SIST-TS CEN ISO/TS 16558-2:2015

Soil quality - Risk-based petroleum hydrocarbons - Part 2: Determination of aliphatic and aromatic fractions of semi-volatile petroleum hydrocarbons using gas chromatography with flame ionisation detection (GC/FID) (ISO/TS 16558-2:2015)

This part of ISO xxxxx specifies a method for the quantitative determination of the total extractable semivolatile, the semi-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 C10 to C40 as well as the aromatic fraction C10 to C40. For sub-fractions lower limits of determination can be reached. With this method all hydrocarbons with a boiling range of 174 °C to 525 °C, n-alkanes between C10H22 to C40H82, isoalkanes, cycloalkanes, alkyl benzenes, and alkyl naphthalenes and polycyclic aromatic compounds are determined as total extractable semi-volatile petroleum hydrocarbons C10 to C40; besides that semi-volatile aliphatic and aromatic fractions are specified.

Bodenbeschaffenheit - Mineralölkohlenwasserstoffe für die Risikobeurteilung - Teil 2: Bestimmung aliphatischer und aromatischer Fraktionen schwerflüchtiger Mineralölkohlenwasserstoffe mittels Gaschromatographie mit Flammenionisationsdetektion (GC/FID) (ISO/TS 16558-2:2015)

Dieser Teil von ISO 16558 legt ein Verfahren zur quantitative Bestimmung des Gesamtgehalts an extrahierbaren schwach flüchtigen, an schwerflüchtigen aliphatischen und aromatischen Fraktionen des Mineralölkohlenwasserstoffs (Petroleum-Kohlenwasserstoff) in feldfrischen Bodenproben mittels Gaschromatographie fest.
Die Ergebnisse der durchgeführten Prüfung können für die Studien zur Risikobeurteilung hinsichtlich der Kontaminationen mit Mineralölkohlenwasserstoffen angewendet werden.
Das Verfahren ist für Mineralölkohlenwasserstoff-Gehalte von etwa 100 mg/kg Boden, angegeben als Trockensubstanz für die gesamte aliphatische Fraktion C10 bis C40 sowie für die aromatische Fraktion von C10 bis C40 geeignet. Bei Teilfraktionen können niedrigere Bestimmungsgrenzen erreicht werden.
Werden geringere Nachweisgrenzen gefordert, kann ein großes Injektionsvolumen verwendet oder die Konzentration des Endextraktes kann vorgenommen werden.
ANMERKUNG   Niedrige Konzentrationen von aliphatischen und aromatischen Fraktionen können in natürlichen nicht kontaminierten organischen Böden, beispielsweise Torfböden, gefunden werden.
Mit diesem Verfahren werden alle Kohlenwasserstoffe mit einem Siedebereich von 174 °C bis 525 °C, n Alkane zwischen C10H22 bis C40H82, Isoalkane, Cycloalkane, Alkylbenzole, Alkylnaphtaline und poly-cyclische aromatische Verbindungen als gesamte extrahierbare schwerflüchtige Mineralölkohlenwasser¬stoffe C10 bis C40 bestimmt. Darüber hinaus werden schwerflüchtige aliphatische und aromatische Fraktionen festgelegt.
Hinsichtlich der Bestimmung flüchtiger aliphatischer und aromatischer Fraktionen von Mineralölkohlen-wasserstoffen in Bodenproben siehe Teil 1 dieser Internationalen Norm.
Die in diesem Teil von ISO 16558 vorgeschlagenen Teilfraktionen haben gezeigt, dass sie für Studien zur Risikobeurteilung geeignet sind. Allerdings können weiterer Teilfraktionen zwischen C10H22 bis C40H82 in Übereinstimmung mit dieser Norm ebenfalls bestimmt werden.
Auf der Grundlage der Peakfolge des Gaschromatogramms und der Siedepunkte der einzelnen im Anhang B 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 2: Détermination des fractions aliphatiques et aromatiques des hydrocarbures de pétrole semi-volatiles par chromatographie en phase gazeuse avec détection d'ionisation de la flamme ((ISO/TS 16558-2:2015)

ISO/TS 16558-2:2015 spécifie une méthode de dosage quantitatif des fractions aliphatiques et aromatiques semi-volatiles extractibles totales des hydrocarbures de pétrole dans des échantillons humides par chromatographie en phase gazeuse.
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/TS 16558-2:2015 propose une méthode applicable à des teneurs en hydrocarbures de pétrole d'environ 100 mg/kg de sol, exprimés sous forme de matière sèche pour la fraction aliphatique C10 à C40 totale ainsi que pour la fraction aromatique C10 à C40. Pour les sous-fractions, des limites de dosage moins élevées peuvent être atteintes.
Si des limites de détection moins élevées sont requises, un plus grand volume d'injection peut être utilisé ou une concentration de l'extrait final peut être effectuée.
NOTE 1       De faibles concentrations en composés aliphatiques et aromatiques peuvent être présentes dans les sols naturels non contaminés riches en matière organique tels que la tourbe.

