SIST EN ISO 22854:2021
(Main)Liquid petroleum products - Determination of hydrocarbon types and oxygenates in automotive-motor gasoline and in ethanol (E85) automotive fuel - Multidimensional gas chromatography method (ISO 22854:2021)
Liquid petroleum products - Determination of hydrocarbon types and oxygenates in automotive-motor gasoline and in ethanol (E85) automotive fuel - Multidimensional gas chromatography method (ISO 22854:2021)
This document specifies the gas chromatographic (GC) method for the determination of saturated,
olefinic and aromatic hydrocarbons in automotive motor gasoline and ethanol (E85) automotive fuel.
Additionally, the benzene and toluene content, oxygenated compounds and the total oxygen content can
be determined.
NOTE 1 For the purposes of this document, the terms % (m/m) and % (V/V) are used to represent respectively
the mass fraction, w, and the volume fraction, φ.
This document defines two procedures, A and B.
Procedure A is applicable to automotive motor gasoline with total aromatics of 19,32 % (V/V) up to
46,29 % (V/V); total olefins from 0,40 % (V/V) up to 26,85 % (V/V); oxygenates from 0,61 % (V/V) up to
9,85 % (V/V); oxygen content from 1,50 % (m/m) to 12,32 % (m/m); benzene content from 0,38 % (V/V)
up to 1,98 % (V/V) and toluene content from 5,85 % (V/V) up to 31,65 % (V/V).
The method has also been tested for individual oxygenates. A precision has been determined for
a total volume of methanol from 1,05 % (V/V) up to 16,96 % (V/V); a total volume of ethanol from
0,50 % (V/V) up to 17,86 % (V/V); a total volume of MTBE from 0,99 % (V/V) up to 15,70 % (V/V), a total
volume of ETBE from 0,99 % (V/V) up to 15,49 % (V/V), a total volume of TAME from 0,99 % (V/V) up to
5,92 % (V/V), and a total volume of TAEE from 0,98 % (V/V) up to 15,59 % (V/V).
Although this test method can be used to determine higher-olefin contents of up to 50 % (V/V), the
precision for olefins was tested only in the range from 0,40 % (V/V) to 26,85 % (V/V).
Although specifically developed for the analysis of automotive motor gasoline that contains oxygenates,
this test method can also be applied to other hydrocarbon streams having similar boiling ranges, such
as naphthas and reformates.
NOTE 2 For Procedure A, applicability of this document has also been verified for the determination of
n-propanol, acetone, and di-isopropyl ether (DIPE). However, no precision data have been determined for these
compounds.
Procedure B describes the analysis of oxygenated groups (ethanol, methanol, ethers, C3 – C5 alcohols)
in ethanol (E85) automotive fuel containing ethanol between 50 % (V/V) and 85 % (V/V). The gasoline
is diluted with an oxygenate-free component to lower the ethanol content to a value below 20 % (V/V)
before the analysis by GC.
The sample can be fully analysed including hydrocarbons. Precision data for the diluted sample are
only available for the oxygenated groups.
NOTE 3 For Procedure B, the precision can be used for an ethanol fraction from about 50 % up to 85 % (V/V).
For the ether fraction, the precision as specified in Table 6 can be used for samples containing at least 11 % (V/V)
of ethers. For the higher alcohol fraction, too few data were obtained to derive a full precision statement and the
data presented in Table 6 are therefore only indicative.
NOTE 4 An overlap between C9 and C10 aromatics can occur. However, the total is accurate. Isopropyl benzene
is resolved from the C8 aromatics and is included with the other C9 aromatics.
Flüssige Mineralölerzeugnisse - Bestimmung der Kohlenwasserstoffgruppen und der sauerstoffhaltigen Verbindungen in Ottokraftstoffen und in Ethanolkraftstoff (E85) - Multidimensionales gaschromatographisches Verfahren (ISO 22854:2021)
Dieses Dokument legt ein Verfahren zur gaschromatographischen Bestimmung (GC) von gesättigten, olefinischen und aromatischen Kohlenwasserstoffen in Ottokraftstoffen und Ethanolkraftstoff (E85) fest. Zusätzlich können die Gehalte an Benzol und Toluol, sauerstoffhaltigen Verbindungen sowie der Gesamt-sauerstoffgehalt bestimmt werden.
ANMERKUNG 1 Für die Zwecke dieses Dokuments wird zur Angabe des Massenanteils, w, einer Substanz der Ausdruck „% (m/m)“ und für den Volumenanteil, φ, einer Substanz der Ausdruck „% (V/V)“ verwendet.
Dieses Dokument definiert zwei Verfahren, A und B.
Verfahren A ist anwendbar für Ottokraftstoffe mit einem Gesamtaromatenanteil von 19,32 % (V/V) bis zu 46,29 % (V/V), einem Gesamtolefinanteil von 0,40 % (V/V) bis zu 26,85 % (V/V), einem Anteil an sauerstoff-haltigen Verbindungen von 0,61 % (V/V) bis zu 9,85 % (V/V), einem Sauerstoffgehalt von 1,50 % (m/m) bis 12,32 % (m/m), einem Benzolgehalt von 0,38 % (V/V) bis zu 1,98 % (V/V) und einem Toluolgehalt von 5,85 % (V/V) bis zu 31,65 % (V/V).
