prEN 18261

Compost and digestate - 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 1) in compost or digestate, using GC-MS, GCMS/MS or HPLC UV DAD/FLD covering a wide range of PAH contamination levels (see Table 1).
When using fluorescence detection, acenaphthylene cannot be measured.
Table 1 — Target analytes of this document
[...table not reproduced...]
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.
This document contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used.
The method may be applied to the analysis of other PAH not specified in the scope, provided suitability is proven by proper in-house validation experiments.

Kompost und Gärreste - 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 (PAKs) (siehe Tabelle 1) in Kompost oder Gärresten mittels GC-MS, GC-MS/MS oder HPLC-UV-DAD/FLD fest, wobei ein breites Spektrum an PAK-Kontaminationsniveaus (siehe Tabelle 1) abgedeckt wird.
Bei Anwendung von Fluoreszenzdetektion kann Acenaphthylen nicht bestimmt werden.
Tabelle 1 — Zielanalyte dieses Dokuments
[...table not reproduced...]
Die Nachweisgrenze hängt von den zu bestimmenden Substanzen, der verwendeten Ausrüstung, der Qualität der für die Extraktion der Probe verwendeten Chemikalien und der Aufreinigung des Extrakts ab.
Dieses Dokument enthält Entscheidungstabellen, die auf den Eigenschaften der Probe basieren, und die anzuwendenden Extraktions- und Aufreinigungsverfahren.
Das Verfahren darf für die Analyse weiterer PAKs angewendet werden, die im Anwendungsbereich nicht genannt sind, sofern die Eignung des Verfahrens durch hinreichende interne Validierungsuntersuchungen bewiesen wurde.

Compost et digestat - Dosage des hydrocarbures aromatiques polycycliques (HAP) par chromatographie en phase gazeuse (CG) et chromatographie liquide à haute performance (HPLC)

Le présent document spécifie différentes méthodes de dosage de 16 hydrocarbures aromatiques polycycliques (HAP) (voir le Tableau 1) dans le compost ou le digestat, faisant appel à des méthodes CG-SM, CG-SM/SM ou HPLC-UV-DAD/FLD couvrant une large gamme de niveaux de contamination par les HAP (voir le Tableau 1).
L’utilisation d’une méthode de détection fluorimétrique ne permet pas le mesurage de l’acénaphtylène.
Tableau 1 — Analytes cibles du présent document
[...table not reproduced...]
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.
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.

Kompost in degestat - Določanje policikličnih aromatskih ogljikovodikov (PAH) s plinsko kromatografijo (GC) in s tekočinsko kromatografijo visoke ločljivosti (HPLC)

General Information

• Status: Not Published
• Publication Date: 13-Apr-2025
• ICS: 65.080 - Fertilizers
• Technical Committee: CEN/TC 223 - Soil improvers and growing media
• Drafting Committee: CEN/TC 223/WG 4 - Analytical methods
• Current Stage: 4020 - Submission to enquiry - Enquiry
• Start Date: 16-Oct-2025
• Due Date: 25-Nov-2023
• Completion Date: 16-Oct-2025
• Directive: 2003/2003 - Regulation (EC) N° 2003/2003 of the European Parlament and of the council of 13 October 2003 relating to fertilisers
• Directive: 2019/1009 - Regulation (EU) 2019/1009 of the European Parliament and of the Council of 5 June 2019 laying down rules on the making available on the market of EU fertilising products and amending Regulations (EC) No 1069/2009 and (EC) No 1107/2009 and repealing Regulation (EC) No 2003/2003
• Mandate: M/564 - Fertilising products in support of Regulation (EU) 2019/1009
• Mandate: M/564 AMD 1 - amending Implementing Decision C(2020) 612 as regards certain harmonised standards and standardisation deliverables, deadlines for their adoption and the duration of the validity of the standardisation request
• Mandate: M/564 AMD 2 - Commission Implementing decision amending Implementing Decision C(2020)612 as regards harmonised standards, the deadlines for the adoption of those standards and the duration of the validity of the standardisation request to the European Committee for Standardisation as regards the EU fertilising products in support of Regulation (EU) 2019/1009 of the European Parliament and of the Council
• Mandate: M/588 - COMMISSION IMPLEMENTING DECISION of 20.9.2022 on a standardisation request to the European Committee for Standardisation as regards methods for the measurements of emissions into the air of polychlorinated dibenzo-pdioxins and furans (PCDDs/PCDFs) and dioxin-like polychlorinated biphenyls (PCBs), total gaseous mercury and formaldehyde in support of Directive 2010/75/EU of the European Parliament and of the Council
• Mandate: M/XXX - COMMISSION IMPLEMENTING DECISION of XXX on a standardisation request to the European Committee for Standardization, to the European Committee for Electrotechnical Standardization and to the European Telecommunications Standards Institute as regards certain measuring instruments in support of Directive 2014/32/EU of the European Parliament and of the Council
• Ref Project: oSIST prEN 18261:2025 - Compost and digestate - Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)