Kakovost tal - Naftni ogljikovodiki, ki predstavljajo tveganje - 2. del: Določevanje alifatskih in aromatskih frakcij polhlapnih naftnih ogljikovodikov s plinsko kromatografijo s plamensko ionizacijsko detekcijo (GC/FID) (ISO/TS 16558-2:2015)

Ta del standarda ISO 16558-2 določa metodo za količinsko določevanje skupnih polhlapnih snovi, ki jih je mogoče ekstrahirati, polhlapnih 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 C10 do C40 in aromatsko frakcijo C10 do C40. Za podfrakcije je mogoče doseči nižje mejne vrednosti določevanja. S to metodo so vsi ogljikovodiki z območjem vrelišča 174 °C do 525 °C, n-alkani med C10H22 in C40H82, izoalkani, cikloalkani, alkilni benzeni in alkilni naftaleni ter policiklične aromatske spojine določeni kot skupni polhlapni naftni ogljikovodiki C10 do C40, ki jih je mogoče ekstrahirati; poleg tega se določijo polhlapne alifatske in aromatske frakcije.

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: CEN ISO/TS 16558-2:2015 - Soil quality - Risk-based petroleum hydrocarbons - Part 2: Determination of aliphatic and aromatic fractions of semi-volatile petroleum hydrocarbons using gas chromatography with flame ionization detection (GC/FID) (ISO/TS 16558-2:2015)

Standards Content (Sample)

SLOVENSKI STANDARD
SIST-TS CEN ISO/TS 16558-2:2015
01-november-2015
.DNRYRVWWDO1DIWQLRJOMLNRYRGLNLNLSUHGVWDYOMDMRWYHJDQMHGHO'RORþHYDQMH
DOLIDWVNLKLQDURPDWVNLKIUDNFLMSROKODSQLKQDIWQLKRJOMLNRYRGLNRYVSOLQVNR
NURPDWRJUDILMRVSODPHQVNRLRQL]DFLMVNRGHWHNFLMR*&),',6276
Soil quality - Risk-based petroleum hydrocarbons - Part 2: Determination of aliphatic and
aromatic fractions of semi-volatile petroleum hydrocarbons using gas chromatography
with flame ionisation detection (GC/FID) (ISO/TS 16558-2:2015)
Bodenbeschaffenheit - Mineralölkohlenwasserstoffe für die Risikobeurteilung - Teil 2:
Bestimmung aliphatischer und aromatischer Fraktionen schwerflüchtiger
Mineralölkohlenwasserstoffe mittels Gaschromatographie mit
Flammenionisationsdetektion (GC/FID) (ISO/TS 16558-2:2015)
Qualité du sol - Hydrocarbures de pétrole à risque - Partie 2: Détermination des fractions
aliphatiques et aromatiques des hydrocarbures de pétrole semi-volatiles par
chromatographie en phase gazeuse avec détection d'ionisation de la flamme ((ISO/TS
16558-2:2015)
Ta slovenski standard je istoveten z: CEN ISO/TS 16558-2:2015
ICS:
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
SIST-TS CEN ISO/TS 16558-2:2015 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN ISO/TS 16558-2:2015


CEN ISO/TS 16558-2
TECHNICAL SPECIFICATION

SPÉCIFICATION TECHNIQUE

September 2015
TECHNISCHE SPEZIFIKATION
ICS 13.080.10
English Version

Soil quality - Risk-based petroleum hydrocarbons - Part 2:
Determination of aliphatic and aromatic fractions of semi-
volatile petroleum hydrocarbons using gas
chromatography with flame ionization detection (GC/FID)
(ISO/TS 16558-2:2015)
Qualité du sol - Hydrocarbures de pétrole à risque - Bodenbeschaffenheit - Mineralölkohlenwasserstoffe
Partie 2: Détermination des fractions aliphatiques et für die Risikobeurteilung - Teil 2: Teil 2: Bestimmung
aromatiques des hydrocarbures de pétrole semi- aliphatischer und aromatischer Fraktionen
volatiles par chromatographie en phase gazeuse avec schwerflüchtiger Mineralölkohlenwasserstoffe mittels
détection d'ionisation de la flamme (ISO/TS 16558- Gaschromatographie mit Flammenionisationsdetektion
2:2015) (GC/FID) (ISO/TS 16558-2:2015)
This Technical Specification (CEN/TS) was approved by CEN on 13 July 2015 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to
submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS
available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in
parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.