Das Verfahren wurde auch für einzelne sauerstoffhaltige Verbindungen geprüft. Die Präzision wurde bestimmt für ein Gesamtvolumen an Methanol von 1,05 % (V/V) bis zu 16,96 % (V/V), ein Gesamtvolumen an Ethanol von 0,50 % (V/V) bis zu 17,86 % (V/V), ein Gesamtvolumen an MTBE von 0,99 % (V/V) bis zu 15,70 % (V/V), ein Gesamtvolumen an ETBE von 0,99 % (V/V) bis zu 15,49 % (V/V), ein Gesamtvolumen an TAME von 0,99 % (V/V) bis zu 5,92 % (V/V) und ein Gesamtvolumen an TAEE von 0,98 % (V/V) bis zu 15,59 % (V/V).
Obwohl dieses Prüfverfahren zur Bestimmung höherer Olefingehalte bis zu 50 % (V/V) angewendet werden kann, wurde die Präzision für Olefine nur im Bereich von 0,40 % (V/V) bis 26,85 % (V/V) ermittelt.
Obwohl dieses Verfahren speziell für die Analyse von Ottokraftstoffen mit sauerstoffhaltigen Verbindungen entwickelt wurde, kann es auch auf andere Kohlenwasserstoffe mit ähnlichen Siedebereichen, wie z. B. Naphthas und Reformate, angewendet werden.
ANMERKUNG 2 Für Verfahren A wurde die Anwendbarkeit dieses Dokuments auch für die Bestimmung von n-Propanol, Aceton und Diisopropylether (DIPE) überprüft. Es wurden jedoch für diese Verbindungen keine Präzisionsdaten bestimmt.
Verfahren B beschreibt die Analyse von sauerstoffhaltigen Verbindungen (Ethanol, Methanol, Ether, C3- bis C5-Alkohole) in Ethanolkraftstoffen (E85) mit einem Ethanolgehalt zwischen 50 % (V/V) und 85 % (V/V). Das Benzin wird mit einer sauerstofffreien Komponente verdünnt, um den Ethanolgehalt vor der GC-Analyse auf einen Wert unter 20 % (V/V) zu senken.
Die Probe kann einschließlich der Kohlenwasserstoffe vollständig analysiert werden. Präzisionsdaten für die verdünnte Probe sind nur für die Gruppe der Sauerstoffverbindungen vorhanden.
ANMERKUNG 3 Für Verfahren B kann die Präzision für einen Ethanolanteil von etwa 50 % (V/V) bis zu 85 % (V/V) verwendet werden. Für den Ethergehalt können die Präzisionsangaben in Tabelle 6 für Proben verwendet werden, deren Ethergehalt bei mindestens 11 % (V/V) liegt. Für höhere Alkoholgehalte wurden zu wenige Daten erhalten, um eine vollständige Präzisionsangabe abzuleiten; in diesem Fall sind die Werte in Tabelle 6 nur als informativ anzusehen.
ANMERKUNG 4 Es kann eine Überlappung zwischen C9- und C10-Aromaten auftreten. Das Gesamtergebnis ist jedoch korrekt. Isopropylbenzol wird von den C8-Aromaten abgetrennt und mit den anderen C9-Aromaten erfasst.
Produits pétroliers liquides - Détermination des groupes d'hydrocarbures et de la teneur en composés oxygénés de l'essence pour moteurs automobiles et du carburant éthanol pour automobiles E85 - Méthode par chromatographie multidimensionnelle en phase gazeuse (ISO 22854:2021)
Le présent document prescrit une méthode pour la détermination par chromatographie en phase gazeuse (CPG) des teneurs en hydrocarbures saturés, oléfiniques et aromatiques dans les essences pour moteurs automobiles et dans les carburants éthanol pour automobiles (E85). En outre, les teneurs en benzène, en composés oxygénés et en oxygène total peuvent être mesurées par cette méthode.
NOTE 1 Pour les besoins du présent document, les termes % (m/m) et % (V/V) sont utilisés pour représenter respectivement la fraction massique, w, et la fraction volumique, φ, d’un produit.
Le présent document définit deux modes opératoires, A et B.
Le mode opératoire A est applicable aux essences pour moteurs automobiles ayant une teneur en aromatiques totaux de 19,32 % (V/V) jusqu’à 46,29 % (V/V), une teneur en oléfines totales de 0,40 % (V/V) jusqu’à 26,85 % (V/V), une teneur en composés oxygénés de 0,61 % (V/V) jusqu’à 9,85 % (V/V), une teneur en oxygène total de 1,50 % (m/m) jusqu’à 12,32 % (m/m), une teneur en benzène de 0,38 % (V/V) jusqu’à 1,98 % (V/V) et une teneur en toluène de 5,85 % (V/V) jusqu’à 31,65 % (V/V).
La méthode a également été testée pour des composés oxygénés individuels. Des données de fidélité ont été déterminées pour un volume total de méthanol de 1,05 % (V/V) à 16,96 % (V/V); un volume total d'éthanol de 0,50 % (V/V) à 17,86 % (V/V); un volume total de MTBE de 0,99 % (V/V) à 15,70 % (V/V), un volume total d'ETBE de 0,99 % (V/V) à 15,49 % (V/V), un volume total de TAME de 0,99 % (V/V) à 5,92 % (V/V), et un volume total de TAEE de 0,98 % (V/V) à 15,59 %(V/V).
