EN ISO 22032:2026

• Abstract:

  This document specifies a method for the determination of selected polybrominated diphenylethers (PBDE) (see Figure 1 and Table 1) in sediment, suspended particulate matter and biota using gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) or with high resolution mass spectrometry (GC-HRMS) in the electron impact (EI), negative ion chemical ionization (NCI) or atmospheric pressure ionization (APCI) mode.; The method is applicable to sediment and suspended particulate matter samples with limits of quantification of 0,2 µg/kg dry mass (dm) for brominated diphenylether (BDE) BDE-28 to BDE-183, of 2 µg/kg dry mass (dm) for BDE‑209.; The method is applicable as well with lower limits of quantification (LOQ), if specific clean-up methods, described in Clause 10, Table 3, method 1 and method 2 in combination with measurement methods GC-MS/MS or GC-HRMS after electron impact ionization (El) or negative ion chemical ionization (NCI) for BDE-209 are used. Depending on the analytical capability of the instrument, limits of quantification down to 0,003 µg/kg dm for BDE-28 to BDE-154 and 0,02 µg/kg dm for BDE-183 and 1 µg/kg dm for BDE-209 and lower are possible.; The method is applicable to biota samples with limits of quantification down to 0,000 2 µg/kg fresh mass (fm) (BDE-28 to BDE-154) and 0,03 μg/kg fresh mass (fm) (BDE-183), if specific clean-up methods, described in Table 4 in combination with measurement methods GC-MS/MS or GC-HRMS after electron impact ionization (El) are used.; Performance data are listed in Annex E.

• Status: Published
• Publication Date: 19-May-2026
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: CEN/TC 230 - Water analysis
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 20-May-2026
• Completion Date: 20-May-2026
• Ref Project: SIST EN ISO 22032:2026 - Water quality - Determination of polybrominated diphenyl ethers (PBDE) in sediment, suspended particulate matter and biota - Method using gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) or with high resolution mass spectrometry (GC-HRMS) (ISO 22032:2026)

• Replaces: EN ISO 22032:2009 - Water quality - Determination of selected polybrominated diphenyl ethers in sediment and sewage sludge - Method using extraction and gas chromatography/mass spectrometry (ISO 22032:2006)
• Effective Date: 05-Apr-2023
• Referred By: EN 17331:2023 - Construction products: Assessment of release of dangerous substances - Content of organic substances - Methods for extraction and analysis
• Effective Date: 27-May-2026
• Referred By: CEN/TS 17331:2019 - Construction products: Assessment of release of dangerous substances - Content of organic substances - Methods for extraction and analysis
• Effective Date: 27-May-2026
• Referred By: EN ISO 5211:2023 - Industrial valves - Part-turn actuator attachments (ISO 5211:2023)
• Effective Date: 28-Jan-2026
• Consolidated By: ISO 22032:2026 - Water quality — Determination of polybrominated diphenyl ethers (PBDE) in sediment, suspended particulate matter and biota — Method using gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) or with high resolution mass spectrometry (GC-HRMS)
• Effective Date: 12-Feb-2026

Overview

EN ISO 22032:2026 is an internationally recognized standard developed by the European Committee for Standardization (CEN) and the International Organization for Standardization (ISO). Titled "Water quality - Determination of polybrominated diphenyl ethers (PBDE) in sediment, suspended particulate matter and biota," this document specifies analytical methods for detecting and quantifying PBDEs in various environmental samples. The standard employs advanced gas chromatography coupled with tandem mass spectrometry (GC-MS/MS) or high-resolution mass spectrometry (GC-HRMS), ensuring high accuracy and low detection limits for diverse PBDE congeners.

PBDEs are persistent organic pollutants (POPs) used as flame retardants in a wide range of consumer and industrial products. Monitoring PBDE levels in aquatic environments is crucial for protecting water quality, aquatic organisms, and human health.

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Key Topics

• Target Analytes: The standard focuses on a specified list of PBDE congeners, which include BDE-28 to BDE-209. These are among the most environmentally significant PBDEs due to their persistence and toxicity.
• Applicable Sample Types: Methods are validated for sediment, suspended particulate matter, and biota (such as aquatic organisms), offering a comprehensive approach for environmental monitoring.
• Detection Techniques:
  • GC-MS/MS (Gas Chromatography coupled with Tandem Mass Spectrometry)
  • GC-HRMS (Gas Chromatography with High Resolution Mass Spectrometry) These techniques, in combination with electron impact (EI), negative ion chemical ionization (NCI), or atmospheric pressure ionization (APCI), allow for accurate identification and quantification even at trace levels.
• Sample Limits: The method supports very low limits of quantification (LOQ), down to 0.0002 µg/kg (fresh mass) for biota and 0.003 µg/kg (dry mass) for sediment and suspended matter, using specific clean-up and calibration practices.
• Sample Clean-up: The standard provides multiple clean-up procedures tailored to the sample matrix and PBDE concentration, enhancing method robustness and reliability.

