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 15009:2012)

This International Standard specifies a method for quantitative gas chromatographic determination of volatile 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 determination 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 determinations apply (expressed on a basis of dry matter):
a) Typical limit of determination when using gas chromatography/flame ionization detection (GC/FID):
— volatile aromatic hydrocarbons: 0,1 mg/kg.
b) Typical limit of determination when using gas chromatography/electron capture detector (GC/ECD):
— volatile halogenated hydrocarbons: 0,01 mg/kg
Lower limits of determination 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 15009:2012)

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 dem Reinheitsgrad des Methanols, mit dem die Bodenprobe extrahiert wird.
Unter den in dieser Internationalen Norm festgelegten Bedingungen gelten für die Bestimmungen folgende Grenzen (angegeben auf Grundlage der Trockensubstanz):
a)   Typische Bestimmungsgrenzen bei Anwendung von Gaschromatographie mit Flammenionisations-detektor (GC/FID):
   für flüchtige aromatische Kohlenwasserstoffe: 0,1 mg/kg.
b)   Typische Bestimmungsgrenzen bei Anwendung von Gaschromatographie mit Elektroneneinfang¬detektor (GC/ECD):
   für flüchtige Halogenkohlenwasserstoffe: 0,01 mg/kg
Niedrigere Bestimmungsgrenzen für einige Verbindungen können mithilfe 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 15009:2012)

Kakovost tal - Določevanje hlapnih aromatskih ogljikovodikov, naftalena in hlapnih halogeniranih ogljikovodikov s plinsko kromatografijo - Metoda "purge-and-trap" s toplotno desorpcijo (ISO 15009:2012)

Ta mednarodni standard opisuje metodo za določevanje hlapnih 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 meja določevanja 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 meje določevanj (izraženo na podlagi suhe snovi):
a) tipična meja določevanja z uporabo plinske kromatografije/plamenske ionizacijske detekcije (GC/FID):
– hlapni aromatski ogljikovodiki: 0,1 mg/kg;
b) tipična meja določevanja z uporabo plinske kromatografije/detektorja na zajetje elektronov (GC/EDC):
– hlapni halogenirani ogljikovodiki: 0,01 mg/kg.
Nižje meje določevanja za nekatere zmesi se lahko dosežejo z masno spektrometrijo (MS) z izbrano detekcijo iona.

General Information

Status
Withdrawn
Public Enquiry End Date
31-Dec-2012
Publication Date
21-Apr-2013
Withdrawal Date
06-Nov-2016
Technical Committee
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
07-Nov-2016
Due Date
30-Nov-2016
Completion Date
07-Nov-2016

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SLOVENSKI STANDARD
SIST EN ISO 15009:2013
01-maj-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 15009:2012)
Bodenbeschaffenheit - Gaschromatographische Bestimmung des Anteils an flüchtigen
aromatischen Kohlenwasserstoffen, Naphthalin und flüchtigen

Halogenkohlenwasserstoffen - Purge-und-Trap-Anreicherung mit thermischer Desorption

(ISO 15009:2012)

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 15009:2012)

Ta slovenski standard je istoveten z: EN ISO 15009:2013
ICS:
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
SIST EN ISO 15009:2013 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 15009:2013
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SIST EN ISO 15009:2013
EUROPEAN STANDARD
EN ISO 15009
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2013
ICS 13.080.10
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 15009:2012)

Qualité du sol - Détermination par chromatographie en Bodenbeschaffenheit - Gaschromatographische

phase gazeuse des teneurs en hydrocarbures aromatiques Bestimmung des Anteils an flüchtigen aromatischen

volatils, en naphtalène et en hydrocarbures halogénés Kohlenwasserstoffen, Naphthalin und flüchtigen

volatils - Méthode par purge et piégeage avec désorption Halogenkohlenwasserstoffen - Purge-und-Trap-

thermique (ISO 15009:2012) Anreicherung mit thermischer Desorption (ISO 15009:2012)

This European Standard was approved by CEN on 21 March 2013.

