|
SIST EN ISO 22032:2009
01-maj-2009
.DNRYRVWYRGH'RORþHYDQMHL]EUDQLKSROLEURPLUDQLKGLIHQLOHWURYYVHGLPHQWLKLQ
EODWXRGSDGQLKYRG3OLQVNDNURPDWRJUDIVNDPHWRGD]PDVQRVSHNWURPHWULMRSR
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Water quality - Determination of selected polybrominated diphenyl ethers in sediment
and sewage sludge - Method using extraction and gas chromatography/mass
spectrometry (ISO 22032:2006)
Wasserbeschaffenheit - Bestimmung ausgewählter polybromierter Diphenylether in
Sediment und Klärschlamm - Verfahren mittels Extraktion und
Gaschromatographie/Massenspektrometrie (ISO 22032:2006)
Qualité de l'eau - Dosage d'une sélection d'éthers diphényliques polybromés dans des
sédiments et des boues d'épuration - Méthode par extraction et chromatographie en
phase gazeuse/spectrométrie de masse (ISO 22032:2006)
Ta slovenski standard je istoveten z: EN ISO 22032:2009
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
SIST EN ISO 22032:2009 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 22032:2009
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SIST EN ISO 22032:2009
EUROPEAN STANDARD
EN ISO 22032
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2009
ICS 13.060.50
English Version
Water quality - Determination of selected polybrominated
diphenyl ethers in sediment and sewage sludge - Method using
extraction and gas chromatography/mass spectrometry (ISO
22032:2006)
Qualité de l'eau - Dosage d'une sélection d'éthers Wasserbeschaffenheit - Bestimmung ausgewählter
diphényliques polybromés dans des sédiments et des polybromierter Diphenylether in Sediment und Klärschlamm
boues d'épuration - Méthode par extraction et - Verfahren mittels Extraktion und
chromatographie en phase gazeuse/spectrométrie de Gaschromatographie/Massenspektrometrie (ISO
masse (ISO 22032:2006) 22032:2006)
This European Standard was approved by CEN on 28 March 2008.
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 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 Management Centre has the same status as the
official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,
Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 22032:2009: E
worldwide for CEN national Members.
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SIST EN ISO 22032:2009
EN ISO 22032:2009 (E)
Contents Page
Foreword .3
2
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SIST EN ISO 22032:2009
EN ISO 22032:2009 (E)
Foreword
The text of ISO 22032:2006 has been prepared by Technical Committee ISO/TC 147 “Water quality” of the
International Organization for Standardization (ISO) and has been taken over as EN ISO 22032:2009 by
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 August 2009, and conflicting national standards shall be withdrawn at
the latest by August 2009.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
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, Cyprus, Czech
Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia,
Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of ISO 22032:2006 has been approved by CEN as a EN ISO 22032:2009 without any modification.
3
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SIST EN ISO 22032:2009
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SIST EN ISO 22032:2009
INTERNATIONAL ISO
STANDARD 22032
First edition
2006-12-15
Water quality — Determination of
selected polybrominated diphenyl ethers
in sediment and sewage sludge —
Method using extraction and gas
chromatography/mass spectrometry
Qualité de l'eau — Dosage d'une sélection d'éthers diphényliques
polybromés dans des sédiments et des boues d'épuration — Méthode
par extraction et chromatographie en phase gazeuse/spectrométrie de
masse
Reference number
ISO 22032:2006(E)
©
ISO 2006
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
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Published in Switzerland
ii © ISO 2006 – All rights reserved
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope . 1
2 Normative references . 2
3 Principle. 2
4 Interferences . 2
5 Reagents and standards . 3
6 Apparatus . 4
7 Sampling and sample pre-treatment. 5
8 Procedure . 5
9 Calibration . 8
10 Test report . 11
Annex A (informative) Clean-up procedures . 12
Annex B (informative) Examples for separation conditions in gas chromatography and mass
spectrometry . 16
Annex C (informative) Typical ions and time windows for electron impact ionization detection. 19
Annex D (informative) Examples of chromatograms and spectra . 20
Annex E (informative) Precision data. 25
Bibliography . 26
© ISO 2006 – All rights reserved iii
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 22032 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods.
iv © ISO 2006 – All rights reserved
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
Introduction
The user should be aware that particular problems could require the specification of additional marginal
conditions.