Bien que cette méthode d’essai puisse être utilisée pour déterminer des teneurs en oléfines plus élevées, jusqu’à 50 % (V/V), la fidélité pour les oléfines n’a été établie que pour des teneurs comprises entre 0,40 % (V/V) et 26,85 % (V/V).
Bien que cette méthode ait été développée pour l’analyse d’essences pour moteurs automobiles qui contiennent des oxygénés, celle-ci peut aussi être appliquée à d’autres bases hydrocarbonées dont l’intervalle d’ébullition est voisin, tels que les naphtas et les réformats.
NOTE 2 Pour le mode opératoire A du présent document, l’applicabilité a été vérifiée pour le dosage du n-propanol, de l’acétone et du di-isopropyl éther (DIPE). Cependant, la fidélité n’a pas été déterminée pour ces composés.
Le mode opératoire B décrit l’analyse des groupes oxygénés (éthanol, méthanol, éthers et alcools C3‑C5) dans des carburants éthanol pour automobiles (E85) contenant de l’éthanol entre 50 % (V/V) et 85 % (V/V). L’essence est diluée avec un composant non oxygéné pour abaisser la teneur en éthanol à une valeur inférieure à 20 % (V/V) avant l’analyse par chromatographie en phase gazeuse (CPG).
L’échantillon peut être totalement analysé y compris les familles d’hydrocarbures. Les valeurs de fidélité pour les échantillons dilués ne sont disponibles que pour les groupes oxygénés.
NOTE 3 Pour le mode opératoire B, les valeurs de fidélité peuvent être utilisées pour une fraction d’éthanol d’environ 50 % (V/V) jusqu’à 85 % (V/V). Pour la fraction éther, la fidélité telle que spécifiée dans le Tableau 6 peut être utilisée pour des échantillons contenant au moins 11 % (V/V) d’éthers. Pour la fraction des alcools supérieurs, trop peu de données ont été recueillies pour établir véritablement des valeurs de fidélité, ainsi les valeurs présentées dans le Tableau 6 ne sont-elles données qu’à titre indicatif.
NOTE 4 Il peut y avoir un chevauchement e
Tekoči naftni proizvodi - Določevanje vrste ogljikovodikov in oksigenatov v motornem bencinu in bencinu na osnovi etanola (E85) - Metoda multidimenzionalne plinske kromatografije (ISO 22854:2021)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 22854:2021
01-oktober-2021
Nadomešča:
SIST EN ISO 22854:2016
Tekoči naftni proizvodi - Določevanje vrste ogljikovodikov in oksigenatov v
motornem bencinu in bencinu na osnovi etanola (E85) - Metoda
multidimenzionalne plinske kromatografije (ISO 22854:2021)
Liquid petroleum products - Determination of hydrocarbon types and oxygenates in
automotive-motor gasoline and in ethanol (E85) automotive fuel - Multidimensional gas
chromatography method (ISO 22854:2021)
Flüssige Mineralölerzeugnisse - Bestimmung der Kohlenwasserstoffgruppen und der
sauerstoffhaltigen Verbindungen in Ottokraftstoffen und in Ethanolkraftstoff (E85) -
Multidimensionales gaschromatographisches Verfahren (ISO 22854:2021)
Produits pétroliers liquides - Détermination des groupes d'hydrocarbures et de la teneur
en composés oxygénés de l'essence pour moteurs automobiles et du carburant éthanol
pour automobiles E85 - Méthode par chromatographie multidimensionnelle en phase
gazeuse (ISO 22854:2021)
Ta slovenski standard je istoveten z: EN ISO 22854:2021
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
75.160.20 Tekoča goriva Liquid fuels
SIST EN ISO 22854:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 22854:2021
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SIST EN ISO 22854:2021
EN ISO 22854
EUROPEAN STANDARD
NORME EUROPÉENNE
August 2021
EUROPÄISCHE NORM
ICS 75.080 Supersedes EN ISO 22854:2016
English Version
Liquid petroleum products - Determination of
hydrocarbon types and oxygenates in automotive-motor
gasoline and in ethanol (E85) automotive fuel -
Multidimensional gas chromatography method (ISO
22854:2021)
Produits pétroliers liquides - Détermination des Flüssige Mineralölerzeugnisse - Bestimmung der
groupes d'hydrocarbures et de la teneur en composés Kohlenwasserstoffgruppen und der sauerstoffhaltigen
oxygénés de l'essence pour moteurs automobiles et du Verbindungen in Ottokraftstoffen und in
carburant éthanol pour automobiles E85 - Méthode par Ethanolkraftstoff (E85) - Multidimensionales
chromatographie multidimensionnelle en phase gaschromatographisches Verfahren (ISO 22854:2021)
gazeuse (ISO 22854:2021)
This European Standard was approved by CEN on 18 July 2021.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, 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: Rue de la Science 23, B-1040 Brussels
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 22854:2021 E
worldwide for CEN national Members.