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
Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 15009:2013: E

worldwide for CEN national Members.
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SIST EN ISO 15009:2013
EN ISO 15009:2013 (E)
Contents Page

Foreword ..............................................................................................................................................................3

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SIST EN ISO 15009:2013
EN ISO 15009:2013 (E)
Foreword

The text of ISO 15009:2012 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the

International Organization for Standardization (ISO) and has been taken over as EN ISO 15009:2013 by

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 October 2013, and conflicting national standards shall be withdrawn at

the latest by October 2013.

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.

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 15009:2012 has been approved by CEN as EN ISO 15009:2013 without any modification.

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SIST EN ISO 15009:2013
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SIST EN ISO 15009:2013
INTERNATIONAL ISO
STANDARD 15009
Second edition
2012-07-01
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 15009:2012(E)
ISO 2012
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SIST EN ISO 15009:2013
ISO 15009:2012(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2012

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,

electronic or mechanical, including photocopying and microfilm, without permission in writing 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 2012 – All rights reserved
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SIST EN ISO 15009:2013
ISO 15009:2012(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 standard compounds .......................................................................................................................... 2

4.3 Standard compounds ......................................................................................................................................... 3

4.4 Methanol (CAS RN 67-56-1) .............................................................................................................................. 4

4.5 Adsorbing agent .................................................................................................................................................. 4

4.6 Cooling water for purge and trap .................................................................................................................... 4

4.7 Inert carrier gas for the gas chromatograph ................................................................................................ 4

4.8 Nitrogen or helium as inert gas for the purge equipment ........................................................................ 4

4.9 Standard solutions .............................................................................................................................................. 4

5 Apparatus .............................................................................................................................................................. 5

6 Sampling, preservation and sample pretreatment ..................................................................................... 7

6.1 General ................................................................................................................................................................... 7

6.2 Sampling using vials prefilled with methanol ............................................................................................. 7

6.3 Sampling using coring tube method .............................................................................................................. 7

7 Procedure .............................................................................................................................................................. 7

7.1 Blank determination ........................................................................................................................................... 7

7.2 Extraction .............................................................................................................................................................. 8

7.3 Purge and trap ...................................................................................................................................................... 8

7.4 Gas chromatographic analysis ........................................................................................................................ 8

8 Calculation ..........................................................................................................................................................10

9 Expression of results ....................................................................................................................................... 11

10 Precision .............................................................................................................................................................. 11

11 Test report ........................................................................................................................................................... 11

Annex A (informative) Relative retention time with respect to ethylbenzene-D10 of volatile aromatic

hydrocarbons and volatile halogenated hydrocarbons on the following columns: CP-Sil 5 CB

and CP-Sil 13 CB ...............................................................................................................................................12

Annex B (normative) Check on internal standards .................................................................................................13

Annex C (informative) Validation ..................................................................................................................................14

Annex D (informative) Information on purge-and-trap instruments ...................................................................17

Bibliography .....................................................................................................................................................................18

© ISO 2012 – All rights reserved iii
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SIST EN ISO 15009:2013
ISO 15009:2012(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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards

adopted by the technical committees are circulated to the member bodies for voting. Publication as an

International Standard requires approval by at least 75 % of the member bodies casting a vote.

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.

ISO 15009 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical

methods and soil characteristics.

This second edition cancels and replaces the first edition (ISO 15009:2002), which has been technically revised.

iv © ISO 2012 – All rights reserved
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SIST EN ISO 15009:2013
INTERNATIONAL STANDARD ISO 15009:2012(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

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 determination 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 determinations apply

(expressed on a basis of dry matter):

a) Typical limit of determination when using gas chromatography/flame ionization detection (GC/FID):

— volatile aromatic hydrocarbons: 0,1 mg/kg.

b) Typical limit of determination when using gas chromatography/electron capture detector (GC/ECD):

— volatile halogenated hydrocarbons: 0,01 mg/kg

Lower limits of determination for some compounds can be achieved by using mass spectrometry (MS) with

selected ion detection.
2 Normative references

The following referenced documents are indispensable for the application of this document. 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 11465:1993/Cor 1:1994, Soil quality — Determination of dry matter and water content on a mass basis —

Gravimetric method — Technical Corrigendum 1

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 2012 – All rights reserved 1
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SIST EN ISO 15009:2013
ISO 15009:2012(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, 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 an

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 FIDs and ECDs, 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 1 This International Standard follows the description of an off-line purge-and-trap method. The use of commercial

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 manufacturer’s

manual, especially regarding the items composing the apparatus which are listed in 5.1.1 to 5.1.9.

