Soil quality - Gas chromatographic determination of volatile aromatic and halogenated hydrocarbons and selected ethers - Static headspace method (ISO 22155:2016)

This International Standard specifies a static headspace method for quantitative gas chromatographic
determination of volatile aromatic and halogenated hydrocarbons and selected aliphatic ethers in soil.
This International Standard is applicable to all types of soil.
The limit of quantification is dependent on the detection system 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 quantifications
apply (expressed on basis of dry matter).
Typical limit of quantification when using GC-FID:
— volatile aromatic hydrocarbons: 0,2 mg/kg;
— aliphatic ethers as methyl tert.-butyl ether(MTBE) and tert.-amyl methyl ether (TAME): 0,5 mg/kg.
Typical limit of quantification when using GC-ECD:
— volatile halogenated hydrocarbons: 0,01 mg/kg to 0,2 mg/kg.
Lower limits of quantification for some compounds can be achieved by using mass spectrometry (MS)
with selected ion detection (see Annex D).

Bodenbeschaffenheit - Gaschromatographische Bestimmung flüchtiger aromatischer Kohlenwasserstoffe, Halogenkohlenwasserstoffe und ausgewählter Ether - Statisches Dampfraum-Verfahren (ISO 22155:2016)

Diese Internationale Norm legt ein statisches Dampfraumverfahren zur gaschromatographischen quantitativen Bestimmung flüchtiger aromatischer Kohlenwasserstoffe, Halogenkohlenwasserstoffe und ausgewählter aliphatischer Ether im Boden fest.
Diese Internationale Norm ist auf alle Bodenarten anwendbar.
Die Bestimmungsgrenze ist abhängig vom angewendeten Nachweissystem und von 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 bei 0,2 mg/kg;
   und für aliphatische Ether, wie Methyl-tert-Butylether (MTBE) und tert-Amylmethylether (TAME) bei 0,5 mg/kg.
Bei Anwendung eines Gaschromatographen mit Elektroneneinfangdetektor (GC-ECD) liegt die typische Bestimmungsgrenze:
   für flüchtige Halogenkohlenwasserstoffe bei 0,01 mg/kg bis 0,2 mg/kg.
Niedrigere Bestimmungsgrenzen für einige Verbindungen können durch Anwendung der Massenspektrometrie (MS) mit selektiver Ionendetektion erreicht werden (siehe Anhang D).

Qualité du sol - Dosage des hydrocarbures aromatiques et halogénés volatils et de certains éthers par chromatographie en phase gazeuse - Méthode par espace de tête statique (ISO 22155:2016)

ISO 22155:2016 spécifie une méthode par espace de tête statique pour la détermination quantitative par chromatographie en phase gazeuse des hydrocarbures aromatiques et halogénés volatils et de certains éthers aliphatiques dans le sol.
ISO 22155:2016 est applicable à tous les types de sol.
La limite de quantification dépend du système de détection 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 quantifications suivantes (exprimées par rapport à la matière sèche) s'appliquent:
Limite de quantification type lorsque le couplage CG-FID est utilisé:
- hydrocarbures aromatiques volatils: 0,2 mg/kg;
- éthers aliphatiques sous forme de méthyl tert.-butyl éther (MTBE) et de tert.-amyl méthyl éther (TAME): 0,5 mg/kg.
Limite de quantification type lorsque le couplage CG-ECD est utilisé:
- hydrocarbures halogénés volatils: 0,01 mg/kg à 0,2 mg/kg.
Des limites de quantification inférieures pour certains composés peuvent être atteintes si l'on utilise la spectrométrie de masse (SM) avec détection sélective des ions (voir Annexe D).

Kakovost tal - Določevanje hlapnih aromatskih in halogeniranih ogljikovodikov in izbranih etrov s plinsko kromatografijo - Metoda s statičnim vzorčevalnikom iz plinske faze (headspace) (ISO 22155:2016)

Ta mednarodni standard določa metodo s statičnim vzorčevalnikom iz plinske faze (headspace) za določevanje hlapnih aromatskih in halogeniranih ogljikovodikov ter izbranih alifatskih etrov v tleh s kvantitativno plinsko kromatografijo.
Ta mednarodni standard se uporablja za vse vrste tal.
Mejna vrednost kvantifikacije je odvisna od uporabljenega sistema za detekcijo 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: 0,2 mg/kg
– alifatski etri kot metil terc-butil eter (MTBE) in terc-amil metil eter (TAME): 0,5 mg/kg
Običajna mejna vrednost kvantifikacije pri uporabi plinske kromatografije/detektorja na zajetje elektronov:
– hlapni halogenirani ogljikovodiki: od 0,01 mg/kg do 0,2 mg/kg
Nižje mejne vrednosti kvantifikacije za nekatere zmesi se lahko dosežejo z masno spektrometrijo (MS) z izbrano detekcijo iona (glej dodatek D).

