SIST EN ISO 15009:2016

SLOVENSKI STANDARD
SIST EN ISO 15009:2016
01-december-2016
1DGRPHãþD
SIST EN ISO 15009:2013
.DNRYRVWWDO'RORþHYDQMHKODSQLKDURPDWVNLKRJOMLNRYRGLNRYQDIWDOHQDLQKODSQLK
KDORJHQLUDQLKRJOMLNRYRGLNRYVSOLQVNRNURPDWRJUDILMR0HWRGDSXUJHDQGWUDSV
WRSORWQRGHVRUSFLMR,62
Soil quality - Gas chromatographic determination of the content of volatile aromatic
hydrocarbons, naphthalene and volatile halogenated hydrocarbons - Purge-and-trap
method with thermal desorption (ISO 15009:2016)
Bodenbeschaffenheit - Gaschromatographische Bestimmung des Anteils an flüchtigen
aromatischen Kohlenwasserstoffen, Naphthalin und flüchtigen
Halogenkohlenwasserstoffen - Purge-und-Trap-Anreicherung mit thermischer Desorption
(ISO 15009:2016)
Qualité du sol - Détermination par chromatographie en phase gazeuse des teneurs en
hydrocarbures aromatiques volatils, en naphtalène et en hydrocarbures halogénés
volatils - Méthode par purge et piégeage avec désorption thermique (ISO 15009:2016)
Ta slovenski standard je istoveten z: EN ISO 15009:2016
ICS:
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST EN ISO 15009:2016 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 15009:2016

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SIST EN ISO 15009:2016


EN ISO 15009
EUROPEAN STANDARD

NORME EUROPÉENNE

March 2016
EUROPÄISCHE NORM
ICS 13.080.10 Supersedes EN ISO 15009:2013
English Version

Soil quality - Gas chromatographic determination of the
content of volatile aromatic hydrocarbons, naphthalene
and volatile halogenated hydrocarbons - Purge-and-trap
method with thermal desorption (ISO 15009:2016)
Qualité du sol - Détermination par chromatographie en Bodenbeschaffenheit - Gaschromatographische
phase gazeuse des teneurs en hydrocarbures Bestimmung des Anteils an flüchtigen aromatischen
aromatiques volatils, en naphtalène et en Kohlenwasserstoffen, Naphthalin und flüchtigen
hydrocarbures halogénés volatils - Méthode par purge Halogenkohlenwasserstoffen - Purge-und-Trap-
et piégeage avec désorption thermique (ISO Anreicherung mit thermischer Desorption (ISO
15009:2016) 15009:2016)
This European Standard was approved by CEN on 23 January 2016.

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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, 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: Avenue Marnix 17, B-1000 Brussels
© 2016 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 15009:2016 E
worldwide for CEN national Members.

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SIST EN ISO 15009:2016
EN ISO 15009:2016 (E)
Contents Page
European foreword . 3
2

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SIST EN ISO 15009:2016
EN ISO 15009:2016 (E)
European foreword
This document (EN ISO 15009:2016) has been prepared by Technical Committee ISO/TC 190 “Soil
quality” in collaboration with Technical Committee CEN/TC 345 “Characterization of soils” 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 September 2016, and conflicting national standards
shall be withdrawn at the latest by September 2016.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent
rights.
This document supersedes EN ISO 15009:2013.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia,
Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands,
Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
Endorsement notice
The text of ISO 15009:2016 has been approved by CEN as EN ISO 15009:2016 without any modification.
3

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SIST EN ISO 15009:2016

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SIST EN ISO 15009:2016
INTERNATIONAL ISO
STANDARD 15009
Third edition
2016-02-15
Soil quality — Gas chromatographic
determination of the content of
volatile aromatic hydrocarbons,
naphthalene and volatile halogenated
hydrocarbons — Purge-and-trap
method with thermal desorption
Qualité du sol — Détermination par chromatographie en phase
gazeuse des teneurs en hydrocarbures aromatiques volatils, en
naphtalène et en hydrocarbures halogénés volatils — Méthode par
purge et piégeage avec désorption thermique
Reference number
ISO 15009:2016(E)
©
ISO 2016

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SIST EN ISO 15009:2016
ISO 15009:2016(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2016, Published in Switzerland
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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2016 – All rights reserved

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SIST EN ISO 15009:2016
ISO 15009:2016(E)