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. CEN ISO/TS 16558-2:2015 E
worldwide for CEN national Members.

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CEN ISO/TS 16558-2:2015 (E)
Contents Page
European foreword . 3

2

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CEN ISO/TS 16558-2:2015 (E)
European foreword
This document (CEN ISO/TS 16558-2:2015) 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.
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 announce this Technical Specification: 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/TS 16558-2:2015 has been approved by CEN as CEN ISO/TS 16558-2:2015 without any
modification.
3

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SIST-TS CEN ISO/TS 16558-2:2015
TECHNICAL ISO/TS
SPECIFICATION 16558-2
First edition
2015-08-15
Soil quality — Risk-based petroleum
hydrocarbons —
Part 2:
Determination of aliphatic and
aromatic fractions of semi-volatile
petroleum hydrocarbons using gas
chromatography with flame ionization
detection (GC/FID)
Qualité du sol — Hydrocarbures de pétrole à risque —
Partie 2: Détermination des fractions aliphatiques et aromatiques
des hydrocarbures de pétrole semi-volatiles par chromatographie en
phase gazeuse avec détection à ionisation de la flamme (CPG-FID)
Reference number
ISO/TS 16558-2:2015(E)
©
ISO 2015

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ISO/TS 16558-2:2015(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

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ISO/TS 16558-2:2015(E)

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Interferences . 2
5 Principle . 2
6 Reagents . 3
7 Apparatus . 4
8 Sampling, sample conservation, and pretreatment . 5
9 Procedure. 5
9.1 Blank . 5
9.2 Extraction . 6
9.2.1 Total petroleum hydrocarbons . 6
9.2.2 Split into aliphatic and aromatic fractions . 6
9.3 Determination by gas chromatography . 7
9.3.1 Test of the performance of the gas chromatographic system . 7
9.3.2 Repeatability test . 7
9.3.3 Calibration . 7
9.3.4 Validity check of the calibration function . 7
9.3.5 Measurement . 7
9.3.6 Integration . 7
9.3.7 Calculation of the total petroleum hydrocarbons. 9
9.3.8 Calculation of the individual extractable fractions . 9
9.4 Quality control . 9
9.4.1 Suitability check of the split procedure . 9
10 Expression of results .10
11 Test report .10
Annex A (informative) Examples of gas chromatograms of total extractable petroleum
hydrocarbon and aliphatic and aromatic fractions in a standard solution and in
soil samples .11
Annex B (informative) Determination of the boiling range of mineral oil hydrocarbons from
the gas chromatogram .14
Annex C (informative) Information on split of aliphatic and aromatic fractions using silicagel .16
Bibliography .20
© ISO 2015 – All rights reserved iii

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ISO/TS 16558-2:2015(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

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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 in this part of ISO 16558 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 ISO 16558 are given in Figure 1.
Key
b
a 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 is not to 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 part of ISO 16558 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

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SIST-TS CEN ISO/TS 16558-2:2015
TECHNICAL SPECIFICATION ISO/TS 16558-2:2015(E)
Soil quality — Risk-based petroleum hydrocarbons —
Part 2:
Determination of aliphatic and aromatic fractions
of semi-volatile petroleum hydrocarbons using gas
chromatography with flame ionization detection (GC/FID)
1 Scope
This part of ISO 16558 specifies a method for the quantitative determination of the total extractable
semi-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.
This part of ISO 16558 provides a method applicable to petroleum hydrocarbon contents from about
100 mg/kg soil expressed as dry matter for the whole aliphatic fraction C to C as well as the
10 40,
aromatic fraction C to C . For sub-fractions, lower limits of determination can be reached.
10 40
If lower detection limits are required, large volume injection can be used or concentration of the final
extract can be carried out.
NOTE 1 Low concentrations of aliphatic and aromatic compounds can be found in natural uncontaminated
organic rich soils like peat soils.
With this method, all hydrocarbons with a boiling range of 174 °C to 525 °C, n-alkanes between C H
10 22
to C H , isoalkanes, cycloalkanes, alkyl benzenes, and alkyl naphthalenes and polycyclic aromatic
40 82
compounds are determined as total extractable semi-volatile petroleum hydrocarbons C to C ;
10 40
besides that, semi-volatile aliphatic and aromatic fractions are specified.
For the determination of volatile aliphatic and aromatic fractions of petroleum hydrocarbons in soil
samples, see ISO 16558-1.
NOTE 2 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 also be determined in conformity with this
10 22 40 82
part 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 B, 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 2015 – All rights reserved 1