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Applications

EN ISO 22032:2026 has broad relevance for environmental monitoring and research in the context of water quality assessment. Key applications include:

• Regulatory Compliance: Supports implementation of EU directives and other regulatory frameworks requiring monitoring of PBDEs in surface waters, sediments, and biota-such as the Urban Waste Water Treatment Directive (91/271/EEC).
• Environmental Monitoring: Enables laboratories and authorities to assess and track PBDE contamination in rivers, lakes, estuaries, and aquatic organisms, providing critical data for ecological risk assessments.
• Pollution Source Identification: Facilitates investigation of point and diffuse sources of PBDEs linked to industrial activities, urban runoff, and waste management practices.
• Research and Development: Provides a robust analytical basis for academic and governmental research projects studying the fate, transport, and bioaccumulation of PBDEs in aquatic ecosystems.
• Risk Assessment: Helps inform decision-making processes to protect wildlife and public health from the risks posed by these persistent organic pollutants.

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Related Standards

Organizations and laboratories may find the following standards useful in conjunction with EN ISO 22032:2026:

• ISO 5667 Series: Guidance on sampling of water, sediments, and suspended solids.
• ISO 8466-1: Water quality-Calibration and evaluation of analytical methods.
• EN 13946, EN 14011, EN 14757, EN 16150, EN 16190, EN 17218: Various standards for sampling and monitoring aquatic organisms and related matrices.
• ISO/TS 13530: Analytical quality control for chemical and physicochemical water analysis.
• EN 16190: Procedures for analyzing dioxins, furans, and other persistent organic pollutants.

---

EN ISO 22032:2026 ensures standardized, high-quality determination of PBDEs in the aquatic environment-supporting effective environmental management, policy compliance, and pollutant control. By adopting these validated methods, stakeholders can produce reliable, comparable results essential for safeguarding water resources and ecosystem health.

SLOVENSKI STANDARD
01-julij-2026
Nadomešča:
SIST EN ISO 22032:2009
Kakovost vode - Določanje polibromiranih difenil etrov (PBDE) v sedimentu,
suspendiranih trdnih delcih in bioti - Metoda s plinsko kromatografijo s tandemsko
masno spektrometrijo (GC-MS/MS) ali masno spektrometrijo visoke ločljivosti (GC-
HRMS) (ISO 22032:2026)
Water quality - Determination of polybrominated diphenyl ethers (PBDE) in sediment,
suspended particulate matter and biota - Method using gas chromatography coupled
with tandem mass spectrometry (GC-MS/MS) or with high resolution mass spectrometry
(GC-HRMS) (ISO 22032:2026)
Wasserbeschaffenheit - Bestimmung von polybromierten Diphenylethern (PBDE) in
Sedimenten, Schwebstoffen und Biota - Verfahren mittels Gaschromatographie
gekoppelt mit Tandem Massenspektrometrie (GC-MS/MS) oder mit der hochauflösenden
Massenspektrometrie (GC-HRMS) (ISO 22032:2026)
Qualité de l'eau - Dosage d'éthers diphényliques polybromés (PBDE) dans les
sédiments, les matières en suspension (particules) et le biote - Méthode par
chromatographie en phase gazeuse couplée à la spectrométrie de masse en tandem
(CG-SM/SM) ou à la spectrométrie de masse haute résolution (CG-SMHR) (ISO
22032:2026)
Ta slovenski standard je istoveten z: EN ISO 22032:2026
ICS:
13.060.50 Preiskava vode na kemične Examination of water for
snovi chemical substances
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN ISO 22032
EUROPEAN STANDARD
NORME EUROPÉENNE
May 2026
EUROPÄISCHE NORM
ICS 13.060.50 Supersedes EN ISO 22032:2009
English Version
Water quality - Determination of polybrominated diphenyl
ethers (PBDE) in sediment, suspended particulate matter
and biota - Method using gas chromatography coupled
with tandem mass spectrometry (GC-MS/MS) or with high
resolution mass spectrometry (GC-HRMS) (ISO
22032:2026)
Qualité de l'eau - Dosage d'éthers diphényliques Wasserbeschaffenheit - Bestimmung von
polybromés (PBDE) dans les sédiments, les matières polybromierten Diphenylethern (PBDE) in
en suspension (particules) et le biote - Méthode par Sedimenten, Schwebstoffen und Biota - Verfahren
chromatographie en phase gazeuse couplée à la mittels Gaschromatographie gekoppelt mit Tandem
spectrométrie de masse en tandem (CG-SM/SM) ou à la Massenspektrometrie (GC-MS/MS) oder mit der
spectrométrie de masse haute résolution (CG-SMHR) hochauflösenden Massenspektrometrie (GC-HRMS)
(ISO 22032:2026) (ISO 22032:2026)
This European Standard was approved by CEN on 17 May 2026.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2026 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 22032:2026 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
This document (EN ISO 22032:2026) has been prepared by Technical Committee ISO/TC 147 "Water
quality" in collaboration with Technical Committee CEN/TC 230 “Water analysis” the secretariat of
which is held by DIN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by November 2026, and conflicting national standards
shall be withdrawn at the latest by November 2026.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 22032:2009.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 22032:2026 has been approved by CEN as EN ISO 22032:2026 without any modification.