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 2
4 Reagents . 2
4.1 Water, free of volatile aromatic and volatile halogenated hydrocarbons . 2
4.2 Internal standards . 2
4.3 Standard compounds . . 3
4.3.1 Volatile aromatic hydrocarbons . 3
4.3.2 Volatile halogenated hydrocarbons . 3
4.4 Methanol . 4
4.5 Adsorbing agent . 4
4.6 Cooling water for purge and trap . 4
4.7 Inert gas for the gas chromatograph . 5
4.8 Nitrogen or helium as inert gas for the purge equipment . 5
4.9 Standard solutions . 5
4.9.1 Standard stock solutions for volatile aromatic and halogenated
compounds in methanol, 4 g/l . 5
4.9.2 Internal standard solutions in methanol, 4 g/l . 5
4.9.3 Calibration solutions . 5
4.10 Methanol containing internal standards . 6
5 Apparatus . 6
6 Sampling, preservation and sample pretreatment . 7
6.1 General . 7
6.2 Sampling using vials pre-filled with methanol . 8
6.3 Sampling using coring tube method . 8
7 Procedure. 8
7.1 Blank determination . 8
7.2 Extraction . 9
7.3 Purge and trap . 9
7.4 Gas chromatographic analysis . 9
7.4.1 Gas chromatographic conditions . 9
7.4.2 Calibration .10
7.4.3 Measurement .11
8 Calculation .12
8.1 Calculation of the concentration of a volatile compound in the water sample .12
8.2 Calculation of the concentration of a volatile compound in the soil sample .12
9 Expression of results .13
10 Precision .13
11 Test report .13
Annex A (informative) Relative retention time with respect to ethylbenzene-D10 of volatile
aromatic hydrocarbons and volatile halogenated hydrocarbons on following
columns: CP-Sil 5 CB and CP-Sil 13 CB .14
Annex B (normative) Check on internal standards .16
Annex C (informative) Validation .17
Annex D (informative) Information on purge and trap instruments.20
© ISO 2016 – All rights reserved iii

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SIST EN ISO 15009:2016
ISO 15009:2016(E)

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.
This third edition cancels and replaces the second edition (ISO 15009:2012), which has been technically
revised.
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SIST EN ISO 15009:2016
INTERNATIONAL STANDARD ISO 15009:2016(E)
Soil quality — Gas chromatographic determination of the
content of volatile aromatic hydrocarbons, naphthalene
and volatile halogenated hydrocarbons — Purge-and-trap
method with thermal desorption
1 Scope
This International Standard specifies a method for quantitative gas-chromatographic determination of
volatile aromatic hydrocarbons, naphthalene and volatile halogenated hydrocarbons in soil.
This International Standard is applicable to all types of soil.
NOTE In the case of unsaturated peaty soils, absorption of the extraction solution may occur.
The lower limit of quantification is dependent on the equipment used and the quality of the methanol
grade used for the extraction of the soil sample.
Under the conditions specified in this International Standard the following limits of quantification
apply (expressed on basis of dry matter):
Typical limit of quantification when using GC-FID:
— Volatile aromatic hydrocarbons: 0,1 mg/kg
Typical limit of quantification when using GC-ECD:
— Volatile halogenated hydrocarbons: 0,01 mg/kg
Lower limits of quantification for some compounds can be achieved by using mass spectrometry (MS)
with selected ion detection.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 4799, Laboratory glassware — Condensers
ISO 10381-1, Soil quality — Sampling — Part 1: Guidance on the design of sampling programmes
ISO 10381-2, Soil quality — Sampling — Part 2: Guidance on sampling techniques
ISO 10381-5, Soil quality — Sampling — Part 5: Guidance on the procedure for the investigation of urban
and industrial sites with regard to soil contamination
ISO 11465, Soil quality — Determination of dry matter and water content on a mass basis —
Gravimetric method
ISO 15680, Water quality — Gas-chromatographic determination of a number of monocyclic aromatic
hydrocarbons, naphthalene and several chlorinated compounds using purge-and-trap and thermal
desorption
ISO 18512, Soil quality — Guidance on long and short term storage of soil samples
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SIST EN ISO 15009:2016
ISO 15009:2016(E)

