EN 17322:2020
(Main)Environmental Solid Matrices - Determination of polychlorinated biphenyls (PCB) by gas chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-ECD)
Environmental Solid Matrices - Determination of polychlorinated biphenyls (PCB) by gas chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-ECD)
This document specifies methods for quantitative determination of seven selected polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in soil, sludge, sediment, treated biowaste, and waste using GC-MS and GC-ECD (see Table 2).
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract.
Under the conditions specified in this document, lower limit of application from 1 μg/kg (expressed as dry matter) for soils, sludge and biowaste to 10 μg/kg (expressed as dry matter) for solid waste can be achieved. For some specific samples the limit of 10 μg/kg cannot be reached.
Sludge, waste and treated biowaste may differ in properties, as well as in the expected contamination levels of PCB and presence of interfering substances. These differences make it impossible to describe one general procedure. This document contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used.
NOTE The analysis of PCB in insulating liquids, petroleum products, used oils and aqueous samples is referred to in EN 61619, EN 12766-1 and EN ISO 6468 respectively.
The method can be applied to the analysis of other PCB congeners not specified in the scope, provided suitability is proven by proper in-house validation experiments.
Feststoffe in der Umwelt - Bestimmung von polychlorierten Biphenylen (PCB) mittels Gaschromatographie und massenspektrometrischer Detektion (GC-MS) oder Elektronen-Einfang-Detektion (GC-ECD)
Dieses Dokument legt Verfahren für die quantitative Bestimmung von sieben ausgewählten polychlorierten Biphenylen (PCB 28, PCB 52, PCB 101, PCB 118, PCB 138, PCB 153 und PCB 180) in Boden, Schlamm, Sediment, behandeltem Bioabfall und Abfall unter Anwendung der GC MS und GC ECD fest (siehe Tabelle 2).
[Tabelle 2]
Die Nachweisgrenze hängt von den zu bestimmenden Stoffen, den verwendeten Geräten, der Qualität der für die Extraktion der Probe verwendeten Chemikalien und der Reinigung des Extrakts ab.
Unter den in diesem Dokument festgelegten Bedingungen kann eine untere Anwendungsgrenze zwischen 1 μg/kg (angegeben als Trockenmasse) für Böden, Schlamm und Bioabfall und 10 μg/kg (angegeben als Trockenmasse) für Feststoffabfall erreicht werden. Bei einigen speziellen Proben kann die Grenze von 10 µg/kg nicht erreicht werden.
Schlamm, Abfall und behandelter Bioabfall können sich hinsichtlich ihrer Eigenschaften sowie hinsichtlich der erwarteten Kontaminationsniveaus von PCB und der Anwesenheit von störenden Stoffen unterscheiden. Aufgrund dieser Unterschiede ist es unmöglich, ein allgemeines Verfahren zu beschreiben. Dieses Dokument enthält Entscheidungstabellen, die auf den Eigenschaften der Probe und den anzuwendenden Extraktions- und Aufreinigungsverfahren basieren.
ANMERKUNG Für die Analyse von PCB in Isolierflüssigkeiten, Mineralölerzeugnissen, Gebrauchtölen und wässrigen Proben wird jeweils auf EN 61619, EN 12766 1 bzw. EN ISO 6468 verwiesen.
Das Verfahren kann für die Analyse weiterer, nicht im Anwendungsbereich festgelegter PCB Kongenere angewendet werden, vorausgesetzt, seine Eignung wurde durch geeignete laborinterne Validierungs¬untersuchungen nachgewiesen.
Matrices solides environnementales - Dosage des polychlorobiphényles (PCB) par chromatographie en phase gazeuse-spectrométrie de masse (CG-SM) ou chromatographie en phase gazeuse avec détection par capture d’électrons (CG-ECD)
Le présent document spécifie les méthodes de dosage, par CG-SM et CG-ECD, de sept polychlorobiphényles choisis (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 et PCB180) dans les sols, les boues, les sédiments, les biodéchets traités et les déchets (voir Tableau 2).
La limite de détection dépend des composés à analyser, de l’équipement utilisé, de la qualité des réactifs chimiques utilisés pour l’extraction de l’échantillon et la purification de l’extrait.