International
Standard
ISO 22032
Second edition
Water quality — Determination of
2026-05
polybrominated diphenyl ethers
(PBDE) in sediment, suspended
particulate matter and biota —
Method using gas chromatography
coupled with tandem mass
spectrometry (GC-MS/MS) or with
high resolution mass spectrometry
(GC-HRMS)
Qualité de l'eau — Dosage d'éthers diphényliques polybromés
(PBDE) dans les sédiments, les matières en suspension
(particules) et le biote — Méthode par chromatographie en phase
gazeuse couplée à la spectrométrie de masse en tandem (CG-SM/
SM) ou à la spectrométrie de masse haute résolution (CG-SMHR)
Reference number
ISO 22032:2026(en) © ISO 2026
ISO 22032:2026(en)
© ISO 2026
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii
ISO 22032:2026(en)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 2
5 Interferences . 3
6 Reagents and standards . . 3
7 Apparatus . 6
8 Sampling and sample pretreatment. 7
9 Procedure . 7
9.1 Extraction of sediment or particulate matter samples by pressurized liquid extraction
(PLE) or Soxhlet . . .7
9.2 Extraction of biota samples .8
9.2.1 PLE, Soxhlet or Twisselmann extraction .8
9.2.2 Cold extraction alternative (biota) .8
10 Clean-up of sample extracts . 8
11 Measurement and integration of the chromatogram .10
12 Calibration .10
12.1 General .10
12.2 Estimation of the linear range .11
12.3 Calibration of the measuring method using an internal standard, .11
12.4 Injection standard .11
13 Identification .11
14 Quantification .11
14.1 Quantification using internal standards, including quality checks of the recovery of the
internal standards .11
14.2 Testing the validity of calibration . 12
15 Expression of results .12
16 Test report .12
Annex A (normative) Program for pressurized liquid extraction .13
Annex B (normative) Clean-up methods .15
Annex C (informative) Typical GC-MS conditions and m/z values for identification and
quantification .20
Annex D (informative) Examples of linearity check and calibration working solutions .26
Annex E (informative) Performance data .28
Bibliography .31

iii
ISO 22032:2026(en)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out through
ISO technical committees. Each member body interested in a subject for which a technical committee
has been established has the right to be represented on that committee. International organizations,
governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely
with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are described
in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the different types
of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the
ISO/IEC Directives, Part 2 (see www.iso.org/directives).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and expressions
related to conformity assessment, as well as information about ISO’s adherence to the World Trade
Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods, in collaboration with the European Committee for Standardization
(CEN) Technical Committee CEN/TC 230, Water analysis, in accordance with the Agreement on technical
cooperation between ISO and CEN (Vienna Agreement).
This second edition cancels and replaces the first edition (ISO 22032:2006), which has been technically
revised.
The main changes are as follows:
— the scope has been expanded to include biota;
— GC-MS/MS has been included as a detection method;
— a description of a clean-up set with manual and automated methods for sediment, for suspended
particulate matter and biota has been included.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.

