ISO 13859:2014
(Main)Soil quality — Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)
Soil quality — Determination of polycyclic aromatic hydrocarbons (PAH) by gas chromatography (GC) and high performance liquid chromatography (HPLC)
ISO 13859:2014 specifies the quantitative determination of 16 PAH in sludge, soil, and treated biowaste using GC-MS and HPLC-UV-DAD/FLD covering a wide range of PAH contamination levels. When using fluorescence detection, acenaphthylene cannot be measured. 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. Typically, a lower limit of application of 0,01 mg/kg (expressed as dry matter) can be ensured for each individual PAH. Sludge, soil, and treated biowaste can differ in properties and also in the expected contamination levels of PAH and presence of interfering substances. These differences make it impossible to describe one general procedure. ISO 13859:2014 contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used. Two general lines are followed, an agitation procedure (shaking) or use of Soxhlet/pressurized liquid extraction.
Qualité du sol — Détermination des hydrocarbures aromatiques polycycliques (HAP) par chromatographie en phase gazeuse (CPG) et chromatographie liquide à haute performance (CLHP)
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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
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
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
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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary information
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
...
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
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
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
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.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
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. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary information
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
...
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