NOTE 2 Other injection techniques, such as static headspace followed by thermal desorption (ISO 22155) or solid-

phase micro-extraction (SPME), can be used, provided that their applicability is proven.

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 standard compounds

4.2.1 For the determination of volatile aromatic hydrocarbons, preferably two internal standard compounds

shall be selected that do not interfere with compounds present in the sample extract.

Examples of suitable internal standards are
— toluene-D8 (CAS RN 2037-26-5),
— ethylbenzene-D10 (CAS RN 25837-05-2), and
— 2-bromofluorobenzene (CAS RN 1072-85-1).
2 © ISO 2012 – All rights reserved
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SIST EN ISO 15009:2013
ISO 15009:2012(E)

4.2.2 For the determination of volatile halogenated hydrocarbons, preferably two internal standard compounds

shall be selected that do not interfere with compounds present in the sample extract.

Examples of suitable internal standards are:
— 1,4-dichlorobutane (CAS RN 110-56-5);
— α,α,α-trifluorotoluene (CAS RN 98-08-8);
— 2-bromofluorobenzene (CAS RN 1072-85-1).
4.3 Standard compounds
4.3.1 Volatile aromatic hydrocarbons
— benzene (CAS RN 71-43-2);
— toluene (CAS RN 108-88-3);
— ethylbenzene (CAS RN 100-41-4);
— o-xylene (CAS RN 95-47-6);
— m-xylene (CAS RN 108-38-3);
— p-xylene (CAS RN 106-42-3);
— styrene (CAS RN 100-42-5);
— naphthalene (CAS RN 91-20-3).
4.3.2 Volatile halogenated hydrocarbons
— dichloromethane (CAS RN 75-09-2);
— trichloromethane (CAS RN 67-66-3);
— tetrachloromethane (CAS RN 56-23-5);
— 1,1-dichloroethane (CAS RN 75-34-3);
— 1,2-dichloroethane (CAS RN 107-06-2);
— 1,1,1-trichloroethane (CAS RN 79-01-6);
— 1,1,2-trichloroethane (CAS RN 79-00-5);
— 1,2-dichloropropane (CAS RN 78-87-5);
— 1,2,3-trichloropropane (CAS RN 98-18-4);
— cis-1,3-dichloropropene (CAS RN 10061-01-5);
— trans-1,3-dichloropropene (CAS RN 10061-02-6);
— cis-1,2-dichloroethene (CAS RN 156-59-2);
— trans-1,2-dichloroethene (CAS RN 156-60-5);
— 3-chloropropene (CAS RN 107-05-1);
— trichloroethene (CAS RN 79-01-6);
— tetrachloroethene (CAS RN 127-18-4);
© ISO 2012 – All rights reserved 3
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SIST EN ISO 15009:2013
ISO 15009:2012(E)
— monochlorobenzene (CAS RN 108-90-7);
— 1,2-dichlorobenzene (CAS RN 95-50-1).
4.4 Methanol (CAS RN 67-56-1)

The methanol used shall not contain more than 100 µg/l of the individual volatile aromatic compounds and not

more than 10 µg/l of the volatile halogenated hydrocarbons that are to be analysed.

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-phenoxide 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 (5.1). A temperature

of about 10 °C is recommended. A cryostat shall be used if the temperature of the cooling water is too high.

4.7 Inert carrier 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 of 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.

Weigh about 100 mg of the individual internal standard compounds (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.

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 in the dark at a temperature of 4 °C ± 2 °C. Prior to

use, they shall be brought to ambient temperature.
4.9.3 Calibration solutions

Calibration solutions containing 0 mg/l to 200 mg/l of each standard (4.3) and the selected internal standard

compounds (4.2), 200 mg/l. The calibration solutions are prepared in methanol.

