SIST EN ISO 16558-1:2015

Soil quality - Risk based petroleum hydrocarbons - Part 1: Determination of aliphatic and aromatic fractions of volatile petroleum hydrocarbons using gas chromatography (static headspace method) (ISO 16558-1:2015)

This part of ISO xxxxx specifies a method for the quantitative determination of the total extractable volatile, the volatile aliphatic and aromatic fractions of petroleum hydrocarbon content in field moist soil samples by gas chromatography. The results of the test carried out can be used for risk assessment studies related to contaminations with petroleum hydrocarbons. The method is applicable to petroleum hydrocarbon contents between XXXX mg/kg and XXXX mg/kg soil expressed as dry matter for the whole aliphatic fraction C5 to C10 as well as the aromatic compounds in the boiling range of C6 to C10. For sub-fractions lower limits of determination can be reached.
With this method all hydrocarbons with a boiling range of 36 °C to 175 °C, n-alkanes between C5H12 to C10H22, isoalkanes, cycloalkanes, BTEX, di- and tri-alkyl benzenes compounds are determined as total volatile petroleum hydrocarbons C5 to C10; besides that volatile aliphatic and aromatic fractions are specified. The sub-fractions proposed in this part of ISO xxxxx have shown to be suitable for risk assessment studies. However other sub-fractions between C5H12 to C10H22 can be determined in conformity with this standard.

Bodenbeschaffenheit - Mineralölkohlenwasserstoffe für die Risikobeurteilung - Teil 1: Bestimmung aliphatischer und aromatischer Fraktionen leicht flüchtiger Mineralölkohlenwasserstoffe mittels Gaschromatographie (statisches Headspace-Verfahren) (ISO 16558-1:2015)

Dieser Teil von ISO 16558 legt ein Verfahren zur quantitative Bestimmung der gesamten extrahierbaren flüchtigen Bestandteile, der leicht flüchtigen aliphatischen und aromatischen Fraktionen des Mineralölkohlen-wasserstoff-Gehalts in feldfrischen Bodenproben mittels Gaschromatographie mit massen¬spektrometrischem Nachweis (GC MS, en: gas chromatography with mass spectrometric detection) fest. Die aromatischen Fraktionen werden durch die Summe der einzelnen aromatischen Verbindungen bestimmt.
Die Ergebnisse der durchgeführten Prüfung können für Studien zur Risikobeurteilung hinsichtlich der Kontaminationen mit Mineralölkohlenwasserstoffen angewendet werden.
Das Verfahren ist für Mineralölkohlenwasserstoff-Gehalte zwischen XXXX mg/kg und XXXX mg/kg Boden, angegeben als Trockensubstanz für die gesamte aliphatische Fraktion C5 bis C10 sowie für die aromatischen Verbindungen im Siedebereich von C6 bis C10 geeignet. Bei Teilfraktionen können niedrigere Bestimmungsgrenzen erreicht werden.
Mit diesem Verfahren werden alle Kohlenwasserstoffe mit einem Siedebereich von 36 °C bis 175 °C, n Alkane zwischen C5H12 und C10H22, Isoalkane, Cycloalkane, BTEX, Di- und Trialkylbenzol-Verbindungen als leicht flüchtige Gesamt-Mineralölkohlenwasserstoffe C5 bis C10 bestimmt. Zusätzlich werden die leicht flüchtigen aliphatischen und aromatischen Fraktionen festgelegt.
Hinsichtlich der Bestimmung von schwerflüchtigen aliphatischen und aromatischen Fraktionen von Mineralölkohlenwasserstoffen in Bodenproben siehe Teil 2 dieser Internationalen Norm.
ANMERKUNG   Die in diesem Teil der ISO 16558 vorgeschlagenen Teilfraktionen haben gezeigt, dass sie für Studien zur Risikobeurteilung geeignet sind. Jedoch können weitere Teilfraktionen zwischen C5H12 und C10H22 in Übereinstimmung mit dieser Internationalen Norm bestimmt werden.
Auf der Grundlage der Peakfolge des Gaschromatogramms und der Siedepunkte der einzelnen im Anhang A angeführten n Alkane können der näherungsweise Siedebereich des Mineralöls und einige qualitative Hinweise zur Zusammensetzung der Kontamination erhalten werden.