iv
ISO 22032:2026(en)
Introduction
This document enables the analysis of polybrominated diphenyl ethers (PBDE) related to 91/271/EEC - the
Urban Waste Water Treatment Directive, the European Union directive concerning the collection, treatment
and discharge of urban waste water and the treatment and discharge of waste water from certain industrial
sectors.
v
International Standard ISO 22032:2026(en)
Water quality — Determination of polybrominated diphenyl
ethers (PBDE) in sediment, suspended particulate matter
and biota — Method using gas chromatography coupled
with tandem mass spectrometry (GC-MS/MS) or with high
resolution mass spectrometry (GC-HRMS)
WARNING — Persons using this document should be familiar with normal laboratory practice. This
document does not purport to address all of the safety problems, if any, associated with its use. It is
the responsibility of the user to establish appropriate safety and health practices.
IMPORTANT — It is absolutely essential that tests conducted in accordance with this document be
carried out by suitably qualified staff.
1 Scope
This document specifies a method for the determination of selected polybrominated diphenylethers (PBDE)
(see Figure 1 and Table 1) in sediment, suspended particulate matter and biota using gas chromatography
coupled with tandem mass spectrometry (GC-MS/MS) or with high resolution mass spectrometry (GC-
HRMS) in the electron impact (EI), negative ion chemical ionization (NCI) or atmospheric pressure ionization
(APCI) mode.
The method is applicable to sediment and suspended particulate matter samples with limits of quantification
of 0,2 µg/kg dry mass (dm) for brominated diphenylether (BDE) BDE-28 to BDE-183, of 2 µg/kg dry mass
(dm) for BDE-209.
The method is applicable as well with lower limits of quantification (LOQ), if specific clean-up methods,
described in Clause 10, Table 3, method 1 and method 2 in combination with measurement methods GC-
MS/MS or GC-HRMS after electron impact ionization (El) or negative ion chemical ionization (NCI) for BDE-
209 are used. Depending on the analytical capability of the instrument, limits of quantification down to
0,003 µg/kg dm for BDE-28 to BDE-154 and 0,02 µg/kg dm for BDE-183 and 1 µg/kg dm for BDE-209 and
lower are possible.
The method is applicable to biota samples with limits of quantification down to 0,000 2 µg/kg fresh mass
(fm) (BDE-28 to BDE-154) and 0,03 μg/kg fresh mass (fm) (BDE-183), if specific clean-up methods, described
in Table 4 in combination with measurement methods GC-MS/MS or GC-HRMS after electron impact
ionization (El) are used.
Performance data are listed in Annex E.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content constitutes
requirements of this document. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
ISO 8466-1:2021, Water quality — Calibration and evaluation of analytical methods — Part 1: Linear calibration
function
ISO/TS 13530, Water quality — Guidance on analytical quality control for chemical and physicochemical water
analysis
ISO 22032:2026(en)
EN 16190, Soil, treated biowaste and sludge — Determination of dioxins and furans and dioxin-like
polychlorinated biphenyls by gas chromatography with high resolution mass selective detection (HR GC-MS)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Principle
Brominated diphenyl ethers are extracted from dried sample material (sediment, suspended particulate
matter, biota) using organic solvents.
Figure 1 — General structure of polybrominated diphenyl ethers
Table 1 — PBDE congeners determined by this method
a b
No. Congener Formula Abbreviation CAS-RN Molar mass
g/mol
1 2,4,4'-Tribromodiphenyl ether C H Br O BDE-28 41318-75-6 406,9
12 7 3
2 2,2',4,4'-Tetrabromodiphenyl ether C H Br O BDE-47 5436-43-1 485,8
12 6 4
3 2,2',4,4',5-Pentabromodiphenyl ether C H Br O BDE-99 60348-60-9 564,7
12 5 5
4 2,2',4,4',6-Pentabromodiphenyl ether C H Br O BDE-100 189084-64-8 564,7
12 5 5
5 2,2',4,4',5,5'-Hexabromodiphenyl ether C H Br O BDE-153 68631-49-2 643,6
12 4 6
6 2,2',4,4',5,6'-Hexabromodiphenyl ether C H Br O BDE-154 207122-15-4 643,6
12 4 6
7 2,2',3,4,4',5',6-Heptabromodiphenyl ether C H Br O BDE-183 207122-16-5 722,5
12 3 7
8 Decabromodiphenyl ether C Br O BDE-209 1163-19-5 959,2
12 10
a
Numbering analogous to IUPAC nomenclature for Polychlorinated Biphenylethers PCB.
b
Chemical Abstracts Service (CAS) Registry Number® is a trademark of the American Chemical Society (ACS). This
information is given for the convenience of users of this document and does not constitute an endorsement by ISO of the product
named. Equivalent products may be used if they can be shown to lead to the same results.
Clean-up of the extract is carried out by various methods as specified in this document. Depending on the
matrix and the concentration of PBDE in the samples five different clean-up methods for sediment samples
and three methods for biota samples can be selected, e.g. column chromatography or gel permeation
chromatography. Options for avoiding dichloromethane and toluene in the sample clean-up are available.
After clean-up and concentration, separation of the brominated diphenyl ethers is accomplished by capillary
gas chromatography. For detection, different types of GC-MS equipment can be used, applying either mass