General Information

Status
Published
Public Enquiry End Date
11-Jan-2015
Publication Date
09-Nov-2016
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
19-Oct-2016
Due Date
24-Dec-2016
Completion Date
10-Nov-2016

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SLOVENSKI STANDARD
SIST EN ISO 22155:2016
01-december-2016
1DGRPHãþD
SIST EN ISO 22155:2013
.DNRYRVWWDO'RORþHYDQMHKODSQLKDURPDWVNLKLQKDORJHQLUDQLKRJOMLNRYRGLNRYLQ
L]EUDQLKHWURYVSOLQVNRNURPDWRJUDILMR0HWRGDVVWDWLþQLPY]RUþHYDOQLNRPL]
SOLQVNHID]H KHDGVSDFH  ,62

Soil quality - Gas chromatographic determination of volatile aromatic and halogenated

hydrocarbons and selected ethers - Static headspace method (ISO 22155:2016)
Bodenbeschaffenheit - Gaschromatographische Bestimmung flüchtiger aromatischer

Kohlenwasserstoffe, Halogenkohlenwasserstoffe und ausgewählter Ether - Statisches

Dampfraum-Verfahren (ISO 22155:2016)

Qualité du sol - Dosage des hydrocarbures aromatiques et halogénés volatils et de

certains éthers par chromatographie en phase gazeuse - Méthode par espace de tête

statique (ISO 22155:2016)
Ta slovenski standard je istoveten z: EN ISO 22155:2016
ICS:
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST EN ISO 22155:2016 en,fr,de

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

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SIST EN ISO 22155:2016
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SIST EN ISO 22155:2016
EN ISO 22155
EUROPEAN STANDARD
NORME EUROPÉENNE
March 2016
EUROPÄISCHE NORM
ICS 13.080.10 Supersedes EN ISO 22155:2013
English Version
Soil quality - Gas chromatographic determination of
volatile aromatic and halogenated hydrocarbons and
selected ethers - Static headspace method (ISO
22155:2016)

Qualité du sol - Dosage des hydrocarbures aromatiques Bodenbeschaffenheit - Gaschromatographische

et halogénés volatils et de certains éthers par Bestimmung flüchtiger aromatischer

chromatographie en phase gazeuse - Méthode par Kohlenwasserstoffe, Halogenkohlenwasserstoffe und

espace de tête statique (ISO 22155:2016) ausgewählter Ether - Statisches Dampfraum-Verfahren

(ISO 22155:2016)
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 22155:2016 E

worldwide for CEN national Members.
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SIST EN ISO 22155:2016
EN ISO 22155:2016 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 22155:2016
EN ISO 22155:2016 (E)
European foreword

This document (EN ISO 22155:2016) 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 22155:2013.

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 22155:2016 has been approved by CEN as EN ISO 22155:2016 without any modification.

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SIST EN ISO 22155:2016
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SIST EN ISO 22155:2016
INTERNATIONAL ISO
STANDARD 22155
Third edition
2016-02-15
Soil quality — Gas chromatographic
determination of volatile aromatic
and halogenated hydrocarbons and
selected ethers — Static headspace
method
Qualité du sol — Dosage des hydrocarbures aromatiques et halogénés
volatils et de certains éthers par chromatographie en phase gazeuse
— Méthode par espace de tête statique
Reference number
ISO 22155:2016(E)
ISO 2016
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SIST EN ISO 22155:2016
ISO 22155:2016(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 22155:2016
ISO 22155:2016(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Principle ........................................................................................................................................................................................................................ 2

4 Reagents ........................................................................................................................................................................................................................ 2

5 Apparatus ..................................................................................................................................................................................................................... 6

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

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

6.2 Sampling using vials pre-filled with methanol ............................................................................................................ 7

6.3 Sampling using coring tube method ..................................................................................................................................... 8

7 Procedure..................................................................................................................................................................................................................... 8

7.1 Blank determination .......................................................................................................................................................................... 8

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

7.3 Head-space analysis............................................................................................................................................................................ 8

7.4 Gas chromatographic analysis ................................................................................................................................................... 9

7.4.1 General...................................................................................................................................................................................... 9

7.4.2 Calibration ..........................................................................................................................................................................10

7.4.3 Measurement ...................................................................................................................................................................11

8 Calculation ...............................................................................................................................................................................................................11

8.1 Calculation of the concentration of a volatile compound in the water sample ............................11

8.2 Calculation of the concentration of a volatile compound in the soil sample ..................................12

9 Expression of results .....................................................................................................................................................................................12

10 Precision ....................................................................................................................................................................................................................12

11 Test report ................................................................................................................................................................................................................12