Qualité du sol - Hydrocarbures de pétrole à risque - Partie 1: Détermination des fractions aliphatiques et aromatiques des hydrocarbures de pétrole volatiles par chromatographie en phase gazeuse (méthode par espace de tête statique) (ISO 16558-1:2015)

ISO 16558-1:2015 spécifie une méthode de dosage quantitatif des fractions aliphatiques et aromatiques volatiles extractibles totales des hydrocarbures de pétrole dans des échantillons humides par chromatographie en phase gazeuse avec détection spectrométrique de masse. Les fractions aromatiques sont dosées par l'ensemble des composés aromatiques individuels.
L'ensemble des fractions aliphatiques (C5 à C10) et aromatiques (C6 to C10) volatiles peut être désigné par l'expression «huile volatile».
Les résultats de l'essai effectué peuvent être utilisés pour les études d'évaluation des risques liées aux contaminations par les hydrocarbures de pétrole.
ISO 16558-1:2015 propose une méthode applicable aux teneurs en hydrocarbures de pétrole d'environ 5 mg/kg de sol, exprimées sous forme de matière sèche pour la fraction aliphatique totale C5 à C10 et d'environ 5 mg/kg de sol, exprimées sous forme de matière sèche pour la fraction aromatique dans le domaine d'ébullition de C6 à C10.
Grace à cette méthode, tous les hydrocarbures ayant une température d'ébullition comprise entre 36 °C et 184 °C, les n-alcanes de C5H12 à C10H22, les isoalcanes, les cycloalcanes, les BTEX et les composés de di- et trialkylbenzène sont dosés sous forme d'hydrocarbures de pétrole volatils totaux C5 à C10. De plus, les fractions aliphatiques et aromatiques volatiles sont spécifiées.
Pour le dosage des fractions aliphatiques et aromatiques semi-volatiles des hydrocarbures de pétrole dans les échantillons de sol, voir l'ISO/TS 16558-2.
NOTE          Les sous-fractions proposées dans la présente partie de l'ISO 16558 se sont révélées adaptées aux études d'évaluation des risques. Cependant, d'autres sous-fractions entre C5H12 et C10H22 peuvent être dosées conformément à la présente partie de l'ISO 16558.
Compte tenu de la forme des pics du chromatogramme en phase gazeuse et du point d'ébullition des différents alcanes indiqués à l'Annexe A, il est possible de déterminer le domaine d'ébullition approximatif des huiles minérales et de recueillir quelques informations qualitatives sur la composition des polluants.

Kakovost tal - Naftni ogljikovodiki, ki predstavljajo tveganje - 1. del: Določevanje alifatskih in aromatskih frakcij hlapnih naftnih ogljikovodikov s plinsko kromatografijo (metoda s statičnim vzorčevalnikom iz plinske faze - headspace) (ISO 16558-1:2015)

Ta del standarda ISO 16558-1 določa metodo za količinsko določevanje skupnih hlapnih snovi, ki jih je mogoče ekstrahirati, hlapnih alifatskih in aromatskih frakcij naftnih ogljikovodikov na terenskih vzorcih vlažnih tal s plinsko kromatografijo. Rezultate izvedenega preskusa je mogoče uporabiti za študije ocene tveganja v zvezi z onesnaženjem z naftnimi ogljikovodiki. Metoda se lahko uporablja za vsebnost naftnih ogljikovodikov med XXXX mg/kg in XXXX mg/kg tal, izraženo kot suha snov, za celotno alifatsko frakcijo C5 do C10 in aromatske spojine v območju vrelišča C6 do C10. Za podfrakcije je mogoče doseči nižje mejne vrednosti določevanja. S to metodo so vsi ogljikovodiki z območjem vrelišča 36 °C do 175 °C, n-alkani med C5H12 in C10H22, izoalkani, cikloalkani, BTEX, dialkil in trialkil benzenske spojine določeni kot skupni hlapni naftni ogljikovodiki C5 do C10; poleg tega se določijo hlapne alifatske in aromatske frakcije. Za podfrakcije, predlagane v tem delu standarda ISO xxxxx, se je izkazalo, da so primerne za študije ocene tveganja. Druge podfrakcije med C5H12 in C10H22 pa je mogoče določiti v skladu s tem standardom.