Dilute the amounts indicated in Table 1 of the solutions obtained according to 6.2 and 6.3 with methanol

(4.4) to 100 ml.
Other volumes of methanol may be used as long as suitability is proven.

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 2012 – All rights reserved
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SIST EN ISO 15009:2013
ISO 15009:2012(E)
Table 1 — Example for preparation of calibration solutions

Calibration solution Internal standard Standard stock Concentration in Quantity in µg/5 µl

solution (4.9.2) solution (4.9.1) the calibration calibration solution
ml ml solution in 100 ml (sample)
mg/l 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 7.2).
5 Apparatus
Usual laboratory glassware, free of interfering compounds.

All glassware shall be cleaned according to the usual procedures for this type of analysis.

5.1 Purge-and-trap apparatus

The instrument described here is for an off-line purge-and-trap method. As mentioned in Note 1 to Clause 3,

commercially available automated systems are allowed provided the requirements of this International Standard

are met. Annex D gives some considerations for the use of such systems.
5.1.1 Round-bottom flask with three angled side necks; volume 100 ml.
5.1.2 Gas inlet tube with a tip of sintered glass.
5.1.3 Ball-and-cup stopcock with a polytetrafluoroethylene (PTFE) ring.
5.1.4 Flow adjustment; the nitrogen flow shall be 40 ml/min ± 2 ml/min.
5.1.5 Inlet tube for the thermocouple.
5.1.6 Allin- or Graham-type condenser (see ISO 4799).
5.1.7 Screw cap with cut-off ring made of silicone rubber with PTFE inlay.
5.1.8 Adsorption tubes

Tubes made of glass or stainless steel, filled with at least 240 mg of adsorbing agent (4.5).

The adsorbent is kept in place by using inert material, e.g. silanized glass fibre. The tubes shall be suitable for

direct use in connection with the apparatus for thermal desorption. The tubes shall be marked on one side. The

tubes shall be provided with caps of inert material, e.g. polyethylene or metal, with screw caps and a PTFE ring,

that allow tight closing after purging.

Before use, the adsorbent shall be activated and purified by slowly heating the tubes to 250 °C and keeping them

at that temperature for 3 h while a nitrogen flow of 10 ml/min is maintained. The adsorbent shall be cooled under

© ISO 2012 – All rights reserved 5
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SIST EN ISO 15009:2013
ISO 15009:2012(E)

nitrogen and the tubes analysed. The result of a blank determination shall not exceed the equivalent of 1 ng of

a compound to be analysed. When the result is higher than this, the adsorbent shall be desorbed once more.

NOTE The use of commercially available tubes is recommended.

Tubes that are used should not be used again, unless the blank determination meets the above-mentioned

requirements.

Care should be taken to avoid cross-contamination. A heavily loaded tube can contaminate a lightly loaded

tube in the sample change platform.
5.1.9 Heating block with thermocouple, suitable for heating 100 ml flasks

5.2 Centrifuge, suitable for centrifuging tubes of 200 ml with such a rotation frequency that the radial

acceleration is 2 000g to 3 000g.
5.3 Centrifuge tubes, with a volume of 200 ml.
5.4 Capillary columns

Fused silica capillary columns with a non-polar or semipolar stationary phase allowing sufficient separation of the

compounds of interest. A thick film of stationary phase increases the efficiency of the more volatile compounds.

Examples are given in 7.4 and Annex A.

5.5 Gas chromatograph, equipped with one or two appropriate detectors. Detectors, such as flame

ionization detectors (FIDs), electron capture detectors (ECDs), photo-ionization detectors (PIDs) or electrolytic

conductivity detectors (ELCDs), and a mass spectrometer (MS) can be used, depending on the substances to

be analysed and their target level of contamination. The mass spectrometer should be capable of operating

over the total mass range of interest and being equipped with a data system capable of quantifying ions using

selected m/z values.
5.6 Apparatus for thermal desorption
The apparatus used shall meet the following requirements:

— a primary desorption oven with adjustable desorption temperature up to 250 °C and adjustable desorption time;

— a cold trap/secondary desorption oven;

— a connecting tube to the gas chromatograph, with adjustable heating up to 150 °C;