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SIST EN ISO 22854:2021
EN ISO 22854:2021 (E)
Contents Page
European foreword . 3
2
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SIST EN ISO 22854:2021
EN ISO 22854:2021 (E)
European foreword
This document (EN ISO 22854:2021) has been prepared by Technical Committee ISO/TC 28 "Petroleum
and related products, fuels and lubricants from natural or synthetic sources" in collaboration with
Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of
petroleum, synthetic and biological origin.” 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 February 2022, and conflicting national standards
shall be withdrawn at the latest by February 2022.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN ISO 22854:2016.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN websites.
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, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
Endorsement notice
The text of ISO 22854:2021 has been approved by CEN as EN ISO 22854:2021 without any modification.
3
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SIST EN ISO 22854:2021
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SIST EN ISO 22854:2021
INTERNATIONAL ISO
STANDARD 22854
Fourth edition
2021-07
Liquid petroleum products —
Determination of hydrocarbon
types and oxygenates in automotive-
motor gasoline and in ethanol (E85)
automotive fuel — Multidimensional
gas chromatography method
Produits pétroliers liquides — Détermination des groupes
d'hydrocarbures et de la teneur en composés oxygénés de l'essence
pour moteurs automobiles et du carburant éthanol pour automobiles
E85 — Méthode par chromatographie multidimensionnelle en phase
gazeuse
Reference number
ISO 22854:2021(E)
©
ISO 2021
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SIST EN ISO 22854:2021
ISO 22854:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021
All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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
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below or ISO’s member body in the country of the requester.
ISO copyright office
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Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2021 – All rights reserved
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SIST EN ISO 22854:2021
ISO 22854:2021(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 2
3 Terms and definitions . 2
4 Principle . 3
5 Reagents and materials . 3
6 Apparatus . 4
7 Sampling . 5
8 Procedure. 5
8.1 Conditioning . 5
8.2 Sample preparation . 5
8.2.1 Procedure B only — Sample dilution . 5
8.2.2 Procedure A and B — Sample cooling . 5
8.3 Test sample injection volume . 5
8.4 V erification of the apparatus and test conditions . 5
8.5 Validation . 5
8.6 Preparation of the test sample . 6
8.7 Preparation of the apparatus and test conditions . 6
9 Calculation . 6
9.1 General . 6
9.2 Calculation as % (m/m) . 6
9.3 Calculation as % (V/V) . 7
9.4 Calculation of total oxygen content in % (m/m) . 9
9.5 Data report according to automotive motor gasoline specification . 9
10 Expression of results . 9
10.1 Procedure A . 9
10.2 Procedure B .10
11 Precision .10
11.1 General .10
11.2 Repeatability, r .10
11.3 Reproducibility, R .10
12 Test report .10
Annex A (informative) Instrument specifications .12
Annex B (informative) Examples of typical chromatograms .15
Bibliography .21
© ISO 2021 – All rights reserved iii
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SIST EN ISO 22854:2021
ISO 22854:2021(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 of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/
iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 28, Petroleum and related products, fuels
and lubricants from natural or synthetic sources, in collaboration with the European Committee for
Standardization (CEN) Technical Committee CEN/TC 19, Gaseous and liquid fuels, lubricants and related
products of petroleum, synthetic and biological origin, in accordance with the Agreement on technical
cooperation between ISO and CEN (Vienna Agreement).
This fourth edition cancels and replaces the third edition (ISO 22854:2016), which has been technically
revised.
The main changes compared to the previous edition are as follows:
— the Scope and precision have been extended in concentration range;
— the precision statement has been updated;
— new examples of typical chromatograms have been added to Annex B;
[7]
— the text has been further harmonized with ASTM D6839 .
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2021 – All rights reserved
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SIST EN ISO 22854:2021
ISO 22854:2021(E)
Introduction
Previous editions of this document were used for determination of saturated, olefinic, aromatic and
oxygenated hydrocarbons in automotive motor gasoline according to European fuel specifications.
An interlaboratory study has shown that the method can be used for gasolines with a higher
concentration of oxygenated compounds, including methanol. The interlaboratory study also provided
data to calculate precision for toluene in gasoline.
Annex B now includes example chromatograms of gasolines with a variety of oxygenates which can be
used for the correct identification of these oxygenates.
[7]
The test method described in this document is harmonized with ASTM D6839 .
© ISO 2021 – All rights reserved v
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SIST EN ISO 22854:2021
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SIST EN ISO 22854:2021
INTERNATIONAL STANDARD ISO 22854:2021(E)
Liquid petroleum products — Determination of
hydrocarbon types and oxygenates in automotive-
motor gasoline and in ethanol (E85) automotive fuel —
Multidimensional gas chromatography method
1 Scope
This document specifies the gas chromatographic (GC) method for the determination of saturated,
olefinic and aromatic hydrocarbons in automotive motor gasoline and ethanol (E85) automotive fuel.
Additionally, the benzene and toluene content, oxygenated compounds and the total oxygen content can
be determined.
NOTE 1 For the purposes of this document, the terms % (m/m) and % (V/V) are used to represent respectively
the mass fraction, w, and the volume fraction, φ.
This document defines two procedures, A and B.
Procedure A is applicable to automotive motor gasoline with total aromatics of 19,32 % (V/V) up to
46,29 % (V/V); total olefins from 0,40 % (V/V) up to 26,85 % (V/V); oxygenates from 0,61 % (V/V) up to
9,85 % (V/V); oxygen content from 1,50 % (m/m) to 12,32 % (m/m); benzene content from 0,38 % (V/V)
up to 1,98 % (V/V) and toluene content from 5,85 % (V/V) up to 31,65 % (V/V).
