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)

ISO 15009:2016 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.

Bodenbeschaffenheit - Gaschromatographische Bestimmung des Anteils an flüchtigen aromatischen Kohlenwasserstoffen, Naphthalin und flüchtigen Halogenkohlenwasserstoffen - Purge-und-Trap-Anreicherung mit thermischer Desorption (ISO 15009:2016)

Diese Internationale Norm legt ein quantitatives gaschromatographisches Verfahren zur Bestimmung von flüchtigen aromatischen Kohlenwasserstoffen, Naphthalin und flüchtigen Halogenkohlenwasserstoffen im Boden fest.
Diese Internationale Norm ist auf alle Bodenarten anwendbar.
ANMERKUNG   Im Fall von ungesättigten Torfböden kann es zur Absorption des Lösungsmittels kommen.
Die untere Bestimmungsgrenze ist abhängig von der verwendeten Prüfeinrichtung und der Qualität des Methanols, mit dem die Bodenprobe extrahiert wird.
Unter den in dieser Internationalen Norm festgelegten Bedingungen gelten folgende Bestimmungsgrenzen (bezogen auf Trockensubstanz):
Bei Anwendung eines Gaschromatographen mit Flammenionisationsdetektor (GC-FID) liegt die typische Bestimmungsgrenze:
—   für flüchtige aromatische Kohlenwasserstoffe: 0,1 mg/kg.
Bei Anwendung eines Gaschromatographen mit Elektronen-Einfang-Detektor (GC-ECD) liegt die typische Bestimmungsgrenze:
—   für flüchtige Halogenkohlenwasserstoffe: 0,01 mg/kg.
Niedrigere Bestimmungsgrenzen für einige Verbindungen können durch Anwendung der Massenspektrometrie (MS) mit selektiver Ionendetektion erreicht werden.

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)

ISO 15009:2016 spécifie une méthode pour la détermination quantitative par chromatographie en phase gazeuse des hydrocarbures aromatiques volatils, du naphtalène et des hydrocarbures halogénés volatils contenus dans les sols.
La présente Norme internationale est applicable à tous les types de sols.
NOTE          En cas de sols tourbeux insaturés, une absorption de la solution d'extraction peut avoir lieu.
La limite inférieure de détermination quantitative dépend du matériel utilisé et de la qualité du méthanol utilisé pour l'extraction de l'échantillon de sol.
Dans les conditions spécifiées dans la présente Norme internationale, les limites de détermination quantitative suivantes (exprimées par rapport à la matière sèche) s'appliquent:
Limite de détermination quantitative type lorsque le couplage CG-FID est utilisé:
-      Hydrocarbures aromatiques volatils: 0,1 mg/kg
Limite de détermination quantitative type lorsque le couplage CG-ECD est utilisé:
-      Hydrocarbures halogénés volatils: 0,01 mg/kg
Des limites de détermination quantitative plus faibles peuvent être atteintes pour certains composés si l'on utilise la spectrométrie de masse (SM) avec détection sélective des ions.

Kakovost tal - Določevanje hlapnih aromatskih ogljikovodikov, naftalena in hlapnih halogeniranih ogljikovodikov s plinsko kromatografijo - Metoda "purge-and-trap" s toplotno desorpcijo (ISO 15009:2016)

Ta mednarodni standard določa metodo za določevanje
hlapnih aromatskih ogljikovodikov, naftalena in hlapnih halogeniranih ogljikovodikov v tleh s kvantitativno plinsko kromatografijo.
Ta mednarodni standard se uporablja za vse vrste tal.
OPOMBA: V primeru nenasičenih šotnih tal lahko pride do absorpcije ekstrakcijske raztopine.
Nižja mejna vrednost kvantifikacije je odvisna od uporabljene opreme in kakovosti stopnje metanola,
ki se uporablja za ekstrakcijo vzorca tal.
Pod pogoji, določenimi v tem mednarodnem standardu, se uporabljajo naslednje mejne vrednosti kvantifikacije
(izraženo na podlagi suhe snovi):
Običajna mejna vrednost kvantifikacije pri uporabi plinske kromatografije/plamenske ionizacijske detekcije:
– hlapni aromatski ogljikovodiki: 0,1 mg/kg
Običajna mejna vrednost kvantifikacije pri uporabi plinske kromatografije/detektorja na zajetje elektronov:
– hlapni halogenirani ogljikovodiki: 0,01 mg/kg
Nižje mejne vrednosti kvantifikacije za nekatere zmesi se lahko dosežejo z masno spektrometrijo (MS)
z izbrano detekcijo iona.

General Information

Status
Published
Publication Date
15-Mar-2016
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
16-Mar-2016
Completion Date
16-Mar-2016

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SLOVENSKI STANDARD
SIST EN ISO 15009:2016
01-december-2016
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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.

---------------------- Page: 1 ----------------------
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

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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.

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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.
iv © ISO 2016 – All rights reserved
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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

© ISO 2016 – All rights reserved 1
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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.

2 © ISO 2016 – All rights reserved
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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
Chemical Abstracts Service Registry Number
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
Chemical Abstracts Service Registry Number
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
Chemical Abstracts Service Registry Number
EC-Number
4.3.2 Volatile halogenated hydrocarbons

Table 4 contains volatile halogenated hydrocarbons for use as standard compounds.

© ISO 2016 – All rights reserved 3
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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
Chemical Abstracts Service Registry Number
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
Chemical Abstracts Service Registry Number
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.

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.

4 © ISO 2016 – All rights reserved
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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).
© ISO 2016 – All rights reserved 5
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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.
...

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