General Information

• Status: Published
• Public Enquiry End Date: 31-Aug-2013
• Publication Date: 05-Oct-2015
• ICS: 13.080.10 - Chemical characteristics of soils
• ICS: 71.040.50 - Physicochemical methods of analysis
• Technical Committee: KAT - Soil quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 18-Sep-2015
• Due Date: 23-Nov-2015
• Completion Date: 06-Oct-2015
• Directive: TP168 - Pravilnik o monitoringu kakovosti tal
• Directive: TP255 - Pravilnik o obratovalnem monitoringu stanja tal
• Ref Project: EN ISO 16558-1:2015 - Soil quality - Risk-based petroleum hydrocarbons - Part 1: Determination of aliphatic and aromatic fractions of volatile petroleum hydrocarbons using gas chromatography (static headspace method) (ISO 16558-1:2015)

Relations

• Amended By: SIST EN ISO 16558-1:2015/A1:2020 - Soil quality - Risk-based petroleum hydrocarbons - Part 1: Determination of aliphatic and aromatic fractions of volatile petroleum hydrocarbons using gas chromatography (static headspace method) - Amendment 1 (ISO 16558-1:2015/Amd 1:2020)
• Effective Date: 01-Nov-2020

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 16558-1:2015
01-november-2015
.DNRYRVWWDO1DIWQLRJOMLNRYRGLNLNLSUHGVWDYOMDMRWYHJDQMHGHO'RORþHYDQMH
DOLIDWVNLKLQDURPDWVNLKIUDNFLMKODSQLKQDIWQLKRJOMLNRYRGLNRYVSOLQVNR
NURPDWRJUDILMRPHWRGDVVWDWLþQLPY]RUþHYDOQLNRPL]SOLQVNHID]HKHDGVSDFH
,62
Soil quality - Risk based petroleum hydrocarbons - Part 1: Determination of aliphatic and
aromatic fractions of volatile petroleum hydrocarbons using gas chromatography (static
headspace method) (ISO 16558-1:2015)
Bodenbeschaffenheit - Mineralölkohlenwasserstoffe für die Risikobeurteilung - Teil 1:
Bestimmung aliphatischer und aromatischer Fraktionen leicht flüchtiger
Mineralölkohlenwasserstoffe mittels Gaschromatographie (statisches Headspace-
Verfahren) (ISO 16558-1:2015)
Qualité du sol - Hydrocarbures de pétrole à risque - Partie 1: Détermination des fractions
aliphatiques et aromatiques des hydrocarbures de pétrole volatiles par chromatographie
en phase gazeuse (méthode par espace de tête statique) (ISO 16558-1:2015)
Ta slovenski standard je istoveten z: EN ISO 16558-1:2015
ICS:
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST EN ISO 16558-1:2015 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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

SIST EN ISO 16558-1:2015

---------------------- Page: 2 ----------------------

SIST EN ISO 16558-1:2015


EN ISO 16558-1
EUROPEAN STANDARD

NORME EUROPÉENNE

September 2015
EUROPÄISCHE NORM
ICS 13.080.10
English Version

Soil quality - Risk-based petroleum hydrocarbons - Part 1:
Determination of aliphatic and aromatic fractions of
volatile petroleum hydrocarbons using gas
chromatography (static headspace method) (ISO 16558-
1:2015)
Qualité du sol - Hydrocarbures de pétrole à risque - Bodenbeschaffenheit - Mineralölkohlenwasserstoffe
Partie 1: Détermination des fractions aliphatiques et für die Risikobeurteilung - Teil 1: Bestimmung
aromatiques des hydrocarbures de pétrole volatiles aliphatischer und aromatischer Fraktionen leicht
par chromatographie en phase gazeuse (méthode par flüchtiger Mineralölkohlenwasserstoffe mittels
espace de tête statique) (ISO 16558-1:2015) Gaschromatographie (statisches Headspace-Verfahren)
(ISO 16558-1:2015)
This European Standard was approved by CEN on 13 June 2015.