— adjustable carrier-gas flow rate up to 40 ml/min.
NOTE Instruments for thermal desorption are commercially available.
5.7 Electronic integrator or automatic recorder

5.8 Syringe, of volume 5 µl, readable to 0,1 µl, and of volume 50 µl, readable to 1 µl.

5.9 Horizontal shaking machine
A shaking machine with horizontal movement (200 to 300 movements per minute).
6 © ISO 2012 – All rights reserved
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SIST EN ISO 15009:2013
ISO 15009:2012(E)
6 Sampling, preservation and sample pretreatment
6.1 General
Sampling shall be carried out in accordance with ISO 10381-1 and ISO 10381-5,
...

SLOVENSKI STANDARD
kSIST FprEN ISO 15009:2012
01-december-2012
[Not translated]

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 15009:2012)
Bodenbeschaffenheit - Gaschromatographische Bestimmung des Anteils an flüchtigen
aromatischen Kohlenwasserstoffen, Naphthalin und flüchtigen

Halogenkohlenwasserstoffen - Purge-und-Trap-Anreicherung mit thermischer Desorption

(ISO 15009:2012)

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 15009:2012)

Ta slovenski standard je istoveten z: FprEN ISO 15009
ICS:
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
kSIST FprEN ISO 15009:2012 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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kSIST FprEN ISO 15009:2012
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kSIST FprEN ISO 15009:2012
EUROPEAN STANDARD
FINAL DRAFT
FprEN ISO 15009
NORME EUROPÉENNE
EUROPÄISCHE NORM
September 2012
ICS 13.080.10
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 15009:2012)

Qualité du sol - Détermination par chromatographie en Bodenbeschaffenheit - Gaschromatographische

phase gazeuse des teneurs en hydrocarbures aromatiques Bestimmung des Anteils an flüchtigen aromatischen

volatils, en naphtalène et en hydrocarbures halogénés Kohlenwasserstoffen, Naphthalin und flüchtigen

volatils - Méthode par purge et piégeage avec désorption Halogenkohlenwasserstoffen - Purge-und-Trap-

thermique (ISO 15009:2012) Anreicherung mit thermischer Desorption (ISO 15009:2012)

This draft European Standard is submitted to CEN members for unique acceptance procedure. It has been drawn up by the Technical

Committee CEN/TC 345.

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, 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.

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
Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprEN ISO 15009:2012: E

worldwide for CEN national Members.
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kSIST FprEN ISO 15009:2012
FprEN ISO 15009:2012 (E)
Contents Page

Foreword ..............................................................................................................................................................3

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kSIST FprEN ISO 15009:2012
FprEN ISO 15009:2012 (E)
Foreword

The text of ISO 15009:2012 has been prepared by Technical Committee ISO/TC 190 “Soil quality” of the

International Organization for Standardization (ISO) and has been taken over as FprEN ISO 15009:2012 by

Technical Committee CEN/TC 345 “Characterization of soils” the secretariat of which is held by NEN.

This document is currently submitted to the Unique Acceptance Procedure.
Endorsement notice

The text of ISO 15009:2012 has been approved by CEN as a FprEN ISO 15009:2012 without any

modification.
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kSIST FprEN ISO 15009:2012
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kSIST FprEN ISO 15009:2012
INTERNATIONAL ISO
STANDARD 15009
Second edition
2012-07-01
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 15009:2012(E)
ISO 2012
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kSIST FprEN ISO 15009:2012
ISO 15009:2012(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2012

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,

electronic or mechanical, including photocopying and microfilm, without permission in writing 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 2012 – All rights reserved
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kSIST FprEN ISO 15009:2012
ISO 15009:2012(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 standard compounds .......................................................................................................................... 2

4.3 Standard compounds ......................................................................................................................................... 3

4.4 Methanol (CAS RN 67-56-1) .............................................................................................................................. 4

4.5 Adsorbing agent .................................................................................................................................................. 4

4.6 Cooling water for purge and trap .................................................................................................................... 4

4.7 Inert carrier gas for the gas chromatograph ................................................................................................ 4

4.8 Nitrogen or helium as inert gas for the purge equipment ........................................................................ 4

