PTV), programmable for large volume injection (LVI). A cold injection technique is recommended; depending on the sensitivity of the instrument large volume injection may be necessary. 6.6 Automatic sampler with option for large volume injection (LVI), including syringes for normal injection (e. g. 1 µl and 2 µl) and for LVI (e. g. 10 µl, 50 µl and 100 µl). 6.7 Capillary columns, for gas chromatography (example chromatograms are given in Annex A). It is advantageous to use non-polar columns (e. g. low-bleed 5 %-phenylsiloxane column), providing thermal stability up to 400 °C; e. g. inner diameter
0,25 mm, length 15 m, film thickness of 0,1 µm is recommended. 6.8 Solid-phase extraction disks (SPE-disks), wide inner diameter: e. g. 40 mm to 60 mm, packed with an appropriate reversed phase adsorbent material, e. g. C18-based or SDB-based adsorbent (for examples, see Annex C). 6.9 Vacuum device for solid-phase extraction, e. g. extraction box or automated workstation for solid-phase extraction procedure capable for processing SPE-disks. 6.10 Evaporation device, such as rotary evaporator, turboevaporator or vacuum concentration device. 6.11 Syringes, 2 µl, 5 µl, 10 µl and 50 µl, volume precision ± 2 %. 6.12 Sample vials; amber glass with fluoropolymer-lined screw-cap is most suitable. 6.13 Glass columns for chromatographic clean-up. 6.14 Pasteur pipettes, made of glass. SIST EN 16694:2015
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