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
© 2015 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 16558-1:2015 E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------

SIST EN ISO 16558-1:2015
EN ISO 16558-1:2015 (E)
Contents Page
European foreword . 3

2

---------------------- Page: 4 ----------------------

SIST EN ISO 16558-1:2015
EN ISO 16558-1:2015 (E)
European foreword
This document (EN ISO 16558-1:2015) 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 March 2016, and conflicting national standards shall
be withdrawn at the latest by March 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.
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 16558-1:2015 has been approved by CEN as EN ISO 16558-1:2015 without any
modification.
3

---------------------- Page: 5 ----------------------

SIST EN ISO 16558-1:2015

---------------------- Page: 6 ----------------------

SIST EN ISO 16558-1:2015
INTERNATIONAL ISO
STANDARD 16558-1
First edition
2015-08-15
Soil quality — Risk-based petroleum
hydrocarbons —
Part 1:
Determination of aliphatic and
aromatic fractions of volatile
petroleum hydrocarbons using gas
chromatography (static headspace
method)
Qualité du sol — Hydrocarbures de pétrole à risque —
Partie 1: Détermination des fractions aliphatiques et aromatiques
des hydrocarbures de pétrole volatiles par chromatographie en phase
gazeuse (méthode par espace de tête statique)
Reference number
ISO 16558-1:2015(E)
©
ISO 2015

---------------------- Page: 7 ----------------------

SIST EN ISO 16558-1:2015
ISO 16558-1:2015(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2015, 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. [phone]
Fax [phone]
[e-mail]
www.iso.org
ii © ISO 2015 – All rights reserved

---------------------- Page: 8 ----------------------

SIST EN ISO 16558-1:2015
ISO 16558-1:2015(E)

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Interferences . 3
5 Principle . 3
6 Reagents . 3
7 Apparatus . 7
8 Sampling, preservation, and sample pretreatment . 8
8.1 General . 8
8.2 Sampling using vials pre-filled with methanol . 8
8.3 Sampling using coring tube method . 9
9 Procedure. 9
9.1 Blank determination . 9
9.2 Extraction . 9
9.3 Headspace-analysis . 9
9.4 Gas chromatographic analysis .10
9.4.1 General.10
9.4.2 Calibration .10
9.4.3 Measurement .12
10 Calculation .12
10.1 Calculation of the concentration in the spiked water sample .12
10.1.1 Volatile aromatic hydrocarbon compounds with internal standard method .12
10.1.2 Volatile aliphatic fractions .12
10.2 Calculation of the concentration of a volatile compound or fraction in the soil sample .13
10.3 Calculation of the concentration of volatile oil in the soil sample .13
11 Expression of results .13
12 Precision .13
13 Test report .13
Annex A (informative) Examples of GC-MS chromatograms of fuels .14
Bibliography .16
© ISO 2015 – All rights reserved iii

---------------------- Page: 9 ----------------------

SIST EN ISO 16558-1:2015
ISO 16558-1:2015(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.
ISO 16558 consists of the following parts, under the general title Soil quality — Risk-based petroleum
hydrocarbons:
— Part 1: Determination of aliphatic and aromatic fractions of volatile petroleum hydrocarbons using gas
chromatography (static headspace method)
— Part 2: Determination of aliphatic and aromatic fractions of semi-volatile petroleum hydrocarbons
using gas chromatography with flame ionization detection (GC/FID) [Technical Specification]
iv © ISO 2015 – All rights reserved

---------------------- Page: 10 ----------------------

SIST EN ISO 16558-1:2015
ISO 16558-1:2015(E)