4.9 Standard solutions .............................................................................................................................................. 4

5 Apparatus .............................................................................................................................................................. 5

6 Sampling, preservation and sample pretreatment ..................................................................................... 7

6.1 General ................................................................................................................................................................... 7

6.2 Sampling using vials prefilled with methanol ............................................................................................. 7

6.3 Sampling using coring tube method .............................................................................................................. 7

7 Procedure .............................................................................................................................................................. 7

7.1 Blank determination ........................................................................................................................................... 7

7.2 Extraction .............................................................................................................................................................. 8

7.3 Purge and trap ...................................................................................................................................................... 8

7.4 Gas chromatographic analysis ........................................................................................................................ 8

8 Calculation ..........................................................................................................................................................10

9 Expression of results ....................................................................................................................................... 11

10 Precision .............................................................................................................................................................. 11

11 Test report ........................................................................................................................................................... 11

Annex A (informative) Relative retention time with respect to ethylbenzene-D10 of volatile aromatic

hydrocarbons and volatile halogenated hydrocarbons on the following columns: CP-Sil 5 CB

and CP-Sil 13 CB ...............................................................................................................................................12

Annex B (normative) Check on internal standards .................................................................................................13

Annex C (informative) Validation ..................................................................................................................................14

Annex D (informative) Information on purge-and-trap instruments ...................................................................17

Bibliography .....................................................................................................................................................................18

© ISO 2012 – All rights reserved iii
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kSIST FprEN ISO 15009:2012
ISO 15009:2012(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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards

adopted by the technical committees are circulated to the member bodies for voting. Publication as an

International Standard requires approval by at least 75 % of the member bodies casting a vote.

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.

ISO 15009 was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 3, Chemical

methods and soil characteristics.

This second edition cancels and replaces the first edition (ISO 15009:2002), which has been technically revised.

iv © ISO 2012 – All rights reserved
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kSIST FprEN ISO 15009:2012
INTERNATIONAL STANDARD ISO 15009:2012(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

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 determination 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 determinations apply

(expressed on a basis of dry matter):

a) Typical limit of determination when using gas chromatography/flame ionization detection (GC/FID):

— volatile aromatic hydrocarbons: 0,1 mg/kg.

b) Typical limit of determination when using gas chromatography/electron capture detector (GC/ECD):

— volatile halogenated hydrocarbons: 0,01 mg/kg

Lower limits of determination for some compounds can be achieved by using mass spectrometry (MS) with

selected ion detection.
2 Normative references

The following referenced documents are indispensable for the application of this document. 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 11465:1993/Cor 1:1994, Soil quality — Determination of dry matter and water content on a mass basis —

Gravimetric method — Technical Corrigendum 1

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 2012 – All rights reserved 1
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kSIST FprEN ISO 15009:2012
ISO 15009:2012(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, 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 an

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 FIDs and ECDs, 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 1 This International Standard follows the description of an off-line purge-and-trap method. The use of commercial

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 manufacturer’s

manual, especially regarding the items composing the apparatus which are listed in 5.1.1 to 5.1.9.

NOTE 2 Other injection techniques, such as static headspace followed by thermal desorption (ISO 22155) or solid-

phase micro-extraction (SPME), can be used, provided that their applicability is proven.

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 standard compounds

4.2.1 For the determination of volatile aromatic hydrocarbons, preferably two internal standard compounds

shall be selected that do not interfere with compounds present in the sample extract.

Examples of suitable internal standards are
— toluene-D8 (CAS RN 2037-26-5),
— ethylbenzene-D10 (CAS RN 25837-05-2), and
— 2-bromofluorobenzene (CAS RN 1072-85-1).
2 © ISO 2012 – All rights reserved
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kSIST FprEN ISO 15009:2012
ISO 15009:2012(E)

4.2.2 For the determination of volatile halogenated hydrocarbons, preferably two internal standard compounds

shall be selected that do not interfere with compounds present in the sample extract.