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SIST EN ISO 22032:2009
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SIST EN ISO 22032:2009
INTERNATIONAL STANDARD ISO 22032:2006(E)
Water quality — Determination of selected polybrominated
diphenyl ethers in sediment and sewage sludge — Method
using extraction and gas chromatography/mass spectrometry
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This standard 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 and to
ensure compliance with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this standard be carried
out by suitably trained staff.
1 Scope
This International Standard specifies a method for the determination of selected polybrominated diphenyl
ethers (PBDE) (see Figure 1 and Table 1) in sediment and sludge using gas chromatography/mass
spectrometry (GC-MS) in the electron impact (EI) or negative ion chemical ionization (NCI) mode.
When using GC-EI-MS, the method is applicable to samples containing 0,05 µg/kg to 25 µg/kg of tetra- to
octabromo congeners and 0,3 µg/kg to 100 µg/kg of decabromo diphenyl ether (BDE-209), respectively.
Approximately ten times lower concentrations can be quantified when using GC-NCI-MS. The risk of
misinterpretation of interfering substances is smaller with EI due to its higher specificity. It is also possible to
analyse other brominated diphenyl ethers according to this International Standard, after verifying its
applicability in each case.
Figure 1 — Chemical formula of polybrominated diphenyl ethers
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
Table 1 — PBDE congeners determined by this method
a
No. Congener Formula Abbreviation Molar mass
g/mol
1 2,2’,4,4’-Tetrabromodiphenyl ether C H BrO BDE-47 485,795 0
12 6 4
2 2,2’,4,4’,5-Pentabromodiphenyl ether C H BrO BDE-99 564,691 1
12 5 5
3 2,2’,4,4’,6-Pentabromodiphenyl ether C H BrO BDE-100 564,691 1
12 5 5
4 2,2’,4,4’,5,6’-Hexabromodiphenyl ether C H BrO BDE-154 643,587 2
12 4 6
5 2,2’,4,4’,5,5’-Hexabromodiphenyl ether C H BrO BDE-153 643,587 2
12 4 6
6 2,2’,3,4,4’,5’,6-Heptabromodiphenyl ether C H BrO BDE-183 722,483 2
12 3 7
7 Decabromodiphenyl ether C BrO BDE-209 959,171 4
12 10
a
Numbering analogous to IUPAC nomenclature for PCB.
2 Normative references
The following referenced documents are indispensable for the application 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 5667-13, Water quality — Sampling — Part 13: Guidance on sampling of sludges from sewage and
water-treatment works
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
Extraction of brominated diphenyl ethers from the dried sample by an organic solvent. Clean-up of the extract
by, e.g. preparative multi-layer silica gel column chromatography. After concentration, separation of the
brominated diphenyl ethers by capillary gas chromatography and detection by either mass spectrometry in the
selected ion monitoring mode using electron impact (EI), or negative ion chemical ionization (NCI). For
determination of the concentration in the sample, an internal standard calibration over the total procedure is
used.
4 Interferences
When applying GC-NCI-MS, 2,2’,4,4’,5,5’-hexabromobiphenyl (BB-153) and tetrabromobisphenol A can co-
elute with BDE-154 and BDE-153, respectively, when using non-polar capillary columns and hence, interfere
with the determination of the corresponding BDE congeners when monitoring the bromide ions m/z = 79 and
m/z = 81. Moreover, naturally produced brominated compounds, such as halogenated bipyrrols and
brominated phenoxyanisols, can be considered as potential interferences.
Sources of contamination are the following: brominated diphenyl ethers used as flame-retardants in organic
polymers. Therefore, contact of the sample or the reagents with these organic polymers shall be avoided.
Transportation paths include airborne dust, vial covers, pasteur pipette fillers and recycled paper.
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
5 Reagents and standards
Only use reagents with negligibly low concentrations of brominated diphenyl ethers compared with the
concentration to be determined and verify by blank determinations. To prevent degradation, store standards in
the dark at temperatures recommended by the manufacturer (calibration solutions should preferably be stored
at approximately −18 °C).
