EN 17503:2022
(Main)Soil, sludge, treated biowaste and waste - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)
Soil, sludge, treated biowaste and waste - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)
This document specifies different methods for quantitative determination of 16 polycyclic aromatic hydrocarbons (PAH) (see Table 2) in soil, sludge, treated biowaste, and waste, using GC-MS or HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels (see Table 2).
NOTE The method can be applied to sediments provided that validity is demonstrated by the user.
When using fluorescence detection, acenaphthylene cannot be measured.
[Table 2 -Target analytes of this document]
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, the lower limit of application from 10 μg/kg (expressed as dry matter) for soils, sludge and biowaste to 100 μg/kg (expressed as dry matter) for solid waste can be achieved. For some specific samples (e.g. bitumen) the limit of 100 μg/kg cannot be reached.
Sludge, waste and treated biowaste can differ in properties as well as in the expected contamination levels of PAH 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.
The method can be applied to the analysis of other PAH not specified in the scope, provided suitability is proven by proper in-house validation experiments.
Sampling is not part of this standard. In dependence of the materials, the following standards need to be considered, e.g. EN 14899, ISO 5667-12 and EN ISO 5667-13.
Boden, Schlamm, behandelter Bioabfall und Abfall - Bestimmung von polycyclischen aromatischen Kohlenwasserstoffen (PAK) mittels Gaschromatographie (GC) und Hochleistungs-Flüssigkeitschromatographie (HPLC)
Dieses Dokument legt verschiedene Verfahren für die quantitative Bestimmung von 16 polycyclischen aromatischen Kohlenwasserstoffen (PAK) (siehe Tabelle 2) in Boden, Schlamm, behandeltem Bioabfall und Abfall mittels GC MS oder HPLC UV DAD/FLD fest, wobei ein breites Spektrum an PAK Kontaminationsniveaus (siehe Tabelle 2) abgedeckt wird.
ANMERKUNG Das Verfahren kann auf Sedimente angewandt werden, sofern der Anwender die Validität nachweist.
Bei Anwendung der Fluoreszenzdetektion kann Acenaphthylen nicht bestimmt werden.
[Tabelle 2]
Die Nachweisgrenze hängt von den zu bestimmenden Substanzen, der verwendeten technischen Ausrüstung, der Qualität der für die Extraktion der Probe verwendeten Chemikalien und der Aufreinigung des Extrakts ab.
Unter den in diesem Dokument festgelegten Bedingungen kann eine untere Anwendungsgrenze zwischen 10 μg/kg (angegeben als Trockenmasse) für Böden, Schlamm und Bioabfall und 100 μg/kg (angegeben als Trockenmasse) für Feststoffabfall erreicht werden. Bei einigen bestimmten Proben (z. B. Bitumen) kann die Grenze von 100 μg/kg nicht erreicht werden.
Schlamm, Abfall und behandelter Bioabfall können sich in Bezug auf ihre Eigenschaften sowie auf die erwarteten PAK Kontaminationsniveaus und das Vorhandensein von störenden Substanzen unterscheiden. Aufgrund dieser Unterschiede ist es unmöglich, ein allgemeines Verfahren darzulegen. Dieses Dokument enthält Entscheidungstabellen, die auf den Eigenschaften der Probe und den anzuwendenden Extraktions und Aufreinigungsverfahren basieren.
Das Verfahren kann für die Analyse weiterer PAK angewendet werden, die im Anwendungsbereich nicht genannt sind, sofern die Eignung des Verfahrens durch hinreichende interne Validierungsuntersuchungen bewiesen wurde.
Die Probenahme ist nicht Bestandteil dieser Norm. In Abhängigkeit von den Materialien bedürfen die folgenden Normen der Berücksichtigung, z. B. EN 14899, ISO 5667 12 und EN ISO 5667 13.