Dans les conditions spécifiées dans le présent document, il est possible d’atteindre une limite inférieure d’application de 1 μg/kg (exprimée sur matière sèche) pour les sols, les boues et les biodéchets à 10 μg/kg (exprimée sur matière sèche) pour les déchets solides. Pour certains échantillons spécifiques, la limite de 10 μg/kg ne peut pas être atteinte.
Les boues, les déchets et les biodéchets traités peuvent présenter des différences en termes de propriétés, de niveaux prévus de contamination par les PCB et de présence de substances interférentes. En raison de ces différences, il est impossible de décrire un mode opératoire général. Le présent document contient des tables de décision basées sur les propriétés de l’échantillon ainsi que sur le mode opératoire d’extraction et de purification à utiliser.
NOTE Pour l’analyse des PCB dans les liquides isolants, les produits pétroliers, les huiles usagées et les échantillons aqueux, se référer respectivement aux normes EN 61619, EN 12766-1 et EN ISO 6468.
La méthode peut être appliquée à l’analyse de congénères de PCB autres que ceux décrits dans le domaine d’application, à condition d’en définir l’applicabilité par des tests de validation internes adaptés.
Trdni matriksi v okolju - Določanje polikloriranih bifenilov (PCB) s plinsko kromatografijo z masno selektivnim detektorjem (GC-MS) ali s plinsko kromatografijo z detektorjem z zajetjem elektronov (GC-ECD)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-november-2020
Nadomešča:
SIST EN 15308:2017
SIST EN 16167:2018+AC:2019
Trdni matriksi v okolju - Določanje polikloriranih bifenilov (PCB) s plinsko
kromatografijo z masno selektivnim detektorjem (GC-MS) ali s plinsko
kromatografijo z detektorjem z zajetjem elektronov (GC-ECD)
Environmental Solid Matrices - Determination of polychlorinated biphenyls (PCB) by gas
chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-
ECD)
Feststoffe in der Umwelt - Bestimmung von polychlorierten Biphenylen (PCB) mittels
Gaschromatographie und massenspektrometrischer Detektion (GC-MS) oder
Elektronen-Einfang-Detektion (GC-ECD)
Matrices solides environnementales - Dosage des polychlorobiphényles (PCB) par
chromatographie en phase gazeuse-spectrométrie de masse (CG-SM) ou
chromatographie en phase gazeuse avec détection par capture d’électrons (CG-ECD)
Ta slovenski standard je istoveten z: EN 17322:2020
ICS:
13.030.10 Trdni odpadki Solid wastes
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
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 17322
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2020
EUROPÄISCHE NORM
ICS 13.030.01; 13.030.10; 13.030.20; 13.080.10 Supersedes EN 15308:2016, EN 16167:2018+AC:2019
English Version
Environmental Solid Matrices - Determination of
polychlorinated biphenyls (PCB) by gas chromatography -
mass selective detection (GC-MS) or electron-capture
detection (GC-ECD)
Matrices solides environnementales - Dosage des Feststoffe in der Umwelt - Bestimmung von
polychlorobiphényles (PCB) par chromatographie en polychlorierten Biphenylen (PCB) mittels
phase gazeuse-spectrométrie de masse (CG-SM) ou Gaschromatographie und massenspektrometrischer
chromatographie en phase gazeuse avec détection par Detektion (GC-MS) oder Elektronen-Einfang-Detektion
capture d'électrons (CG-ECD) (GC-ECD)
This European Standard was approved by CEN on 15 June 2020.
This European Standard was corrected and reissued by the CEN-CENELEC Management Centre on 9 September 2020.