spectrometry in multiple reaction mode, or high resolution mass spectrometry with different ionisation
techniques as electron impact (EI), negative ion chemical ionization (NCI) or atmospheric pressure chemical
ionisation (APCI).
ISO 22032:2026(en)
For the determination of the analyte concentration in the sample, an internal standard calibration is used.
5 Interferences
Non-specific matrix interferences, as well as interferences from other environmental contaminants are
dealt with using the given clean-up procedures.
Sources of contamination of the samples can be the following: brominated diphenyl ethers used as flame-
retardants or for other purposes in organic polymers, used in vial covers, Pasteur pipette fillers, recycled
paper and are possibly transported also via air dust. Therefore, any contact of samples, reagents or any
material used with these organic polymers shall be avoided.
PCB-180 can interfere with BDE-47 if a short column is used. The application of MS/MS detection as
well as avoiding m/z 323,87 in the detection by GC-HRMS allows for separation the compounds via mass
spectrometry.
Interferences with other chlorinated substances can occur, if chromatographic separation is not sufficient
as described in Reference [14]:
— BDE-47 at m/z 323,878 5 with Heptachlorobiphenyl at m/z 323,864 7 such as PCB-180;
— BDE-100 and BDE-99 at m/z 403,787 0 with Octachloronaphthalene at m/z 403,745 0;
— BDE-100 and BDE-99 at m/z 405,784 9 with Heptachlorodibenzofurans at m/z 405,784 7.
MS/MS detection at optional m/z values (see Table C.1) can solve the problem. Therefore, careful evaluation
of instrumentation, masses and mass transitions used in MS shall be done.
Further interferences from BDE-congeners not listed in this document, as well as by other brominated
compounds can be found in Reference [15]. Coelutions can occur especially when using short columns and
short oven programs. Such potential interferences depending on the analytical column are:
— BDE-16, BDE-33 interfering with BDE-28;
— BDE-184, BDE-182 and BDE-175 interfering with BDE-183.
These and further interferences should be overcome by a sufficient chromatographic separation.
6 Reagents and standards
Use only reagents and materials with negligibly low concentrations of brominated diphenyl ethers, verify
this in every analysis series by blank determinations over the total procedure. The blank over the total
procedure shall be less than the reported limit of detection (see the definition of the limit of detection in
ISO/TS 13530). If necessary, traces of PBDE in solid materials can be reduced by heating at 400 °C.
6.1 Solvents for extraction, preparation of stock solutions and clean-up.
6.1.1 n-Heptane, C H .
7 16
6.1.2 Toluene, C H .
7 8
6.1.3 Acetone (2-propanone), C H O.
3 6
6.1.4 Dichloromethane, CH Cl .
2 2
6.1.5 Cyclohexane, C H .
6 12
6.1.6 Dodecane, C H for automatized clean-up or as a keeper.
12 26,
ISO 22032:2026(en)
6.1.7 n-Hexane, C H .
6 14
6.1.8 Ethanol, C H O.
2 6
6.1.9 Ethyl acetate, C H O .
4 8 2
6.2 Reference stock solutions.
See Table 1. Solutions of reference substances are commercially available.
Store the prepared solutions in a refrigerator at (5 ± 3) °C, alternatively according to the manufacturer.
6.3 Internal standard stock solutions.
Solutions of C-labelled reference substances for use as internal standards are commercially available.
Store the prepared solutions in a refrigerator at (5 ± 3) °C, alternatively according to the manufacturer.
See Table 2.
Table 2 — List of C-labelled internal standards
No Name Formula Abbreviation Molar mass
g/mol
13 13 13
1 2,4,4'-Tribromo[ C ]diphenyl ether C H Br O C-BDE-28 418,8
12 12 7 3
13 13 13
2 2,2',4,4'-Tetrabromo[ C ]diphenyl ether C H Br O C-BDE-47 497,7
12 12 6 4
13 13 13
3 2,2',4,4',5-Pentabromo[ C ]diphenyl ether C H Br O C-BDE-99 576,6
12 12 5 5
13 13 13
4 2,2',4,4',6-Pentabromo[ C ]diphenyl ether C H Br O C-BDE-100 576,6
12 12 5 5
13 13 13
5 2,2',4,4',5,5'-Hexabromo[ C ]diphenyl ether C H Br O C-BDE-153 655,5
12 12 4 6
13 13 13
6 2,2',4,4',5,6'-Hexabromo[ C ]diphenyl ether C H Br O C-BDE-154 655,5
12 12 4 6
13 13 13
7 2,2',3,4,4',5',6-Heptabromo[ C ]diphenyl ether C H Br O C-BDE-183 734,4
12 12 3 7
13 13 13
8 Decabromo[ C ]diphenyl ether C Br O C-BDE-209 971,1
12 12 10
6.4 Internal standard working solutions for calibration and addition to the samples, see Annex D.
6.5 Sodium sulfate, Na SO , anhydrous powdered baked in oven (7.5) for 4 hours at 400 °C.
2 4
6.6 Water, free of blanks and potential interferences.
6.7 Extraction filters, e.g. cellulose for PLE-extractor.
6.8 Soxhlet thimbles, (e.g. 27 mm × 100 mm) (pre-cleaned).
6.9 Sand (blank free), e.g. Ottawa sand or sea sand for blank analysis over the total procedure and as a
filling of the extraction cells; alternative: glass granulate.
6.10 Basic alumina, (Al O ), activity Super I, particle size 0,063 mm to 0,2 mm, pH 10 (100 g/l, H O, 20 °C)
2 3 2
3 1)
(in slurry) density 3,94 g/cm , e.g. MP Alumina B – Super I for Dioxin Analysis 1344-28-1 (mpbio.com),
avoid long storage and contact with air humidity.
1) This information is given for the convenience of users of this document and does not constitute an endorsement by
ISO of the product named. Equivalent products may be used if they can be shown to lead to the same results.