Annex A (informative) Relative retention times with respect to ethylbenzene-D10 of

volatile aromatic hydrocarbons and volatile halogenated hydrocarbons —

Examples of suitable target and qualifier ions ..................................................................................................................13

Annex B (normative) Check on internal standards ............................................................................................................................15

Annex C (informative) Validation (general) ...............................................................................................................................................16

Annex D (informative) Performance characteristics ........................................................................................................................19

Bibliography .............................................................................................................................................................................................................................21

© ISO 2016 – All rights reserved iii
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SIST EN ISO 22155:2016
ISO 22155:2016(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 22155:2011), which has been technically

revised.
iv © ISO 2016 – All rights reserved
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SIST EN ISO 22155:2016
INTERNATIONAL STANDARD ISO 22155:2016(E)
Soil quality — Gas chromatographic determination of
volatile aromatic and halogenated hydrocarbons and
selected ethers — Static headspace method
1 Scope

This International Standard specifies a static headspace method for quantitative gas chromatographic

determination of volatile aromatic and halogenated hydrocarbons and selected aliphatic ethers in soil.

This International Standard is applicable to all types of soil.

The limit of quantification is dependent on the detection system 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 quantifications

apply (expressed on basis of dry matter).
Typical limit of quantification when using GC-FID:
— volatile aromatic hydrocarbons: 0,2 mg/kg;

— aliphatic ethers as methyl tert.-butyl ether(MTBE) and tert.-amyl methyl ether (TAME): 0,5 mg/kg.

Typical limit of quantification when using GC-ECD:
— volatile halogenated hydrocarbons: 0,01 mg/kg to 0,2 mg/kg.

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

with selected ion detection (see Annex D).
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 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 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 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography and

mass spectrometry
© ISO 2016 – All rights reserved 1
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SIST EN ISO 22155:2016
ISO 22155:2016(E)
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. An aliquot of the methanol extract is transferred into a

headspace vial with a defined amount of water and sealed. The temperature of the vials is stabilized in

a thermostatic system to a temperature within the range 50 °C to 80 °C to achieve specified equilibrium

conditions. Gas chromatographic analysis of the volatile compounds in gaseous phase in equilibrium with

the water in the vials is carried out by using headspace injection and an appropriate capillary column.

Volatile organic compounds are detected with appropriate detectors 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 is made by comparison of

retention times and peak heights (or peak areas) comparing to the internal standard added.

When using non-specific detectors 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.
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 organic compounds

Water, free from volatile organic contaminants shall show negligible interferences in comparison with

the smallest concentration to be determined. 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.

Table 1 — Examples of suitable internal standards
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.

2 © ISO 2016 – All rights reserved
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SIST EN ISO 22155:2016
ISO 22155:2016(E)
Table 2 — Examples of suitable internal standards
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.

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
Chemical Abstracts Service Registry Number.
EC-Number.
© ISO 2016 – All rights reserved 3
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SIST EN ISO 22155:2016
ISO 22155:2016(E)
Table 4 (continued)
a b
Compound name CAS-RN EC-N
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 Aliphatic ethers
Table 5 contains aliphatic ethers for use as standard compounds.
Table 5 — Examples of aliphatic ethers suitable as standards compounds
a b
Compound name CAS-RN EC-N
methyl tert.-butyl ether (MTBE) 1634–04–4 216–653–1
tert.-amyl methyl ether (TAME) 994–05–8 213–611–4
Chemical Abstracts Service Registry Number.
EC-Number.

NOTE This method can also be used for volatile organic compounds not included in this International

Standard, provided it has been validated for each new compound.
4.5 Methanol

Methanol (see Table 6) is used as solvent for the extraction of soil samples and for the preparation of

standard solutions.
Table 6 — Registration data
a b
Compound name CAS-RN EC-N
Methanol 67–56–1 200–659–6
Chemical Abstracts Service Registry Number.
EC-Number.

NOTE Other solvents which are readily soluble in water and do not interfere with the analytical process can

be used as well, for example dimethylformamide (DMF) and dimethylsulfoxide (DMSO).

4.6 Gases for gas chromatography

Helium, nitrogen or argon-methane mixture ultrapure. Other gases for gas chromatography shall be

used in accordance with the instrument manufacturer’s instructions.
4 © ISO 2016 – All rights reserved
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SIST EN ISO 22155:2016
ISO 22155:2016(E)
4.7 Standard solutions
4.7.1 Standard stock solutions for the volatile compounds in methanol

Prepare the stock solutions by adding defined amounts (e.g. 100 µl) of each standard compound (4.3,

4.4 and 4.5) with a microlitre syringe (5.8). Immerse the tip of the needle in the solvent methanol and

weigh with an accuracy of 0,1 mg.