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ISO 11465, Soil quality — Determination of dry matter and water content on a mass basis —
Gravimetric method
ISO 14507, Soil quality — Pretreatment of samples for determination of organic contaminants
ISO 16703, Soil quality — Determination of content of hydrocarbon in the range C10 to C40 by gas
chromatography
ISO 18512, Soil quality — Guidance on long and short term storage of soil samples
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
total extractable semi-volatile petroleum hydrocarbon content by gas chromatography
sum of compounds extractable with acetone/n-heptane (2+1) that can be detected with a flame
ionization detector and chromatographed on a non-polar capillary column with retention times
between those of n-decane (C H ) and n-tetracontane (C H )
10 22 40 82
Note 1 to entry: Substances that comply with that definition are mainly long chain or branched aliphatic, alicyclic,
lower polycyclic, or alkyl substituted aromatic hydrocarbons.
3.2
semi-volatile aliphatic fraction of petroleum hydrocarbons
fraction of the total semi-volatile petroleum hydrocarbons which are eluted with pentane, hexane, or
heptane after adsorption on silicagel
Note 1 to entry: This is a method defined in this part of ISO 16558. It is unknown and unpredictable if the same
compounds will elute from the silicagel with other solvents.
3.3
semi-volatile aromatic fraction of petroleum hydrocarbons
fraction of the total semi-volatile petroleum hydrocarbons which are eluted with dichloromethane or
with a 1:1 mixture of dichloromethane and n-heptane after adsorption on silicagel
Note 1 to entry: This is a method defined in this part of ISO 16558. It is unknown and unpredictable if the same
compounds will elute from the silicagel with other solvents.
4 Interferences
Compounds not related to petroleum hydrocarbon contaminations with a boiling point between C
10
and C (e.g. halogenated hydrocarbons) might interfere with the determination.
40
5 Principle
A known amount of the homogenized soil sample is extracted by mechanical shaking or sonication
with acetone/n-heptane. The organic layer is separated and washed twice with water. An aliquot of the
extract is analysed by capillary gas chromatography with flame ionization detection. The total peak
area between the range defining standards n-decane and n-tetracontane is measured as the amount of
total extractable semi-volatile petroleum. The extract is split into two fractions containing, respectively,
the aliphatic and aromatic hydrocarbons using a column containing silicagel. The fractions are also
analysed by gas chromatography.
Instead of n-heptane, another single hydrocarbon solvent or technical mixture of hydrocarbons, boiling
range 36 °C to 99 °C, can be used.
2 © ISO 2015 – All rights reserved