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, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATIO N
EUROPÄISCHES KOMITEE FÜR NORMUN G
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17322:2020 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 6
4 Principle . 7
5 Interferences . 8
5.1 Interference with sampling and extraction . 8
5.2 Interference with GC . 8
6 Safety remarks . 8
7 Reagents . 9
7.1 General . 9
7.2 Reagents for extraction . 9
7.3 Reagents for clean-up . 9
7.4 Gas chromatographic analysis . 12
7.5 Standards . 12
7.6 Preparation of standard solutions . 14
8 Apparatus . 15
8.1 Extraction and clean-up procedures . 15
8.2 Gas chromatograph . 16
9 Sample storage and preservation . 16
9.1 Sample storage . 16
9.2 Sample pre-treatment . 16
10 Procedure. 17
10.1 Blank test . 17
10.2 Extraction . 17
10.3 Concentration . 20
10.4 Clean-up of the extract . 20
10.5 Addition of the injection standard . 24
10.6 Gas chromatographic analysis (GC) . 24
10.7 Mass spectrometry (MS) . 24
10.8 Electron capture detection (ECD) . 28
11 Performance characteristics . 30
12 Precision . 30
13 Test report . 30
Annex A (informative) Repeatability and reproducibility data . 31
A.1 Materials used in the inter-laboratory comparison study . 31
A.2 Inter-laboratory comparison results . 32
Annex B (informative) Examples for gas chromatographic conditions and retention times
of PCBs . 36
Annex C (informative) Calculation method for the estimation of total PCB content . 37
Bibliography . 45
European foreword
This document (EN 17322:2020) has been prepared by Technical Committee CEN/TC 444
“Environmental characterization of solid matrices”, the secretariat of which is held by NEN.
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 January 2021, and conflicting national standards shall
be withdrawn at the latest by January 2021.
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 16167:2018+AC:2019 and EN 15308:2016.
This document is the result of the merging of EN 16167:2018+AC:2019 and EN 15308:2016, with minor
technical modifications.
According to the CEN-CENELEC Internal Regulations, the national standards organisations 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, Turkey and the United
Kingdom.
Introduction
Polychlorinated biphenyls (PCB) have been widely used as additives in industrial applications where
chemical stability has been required. This stability on the other hand creates environmental problems
when PCB are eventually released into the environment. Since some of these PCB compounds are highly
toxic, their presence in the environment (air, water, soil, sediment and waste) is regularly monitored and
controlled. At present determination of PCB is carried out in these matrices in most of the routine
laboratories following the preceding steps for sampling, pre-treatment, extraction and clean-up, by
measurement of specific PCB by means of gas chromatography in combination with mass spectrometric
detection (GC-MS) or gas chromatography with electron capture detector (GC-ECD).
This document was developed by merging of EN 16167:2018+AC:2019, initially elaborated as a CEN
Technical Specification in the European project 'HORIZONTAL' and validated by CEN/TC 400 with the
support of BAM, with EN 15308, published by CEN/TC 292.
Considered the different matrices and possible interfering compounds, this document does not contain
one single possible way of working. Several choices are possible, in particular relating to clean-up.
Detection with both MS-detection and ECD-detection is possible. Two different extraction procedures are
described and 9 clean-up procedures. The use of internal and injection standards is described in order to
have an internal check on choice of the extraction and clean-up procedure. The method is as far as
possible in agreement with the method described for PAH (EN 16181:2018 and EN 15527:2008). It has
been tested for ruggedness.
This document is applicable and validated for several types of matrices as indicated in Table 1 (see also
Annex A for the results of the validation).
Table 1 — Matrices for which this European Standard is applicable and validated
Matrix Materials used for validation
Soil Sandy soil
Mix of soil from the vicinity of Berlin, Germany and PCB-free
German reference soil
Sludge Mix of municipal waste water treatment plant sludge from
North Rhine Westphalia, Germany
Biowaste Mix of compost from the vicinity of Berlin, Germany and
sludge from North Rhine Westphalia, Germany
Waste Contaminated soil, building debris, waste wood, sealant
waste, electronic waste, shredder light fraction, cable
shredder waste
WARNING — Persons using this document should be familiar with usual 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 and to ensure compliance
with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted acco
...