Examples of suitable internal standards are:
— 1,4-dichlorobutane (CAS RN 110-56-5);
— α,α,α-trifluorotoluene (CAS RN 98-08-8);
— 2-bromofluorobenzene (CAS RN 1072-85-1).
4.3 Standard compounds
4.3.1 Volatile aromatic hydrocarbons
— benzene (CAS RN 71-43-2);
— toluene (CAS RN 108-88-3);
— ethylbenzene (CAS RN 100-41-4);
— o-xylene (CAS RN 95-47-6);
— m-xylene (CAS RN 108-38-3);
— p-xylene (CAS RN 106-42-3);
— styrene (CAS RN 100-42-5);
— naphthalene (CAS RN 91-20-3).
4.3.2 Volatile halogenated hydrocarbons
— dichloromethane (CAS RN 75-09-2);
— trichloromethane (CAS RN 67-66-3);
— tetrachloromethane (CAS RN 56-23-5);
— 1,1-dichloroethane (CAS RN 75-34-3);
— 1,2-dichloroethane (CAS RN 107-06-2);
— 1,1,1-trichloroethane (CAS RN 79-01-6);
— 1,1,2-trichloroethane (CAS RN 79-00-5);
— 1,2-dichloropropane (CAS RN 78-87-5);
— 1,2,3-trichloropropane (CAS RN 98-18-4);
— cis-1,3-dichloropropene (CAS RN 10061-01-5);
— trans-1,3-dichloropropene (CAS RN 10061-02-6);
— cis-1,2-dichloroethene (CAS RN 156-59-2);
— trans-1,2-dichloroethene (CAS RN 156-60-5);
— 3-chloropropene (CAS RN 107-05-1);
— trichloroethene (CAS RN 79-01-6);
— tetrachloroethene (CAS RN 127-18-4);
© ISO 2012 – All rights reserved 3
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kSIST FprEN ISO 15009:2012
ISO 15009:2012(E)
— monochlorobenzene (CAS RN 108-90-7);
— 1,2-dichlorobenzene (CAS RN 95-50-1).
4.4 Methanol (CAS RN 67-56-1)

The methanol used shall not contain more than 100 µg/l of the individual volatile aromatic compounds and not

more than 10 µg/l of the volatile halogenated hydrocarbons that are to be analysed.

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-phenoxide 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 (5.1). A temperature

of about 10 °C is recommended. A cryostat shall be used if the temperature of the cooling water is too high.

4.7 Inert carrier 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 of 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.

Weigh about 100 mg of the individual internal standard compounds (4.2.1 and 4.2.2), accurate to 0,1 mg, into a

closed septum ask fl containing 25 ml of methanol. Using a syringe, transfer the standard compounds into the askfl .

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 in the dark at a temperature of 4 °C ± 2 °C. Prior to

use, they shall be brought to ambient temperature.
4.9.3 Calibration solutions

Calibration solutions containing 0 mg/l to 200 mg/l of each standard (4.3) and the selected internal standard

compounds (4.2), 200 mg/l. The calibration solutions are prepared in methanol.

Dilute the amounts indicated in Table 1 of the solutions obtained according to 6.2 and 6.3 with methanol

(4.4) to 100 ml.
Other volumes of methanol may be used as long as suitability is proven.

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 2012 – All rights reserved
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kSIST FprEN ISO 15009:2012
ISO 15009:2012(E)
Table 1 — Example for preparation of calibration solutions

Calibration solution Internal standard Standard stock Concentration in Quantity in µg/5 µl

solution (4.9.2) solution (4.9.1) the calibration calibration solution
ml ml solution in 100 ml (sample)
mg/l 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 7.2).
5 Apparatus
Usual laboratory glassware, free of interfering compounds.

All glassware shall be cleaned according to the usual procedures for this type of analysis.

5.1 Purge-and-trap apparatus

The instrument described here is for an off-line purge-and-trap method. As mentioned in Note 1 to Clause 3,

commercially available automated systems are allowed provided the requirements of this International Standard

are met. Annex D gives some considerations for the use of such systems.
5.1.1 Round-bottom flask with three angled side necks; volume 100 ml.
5.1.2 Gas inlet tube with a tip of sintered glass.
5.1.3 Ball-and-cup stopcock with a polytetrafluoroethylene (PTFE) ring.
5.1.4 Flow adjustment; the nitrogen flow shall be 40 ml/min ± 2 ml/min.
5.1.5 Inlet tube for the thermocouple.
5.1.6 Allin- or Graham-type condenser (see ISO 4799).
5.1.7 Screw cap with cut-off ring made of silicone rubber with PTFE inlay.
5.1.8 Adsorption tubes

Tubes made of glass or stainless steel, filled with at least 240 mg of adsorbing agent (4.5).