The method has also been tested for individual oxygenates. A precision has been determined for
a total volume of methanol from 1,05 % (V/V) up to 16,96 % (V/V); a total volume of ethanol from
0,50 % (V/V) up to 17,86 % (V/V); a total volume of MTBE from 0,99 % (V/V) up to 15,70 % (V/V), a total
volume of ETBE from 0,99 % (V/V) up to 15,49 % (V/V), a total volume of TAME from 0,99 % (V/V) up to
5,92 % (V/V), and a total volume of TAEE from 0,98 % (V/V) up to 15,59 % (V/V).
Although this test method can be used to determine higher-olefin contents of up to 50 % (V/V), the
precision for olefins was tested only in the range from 0,40 % (V/V) to 26,85 % (V/V).
Although specifically developed for the analysis of automotive motor gasoline that contains oxygenates,
this test method can also be applied to other hydrocarbon streams having similar boiling ranges, such
as naphthas and reformates.
NOTE 2 For Procedure A, applicability of this document has also been verified for the determination of
n-propanol, acetone, and di-isopropyl ether (DIPE). However, no precision data have been determined for these
compounds.
Procedure B describes the analysis of oxygenated groups (ethanol, methanol, ethers, C3 – C5 alcohols)
in ethanol (E85) automotive fuel containing ethanol between 50 % (V/V) and 85 % (V/V). The gasoline
is diluted with an oxygenate-free component to lower the ethanol content to a value below 20 % (V/V)
before the analysis by GC.
The sample can be fully analysed including hydrocarbons. Precision data for the diluted sample are
only available for the oxygenated groups.
NOTE 3 For Procedure B, the precision can be used for an ethanol fraction from about 50 % up to 85 % (V/V).
For the ether fraction, the precision as specified in Table 6 can be used for samples containing at least 11 % (V/V)
of ethers. For the higher alcohol fraction, too few data were obtained to derive a full precision statement and the
data presented in Table 6 are therefore only indicative.
NOTE 4 An overlap between C9 and C10 aromatics can occur. However, the total is accurate. Isopropyl benzene
is resolved from the C8 aromatics and is included with the other C9 aromatics.
© ISO 2021 – All rights reserved 1
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SIST EN ISO 22854:2021
ISO 22854:2021(E)
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3170, Petroleum liquids — Manual sampling
ISO 3171, Petroleum liquids — Automatic pipeline sampling
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
hydrocarbon
hydrocarbon group
HG
family of hydrocarbons such as saturated hydrocarbons, olefinic hydrocarbons
3.1.1
saturate
saturated hydrocarbon
type of hydrocarbon (3.1) that contains no double bonds with a carbon number of 3 to 12
EXAMPLE n-Paraffins, iso-paraffins, naphthenes and poly-naphthenes.
3.1.2
olefin
olefinic hydrocarbon
type of hydrocarbon (3.1) that contains double or triple bonds with a carbon number of 3 to 10
EXAMPLE n-Olefins, iso-olefins and cyclic olefins.
3.1.3
aromatic
aromatic hydrocarbon
type of cyclic hydrocarbon (3.1) with alternating double and single bonds between carbon atoms
forming the rings
EXAMPLE Benzene, toluene and higher homologous series with a carbon number of 6 to 10 and naphthalenes,
with a carbon number of up to 12.
3.2
oxygenate
oxygenated compound
type of hydrocarbon (3.1) that contains an oxygen group, the addition of which is allowed according to
current petrol specifications
EXAMPLE Alcohols and ethers.
Note 1 to entry: See Note 2 to Clause 1.
2 © ISO 2021 – All rights reserved
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SIST EN ISO 22854:2021
ISO 22854:2021(E)
4 Principle
4.1 Procedure A and Procedure B use the same separation technique and analysis procedure. The
difference between the two procedures is that for Procedure B the sample is diluted. The diluting solvent
is not considered in the integration. This makes it possible to report the results of the undiluted sample
after normalization to 100 %.
4.2 The automotive motor gasoline sample being analysed is separated into hydrocarbon groups by
means of GC analysis using special column-coupling and column-switching procedures.
The automotive motor gasoline sample is injected into the GC system and, after vaporization, is
separated into the different groups. Detection is always done by a flame ionization detector (FID).
4.3 The mass concentration of each detected compound or hydrocarbon group is determined by
the application of relative response factors (see 9.2) to the area of the detected peaks, followed by
normalization to 100 %. For automotive motor gasoline samples containing oxygenates that cannot
be determined by this test method, the hydrocarbon results are normalized to 100 % minus the value
of oxygenates as determined by another method. The liquid volume concentration of each detected
compound or hydrocarbon group is determined by the application of density values (see 9.3) to the
calculated mass concentration of the detected peaks followed by normalization to 100 %.
IMPORTANT — It is essential to the correct execution of the method that great care be taken to
ensure that all compounds are correctly identified. This is especially true for the identification
of oxygenated compounds because of their wide range of response factors. It is, therefore,
highly recommended for correct identification to verify possibly unknown oxygenates using a
reference mixture that contains these pure compounds.
4.4 After this analysis, the automotive motor gasoline is separated into hydrocarbon groups and then
by carbon number. Using the corresponding relative response factors, the mass distributions of the
groups in the automotive motor gasoline sample can be calculated.