Sols, boues, biodéchets traités et déchets - Dosage des hydrocarbures aromatiques polycycliques (HAP) par chromatographie en phase gazeuse et chromatographie liquide à haute performance
Le présent document spécifie différentes méthodes de dosage de 16 hydrocarbures aromatiques polycycliques (HAP) (voir Tableau 2) dans les sols, les boues, les biodéchets traités et les déchets faisant appel à des méthodes CG-SM ou HPLC-UV-DAD/FLD couvrant une large gamme de niveaux de contamination par les HAP (voir Tableau 2).
NOTE La méthode peut être appliquée aux sédiments sous réserve que l’utilisateur ait démontré la validité.
L’utilisation d’une méthode de détection fluorimétrique ne permet pas le mesurage de l’acénaphtylène.
[Tableau 2 - Analytes cible du présent document]
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, la limite inférieure d’application allant de 10 μg/kg (exprimée par rapport à la matière sèche) pour les sols, boues et biodéchets jusqu’à 100 μg/kg (exprimée par rapport à la matière sèche) pour les déchets solides peut être atteinte. Pour certains échantillons particuliers (bitume, par exemple), la limite de 100 μg/kg ne peut pas être atteinte.
Les boues, les déchets et les biodéchets traités peuvent présenter des propriétés, des niveaux de contamination différents par les HAP attendus et des 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.
La méthode peut être appliquée à l’analyse d’autres HAP non spécifiés dans le domaine d’application, à condition que son adéquation ait été prouvée par des expériences de validation interne.
L’échantillonnage n’est pas couvert par la présente norme. Selon le type de matériau, il est nécessaire de prendre en compte par exemple les normes suivantes : l’EN 14899, l’ISO 5667-12 et l’EN ISO 5667-13.
Tla, blato, obdelani biološki odpadki in odpadki - Določevanje policikličnih aromatskih ogljikovodikov (PAH) s plinsko kromatografijo (GC) in s tekočinsko kromatografijo visoke ločljivosti (HPLC)
Ta evropski standard določa metodo za kvantitativno določevanje 16 policikličnih aromatskih ogljikovodikov (PAH) (glej preglednico) v tleh, blatu, usedlinah, obdelanih bioloških odpadkih in odpadkih z metodama GC-MS in HPLC-UV-DAD/FLD, ki zajemata široko območje ravni onesnaženja PAH (glej preglednico 2).
S fluorescenčnim zaznavanjem ni mogoče izmeriti acenaftilena.
Preglednica – Ciljni analiti tega evropskega standarda
Ciljni analit CAS-RNa
Naftalen 91–20–3
Acenaften 83–32–9
Acenaftilen 208–96–8
Fluoren 86–73–7
Antracen 120–12–7
Fenantren 85–01–8
Fluoranten 206-44-0
Piren 129-00-0
Benz[a]antracen 56–55–3
Krizen 218–01–9
Benzo[b]fluoranten 205–99–2
Benzo[k]fluoranten 207–08–9
Benzo[a]piren 50–32–8
Indeno[1,2,3-cd]piren 193–39–5
Dibenzo[a,h]antracen 53–70–3
Benzo[ghi]perilen 191–24–2
a Registrska številka Chemical Abstracts Service CAS-RN.
Meja detekcije je odvisna od determinant, uporabljene opreme, kakovosti kemikalij, uporabljenih za ekstrakcijo vzorca in očiščenje izvlečka.
Pod pogoji, določenimi v tem evropskem standardu, je mogoče doseči spodnjo mejo uporabe od 10 μg/kg (izraženo kot suha snov) za tla, blato in biološke odpadke do 100 μg/kg (izraženo kot suha snov) za trdne odpadke. Za nekatere specifične vzorce (npr. bitumen) ni mogoče doseči meje 100 μg/kg.