Introduction
ISO 11504 establishes a basis for the choice of fractions and individual compounds when carrying out
analysis for petroleum hydrocarbons in soils and soil-like materials including sediments. It provides
guidance for the appropriate use of the analytical results in risks assessment. This part of ISO 16558
specifies methods for the quantitative determination of the appropriate fractions of aliphatic and
aromatic compounds. The methods described are based on existing standards [mineral oil (ISO 16703)
and volatile hydrocarbons (ISO 22155)].
The general use and relation between the two different parts of this International Standard is given in
Figure 1.
Key
a b
Florisil® clean-up: Only to be applied in case the test according to ISO 16703 is carried out. If the aliphatic
and aromatic fractions have to be analysed, florisil clean-up should not be carried out. Florisil® is a trade
name for a prepared diatomaceous substance mainly consisting of anhydrous magnesium silicate.
b
Florisil® 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.
Figure 1 — Use of different analytical International Standards during risk assessment of
petroleum hydrocarbons
© ISO 2015 – All rights reserved v

---------------------- Page: 11 ----------------------

SIST EN ISO 16558-1:2015

---------------------- Page: 12 ----------------------

SIST EN ISO 16558-1:2015
INTERNATIONAL STANDARD ISO 16558-1:2015(E)
Soil quality — Risk-based petroleum hydrocarbons —
Part 1:
Determination of aliphatic and aromatic fractions
of volatile petroleum hydrocarbons using gas
chromatography (static headspace method)
1 Scope
This part of ISO 16558 specifies a method for the quantitative determination of the total extractable
volatile, the volatile aliphatic, and aromatic fractions of petroleum hydrocarbon content in field moist
soil samples by gas chromatography with mass spectrometric detection. The aromatic fractions are
determined by the sum of individual aromatic compounds.
The sum of the volatile aliphatic (C to C ) and aromatic (C to C ) fractions can be referred to as
5 10 6 10
“volatile oil”.
The results of the test carried out can be used for risk assessment studies related to contaminations
with petroleum hydrocarbons.
This part of ISO 16558 provides a method applicable to petroleum hydrocarbon contents from about
5 mg/kg soil expressed as dry matter for the whole aliphatic fraction C to C and about 5 mg/kg soil
5 10
expressed as dry matter for the aromatic fraction in the boiling range of C to C .
6 10
With this method, all hydrocarbons with a boiling range of 36 °C to 184 °C, n-alkanes between C H to
5 12
C H , isoalkanes, cycloalkanes, BTEX, and di- and tri-alkyl benzenes compounds are determined as
10 22
total volatile petroleum hydrocarbons C to C . In addition, volatile aliphatic and aromatic fractions
5 10
are specified.
For the determination of semi-volatile aliphatic and aromatic fractions of petroleum hydrocarbons in
soil samples, see ISO/TS 16558-2.
NOTE The sub-fractions proposed in this part of ISO 16558 have shown to be suitable for risk assessment
studies. However, other sub-fractions between C H to C H can be determined in conformity with this part
5 12 10 22
of ISO 16558.
On the basis of the peak pattern of the gas chromatogram and of the boiling points of the individual
n-alkanes listed in Annex A, the approximate boiling range of the mineral oil and some qualitative
information on the composition of the contamination can be achieved.
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 8466-1, Water quality — Calibration and evaluation of analytical methods and estimation of
performance characteristics — Part 1: Statistical evaluation of the linear calibration function
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 2015 – All rights reserved 1

---------------------- Page: 13 ----------------------

SIST EN ISO 16558-1:2015
ISO 16558-1:2015(E)