SLOVENSKI STANDARD
01-november-2020
Nadomešča:
SIST EN 15308:2017
SIST EN 16167:2018+AC:2019
Trdni matriksi z vidika okolja - Določevanje polikloriranih bifenilov (PCB) s plinsko
kromatografijo z masno selektivnim detektorjem (GC-MS) ali s plinsko
kromatografijo z detektorjem z zajetjem elektronov (GC-ECD)
Environmental Solid Matrices - Determination of polychlorinated biphenyls (PCB) by gas
chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-
ECD)
Feststoffe in der Umwelt - Bestimmung von polychlorierten Biphenylen (PCB) mittels
Gaschromatographie und massenspektrometrischer Detektion (GC-MS) oder
Elektronen-Einfang-Detektion (GC-ECD)
Matrices solides environnementales - Dosage des polychlorobiphényles (PCB) par
chromatographie en phase gazeuse-spectrométrie de masse (CG-SM) ou
chromatographie en phase gazeuse avec détection par capture d’électrons (CG-ECD)
Ta slovenski standard je istoveten z: EN 17322:2020
ICS:
13.030.10 Trdni odpadki Solid wastes
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
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 17322
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2020
EUROPÄISCHE NORM
ICS 13.030.01; 13.030.10; 13.030.20; 13.080.10 Supersedes EN 15308:2016, EN 16167:2018+AC:2019
English Version
Environmental Solid Matrices - Determination of
polychlorinated biphenyls (PCB) by gas chromatography -
mass selective detection (GC-MS) or electron-capture
detection (GC-ECD)
Matrices solides environnementales - Dosage des Feststoffe in der Umwelt - Bestimmung von
polychlorobiphényles (PCB) par chromatographie en polychlorierten Biphenylen (PCB) mittels
phase gazeuse-spectrométrie de masse (CG-SM) ou Gaschromatographie und massenspektrometrischer
chromatographie en phase gazeuse avec détection par Detektion (GC-MS) oder Elektronen-Einfang-Detektion
capture d'électrons (CG-ECD) (GC-ECD)
This European Standard was approved by CEN on 15 June 2020.
This European Standard was corrected and reissued by the CEN-CENELEC Management Centre on 9 September 2020.
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, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATIO N
EUROPÄISCHES KOMITEE FÜR NORMUN G
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17322:2020 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 6
4 Principle . 7
5 Interferences . 8
5.1 Interference with sampling and extraction . 8
5.2 Interference with GC . 8
6 Safety remarks . 8
7 Reagents . 9
7.1 General . 9
7.2 Reagents for extraction . 9
7.3 Reagents for clean-up . 9
7.4 Gas chromatographic analysis . 12
7.5 Standards . 12
7.6 Preparation of standard solutions . 14
8 Apparatus . 15
8.1 Extraction and clean-up procedures . 15
8.2 Gas chromatograph . 16
9 Sample storage and preservation . 16
9.1 Sample storage . 16
9.2 Sample pre-treatment . 16
10 Procedure. 17
10.1 Blank test . 17
10.2 Extraction . 17
10.3 Concentration . 20
10.4 Clean-up of the extract . 20
10.5 Addition of the injection standard . 24
10.6 Gas chromatographic analysis (GC) . 24
10.7 Mass spectrometry (MS) . 24
10.8 Electron capture detection (ECD) . 28
11 Performance characteristics . 30
12 Precision . 30
13 Test report . 30
Annex A (informative) Repeatability and reproducibility data . 31
A.1 Materials used in the inter-laboratory comparison study . 31
A.2 Inter-laboratory comparison results . 32
Annex B (informative) Examples for gas chromatographic conditions and retention times
of PCBs . 36
Annex C (informative) Calculation method for the estimation of total PCB content . 37
Bibliography . 45
European foreword
This document (EN 17322:2020) has been prepared by Technical Committee CEN/TC 444
“Environmental characterization of solid matrices”, the secretariat of which is held by NEN.
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 January 2021, and conflicting national standards shall
be withdrawn at the latest by January 2021.
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 16167:2018+AC:2019 and EN 15308:2016.
This document is the result of the merging of EN 16167:2018+AC:2019 and EN 15308:2016, with minor
technical modifications.
According to the CEN-CENELEC Internal Regulations, the national standards organisations 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, Turkey and the United
Kingdom.