Blato, odpadki in obdelani biološki odpadki se lahko razlikujejo glede lastnosti in tudi glede predvidenih stopenj onesnaženja s policikličnimi aromatskimi ogljikovodiki ter prisotnosti motečih snovi. Zaradi teh razlik ni možen opis enotnega splošnega postopka. Ta evropski standard vključuje tabele odločanja, ki temeljijo na lastnostih vzorca, ter postopek za ekstrakcijo in očiščenje, ki ga je treba uporabiti.
Metoda se lahko uporablja za analize drugih policikličnih aromatskih ogljikovodikov, ki ne spadajo na področje uporabe tega standarda, če je njena ustreznost dokazana s primernimi internimi poskusi za validacijo.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-marec-2023
Nadomešča:
SIST EN 15527:2009
SIST EN 16181:2018
SIST ISO 13877:1999
Tla, blato, obdelani biološki odpadki in odpadki - Določevanje policikličnih
aromatskih ogljikovodikov (PAH) s plinsko kromatografijo (GC) in s tekočinsko
kromatografijo visoke ločljivosti (HPLC)
Soil, sludge, treated biowaste and waste - Determination of polycyclic aromatic
hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid
chromatography (HPLC)
Boden, Schlamm, behandelter Bioabfall und Abfall - Bestimmung von polycyclischen
aromatischen Kohlenwasserstoffen (PAK) mittels Gaschromatographie (GC) und
Hochleistungs-Flüssigkeitschromatographie (HPLC)
Sols, boues, biodéchets traités et déchets - Dosage des hydrocarbures aromatiques
polycycliques (HAP) par chromatographie en phase gazeuse et chromatographie liquide
à haute performance
Ta slovenski standard je istoveten z: EN 17503:2022
ICS:
13.030.01 Odpadki na splošno Wastes in general
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 17503
EUROPEAN STANDARD
NORME EUROPÉENNE
February 2022
EUROPÄISCHE NORM
ICS 13.030.01; 13.080.10 Supersedes EN 15527:2008, EN 16181:2018
English Version
Soil, sludge, treated biowaste and waste - Determination of
polycyclic aromatic hydrocarbons (PAH) by gas
chromatography (GC) and high performance liquid
chromatography (HPLC)
Sols, boues, biodéchets traités et déchets - Dosage des Boden, Schlamm, behandelter Bioabfall und Abfall -
hydrocarbures aromatiques polycycliques (HAP) par Bestimmung von polycyclischen aromatischen
chromatographie en phase gazeuse et Kohlenwasserstoffen (PAK) mittels
chromatographie liquide à haute performance Gaschromatographie (GC) und Hochleistungs-
Flüssigkeitschromatographie (HPLC)
This European Standard was approved by CEN on 3 January 2022.
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 NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17503:2022 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 6
3 Terms and definitions . 6
4 Principle . 8
5 Interferences . 8
6 Safety remarks . 9
7 Reagents . 10
8 Apparatus . 14
9 Sample storage and preservation . 15
10 Procedure . 16
11 Performance characteristics. 29
12 Precision . 29
13 Test report . 30
Annex A (informative) Repeatability and reproducibility data . 31
A.1 Materials used in the interlaboratory comparison study . 31
A.2 Interlaboratory comparison results . 32
Annex B (informative) Examples of instrumental conditions and chromatograms . 39
B.1 Measurement of PAH with GC-MS . 39
B.2 Measurement of PAH with HPLC fluorescence . 45
B.3 Example for measurement conditions of PAH with GC-MS/MS . 51
Bibliography . 53
European foreword
This document (EN 17503:2022) 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 August 2022, and conflicting national standards shall be
withdrawn at the latest by August 2022.