ISO 22032:2026(en)
6.11 Basic alumina, (Al O ), activity I, particle size 0,063 mm to 0,2 mm, pH 8,5 to pH 10,5 (100 g/l, H O,
2 3 2
20 °C) (in slurry) density 4 g/cm , (20 °C), pore size 9 nm, avoid long storage and contact with air humidity.
6.12 Silica 60, (70 mesh to 230 mesh).
6.13 Silver nitrate, (AgNO ).
6.14 Sulfuric acid, H SO , 95 % to 97 %.
2 4
6.15 Hydrochloric acid, HCl, 2 mol/l.
6.16 Material for fixing the adsorbent materials in the clean-up columns, e.g. quartz wool or glass
wool, silanised glass wool.
6.17 Copper powder, grain size < 63 µm.
6.18 Silica-sulfuric acid.
Add 44 g sulfuric acid (6.14) dropwise to 56 g silica (6.12). Subsequently shake for 30 min. Store tightly
closed in brown glass bottles. The mixture is stable for at least 1 month.
6.19 Silica-silver nitrate.
Dissolve 10 g AgNO (6.13) in 40 ml water (6.6), add solution stepwise to 90 g silica (6.12) and stir, activate
at 125 °C for 5 hours. Store tightly closed in brown glass bottles. The mixture is stable at least for 1 month.
6.20 Operating gases, for GC-MS, of high purity and in accordance with manufacturer’s specifications.
6.21 Nitrogen, N , for concentrating of extracts.
6.22 Linearity check and calibration working solutions.
Considering the working range and the sample amount, prepare calibration solutions using syringes (7.17)
with the lowest point corresponding to the LOQ of the method (example given in Annex D). The concentration
of the internal standard should be between the medium and the top level of the calibration range (example
given in Annex D).
6.23 Injection standards.
The following C-labelled injection standards are commercially available and have proven to be practicable:
13 13
— 3,3',4,4'-Tetrabromo( C )diphenyl ether ( C-BDE-77);
13 13
— 3,3',4,5'-Tetrabromo( C )diphenyl ether ( C-BDE-79);
13 13
— 2,3’,4,4’,5-Pentabromo( C )diphenyl ether ( C-BDE-118);
13 13
— 2,2',3,4,4',5-Hexabromo( C )diphenyl ether ( C-BDE-137);
13 13
— 2,2',3,4,4',5’-Hexabromo( C )diphenyl ether ( C-BDE-138);
13 13
— 2,2',3,4,4',6-Hexabromo( C )diphenyl ether ( C-BDE-139);
13 13
— 2,2',3,4,4',5,5'-Heptabromo( C )diphenyl ether ( C-BDE-180);
13 13
— 2,3,3',4,4',5,6-Heptabromo( C )diphenyl ether ( C-BDE-190);
13 13
— 2,2',3,4,4',5,5',6-Octabromo( C )diphenyl ether ( C-BDE-203);
ISO 22032:2026(en)
13 13
— 2,3,3',4,4',5,5',6-Octabromo( C )diphenyl ether ( C-BDE-205);
13 13
— 2,2',3,3',4,4',5,5',6-Nonabromo( C )diphenyl ether ( C-BDE-206).
Use commercially available solutions (6.2, 6.3) (e.g. in nonane, toluene or iso-octane) or prepare stock
solutions, e.g. by dissolving 10 mg of each of the reference substances in n-heptane (6.1.1) in an amber, 10-ml
volumetric flask (7.15) and bring to volume (concentration: 1 mg/ml).
Examples for calibration working solutions are given in Annex D. For the linearity check use at least
six concentration levels.
The solutions may be stored in a refrigerator at (5 ± 3) °C in the dark for at least 1 year. Check the
concentration of the calibration solutions against an independently prepared standard prior to use.
7 Apparatus
Clean all glassware at least by rinsing with acetone (2-propanone) (6.1.3).
7.1 Wide-necked bottle, 1 000 ml up to 5 000 ml capacity, for wet sediment, particulate matter or biota.
7.2 Freeze drying apparatus.
7.3 Deep freezer.
7.4 Mortar and pestle, or a grinding mill.
7.5 Drying ovens, capable of maintaining temperatures in the ranges of 100 °C to 400 °C for baking of
clean-up materials, for baking of glassware and for dry residue determination of samples.
7.6 Sieve shaker with appropriate sieve meshes (aperture size), 2 mm.
7.7 Desiccator.
7.8 Pressurized liquid extractor (PLE) and appropriate filter materials suited for the device,
alternatively Soxhlet extraction apparatus, consisting of round bottom flasks (e.g. 250 ml), Soxhlet
extractors and Soxhlet thimbles (e.g. 27 mm × 100 mm) see 6.8, vertical condensers (e.g. 300 mm) and
heating apparatus or Twisselmann extraction system.
7.9 Evaporation device, e.g. rotary evaporator or concentration device with suitable gases 6.21.
7.10 Automatic sample processing system, e.g. DexTech/DexTech Plus from LC-Tech, MiuraTM GO-2HT
2)
(Miura Co. Ltd).
7.11 Small glass columns for chromatographic clean-up, 1 cm inner diameter, approximately 12 mm ×
140 mm with a stopcock.
7.12 Big glass columns for chromatographic clean-up, > 2 cm inner diameter, approximately 25 mm ×
150 mm with a stopcock.
7.13 Ready to use columns for automatized clean-up from, e.g. LC-Tech or Miura-system: see Clause B.7.
2) DexTech/DexTech Plus from LC-Tech, MiuraTM GO-2HT (Miura Co. Ltd) are automatic sample processing systems.
This information is given for the convenience of users of this document and does not constitute an endorsement by ISO
of the automatic sample processing systems. Equivalent systems may be used if they can be shown to lead to the same
results.
ISO 22032:2026(en)
7.14 Gel permeation chromatography (GPC) clean-up system (with modular design), pump, sampling
injector, sample rack; fraction collector, column: e.g. Ashahipak GF 310 HQ 7,5 mm × 300 mm, 5 µm particle
size.
7.15 Volumetric flasks, 1 ml, 2 ml, 10 ml and 25 ml, preferable amber glass.
7.16 Pasteur pipettes, e.g. 2 ml.
7.17 Syringes, 2 µl, 5 µl, 10 µl and 50 µl, volume precision ±2 %.
7.18 GC-sample vials, e.g. 2 ml, amber glass with a micro insert and a fluoropolymer-lined screw-cap is
most suitable.
7.19 Gas chromatograph, with operating gases 6.20 with a splitless injection port or a temperature
programmable injection port, coupled to a tandem mass spectrometer (GC-MS/MS) or GC-HRMS with
electron impact or chemical ionization and appropriate reactant gas (e.g. CH ) or atmospheric pressure
ionization.
7.20 Analytical column, fused silica column with non-polar low bleed separating phase (see Annex C for
examples); inner diameter < 0,25 mm, length 15 m, film thickness of 0,1 µm is recommended.
8 Sampling and sample pretreatment
Take samples, see e.g. ISO 5667-12, ISO 5667-13 or ISO 5667-17, in a bottle (7.1). Store and transport in
the dark at approximately 4 °C (see ISO 5667-15). Pre-treat the samples immediately in the laboratory by
homogenizing and freeze-drying (7.2), alternatively mix them with sodium sulfate (6.5). If an immediate
pre-treating is not possible, samples can be frozen (7.3) and stored in a freezer at a temperature below −15 °C
(see ISO 5667-15). Deagglomerize the dried samples using apparatus e.g. (7.4) and sieve it using device (7.6)
according to the analytical task.
Take and pretreat biota samples, see e.g. EN 14011, EN 14757, EN 16150, EN 17218, ISO 10870 or EN 13946,
immediately either before or after homogenizing by freezing. Freeze dry to remove water and to enhance
the surface for later extraction.
Store the dried samples protected against air humidity, e.g. in a desiccator (7.7).
9 Procedure
9.1 Extraction of sediment or particulate matter samples by pressurized liquid extraction
(PLE) or Soxhlet
Place the filter (6.7) or thimble (6.8) and, if applicable, the sand (6.9) in the extractor according to the
instructions for the extractor (PLE) (7.8) or Soxhlet extractor (7.8). Transfer a suitable amount, e.g. 5 g, of
the pre-treated, dry sample into the prepared extractor cell. Add a suitable amount of the internal standard
working solution (6.4) prepared from the internal standard stock solutions (6.3) to the sample and add 2 ml
of the extraction solvent (6.1) to avoid losses of the internal standard. Add sand (6.9) on the top.
The extraction programs and solvents for PLE or Soxhlet given in Clauses A.1 and A.3 shall be applied.
Protect samples and extracts carefully from sunlight to avoid photodegradation of the PBDE, especially
BDE-209.
NOTE 1 Other extraction techniques can be used after performing comparability exercise with PLE and the given
program or Soxhlet extraction. Extraction of BDE-209 requires specific attention and, sometimes, longer extraction
times than for other PBDE congeners.
NOTE 2 Other extraction solvents, can be used after performing comparability exercise.