Introduction
Polychlorinated biphenyls (PCB) have been widely used as additives in industrial applications where
chemical stability has been required. This stability on the other hand creates environmental problems
when PCB are eventually released into the environment. Since some of these PCB compounds are highly
toxic, their presence in the environment (air, water, soil, sediment and waste) is regularly monitored and
controlled. At present determination of PCB is carried out in these matrices in most of the routine
laboratories following the preceding steps for sampling, pre-treatment, extraction and clean-up, by
measurement of specific PCB by means of gas chromatography in combination with mass spectrometric
detection (GC-MS) or gas chromatography with electron capture detector (GC-ECD).
This document was developed by merging of EN 16167:2018+AC:2019, initially elaborated as a CEN
Technical Specification in the European project 'HORIZONTAL' and validated by CEN/TC 400 with the
support of BAM, with EN 15308, published by CEN/TC 292.
Considered the different matrices and possible interfering compounds, this document does not contain
one single possible way of working. Several choices are possible, in particular relating to clean-up.
Detection with both MS-detection and ECD-detection is possible. Two different extraction procedures are
described and 9 clean-up procedures. The use of internal and injection standards is described in order to
have an internal check on choice of the extraction and clean-up procedure. The method is as far as
possible in agreement with the method described for PAH (EN 16181:2018 and EN 15527:2008). It has
been tested for ruggedness.
This document is applicable and validated for several types of matrices as indicated in Table 1 (see also
Annex A for the results of the validation).
Table 1 — Matrices for which this European Standard is applicable and validated
Matrix Materials used for validation
Soil Sandy soil
Mix of soil from the vicinity of Berlin, Germany and PCB-free
German reference soil
Sludge Mix of municipal waste water treatment plant sludge from
North Rhine Westphalia, Germany
Biowaste Mix of compost from the vicinity of Berlin, Germany and
sludge from North Rhine Westphalia, Germany
Waste Contaminated soil, building debris, waste wood, sealant
waste, electronic waste, shredder light fraction, cable
shredder waste
WARNING — Persons using this document should be familiar with usual 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 and to ensure compliance
with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests condu
...
SLOVENSKI STANDARD
01-november-2020
Nadomešča:
SIST EN 15308:2017
SIST EN 16167:2018+AC:2019
Trdni matriksi z vidika okolja - Določevanje polikloriranih bifenilov (PCB) s plinsko
kromatografijo z masno selektivnim detektorjem (GC-MS) ali s plinsko
kromatografijo z detektorjem z zajetjem elektronov (GC-ECD)
Environmental Solid Matrices - Determination of polychlorinated biphenyls (PCB) by gas
chromatography - mass selective detection (GC-MS) or electron-capture detection (GC-
ECD)
Feststoffe in der Umwelt - Bestimmung von polychlorierten Biphenylen (PCB) mittels
Gaschromatographie und massenspektrometrischer Detektion (GC-MS) oder
Elektronen-Einfang-Detektion (GC-ECD)
Matrices solides environnementales - Dosage des polychlorobiphényles (PCB) par
chromatographie en phase gazeuse-spectrométrie de masse (CG-SM) ou
chromatographie en phase gazeuse avec détection par capture d’électrons (CG-ECD)
Ta slovenski standard je istoveten z: EN 17322:2020
ICS:
13.030.10 Trdni odpadki Solid wastes
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
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 17322
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2020
EUROPÄISCHE NORM
ICS 13.030.01; 13.030.10; 13.030.20; 13.080.10 Supersedes EN 15308:2016, EN 16167:2018+AC:2019
English Version
Environmental Solid Matrices - Determination of
polychlorinated biphenyls (PCB) by gas chromatography -
mass selective detection (GC-MS) or electron-capture
detection (GC-ECD)
Matrices solides environnementales - Dosage des Feststoffe in der Umwelt - Bestimmung von
polychlorobiphényles (PCB) par chromatographie en polychlorierten Biphenylen (PCB) mittels
phase gazeuse-spectrométrie de masse (CG-SM) ou Gaschromatographie und massenspektrometrischer
chromatographie en phase gazeuse avec détection par Detektion (GC-MS) oder Elektronen-Einfang-Detektion
capture d'électrons (CG-ECD) (GC-ECD)
This European Standard was approved by CEN on 15 June 2020.
This European Standard was corrected and reissued by the CEN-CENELEC Management Centre on 9 September 2020.