5.1 Solvents for extraction, clean-up and preparation of stock solutions.
A variety of solvents may be used depending on the particular sample matrix to be analysed and the
availability of commercial standard solution, e.g. toluene (C H ), or acetone (propanone, C H O), or a mixture
7 8 3 6
of acetone (propanone, C HO) and hexane (C H ), or heptane (C H ), or iso-octane
3 6 6 14 7 16
(2,2,4-trimethylpentane, C H ), or nonane (C H ), or dichloromethane (CH Cl ) for residual analysis.
8 18 9 20 2 2
5.2 Reference substances.
See Table 1. Solutions of reference substances are commercially available.
5.3 Internal standard substances.
Solutions of reference substances for use as internal standards for electron impact ionization (Table 2,
substances 1 to 5) and for negative ion chemical ionization (Table 2, substances 6, 7 and 8) are commercially
available.
Table 2 — Examples of internal standards
No Name Formula Abbreviation Molar mass
g/mol
Internal standards for GCMS with electron impact ionization
13 13 13
1 2,2’,4,4’-Tetrabromo[ C ]diphenyl ether C H Br O C-BDE-47 497,703 5
12 12 6 4
13 13 13
2 2,2’,4,4’,5-Pentabromo[ C ]diphenyl ether C H Br O C-BDE-99 576,599 5
12 12 5 5
13 13 13
3 2,2’,4,4’,5,5’-Hexabromo[ C ]diphenyl ether C H Br O C-BDE-153 655,495 5
12 12 4 6
13 13 13
4 2,2’,3,4,4’,5’,6-Heptabromo[ C ]diphenyl ether C H Br O C-BDE-183 734,391 6
12 12 3 7
13 13 13
5 Decabromo[ C ]diphenyl ether C Br O C-BDE-209 971,079 7
12 12 10
a
Internal standards for GCMS with negative ion chemical ionization
6 3,3’,4,4’-Tetrabromodiphenyl ether C H Br O BDE-77 485,795 0
12 6 4
7 2,2’,3,4,4’,5,6-Heptabromodiphenyl ether C H Br O BDE-181 722,483 2
12 3 7
13 13 13
8 Decabromo[ C ]diphenyl ether C Br O C-BDE-209 971,079 7
12 12 10
a
Check for interferences when non-labelled PBDE is used as an internal standard. Other BDE congeners are suitable as
internal standards, e.g. BDE-140.
5.4 Sodium sulfate, anhydrous, Na SO , powdered.
2 4
5.5 Operating gases, for gas chromatography/mass spectrometry, of high purity and in accordance with
manufacturer’s specifications.
5.6 Nitrogen, of high purity, at least 99,999 % by volume, for drying and for concentration by evaporation.
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
5.7 Solutions of the single reference substances / internal standards.
Use commercially available solutions (may be in nonane, toluene or iso-octane) or prepare stock solutions,
e.g. by dissolving 10 mg of each of the reference substances (5.2, 5.3) in toluene (5.1) in an amber, 10-ml
volumetric flask and bring to volume (concentration: 1 mg/ml). Store at approximately −18 °C in the dark.
5.8 Multicomponent stock solution of reference substances.
Accurately transfer between 100 µl to 500 µl of each single standard solution (5.7) into an amber, 10-ml
volumetric flask and bring to volume with the appropriate solvent, e.g. toluene, or nonane, or iso-octane (5.1).
(Concentrations are between 10 µg/ml and 50 µg/ml per substance.)
5.9 Calibration solutions for multicomponent-multilevel calibration.
Prepare, e.g. seven calibration solutions with concentrations according to the detection capacity of the mass
spectrometer. Combine the multicomponent stock solutions of reference substances (5.8), internal standards
(5.10) and, if necessary, injection standard (5.12) to produce the solutions (e.g. shown in Table 5) by
appropriate dilution with the appropriate solvent, e.g. toluene, or nonane, or iso-octane (5.1).
In order to avoid potential photodegradation, store the solutions in the dark. Check the concentrations of
calibration solutions before use.
Use one of the calibration solutions to optimize the GC-MS system and to determine the retention times. As
an alternative, determine and use relative retention times.