ISO 22032:2026(en)
Concentrate the extract from the extractor gently (at a temperature of 40 °C) to 1 ml ± 0,5 ml using a suitable
evaporation device (7.9).
9.2 Extraction of biota samples
9.2.1 PLE, Soxhlet or Twisselmann extraction
Place the filter (6.7) or thimble (6.8) and the sand (6.9) in the extractor according to the instructions for
the extractor (PLE) or alternative extractor (7.8). Transfer a suitable amount, 2 g to 5 g, of the dried biota
sample, into the prepared extractor cell. Add the internal standard working solution (6.4) to the sample and
add 2 ml of the extraction solvent to avoid losses of the internal standard. Add sand on the top, if applicable.
The internal standards can be added also after fat extraction, if an appropriate validation of the quantitative
extraction is given.
The extraction programs and solvents for PLE or Soxhlet given in Clauses A.2 and A.4 shall be applied.
Protect samples and extracts carefully from sunlight to avoid photodegradation of the PBDE, especially
BDE-209.
NOTE 1 Other extraction techniques, such as ultrasonic extraction, can be used after performing comparability
exercise with PLE and the given program or Soxhlet extraction. Extraction of BDE-209 requires specific attention and,
sometimes, longer extraction times than other PBDE congeners.
Make sure that exhaustive extraction is achieved.
NOTE 2 Other extraction solvents, can be used after performing comparability exercise.
Concentrate the extract from the extractor gently (at a temperature of 40 °C) to 1 ml ± 0,5 ml using a suitable
evaporation device (7.9).
9.2.2 Cold extraction alternative (biota)
This procedure describes a cold extraction of fat by means of dichloromethane/cyclohexane (a volume
fraction of 1:1) (6.1.4 and 6.1.5).
A mixture of (30,0 ± 0,1) g of the wet sample, 70 g sodium sulfate (6.5), 30 g glass granulate or as an
alternative sea sand (6.9) and the internal standard solution (6.4) are put in a mortar (7.4). The mixture is
finely ground using the pestle to produce a powder. Approximately 5 g of sodium sulfate (6.5) is filled into a
chromatographic glass column (7.11) sealed with a plug of silanised glass wool (6.16). Afterwards the finely
ground sample powder is added to the column. Extract with 350 ml of a dichloromethane/cyclohexane (a
volume ratio of 1:1) mixture and collect the eluate in a 500 ml round bottom flask. This eluate is carefully
concentrated by means of an evaporation device (7.9) at a temperature of (40 ± 5) °C.
Remove the solvent entirely.
10 Clean-up of sample extracts
Depending on the matrix and the concentration of PBDE in the samples, one of five different clean-up methods
for sediment samples (see Table 3) and one of three methods for biota samples (see Table 4) shall be selected,
e.g. column chromatographic methods, or combined methods using GPC or avoiding dichloromethane and
toluene. One of the methods is identical to ISO 18635 for short chain polychlorinated paraffins (SCCP)
analysis in sediment and allows for enhancement of laboratory efficiency.
Before applying the method, the elution volume shall be checked. The clean-up columns are always prepared
before solvent addition, hence do not prepare by the slurry technique.