5 Reagents and materials
5.1 Gases
Installation of suitable moisture filters is recommended for hydrogen, helium and nitrogen lines.
5.1.1 Hydrogen, 99,995 % pure.
WARNING — Hydrogen is explosive when mixed with air at concentration between 4 % (V/V)
and 75 % (V/V). Refer to the equipment manufacturers’ manuals concerning leaks in the system.
5.1.2 Helium or nitrogen, 99,995 % pure.
The system’s operating parameters such as column and trap temperatures, carrier gas flows and valve
switching times are depending on the type of carrier gas used. The use of nitrogen as carrier gas is
not possible on all configurations. Contact the equipment manufacturer for specific information or
instructions on the use of nitrogen.
5.1.3 Compressed air.
5.2 Vials, airtight and inert, e.g. with rubber-membrane caps covered with self-sealing
polytetrafluoroethylene (PTFE).
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SIST EN ISO 22854:2021
ISO 22854:2021(E)
5.3 Reference solutions, finished automotive motor gasoline(s) used as reference and which contain
components and concentration levels comparable to those of the test sample.
The composition of the reference solution should have been determined in a round robin or by other
methods.
WARNING — The reference solutions are flammable and harmful if inhaled.
5.4 Diluting solvent, used in Procedure B, shall not interfere with any other component in gasoline
being analysed. Dodecane (C H ) or tridecane (C H ) are recommended solvents.
12 26 13 28
6 Apparatus
6.1 Gas chromatograph, computer-controlled, multidimensional GC equipment, injector, FID, suitable
columns, traps and hydrogenation catalysts, of which an example is given in Annex A.
6.2 Switching valves, suitable switching valves that are used for the transfer of compounds from one
column to the other in the gas chromatograph.
They shall have a chemically inactive surface and a small dead volume.
6.3 Traps, suitable short columns (see Annex A for an example) used for retaining certain selected
chemical groups of the automotive motor gasoline using temperature control.
The absorption of the trapped compounds shall be reversible.
EXAMPLE A typical sequence is the following:
— The alcohols and higher-boiling aromatics are absorbed in a trap (sulfate column I). The remaining aromatics
are separated from the other components by means of a polar column (for example, OV 275).
— The ethers are separated from the remaining fraction by means of another trap (sulfate column II).
— The olefins are separated from the saturates by the olefin trap (for example, silver salt) in two steps. This is
necessary due to the limited capacity of such traps to retain high amounts of butene or total olefins. If the
trap capacity is sufficient for the olefin concentration, the separation can be performed in one step.
— The remaining saturated hydrocarbons are separated into paraffins and naphthenes according to their
carbon number using a 13X molecular sieve column.
— The ethers are then eluted from the trap (sulfate column II) and separated and detected according to boiling
point.
— The olefins are desorbed from the olefin trap and hydrogenated in the Pt-column. They are separated and
detected as the corresponding saturated compounds using a 13X molecular sieve.
— The alcohols and higher-boiling aromatics are eluted from the polar column and the trap (sulfate column I),
separated using a non-polar column (for
...
SLOVENSKI STANDARD
oSIST prEN ISO 22854:2020
01-maj-2020
Tekoči naftni proizvodi - Določevanje vrste ogljikovodikov in oksigenatov v
motornem bencinu in bencinu na osnovi etanola (E85) - Metoda
multidimenzionalne plinske kromatografije (ISO/DIS 22854:2020)
Liquid petroleum products - Determination of hydrocarbon types and oxygenates in
automotive-motor gasoline and in ethanol (E85) automotive fuel - Multidimensional gas
chromatography method (ISO/DIS 22854:2020)
Flüssige Mineralölerzeugnisse - Bestimmung der Kohlenwasserstoffgruppen und der
sauerstoffhaltigen Verbindungen in Ottokraftstoffen und in Ethanolkraftstoff (E85) -
Multidimensionales gaschromatographisches Verfahren (ISO/DIS 22854:2020)
Produits pétroliers liquides - Détermination des groupes d'hydrocarbures et des
composés oxygénés de l'essence pour moteurs automobiles et du carburant pour
automobiles éthanol (E85) - Méthode par chromatographie multidimensionelle en phase
gazeuse (ISO/DIS 22854:2020)
Ta slovenski standard je istoveten z: prEN ISO 22854
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
75.160.20 Tekoča goriva Liquid fuels
oSIST prEN ISO 22854:2020 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 22854:2020
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oSIST prEN ISO 22854:2020
DRAFT INTERNATIONAL STANDARD
ISO/DIS 22854
ISO/TC 28 Secretariat: NEN
Voting begins on: Voting terminates on:
2020-03-13 2020-06-05
Liquid petroleum products — Determination of
hydrocarbon types and oxygenates in automotive-
motor gasoline and in ethanol (E85) automotive fuel —
Multidimensional gas chromatography method
Produits pétroliers liquides — Détermination des groupes d'hydrocarbures et des composés oxygénés de
l'essence pour moteurs automobiles et du carburant pour automobiles éthanol (E85) — Méthode par
chromatographie multidimensionelle en phase gazeuse
ICS: 75.080
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 22854:2020(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2020
---------------------- Page: 3 ----------------------
oSIST prEN ISO 22854:2020
ISO/DIS 22854:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020
All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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
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Email: copyright@iso.org
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Published in Switzerland