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, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATIO N
EUROPÄISCHES KOMITEE FÜR NORMUN G
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17322:2020 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 6
4 Principle . 7
5 Interferences . 8
5.1 Interference with sampling and extraction . 8
5.2 Interference with GC . 8
6 Safety remarks . 8
7 Reagents . 9
7.1 General . 9
7.2 Reagents for extraction . 9
7.3 Reagents for clean-up . 9
7.4 Gas chromatographic analysis . 12
7.5 Standards . 12
7.6 Preparation of standard solutions . 14
8 Apparatus . 15
8.1 Extraction and clean-up procedures . 15
8.2 Gas chromatograph . 16
9 Sample storage and preservation . 16
9.1 Sample storage . 16
9.2 Sample pre-treatment . 16
10 Procedure. 17
10.1 Blank test . 17
10.2 Extraction . 17
10.3 Concentration . 20
10.4 Clean-up of the extract . 20
10.5 Addition of the injection standard . 24
10.6 Gas chromatographic analysis (GC) . 24
10.7 Mass spectrometry (MS) . 24
10.8 Electron capture detection (ECD) . 28
11 Performance characteristics . 30
12 Precision . 30
13 Test report . 30
Annex A (informative) Repeatability and reproducibility data . 31
A.1 Materials used in the inter-laboratory comparison study . 31
A.2 Inter-laboratory comparison results . 32
Annex B (informative) Examples for gas chromatographic conditions and retention times
of PCBs . 36
Annex C (informative) Calculation method for the estimation of total PCB content . 37
Bibliography . 45
European foreword
This document (EN 17322:2020) has been prepared by Technical Committee CEN/TC 444
“Environmental characterization of solid matrices”, the secretariat of which is held by NEN.
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 January 2021, and conflicting national standards shall
be withdrawn at the latest by January 2021.
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 16167:2018+AC:2019 and EN 15308:2016.
This document is the result of the merging of EN 16167:2018+AC:2019 and EN 15308:2016, with minor
technical modifications.
According to the CEN-CENELEC Internal Regulations, the national standards organisations 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, Turkey and the United
Kingdom.
Introduction
Polychlorinated biphenyls (PCB) have been widely used as additives in industrial applications where
chemical stability has been required. This stability on the other hand creates environmental problems
when PCB are eventually released into the environment. Since some of these PCB compounds are highly
toxic, their presence in the environment (air, water, soil, sediment and waste) is regularly monitored and
controlled. At present determination of PCB is carried out in these matrices in most of the routine
laboratories following the preceding steps for sampling, pre-treatment, extraction and clean-up, by
measurement of specific PCB by means of gas chromatography in combination with mass spectrometric
detection (GC-MS) or gas chromatography with electron capture detector (GC-ECD).
This document was developed by merging of EN 16167:2018+AC:2019, initially elaborated as a CEN
Technical Specification in the European project 'HORIZONTAL' and validated by CEN/TC 400 with the
support of BAM, with EN 15308, published by CEN/TC 292.
Considered the different matrices and possible interfering compounds, this document does not contain
one single possible way of working. Several choices are possible, in particular relating to clean-up.
Detection with both MS-detection and ECD-detection is possible. Two different extraction procedures are
described and 9 clean-up procedures. The use of internal and injection standards is described in order to
have an internal check on choice of the extraction and clean-up procedure. The method is as far as
possible in agreement with the method described for PAH (EN 16181:2018 and EN 15527:2008). It has
been tested for ruggedness.
This document is applicable and validated for several types of matrices as indicated in Table 1 (see also
Annex A for the results of the validation).
Table 1 — Matrices for which this European Standard is applicable and validated
Matrix Materials used for validation
Soil Sandy soil
Mix of soil from the vicinity of Berlin, Germany and PCB-free
German reference soil
Sludge Mix of municipal waste water treatment plant sludge from
North Rhine Westphalia, Germany
Biowaste Mix of compost from the vicinity of Berlin, Germany and
sludge from North Rhine Westphalia, Germany
Waste Contaminated soil, building debris, waste wood, sealant
waste, electronic waste, shredder light fraction, cable
shredder waste
WARNING — Persons using this document should be familiar with usual 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 and to ensure compliance
with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests condu
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