The adsorbent is kept in place by using inert material, e.g. silanized glass fibre. The tubes shall be suitable for

direct use in connection with the apparatus for thermal desorption. The tubes shall be marked on one side. The

tubes shall be provided with caps of inert material, e.g. polyethylene or metal, with screw caps and a PTFE ring,

that allow tight closing after purging.

Before use, the adsorbent shall be activated and purified by slowly heating the tubes to 250 °C and keeping them

at that temperature for 3 h while a nitrogen flow of 10 ml/min is maintained. The adsorbent shall be cooled under

© ISO 2012 – All rights reserved 5
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kSIST FprEN ISO 15009:2012
ISO 15009:2012(E)

nitrogen and the tubes analysed. The result of a blank determination shall not exceed the equivalent of 1 ng of

a compound to be analysed. When the result is higher than this, the adsorbent shall be desorbed once more.

NOTE The use of commercially available tubes is recommended.

Tubes that are used should not be used again, unless the blank determination meets the above-mentioned

requirements.

Care should be taken to avoid cross-contamination. A heavily loaded tube can contaminate a lightly loaded

tube in the sample change platform.
5.1.9 Heating block with thermocouple, suitable for heating 100 ml flasks

5.2 Centrifuge, suitable for centrifuging tubes of 200 ml with such a rotation frequency that the radial

acceleration is 2 000g to 3 000g.
5.3 Centrifuge tubes, with a volume of 200 ml.
5.4 Capillary columns

Fused silica capillary columns with a non-polar or semipolar stationary phase allowing sufficient separation of the

compounds of interest. A thick film of stationary phase increases the efficiency of the more volatile compounds.

Examples are given in 7.4 and Annex A.

5.5 Gas chromatograph, equipped with one or two appropriate detectors. Detectors, such as flame

ionization detectors (FIDs), electron capture detectors (ECDs), photo-ionization detectors (PIDs) or electrolytic

conductivity detectors (ELCDs), and a mass spectrometer (MS) can be used, depending on the substances to

be analysed and their target level of contamination. The mass spectrometer should be capable of operating

over the total mass range of interest and being equipped with a data system capable of quantifying ions using

selected m/z values.
5.6 Apparatus for thermal desorption
The apparatus used shall meet the following requirements:

— a primary desorption oven with adjustable desorption temperature up to 250 °C and adjustable desorption time;

— a cold trap/secondary desorption oven;

— a connecting tube to the gas chromatograph, with adjustable heating up to 150 °C;

— adjustable carrier-gas flow rate up to 40 ml/min.
NOTE Instruments for thermal desorption are commercially available.
5.7 Electronic integrator or automatic recorder

5.8 Syringe, of volume 5 µl, readable to 0,1 µl, and of volume 50 µl, readable to 1 µl.

5.9 Horizontal shaking machine
A shaking machine with horizontal movement (200 to 300 movements per minute).
6 © ISO 2012 – All rights reserved
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kSIST FprEN ISO 15009:2012
ISO 15009:2012(E)
6 Sampling, preservation and sample pretreatment
6.1 General

Sampling shall be carried out in accordance with ISO 10381-1 and ISO 10381-5, as appropriate, using

equipment according to ISO 10381-2, after coordination with the analytical laboratory.

Samples shall be analysed as soon as possible upon their receipt in the laboratory. If it is necessary to store

samples, they shall be stored in cool conditions in accordance with ISO 18512. Samples are not pretreated.

Exposure of samples to air, even during sampling, shall be avoided.

Samples for the determination of volatile compounds can be obtained using several techniques. It is strongly

recommended that one of the procedures described in 6.2 and 6.3 be used.
Determine the dry matter content of the field-moist samp
...

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