ii © ISO 2020 – All rights reserved
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oSIST prEN ISO 22854:2020
ISO/DIS 22854:2020(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 2
3 Terms and definitions . 2
4 Principle . 3
5 Reagents and materials . 3
6 Apparatus . 4
7 Sampling . 5
8 Procedure. 5
8.1 Conditioning . 5
8.2 Sample preparation . 5
8.2.1 Procedure B only − Sample dilution . 5
8.2.2 Procedure A and B − Sample cooling . 5
8.3 Test sample injection volume . 5
8.4 V erification of the apparatus and test conditions . 5
8.5 Validation . 6
8.6 Preparation of the test sample . 6
8.7 Preparation of the apparatus and test conditions . 6
9 Calculation . 6
9.1 General . 6
9.2 Calculation as % (m/m) . 6
9.3 Calculation as % (V/V) . 8
9.4 Calculation of total oxygen content in % (m/m) . 9
9.5 Data report according to automotive motor gasoline specification . 9
10 Expression of results .10
10.1 Procedure A .10
10.2 Procedure B .10
11 Precision .10
11.1 General .10
11.2 Repeatability, r .10
11.3 Reproducibility, R .10
12 Test report .11
Annex A (informative) Instrument specifications .12
Annex B (informative) Examples of typical chromatograms .14
Bibliography .20
© ISO 2020 – All rights reserved iii
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oSIST prEN ISO 22854:2020
ISO/DIS 22854:2020(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 of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see www .iso .org/
iso/ foreword .html.
This document was prepared by Technical Committee ISO/TC 28, Petroleum and related products, fuels
and lubricants from natural or synthetic sources.
This fourth edition cancels and replaces the third edition (ISO 22854:2016), which has been technically
revised.
The main changes compared to the previous edition are as follows:
— new examples of typical chromatograms in Annex B.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
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oSIST prEN ISO 22854:2020
ISO/DIS 22854:2020(E)
Introduction
This document is a small update of the second edition (ISO 22854:2014), which in turn was a revision
to extend the scope of the first edition. Originally ISO 22854:2008 (and its predecessor EN 14517:2004)
was used for determination of saturated, olefinic, aromatic and oxygenated hydrocarbons in automotive
motor gasoline according to European fuel specifications. Recent round-robin work has shown that the
scope of the method can be updated without alteration to include petrol with higher oxygen percentages
than mentioned in the first edition and will now be applicable for automotive motor gasoline up to and
including E10.
An interlaboratory study organized by CEN has shown that the method can also be used for high-
ethanol gasoline [also called ethanol (E85) automotive fuel], provided that the sample is diluted with a
component that will not interfere with any of the components or group of components that need to be
analysed. Details of how to perform such analysis are given in 8.2.
The derived precision data for methanol do not comply with the precision calculation as presented in
this document. No precision calculation for methanol has been established as the need for such data has
not been expressed. If methanol is present in the automotive motor gasoline sample, it is recommended
[1]
that its contents is verified by the use of an appropriate test method, for instance as given in EN 228 .
[2]
The test method described in this document is harmonized with ASTM D6839 .
© ISO 2020 – All rights reserved v
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oSIST prEN ISO 22854:2020
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oSIST prEN ISO 22854:2020
DRAFT INTERNATIONAL STANDARD ISO/DIS 22854:2020(E)
Liquid petroleum products — Determination of
hydrocarbon types and oxygenates in automotive-
motor gasoline and in ethanol (E85) automotive fuel —
Multidimensional gas chromatography method
1 Scope
This document specifies the gas chromatographic (GC) method for the determination of saturated,
olefinic and aromatic hydrocarbons in automotive motor gasoline and ethanol (E85) automotive
fuel. Additionally, the benzene content, oxygenate compounds and the total oxygen content can be
determined.
NOTE 1 For the purposes of this document, the terms % (m/m) and % (V/V) are used to represent respectively
the mass fraction, µ, and the volume fraction, φ.
This document defines two procedures, A and B.
Procedure A is applicable to automotive motor gasoline with total aromatics of up to 50 % (V/V); total
olefins from about 1,5 % (V/V) up to 30 % (V/V); oxygenates from 0,8 % (V/V) up to 15 % (V/V); total
oxygen from about 1,5 % (m/m) to about 3,7 % (m/m); and benzene of up to 2 % (V/V). The system can
be used for ethers with 5 or more C atoms up to 22 % (V/V) but the precision has not been established
up to this level.
Although this test method can be used to determine higher-olefin contents of up to 50 % (V/V), the
precision for olefins was tested only in the range from about 1,5 % (V/V) to about 30 % (V/V).
Although specifically developed for the analysis of automotive motor gasoline that contains oxygenates,
this test method can also be applied to other hydrocarbon streams having similar boiling ranges, such
as naphthas and reformates.
NOTE 2 For Procedure A, precision data have been established for the oxygenate compounds in automotive
motor gasoline samples containing ethyl-tert-butyl ether (ETBE), methyl-tert-butyl ether (MTBE), tert-amyl-
methyl ether (TAME), iso-propanol, iso-butanol, tert-butanol, methanol and ethanol. The derived precision data
for methanol do not comply with the precision calculation as presented in this document. Applicability of this
document has also been verified for the determination of n-propanol, acetone, and di-isopropyl ether (DIPE).