Standards Content (Sample)

SLOVENSKI STANDARD
01-december-2025
Kompost in degestat - Določanje policikličnih aromatskih ogljikovodikov (PAH) s
plinsko kromatografijo (GC) in s tekočinsko kromatografijo visoke ločljivosti
(HPLC)
Compost and digestate - Determination of polycyclic aromatic hydrocarbons (PAH) by
gas chromatography (GC) and high performance liquid chromatography (HPLC)
Kompost und Gärreste - Bestimmung von polycyclischen aromatischen
Kohlenwasserstoffen (PAK) mittels Gaschromatographie (GC) und Hochleistungs-
Flüssigkeitschromatographie (HPLC)
Compost et digestat - Dosage des hydrocarbures aromatiques polycycliques (HAP) par
chromatographie en phase gazeuse (CG) et chromatographie liquide à haute
performance (HPLC)
Ta slovenski standard je istoveten z: prEN 18261
ICS:
65.080 Gnojila Fertilizers
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2025
ICS 65.080
English Version
Compost and digestate - Determination of polycyclic
aromatic hydrocarbons (PAH) by gas chromatography
(GC) and high performance liquid chromatography (HPLC)
Compost et digestat - Dosage des hydrocarbures Kompost und Gärreste - Bestimmung von
aromatiques polycycliques (HAP) par chromatographie polycyclischen aromatischen Kohlenwasserstoffen
en phase gazeuse (CG) et chromatographie liquide à (PAK) mittels Gaschromatographie (GC) und
haute performance (HPLC) Hochleistungs-Flüssigkeitschromatographie (HPLC)
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 223.
If this draft becomes a European Standard, 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.

This draft European Standard was established by CEN 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.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2025 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 18261:2025 E
worldwide for CEN national Members.

Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 7
4 Principle . 9
5 Interferences . 9
5.1 Interference with containers . 9
5.2 Interference with GC-MS . 10
5.3 Interference with the HPLC . 10
6 Safety remarks . 10
7 Reagents . 10
7.1 General. 10
7.2 Reagents for extraction . 11
7.3 Reagents for clean-up . 11
7.4 Reagents for chromatographic analysis . 12
7.5 Standards . 12
7.5.1 General. 12
7.5.2 Calibration substances and internal standards . 12
7.5.3 Injection standard . 13
7.6 Preparation of standard solutions. 14
7.6.1 General. 14
7.6.2 Preparation of calibration standard solutions for GC-MS . 14
7.6.3 Preparation of internal standard solution for GC-MS . 14
7.6.4 Preparation of injection standard solution for GC-MS . 14
7.6.5 Preparation of calibration standard solutions for HPLC . 14
7.6.6 Preparation of extraction standard solution for HPLC . 15
8 Apparatus . 15
8.1 Extraction and clean-up procedures . 15
8.2 Gas chromatograph . 16
8.2.1 General. 16
8.2.2 Capillary columns . 16
8.3 High-performance liquid chromatograph . 16
8.3.1 General. 16
8.3.2 Analytical separation column. 16
9 Sampling . 16
10 Sample storage and preservation . 17
10.1 Sample storage . 17
10.2 Sample pre-treatment . 17
11 Procedure . 17
11.1 Safety . 17
11.2 Blank test . 18
11.3 Extraction . 18
11.3.1 General . 18
11.3.2 Extraction procedure 1: acetone/hexane-like solvent and agitation or sonication . 18
11.3.3 Extraction procedure 2: Soxhlet extraction . 19
11.3.4 Extraction procedure 3: Pressurized liquid extraction (PLE) . 19
11.3.5 Extraction procedure 3: acetone/hexane-like solvent/sodium chloride and agitation
................................................................................................................................................................... 19
11.4 Concentration . 20
11.4.1 General . 20
11.4.2 For HPLC analysis . 20
11.5 Clean-up of the extract . 21
11.5.1 General . 21
11.5.2 Clean-up A – Aluminium oxide . 21
11.5.3 Clean-up B – Silica gel . 22
11.5.4 Clean-up C – Gel permeation chromatography . 22
11.6 Addition of the injection standard . 22
11.7 GC-MS analysis . 22
11.7.1 Settings of the gas chromatograph . 22
11.7.2 Mass spectrometric (MS) conditions . 23
11.7.3 Calibration of the method using an internal standard . 24
11.7.4 Measurement . 25
11.7.5 Identification . 25
11.7.6 Check on method performance . 26
11.7.7 Calculation . 27
11.8 High-performance liquid chromatographic analysis (HPLC) . 27
11.8.1 General . 27
11.8.2 Setting the HPLC . 28
11.8.3 Detection . 28
11.8.4 Calibration. 29
11.8.5 Measurement . 29
11.8.6 Calculation . 30
12 Performance characteristics . 30
13 Precision . 30
14 Test report .
...