ISO 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography and
mass spectrometry
3 Principle
Test samples are taken from an untreated field moist soil sample. To prevent losses of the volatiles,
samples are taken as undisturbed as possible in the field with a tube corer or by adding methanol
immediately in the field.
The test sample is extracted with methanol. After centrifugation, if necessary, part of the methanol
extract is brought into a purge vessel filled with water. The volatile compounds are purged with
nitrogen or helium and adsorbed on a suitable adsorbing agent. The adsorbed compounds are
desorbed thermally and by means of a carrier gas flow, whether or not via a cold trap, brought into
a gas chromatograph. The various compounds are separated by using a capillary column with an
immobile phase of low polarity. Volatile organic compounds are detected with appropriate detectors
such as: mass spectrometric detector (MS), flame ionization detector (FID), electron capture detector
(ECD), photo ionization detector (PID) or electrolytic conductivity detector (ELCD). Identification and
quantification takes place by comparison of retention times and peak heights (or peak areas) towards
internal standard added with the corresponding variables of an external standard solution. The
efficiency of the procedure depends on the composition of the soil that is investigated. The described
procedure does not take into account incomplete extraction caused by structure and composition of the
soil sample.
When using non-specific detectors such as FID and ECD, the confirmation of the identity of the detected
compounds and their concentrations should be done by repeating the gas chromatographic analysis
using a column of different polarity. When using gas chromatography-mass spectrometry (GC-MS), the
identity confirmation and the quantification can be done in a single run.
NOTE This International Standard follows the description of an ‘off-line purge and trap’ method. The use
of commercially available online instruments is allowed provided that equivalent results are obtained during
validation of this equipment. With such an instrument purge and trap occurs on line with gas chromatography
and detection. Follow the manual of the manufacturer especially regarding the items 5.2.1 to 5.2.9.
4 Reagents
All reagents shall be of recognized analytical grade. Verify whether the reagents are applicable for this
specific purpose and free of interfering compounds.
4.1 Water, free of volatile aromatic and volatile halogenated hydrocarbons
Usually boiler water with a temperature of at least 80 °C and 1 day old can be applied. Purging with
an inert gas, e.g. a flow of 10 ml/min of nitrogen for 30 min, is another means of removing interfering
compounds from water. A sufficient amount of water from the same batch should be available to
complete each batch of analyses, including all preparations.
4.2 Internal standards
4.2.1 For the determination of volatile aromatic hydrocarbons preferably two internal standards shall
be selected from Table 1. They shall not interfere with compounds present in the sample extract.
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SIST EN ISO 15009:2016
ISO 15009:2016(E)

Table 1 — Examples of suitable internal standards for the determination of volatile aromatic
hydrocarbons
a b
Compound name CAS-RN EC-N
Toluene-D8 2037–26–5 218–009–5
Ethylbenzene-D10 25837–05–2 247–292–8
2-Bromofluorobenzene 1072–85–1 214–018–3
a
 Chemical Abstracts Service Registry Number
b
 EC-Number
4.2.2 For the determination of volatile halogenated hydrocarbons preferably two internal standards
shall be selected from Table 2. They shall not interfere with compounds present in the sample extract.
Table 2 — Examples of suitable internal standards for the determination of volatile
halogenated hydrocarbons
a b
Compound name CAS-RN EC-N
1,4-Dichlorobutane 110–56–5 203–778–1
α,α,α-Trifluorotoluene 98–08–8 202–635–0
2-Bromofluorobenzene 1072–85–1 214–018–3
a
 Chemical Abstracts Service Registry Number
b
 EC-Number
4.3 Standard compounds
4.3.1 Volatile aromatic hydrocarbons
Table 3 contains volatile aromatic hydrocarbons for use as standard compounds.
Table 3 — Examples of volatile aromatic hydrocarbons suitable as standard compounds
a b
Compound name CAS-RN EC-N
Benzene 71–43–2 202–753–7
Toluene 108–88–3 203–625–9
Ethylbenzene 100–41–4 202–849–4
o-Xylene 95–47–6 202–422–2
m-Xylene 108–38–3 203–576–3
p-Xylene 106–42–3 203–396–5
Styrene 100–42–5 202–851–5
Naphthalene 91–20–3 202–049–5
a
 Chemical Abstracts Service Registry Number
b
 EC-Number
4.3.2 Volatile halogenated hydrocarbons
Table 4 contains volatile halogenated hydrocarbons for use as standard compounds.
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SIST EN ISO 15009:2016
ISO 15009:2016(E)