5.10 Stock solution of the internal standards.
Prepare a stock solution of the internal standards at an appropriate concentration in, e.g. toluene or iso-octane
(2,2,4-trimethylpentane). Dilute this stock solution. See Table 5 for suggested concentrations of calibration
solutions and sample extracts.
5.11 Clean-up material.
See Annex A.
5.12 Injection standard.
Use an injection standard, e.g. dibromooctafluorobiphenyl (C Br F ), to determine recovery rates for the
12 2 8
internal standard in each sample.
5.13 Baked sand.
Bake sand for at least 8 h at 400 °C.
6 Apparatus
Clean all glassware by rinsing with acetone (propanone) (5.1). Heating the glassware to 400 °C will reduce
blanks. Recalibrate volumetric apparatus prior to use if heated.
6.1 Wide-necked bottle, 1 000 ml up to 5 000 ml capacity, for wet sediment or sludge.
6.2 Freeze drying apparatus.
6.3 Deep freezer.
6.4 Mortar and pestle, or a grinding mill.
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
6.5 Drying ovens, capable of maintaining temperatures in the ranges of 100 °C to 400 °C for baking and
storage of clean-up materials, for baking of glassware and for dry residue determination of samples.
6.6 Sieve shaker with appropriate sieve meshes (aperture size), e.g. 2 mm.
6.7 Desiccator.
6.8 Soxhlet extraction apparatus, consisting of round bottom flasks (e.g. 250 ml), Soxhlet extractors and
Soxhlet thimbles (e.g. 27 mm × 100 mm), vertical condensers (e.g. 300 mm) and heating apparatus.
6.9 Evaporation device, e.g. rotary evaporator, turbo evaporator or vacuum concentration device.
6.10 Glass columns for chromatographic clean-up.
6.11 Volumetric cylinders, 250 ml and 500 ml.
6.12 Volumetric flasks, 1 ml, 2 ml, 10 ml, and 25 ml.
6.13 Pasteur pipettes, e.g. 2 ml.
6.14 Syringes, 2 µl, 5 µl, 10 µl and 50 µl, volume precision ± 2 %.
6.15 Sample vials.
Amber glass with fluoropolymer-lined screw-cap is most suitable.
6.16 Gas chromatograph, with either a splitless injection port or an on-column injection port coupled to a
mass spectrometer (GC-MS) with electron impact or chemical ionization and appropriate reactant gas
(e.g. CH ).
4
6.17 Analytical column.
Fused silica column with non-polar low bleed separating phase (see Annex B for examples), e.g. inner
diameter < 0,25 mm, length 15 m to at maximum 30 m (shorter columns for higher brominated congeners).
A film thickness of 0,1 µm is recommended.
7 Sampling and sample pre-treatment
Take samples as specified in ISO 5667-13 in a bottle (6.1). Store and transport in the dark at approximately
4 °C. Pre-treat the samples immediately in the laboratory by homogenizing and freeze-drying. Grind the
samples using apparatus (6.4) and sieve them using a sieve shaker (6.6) according to the analytical task.
8 Procedure
8.1 Extraction
Transfer a suitable mass, e.g. 5 g to 10 g, of the pre-treated, dry sample into a Soxhlet thimble. Depending on
the expected concentration in the sample, add 100 µl to 1 000 µl of the internal standard solution (5.10), to the
Soxhlet thimble. Place the thimble in the Soxhlet extractor. The various solvents given in 5.1 produce similar
extraction efficiencies after a 16 h Soxhlet extraction. Certain sample matrices may require a more polar
solvent to efficiently extract the PDBE congeners, e.g. a mixture of acetone (propanone) and hexane, or
dichloromethane.
Other extraction techniques, e.g. accelerated solvent extraction, and shorter extraction times may be used
after performing comparability exercise with a 16 h Soxhlet extraction.
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
Fill the round-bottomed flask with, e.g. 100 ml of the solvent (5.1) and connect it to the Soxhlet extractor. The
addition of boiling chips is useful. Lower the flask into the heating apparatus. Adjust the temperature of the
heating device until the refluxing solvent reaches the lower part of the vertical condenser. Extract the sample
for 16 h.
After the extraction is complete, concentrate the extract nearly to dryness using a suitable evaporation device
(6.9).
