ISO 13859:2014

INTERNATIONAL ISO
STANDARD 13859
First edition
2014-02-01
Soil quality — Determination of
polycyclic aromatic hydrocarbons
(PAH) by gas chromatography
(GC) and high performance liquid
chromatography (HPLC)
Qualité du sol — Détermination des hydrocarbures aromatiques
polycycliques (HAP) par chromatographie en phase gazeuse (CPG) et
chromatographie liquide à haute performance (CLHP)
Reference number
©
ISO 2014
© ISO 2014
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ii © ISO 2014 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 2
3 Terms and definitions . 2
4 Principle . 3
5 Interferences . 3
5.1 Interference with sampling and extraction . 3
5.2 Interference with GC-MS . 4
5.3 Interferences with the HPLC . 4
6 Safety remarks . 4
7 Reagents . 5
7.1 General . 5
7.2 Reagents for extraction . 5
7.3 Reagents for clean-up . 5
7.4 Reagents for chromatographic analysis . 6
7.5 Standards . 7
7.6 Preparation of standard solutions . 8
7.7 Preparation of internal standard solutions . 9
7.8 Preparation of injection standard solution . 9
8 Apparatus . 9
9 Sample storage and preservation .11
9.1 Sample storage .11
9.2 Sample pretreatment .11
10 Procedure.11
10.1 Blank test .11
10.2 Extraction .12
10.3 Concentration or dilution .14
10.4 Clean-up of the extract .15
10.5 Addition of the injection standard .16
10.6 Gas chromatographic analysis (GC) .17
10.7 High performance liquid chromatographic analysis (HPLC) .20
11 Performance characteristics .23
12 Precision .23
13 Test report .23
Annex A (informative) Repeatability and reproducibility data .24
Annex B (informative) Examples of instrumental conditions and chromatograms .27
Bibliography .37
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
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electrotechnical standardization.
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different types of ISO documents should be noted. This document was drafted in accordance with the
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The committee responsible for this document is ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical
methods and soil characteristics.
iv © ISO 2014 – All rights reserved

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 preceding steps for sampling, pretreatment, 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.
It is to be underlined that the target contamination level of PAH can lie in the range of about 0,01 mg/kg
per individual PAH (agricultural soil and sediment) to about 200 mg/kg and higher (e.g. contaminated
soil at coking plant sites or waste). The use of internal and injection standards is described in order to
have an internal check on execution of the extraction and clean-up procedure. The method is as far as
possible in agreement with the method described for PCBs (see EN 16167).
This International Standard is the result of a desk study “Horizontal International Standard for
determination of PAH in sludge, soil, and biowaste” in the project “Horizontal” and aims at evaluating
the latest developments in assessing PAH in sludge, soil, treated biowaste, and neighbouring fields. After
an evaluation study, in which the ruggedness of the method was studied, a European-wide validation
of the draft standard has taken place. The results of the desk studies as well as the evaluation and
validation studies have been subject to discussions with all parties concerned in CEN.
This International Standard 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 International Standard is applicable and validated
Matrix Materials used for validation
Sludge Municipal sludge
Biowaste Fresh compost
INTERNATIONAL STANDARD ISO 13859:2014(E)
Soil quality — Determination of polycyclic aromatic
hydrocarbons (PAH) by gas chromatography (GC) and high
performance liquid chromatography (HPLC)
WARNING — Persons using this International Standard should be familiar with usual laboratory
practice. This International 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 International
Standard be carried out by suitably trained staff.
1 Scope
This International Standard specifies the quantitative determination of 16 PAH (see Table 2) in
sludge, soil, and treated biowaste using GC-MS and HPLC-UV-DAD/FLD covering a wide range of PAH
contamination levels (see also Annex B).
When using fluorescence detection, acenaphthylene cannot be measured.
Table 2 — Polycyclic aromatic hydrocarbons which can be analysed using this International
Standard
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
...