ISO 11465, Soil quality — Determination of dry matter and water content on a mass basis —
Gravimetric method
ISO 18512, Soil quality — Guidance on long and short term storage of soil samples
ISO 22155, Soil quality — Gas chromatographic determination of volatile aromatic and halogenated
hydrocarbons and selected ethers — Static headspace method
ISO 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography and
mass spectrometry
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
total content of volatile petroleum hydrocarbon fractions by gas chromatography
sum of compounds extractable with methanol that can be measured by headspace gas chromatography
with a mass spectrometric detector and eluted on a non-polar capillary column with retention times
between those of n-pentane (C H ) EC 5 and hexane (C H ) EC 6, between EC 6 and n-octane (C H )
5 12 6 14 8 18
EC 8, and between EC 8 and 1,2-diethylbenzene (C H ) EC 10
10 14
Note 1 to entry: Substances that comply with that definition are mainly short chain or branched, olefenic,
alicyclic, aliphatic hydrocarbons, and BTEX or alkyl substituted aromatic hydrocarbons.
3.2
volatile aromatic compounds and fraction between EC numbers 9 to 10 of petroleum hydrocarbons
single mono-aromatic BTEX compounds and the fraction between EC numbers 9 to 10 containing di-
and tri-alkylated aromatic compounds which can be measured by headspace gas chromatography with
a mass spectrometric detector
Note 1 to entry: For example compounds, see Table 1.
3.3
volatile aliphatic fractions of petroleum hydrocarbons
quantitative values for the aliphatic fractions of the volatile petroleum hydrocarbons (olefenic, alicyclic
branched, and paraffinic short hydrocarbons) between EC numbers 5 to 6, 6 to 8, and 8 to 10 which can
be measured with headspace gas chromatography with a mass spectrometric detector
Note 1 to entry: For example compounds, see Table 1.
Table 1 — EC number ranges and respective example aliphatic and aromatic compounds
Structure EC number range Boiling Example compounds
type Carbon number of range
n-alkanes
°C
Aliphatic 5 to 6 ≥ 36 to 69 Pentane, 2- and 3-methylpentane, 2,2- and
compounds 2,3-dimethylbutane, cyclopentane,
2,3-dimethyl-butadiene, hexane
> 6 to 8 > 69 to 128 Cyclohexane, methylcyclopentane,
dimethyl-cyclopentane, methyl- and
dimethyl-cyclohexane, branched C - and
7
C -alkane
8
> 8 to 10 > 128 to 175 n-nonane, 2-methylnonane,
1,1,3-trimethyl-cyclohexane,
2,3-dimethylheptane, n-decane
2 © ISO 2015 – All rights reserved

---------------------- Page: 14 ----------------------

SIST EN ISO 16558-1:2015
ISO 16558-1:2015(E)

Table 1 (continued)
Structure EC number range Boiling Example compounds
type Carbon number of range
n-alkanes
°C
Aromatic > 6 to 9 > 69 to 151 BTEX single compounds, styrene
compounds
> 9 to 10 > 151 to 184 Allylbenzene, i- and n-propylbenzene, 2- and 3-
and 4-ethyltoluene, 1,2- and 1,3-diethylbenzene,
1,2,3- and 1,2,4- and 1,3,5-trimethylbenzene,
isopropenylbenzene
4 Interferences
Compounds not related to petroleum hydrocarbon contaminations with boiling point between C and C
5 10
(e.g. halogenated hydrocarbons and ethers as MTBE and TAME) can interfere with the aliphatic fractions.
5 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 (see ISO 22155 for further information).
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. The compounds are detected with a mass spectrometric detector (MS).
The procedure as described in ISO 22155 is followed for determination of the individual aromatic
compounds. Several aromatic fractions are then determined by summation of individual aromatic
compounds.
On the basis of the peak pattern of the gas chromatogram and of the boiling points of the individual
n-alkanes between C H to C H (retention time standard), the sub-fractions of the volatile aliphatic
5 12 10 22
hydrocarbons can be fixed and the peak areas of the sub-fractions can be integrated and hence used for
quantification.
The total peak areas between the EC range defining standards between n-pentane and n-decane is
measured and the content of the volatile aliphatic hydrocarbons in the sample is quantified against an
external standard mix consisting of different types of volatile aliphatic compounds which are typical
for petroleum hydrocarbons.
6 Reagents
All reagents shall be of recognized analytical grade. Verify whether the reagents are applicable for this
specific purpose and free of interfering compounds.
6.1 Water, free of volatile organic compounds.
Water, free from organic contaminants. It shall show negligible interferences in comparison with the
smallest concentration to be determined. Sufficient water from the same batch should be available to
complete each batch of analyses including all preparations.
Water can be heated in a round bottom flask for about 30 min to remove remains of volatile compounds.
© ISO 2015 – All rights reserved 3