ISO 22032:2026(en)
Table 3 — Clean-up methods for sediments and suspended particle matter
(see Annex B)
Clean-up method Method 1 Method 2 Method 3 Method 4 Method 7
Low concentra- Low concentra-
Medium concen- tion of matrix tion of matrix High concentra-
High concentration
Matrix tration of matrix constituents, e.g. constituents, e.g. tion of matrix
of matrix constitu-
characterisation constituents, sometimes in sometimes in constituents,
ents, possibly PCB
possibly PCB suspended partic- suspended partic- lipids, PCB
ulate matter ulate matter
No use of dichlo-
Use of dichlo- Use of dichlo-
romethane and
Additional = clean-up in
romethane and Use of toluene romethane and
toluene
information ISO 18635
toluene toluene
No sulfur removal
Column chro-
Column chromato-
matographic
graphic clean-up
clean-up with
with sulfur re-
sulfur removal
moval using layers
Clean-up step using layers of
of silica-sulfuric
silica-sulfuric
acid and silica-sil-
acid and silica-sil-
ver nitrate (see
ver nitrate (see
Clause B.1)
Clause B.1)
Column chroma-
tographic clean-
up with silica-sul-
Clean-up step
furic acid in a
small column
(see Clause B.2)
Column chromato-
graphic clean-up
with Alumi-
na B Super I (see
Clean-up step
Clause B.3)
Use of dichlo-
romethane
Column chroma-
tographic clean-
up with Alumina
Clean-up step
and activated
copper powder
(see Clause B.4)
Gel chromato-
Clean-up step graphic clean-up
(see Clause B.5)
Biota automated
Clean-up step  clean-up (see
Clause B.7)
NOTE For samples containing high amounts of sulfur: gel permeation chromatography is more efficient for sulfur
removal than using copper powder.
Concentrate (7.9) the final eluate gently to a volume of about 0,5 ml to 1 ml and dry it with sodium sulfate
(6.5), if necessary. For further concentration a keeper can be added to avoid evaporation to dryness, e.g.
10 µl dodecane (6.1.6) for a final volume of e.g. 100 µl. Transfer the extract to a GC-vial (7.18).

ISO 22032:2026(en)
Table 4 — Clean-up methods for biota
Clean-up method Method 5 Method 6 Method 7
Matrix High concentration of matrix High concentration of matrix High concentration of matrix
characterisation constituents, lipids, PCB constituents, lipids, PCB constituents, lipids, PCB
Additional Use of dichloromethane and
Use of dichloromethane No use of dichloromethane
information toluene
Column chromatographic Column chromatograp
...