Table 4 — Examples of volatile halogenated hydrocarbons suitable as standard compounds
a b
Compound name CAS-RN EC-N
Dichloromethane 75–09–2 200–838–9
Trichloromethane 67–66–3 200–663–8
Tetrachloromethane 56–23–5 200–262–8
1,1-Dichloroethane 75–34–3 200–863–5
1,2-Dichloroethane 107–06–2 203–458–1
1,1,1-Trichloroethane 71–55–6 200–756–3
1,1,2-Trichloroethane 79–00–5 201–166–9
1,2-Dichloropropane 78–87–5 201–152–2
1,2,3-Trichloropropane 98–18–4 202–486–1
cis-1,3-Dichloropropene 10061–01–5 233–195–8
trans-1,3-Dichloropropene 10061–02–6 208–826–5
cis-1,2-Dichloroethene 156–59–2 205–859–7
trans-1,2-Dichloroethene 156–60–5 205–860–2
3-Chloropropene 107–05–1 203–457–6
Trichloroethene 79–01–6 201–61–04
Tetrachloroethene 127–18–4 204–825–9
Monochlorobenzene 108–90–7 203–628–5
1,2-Dichlorobenzene 95–50–1 202–425–9
a
 Chemical Abstracts Service Registry Number
b
 EC-Number
4.4 Methanol
Methanol (see Table 5) is used as solvent for the extraction of soil samples and for the preparation of
standard solutions.
Table 5 — Registration data
a b
Compound name CAS-RN EC-N
Methanol 67–56–1 200–659–6
a
 Chemical Abstracts Service Registry Number
b
 EC-Number
4.5 Adsorbing agent
Polymer of 2,6-diphenyl-p-phenoxide (40 mesh to 60 mesh) of a grade suitable for thermal desorption.
1)
NOTE 1 2,6-diphenyl-p-phenylene oxide (CAS-RN 24938–68–9) is commercially available as Tenax TA .
NOTE 2 Other adsorbing agents may be used provided that their suitability has been tested.
4.6 Cooling water for purge and trap
The temperature of the cooling water depends on the dimensions of the purge and trap equipment (5.2).
A temperature of about 10 °C is recommended. A cryostat shall be used if the temperature of the cooling
water is too high.
1) Tenax TA is an example of a suitable product available commercially. This information is given for the
convenience of users of this International Standard and does not constitute an endorsement by ISO of this product.
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SIST EN ISO 15009:2016
ISO 15009:2016(E)

4.7 Inert gas for the gas chromatograph
Helium, nitrogen or argon-methane mixture ultra-pure. Other gases for gas chromatography shall be
used in accordance with the instrument manufacturer’s instructions.
4.8 Nitrogen or helium as inert gas for the purge equipment
4.9 Standard solutions
4.9.1 Standard stock solutions for volatile aromatic and halogenated compounds in
methanol, 4 g/l
Weigh about 100 mg of the individual standard compounds (4.3) with an accuracy of 0,1 mg into a
closed septum flask containing 25 ml methanol. Transfer the standard compounds into the flask by
using a syringe.
NOTE The stock solution is stable for about 6 months when stored at −18°C.
4.9.2 Internal standard solutions in methanol, 4 g/l
The containers containing the solutions shall be marked or weighed so that any evaporation losses of
the solvent may be recognized. The solutions shall be stored at a temperature of (4 ± 2) °C in the dark.
Prior to use, they shall be brought to ambient temperature.
Weigh about 100 mg of the individual internal standards (4.2.1 and 4.2.2) accurate to 0,1 mg into a
closed septum flask containing 25 ml of methanol. Using a syringe, transfer the standard compounds
into the flask.
4.9.3 Calibration solutions
Calibration solutions containing 0 mg/l to 200 mg/l of each standard (4.3) and the selected internal
standards (4.2), 200 mg/l. The calibration solutions are prepared in methanol.
Dilute the amounts indicated in Table 6 of the solutions obtained according to 4.9.2 and 4.9.1 with
methanol (4.4) to 100 ml.
Other volumes of methanol may be used, as long as suitability is proven.
Table 6 — Example for preparation of calibration solutions
Calibration Internal standard Standard stock Concentration in the Quantity in µg/5 µl
solution solution (4.9.2) solution (4.9.1) calibration solution calibration solution in
ml ml mg/l 100 ml (sample) water
1 5 0 0 0
2 5 1 40 0,2
3 5 2 80 0,4
4 5 3 120 0,6
5 5 4 160 0,8
6 5 5 200 1,0
The total volume of the methanol used for calibration shall be the same as that which will be taken for
the methanol extract of the soil sample (see 7.3).
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SIST EN ISO 15009:2016
ISO 15009:2016(E)

4.10 Methanol containing internal standards
Prepare methanol containing a suitable concentration of the internal standards (e.g. 0,4 µg/ml). The
concentration shall be such that the end concentration in the water extract in the purge vessel is of the
same level as in the calibration solutions.
5
...