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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.
1)
6.1 Acetone, (CH ) CO (CAS-RN 67-64-1).
3 2
6.2 n-Heptane, C H (CAS-RN 142-82-5).
7 16
Instead of n-heptane, another single hydrocarbon solvent or technical mixture of hydrocarbons, boiling
range 36 °C to 99 °C, may be used.
6.3 Dichloromethane, CH Cl (CAS-RN 75-09-2).
2 2
6.4 Silicagel, particle size 63 µm to 200 µm (70 mesh to 230 mesh) heated for at least 16 h at 140 °C
and stored in a desiccator over a molecular sieve.
6.5 Anhydrous sodium sulfate, Na SO , heated for at least 2 h at 550 °C.
2 4
6.6 Retention time window (RTW) standard solution, is the range defining standard solution
containing n-tetracontane and n-decane.
Weigh (30 ± 1) mg of n-tetracontane into a 1 l volumetric flask, dissolve completely in an appropriate
volume of n-heptane (6.2), add 30 µl of n-decane (about 21 mg), mix well, fill up to volume with n-heptane
and homogenize. This solution shall be used for all dilution steps of the hydrocarbon standard (6.7) and
be stored at room temperature.
NOTE n-tetracontane is only moderately soluble in n-heptane. Slight warming and/or sonication accelerates
the dissolution process.
6.7 Hydrocarbon standard solution for calibration.
Mix approximately equal masses of two different types of mineral oil. Weigh accurately this mixture
and dissolve in the RTW standard solution (6.6) to give a hydrocarbon content of about 8 g/l.
Preparation of the calibration solutions can be done by diluting an aliquot of this standard solution
(6.7) with the internal standard solution (6.6).
The first oil type should show discrete peaks (e.g. a diesel fuel) in the gas chromatogram, as can be seen
in Figure A.1 (left part of the chromatogram). The second type should have a boiling range higher than
the first one and should show a hump in the gas chromatogram, as can be seen in Figure A.1 (right part
of the chromatogram). A suitable oil of this type is, for example, a lubricating oil without any additives.
NOTE General purpose hydrocarbon standards for calibration can be obtained from many commercial
organizations. Calibration standards specific to this part of ISO 16558 can be purchased e.g. from Bundesanstalt
für Materialforschung und -prüfung, Fachgruppe I.2, Richard-Willstätter-Strasse 11 D-12489 Berlin, Germany,
or VSL BV, Thijsseweg 11, 2600 Delft, Netherlands (product RIVM-NMi-001). This information is given for the
convenience of users of this part of ISO 16558 and does not constitute an endorsement by ISO of this product.
6.8 Control solution.
Prepare an independent control solution according to 6.7 with a hydrocarbon concentration of about in
the middle of the working range System performance standard solution.
1) CAS-RN: Chemical Abstracts Service Registry Number.
© ISO 2015 – All rights reserved 3

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ISO/TS 16558-2:2015(E)

6.9 Retention time standard solution.
Prepare a mixture of equal amounts, on a mass basis, of the n-alkanes with carbon numbers from C
10
to C , dissolved in n-heptane (6.2), to give concentrations of about 50 mg/l of each n-alkane. Store at
40
room temperature.
NOTE 1 This solution is also used to verify the suitability of the gas chromatographic system for the resolution
of n-alkanes, as well as for the detector response.
NOTE 2 This solution is used to give information of the retention times of the n-alkanes to characterize the
hydrocarbons in the samples.
6.10 Preparation of the silicagel column.
Push a plug of pre-washed glass wool or a PTFE frit down into the column (7.10). Add successively 3 g of
silicagel (6.4) and 2 g sodium sulfate (6.5). Prepare the column immediately before use.
NOTE Commercially available cartridges are also applicable.
6.11 Control solution silicagel column efficiency.
6.11.1 Control solution aliphatic split.
Prepare a mixture of equal amounts, on a mass basis, of the n-alkanes with carbon numbers from C
10
to C , dissolved in n-heptane (6.2), to give concentrations of about 50 mg/l of each n-alkane. Store at
40
room temperature.
6.11.2 Control solution aromatic split.
Prepare a mixture of equal amounts, on a mass basis, polycyclic aromatic hydrocarbons containing
16 PAH according to EPA in n-heptane (6.2), to give mass concentrations of about 50 mg/l of each
compound. Store at room temperature.
7 Apparatus
7.1 Usual laboratory glassware, which shall be heated 2 h in an oven at 200 °C to 300 °C and after
cooling, rinsed with acetone (6.1) and dried before use.
The cleaning procedure of the glassware can be replaced by any method if it shows (e.g. by blank
samples) that the glassware does not give a positive contribution to the concentration of the compounds
of interest in this part of ISO 16558.
7.2 Devices for extraction.
Mechanical shaker, horizontal movement, at least 120 shaking movements per minute. Alternatively, an
ultrasonic bath can be used.
7.3 Laboratory centrifuge, capable of producing an acceleration of at least 1 500 g.
7.4 Gas chromatograph, equipped with a non-discriminating injection system (preferably on-column
or programmable temperature vaporization injection-PTV), a capillary column, and a flame ionization
detector (FID).
NOTE The use of a large volume injection system can improve the limit of detection considerably.
7.5 Capillary column, a fused silica capillary column with one of the following stationary phases
and dimensions:
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SIST-TS CEN ISO/TS 16558-2:2015
ISO/TS 16558-2:2015(E)

— stationary phase: non-polar, e.g. immobilized 100 % dimethyl polysiloxane,
95 %-dimethyl-5 %-diphenyl polysiloxane, modified siloxane polymer;
— length: 10 m to 25 m;
— internal diameter: 0,1 mm to 0,32 mm;
— film th
...