---------------------- Page: 15 ----------------------

SIST EN ISO 16558-1:2015
ISO 16558-1:2015(E)

1)
6.2 Methanol (CAS-RN 67-56-1).
Solvent for the extraction of soil samples and for the preparation of standard solutions.
6.3 Internal standard compounds.
For the determination of volatile aromatic hydrocarbons by GC-MS, two or more internal standards
shall be selected. They shall not interfere with compounds present in the methanol extract.
Examples of suitable internal standards are the following:
a) toluene-D8 (CAS-RN 2037-26-5);
b) ethylbenzene-D10 (CAS-RN 25837-05-2);
c) 1,3,5-trimethylbenzene D3 (CAS-RN 38574-14-0).
Example of suitable non-deuterated internal standard:
— ααα-trifluorotoluene (CAS-RN 98-08-8).
6.4 Retention time standard solution.
It is the fraction range defining standard solution containing n-pentane, n-hexane, n-heptane, n-octane,
n-nonane, and n-decane.
Prepare a mixture of equal amounts, on a mass basis, of the n-alkanes with carbon numbers from C
5
to C , dissolved in methanol (6.2), to give concentrations of about 50 mg/l of each n-alkane. Store at
10
room temperature.
NOTE This solution is used to give information of the retention times of the n-alkanes to define the volatile
hydrocarbon fractions in the samples.
6.5 Volatile aromatic hydrocarbon standards between EC numbers range 6 to 10 for calibration
of headspace GC-MS system.
Compound CAS-RN
EC number range 6 to 9
benzene 71–43–2
toluene 108–88–3
ethylbenzene 100–41–4
o-xylene 95–47–6
m-xylene 108–38–3
p-xylene 106–42–3
styrene 100–42–5
EC number range 9 to 10
allylbenzene 300–57–2
isoproprenylbenzene 98–83–9
1) CAS-RN: Chemical Abstracts Service Registry Number.
4 © ISO 2015 – All rights reserved

---------------------- Page: 16 ----------------------

SIST EN ISO 16558-1:2015
ISO 16558-1:2015(E)

2-ethyltoluene 611–14–3
3-ethyltoluene 620–14–4
4-ethyltoluene 622–96–8
1,2,3-trimethylbenzene 526–73–8
1,2,4-trimethylbenzene 95–63–6
1,3,5-trimethylbenzene 108–67–8
isopropylbenzene 98–82–8
sec-butylbenzene 135–98–8
1,2-diethylbenzene 135–01–3
1,3-diethylbenzene 141–93–5
The detector responses of these selected compounds are measured by headspace gas chromatography
with a mass spectrometric detector (electron ionization with selected ion monitoring of mass fragments
m/z 78 for benzene and m/z 91 for toluene, ethylbenzene, and xylenes, m/z 104 for styrene, and
m/z 91+105+117+118+119+120+134 for di- and tri-alkylated benzene), which are used for quantification.
6.6 Volatile aliphatic hydrocarbon standards between EC numbers range 5 to 10 for calibration
of headspace GC-MS system.
Aliphatic compound CAS-RN
n-pentane 109–66–0
n-hexane 110–54–3
n-heptane 142–82–5
n-octane 111–65–9
n-nonane 111–84–2
n-decane 124–18–5
Cyclopentane 287–92–3
2-methylpentane 107–83–5
3-methylpentane 96–14–0
methylcyclopentane 96–37–7
2,2-dimethylpentane 590–35–2
2,3-dimethylbutane 79–29–8
Trans-Pentadiene 2004–70–8
Cyclohexane 110–82–7
Methylcyclohexane 108–87–2
1,1-Dimethylcyclohexane 590–66–9
© ISO 2015 – All rights reserved 5

---------------------- Page: 17 ----------------------

SIST EN ISO 16558-1:2015
ISO 16558-1:2015(E)

The detector responses of these selected compounds are measured by headspace gas chromatography
with a mass spectrometric detector (electron ionization with selected ion monitoring of mass fragments
m/z 41+43+55+56+57+69+70+71 for olefenic, alicyclic branched, and paraffinic short hydrocarbons),
...