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 15527:2008 and EN 16181:2018.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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
Polycyclic aromatic hydrocarbons (PAH) are ubiquitous because they are released in appreciable
quantities every year into the environment through the combustion of organic matters such as coal, fuel
oils, petrol, wood, refuse and plant materials. Since some of these PAH compounds are carcinogenic or
mutagenic, their presence in the environment (air, water, soil, sediment and waste) is regularly
monitored and controlled. At present determination of PAH is carried out in these matrices in most of the
routine laboratories following the prescribed steps specified for sampling, pre-treatment, extraction,
clean-up by measurement of specific PAH by means of gas chromatography in combination with mass
spectrometric detection (GC-MS) or by high performance liquid chromatography (HPLC) in combination
with UV-DAD- or fluorescence detection (HPLC-UV-DAD/FLD). Both the GC-MS and the HPLC methods
are included in this horizontal standard.
This document was developed by the merging of EN 16181:2018, 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 15527, 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.
Quantification with both GC-MS-detection and HPLC-DAD-UV/FLD is possible. Four different extraction
procedures are described and three 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 polychlorinated biphenyls (PCB)
in EN 17322. 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 document is applicable and validated
Matrix Materials used for validation
Soil Sandy soil
Mix of soil from an industrial area in Brandenburg, Germany and
PAH-free German reference soil
Sludge Mix of municipal waste water treatment plant sludge from the
vicinity of Berlin, Germany
Biowaste Mix of compost from the vicinity of Berlin, Germany
Contaminated soil, building debris, waste wood, roofing tar,
Waste
shredder light fraction
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.
WARNING — It is absolutely essential that tests conducted according to this document be carried out by
suitably trained staff.
1 Scope
This document specifies different methods for quantitative determination of 16 polycyclic aromatic
hydrocarbons (PAH) (see Table 2) in soil, sludge, treated biowaste, and waste, using GC-MS or HPLC-UV-
DAD/FLD covering a wide range of PAH contamination levels (see Table 2).
NOTE The method can be applied to sediments provided that validity is demonstrated by the user.
When using fluorescence detection, acenaphthylene cannot be measured.
Table 2 —Target analytes of this document
a
Target analyte
CAS-RN
Naphthalene 91–20–3
Acenaphthene 83–32–9
Acenaphthylene 208–96–8
Fluorene 86–73–7
Anthracene 120–12–7
Phenanthrene 85–01–8
Fluoranthene 206–44–0
Pyrene 129–00–0
Benz[a]anthracene 56–55–3
Chrysene 218–01–9
Benzo[b]fluoranthene 205–99–2
Benzo[k]fluoranthene 207–08–9
Benzo[a]pyrene 50–32–8
Indeno[1,2,3-cd]pyrene 193–39–5
Dibenz[a,h]anthracene 53–70–3
Benzo[ghi]perylene 191–24–2
a
CAS-RN Chemical Abstracts Service Registry Number.
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, the lower limit of application from 10 μg/kg (expressed
as dry matter) for soils, sludge and biowaste to 100 μg/kg (expressed as dry matter) for solid waste can
be achieved. For some specific samples (e.g. bitumen) the limit of 100 μg/kg cannot be reached.
Sludge, waste and treated biowaste can differ in properties as well as in the expected contamination
levels of PAH 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.
The method can be applied to the analysis of other PAH not specified in the scope, provided suitability is
proven by proper in-house validation experiments.
Sampling is not part of this standard. In dependence of the materials, the following standards need to be
considered, e.g. EN 14899, ISO 5667-12 and EN ISO 5667-13.
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.
EN 15002, Characterization of waste — Preparation of test portions from the laboratory sample
EN 15934, Sludge, treated biowaste, soil and waste — Calculation of dry matter fraction after
determination of dry residue or water content
EN 16179, Sludge, treated biowaste and soil — Guidance for sample pretreatment
EN ISO 5667-15, Water quality — Sampling — Part 15: Guidance on the preservation and handling of
sludge and sediment samples (ISO 5667-15)
EN ISO 16720, Soil quality — Pretreatment of samples by freeze-drying for subsequent analysis (ISO 16720)
EN ISO 22892, Soil quality — Guidelines fo
...
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