Protect samples and extracts carefully from sunlight to avoid photodegradation of the decabromo diphenyl
ether (C Br O).
12 10
Extraction of BDE-209 requires specific attention and, sometimes, longer extraction times than other PBDE
congeners. Use toluene as an extraction solvent for extraction of BDE-209. During concentration, use toluene
as a keeper.
8.2 Clean-up
Depending on the different sample matrices encountered, a variety of sample extract clean-up procedures
may be suitable. Examples of clean-up procedures are given in Annex A. The recovery efficiency of all internal
standards (see also 9.3 and 9.5) shall be 60 % or better. In most cases, use of a clean-up column given in A.1
followed by the procedure in A.2 is successful.
8.3 Measurement
Optimize the operating conditions of the GC-MS system, e.g. according to the manufacturer’s instructions.
Examples of the gas chromatographic conditions are given in Annex B.
Prior to analysis, establish the operating conditions and verify the GC-MS system performance and the
calibration for all analytes and their internal standards by analysis of a calibration standard.
Add the injection standard (5.12), if necessary, and analyse the sample with GC-MS.
Especially for the analysis of BDE-209, minimise the exposure of the samples to high temperatures for long
periods of times during the injection and separation stages, because of the thermal degradation of BDE-209 at
temperatures higher than 300 °C. Optimize the injection step, paying special attention to the peak height of
BDE-209.
8.4 Blank determination
Analyse as a blank, a clean Soxhlet thimble in exactly the same way as the sample, but replacing the sample
by the appropriate amount of baked sand (5.13). The concentration of PBDE in the blank should be negligible,
compared with the concentrations of PBDEs to be determined.
8.5 Identification
Consider an analyte to be identified,
⎯ if the retention time of the analyte in the mass chromatogram of the sample is the same as the retention
time of the reference substance in the mass chromatogram of the calibration standard solution measured
under identical experimental conditions (the deviation shall be below 1 %, and not exceeding 12 s), and
⎯ if the ratio of the quantification and qualifier mass is within ± 10 % of the theoretical bromine isotope ratio.
See Table 3 for typical ions when negative ion chemical ionization detection used.
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
Table 3 — Ions for negative ion chemical ionization detection
Compound Ions for quantification Ions for qualification
BDE-47 79 81
BDE-99 79 81
BDE-100 79 81
BDE-154 79 81
BDE-153 79 81
BDE-183 79 81
a
BDE-209 486,7 484,7
Internal standards
BDE-77 79 81
BDE-181 79 81
13
C-BDE-209 494,7 496,7
a
Do not use the ion 488,7 because of overlapping with a fragment ion from
13
C-BDE-209.
The following ions (Table 4) are proposed for electron impact ionization detection. The values in brackets are
the percent ratio between the most intensive qualifier ion and the second qualifier ion. Use two representative
masses with a recognizable bromine-pattern for identification of each compound. It is also possible to use
more than one ion for quantification.
Table 4 — Ions for electron impact ionization detection
Compound Ions for quantification Ions for qualification
BDE-47 325,9 483,7 (69,5), 485,7 (100)
BDE-99 405,7 563,6 (100), 565,6 (98)
BDE-100 405,7 563,6 (100), 565,6 (98)
BDE-153 485,7 641,5 (100), 643,5 (73,4)
BDE-154 485,7 641,5 (100), 643,5 (73,4)
BDE-183 563,6 721,4 (100), 723,4 (93,6)
BDE-209 799,3 (100) 959,1 (25), 797,3 (81)
13
C-BDE-47 339,9 495,7 (69.5), 497,7 (100)
13
C-BDE-99 417,7 575,6 (100), 577,6 (98)
13
C-BDE-153 497,7 653,5 (100), 655,5 (73,4)
13
C-BDE-209 811,3 (100) 971,1 (25), 809,3 (81)
Check that the ions used are free from interferences caused by matrix components.
See Annex C for other ions that may be used and suggested time windows.
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SIST EN ISO 22032:2009
ISO 22032:2006(E)
9 Calibration
9.1 General
Modern mass spectrometric detection provides linear correlations between the concentrations of single
substances and the corresponding responses over several decades of concentration. This facilitates an
effective means of calibration. It is necessary to carry out the following steps
...