NOTE 1 A convenient concentration (4 mg/ml) of the standard stock solution is obtained by weighing 100 mg

of the standard substance and dissolving it in 25 ml of the solvent. The stock solution is stable for about 6 m when

stored at −18 °C.

NOTE 2 For practical reasons, mixed standard stock solutions can also be prepared.

4.7.2 Internal standard stock solutions in methanol

The containers containing the solutions shall be 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.

Prepare the internal standard stock solutions with the individual internal standard compounds (4.2.1

and 4.2.2) in the same procedure as in 4.7.1.
4.7.3 Intermediate mixed standard solutions

Prepare intermediate mixed standard solutions by mixing a defined volume of each individual standard

stock solution or a mixed standard stock solution and dilute with methanol.
NOTE A typical concentration is 40 µg/ml.

Store the intermediate mixed standard solutions at (4 ± 2) °C not longer than 3 m.

4.7.4 Working standard solutions

Prepare at least five different concentrations (e.g. from 0,2 µg/ml to 3,2 µg/ml) by suitable dilutions of

the intermediate mixed standard solutions adding 50 µl to 500 µl of 4.7.3 to methanol (10 ml) using a

microlitre syringe (5.8).
4.7.5 Working internal standard solutions

Prepare the internal standard solutions of defined concentration (e.g. 0,4 µg/ml) as described in 4.7.3.

4.7.6 Aqueous calibration standard solutions

Prepare the calibration solutions (see Table 7) by adding a defined amount (e.g. 50 µl) of working

standard solutions and internal standard solutions to a defined volume (e.g. 10 ml) of water in an

appropriate headspace vial. Use a syringe and immerse the top of the needle in the water. Seal the vial

tightly with a crimp cap fitted with polytetrafluoroethylene (PTFE) coated septum. The total volume of

the methanol used for calibration shall be the same which will be taken for the methanol extract of the

soil sample (see 7.3). Make sure that the content of the organic solvent in the final aqueous calibration

standard solution does not exceed the volume fraction of 2 %.
© ISO 2016 – All rights reserved 5
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SIST EN ISO 22155:2016
ISO 22155:2016(E)
Table 7 — Example for the preparation of calibration solutions
Calibration Working Working Concentration Quantity in Concentration
solution standard internal in working calibration in aqueous
solution (4.7.4) standard standard solu- solution of 10 ml calibration
standards tion (sample) water solution
(4.7.5)
µl µl µg/ml ng µg/l
1 50 50 (methanol) 0 0 0
2 50 50 0,2 10 1
3 50 50 0,4 20 2
4 50 50 0,8 40 4
5 50 50 1,6 80 8
6 50 50 3,2 160 16
4.8 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 headspace vial is of

the same level as in the calibration standards.
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 Glass vials with suitable septum.

Glass vials (50 ml to 100 ml) and screw cap, fitted with a PTFE-coated septum for field moist soil

samples taken in the field. Glass vials (10 ml for 5 ml water and 22 ml for 10 ml water) with a PTFE-

coated septum and crimped metallic cap, compatible with the headspace system connected to an

appropriate gas chromatographic system. The vials shall be capable of being hermetically sealed in the

field as well as at elevated temperatures.
5.2 Crimping pliers.
5.3 Headspace system.

This method was developed for using a totally automated equilibrium headspace analyser available

from several commercial sources. The system used shall meet the following specifications.

The system shall be capable of keeping the vials at a constant temperature (between 50 °C and 80 °C).

The system shall be capable of transferring accurately a representative portion of the headspace into a

gas chromatograph fitted with capillary columns.
5.4 Shaking machine, with horizontal movement (200 to 300 movements per minute).
5.5 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

separation of more volatile compounds.
Examples are given in 7.4.1.
6 © ISO 2016 – All rights reserved
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SIST EN ISO 22155:2016
ISO 22155:2016(E)

5.6 Gas chromatograph, equipped with one or two appropriate detectors. Detectors like flame

ionization detector (FID), electron capture detector (ECD), photo ionization detector (PID) or electrolytic

conductivity detector (ELCD) and mass spectrometer (MS) can be used, depending on the substances to

be analysed and their target level of contamination. The mass spectrometer should be able 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.
5.7 Electronic integrator or computer with chromatographic software.
5.8 Syringe, volume 5 µl, 10 µl, 50 µl, 100 µl, 250 µl, and 500 µl.

5.9 Centrifuge, with a capacity of a rotation frequency that results into a radial acceleration of at

least 2000g.
6 Sampling, preservation, and sample pretreatment
6.1 General

Sampling shall be carried out according to ISO 10381-1 using equipment according to ISO 10381-2 after

coordination with the analytical laboratory.

Samples shall be stored cool according to ISO 18512 (2 °C to 8 °C). Samples are not pretreated. Exposure

of samples to air, even during sampling, shall be avoided as far as possible.
Sampling fo
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