However, no precision data have been determined for these compounds.
Procedure B describes the procedure for the analysis of oxygenated groups (ethanol, methanol,
ethers, C3 – C5 alcohols) in ethanol (E85) automotive fuel containing ethanol between 50 % (V/V)
and 85 % (V/V). The gasoline is diluted with an oxygenate-free component to lower the ethanol content
to a value below 20 % (V/V) before the analysis by GC. If the ethanol content is unknown, it is advisable
to use a dilution of 4:1 when analysing the sample.
The sample can be fully analysed including hydrocarbons. Precision data for the diluted sample are
only available for the oxygenated groups.
NOTE 3 For Procedure B, the precision can be used for an ethanol fraction from about 50 % (V/V) up to
85 % (V/V). For the ether fraction, the precision as specified in Table 6 can be used for samples containing at
least 11 % (V/V) of ethers. For the higher alcohol fraction, too few data were obtained to derive a full precision
statement and the data presented in Table 6 are therefore only indicative.
NOTE 4 While developing this test method, the final boiling point was limited to 215 °C.
NOTE 5 An overlap between C9 and C10 aromatics can occur. However, the total is accurate. Isopropyl benzene
is resolved from the C8 aromatics and is included with the other C9 aromatics.
© ISO 2020 – All rights reserved 1
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oSIST prEN ISO 22854:2020
ISO/DIS 22854:2020(E)
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 3170, Petroleum liquids — Manual sampling
ISO 3171, Petroleum liquids — Automatic pipeline sampling
ISO 4259, Petroleum products — Determination and application of precision data in relation to
methods of test
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
3.1
hydrocarbon group
family of hydrocarbons such as saturated hydrocarbons, olefinic hydrocarbons, etc
3.1.1
saturated hydrocarbon
saturate
type of hydrocarbon that contains no double bonds with a carbon number of 3 to 12
EXAMPLE n-Paraffins, iso-paraffins, naphthenes and poly-naphthenes.
3.1.2
olefinic hydrocarbon
olefin
type of hydrocarbon that contains double or triple bonds with a carbon number of 3 to 10
EXAMPLE n-Olefins, iso-olefins and cyclic olefins.
3.1.3
aromatic hydrocarbon
aromatic
type of cyclic hydrocarbon with alternating double and single bonds between carbon atoms forming
the rings
EXAMPLE Benzene, toluene and higher homologous series with a carbon number of 6 to 10 and naphthalenes,
with a carbon number of up to 12.
3.2
oxygenate
oxygenated compound
type of hydrocarbon that contains an oxygen group, the addition of which is allowed according to
current petrol specifications
EXAMPLE Alcohols and ethers.
Note 1 to entry: See Clause 1, Note 2.
2 © ISO 2020 – All rights reserved
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ISO/DIS 22854:2020(E)
3.3
partial group
PG
one carbon number in an individual group, being either a single compound like toluene or an
isomeric mixture
EXAMPLE n-Butane and iso-butane.
4 Principle
4.1 Procedure A and Procedure B use the same separation technique and analysis procedure. The
difference between the parts is that for Procedure B the sample is diluted. The diluting solvent is not
considered in the integration. This makes it possible to report the results of the undiluted sample after
normalization to 100 %.
4.2 The automotive motor gasoline sample being analysed is separated into hydrocarbon groups by
means of GC analysis using special column-coupling and column-switching procedures.
The automotive motor gasoline sample is injected into the GC system and, after vaporization, is
separated into the different groups. Detection is always done by a flame ionization detector (FID).
4.3 The mass concentration of each detected compound or hydrocarbon group is determined by
the application of relative response factors (see 9.2) to the area of the detected peaks, followed by
normalization to 100 %. For automotive motor gasoline samples containing oxygenates that cannot
be determined by this test method, the hydrocarbon results are normalized to 100 % minus the value
of oxygenates as determined by another method. The liquid volume concentration of each detected
compound or hydrocarbon group is determined by the application of density values (see 9.3) to the
calculated mass concentration of the detected peaks followed by normalization to 100 %.
IMPORTANT — It is essential to the correct execution of the method that great care be taken to
ensure that all compounds are correctly identified. This is especially true for the identification of
oxygen - containing compounds because of their wide range of response factors. It is, therefore,
highly recommended for correct identification to verify possibly unknown oxygenates using a
reference mixture that contains these pure compounds.
4.4 After this analysis, the automotive motor gasoline is separated into hydrocarbon groups and then
by carbon number. By the use of the corresponding relative response factors, the mass distributions of
the groups in the automotive motor gasoline sample can be calculated.
5 Reagents and materials
5.1 Gases
Installation of suitable moisture filters is recommended for hydrogen, helium and nitrogen lines.
5.1.1 Hydrogen, 99,995 % pure.
DANGER — Hydrogen is explosive when mixed with air at concentration between 4 % (V/V) and
75 % (V/V). See the equipment manufacturers’ manuals concerning leaks in the system.
5.1.2 Helium or nitrogen, 99,995 % pure.
The system’s operating parameters such as column and trap temperatures, carrier gas flows and valve
switching times are depending on the type of carrier gas used. The use of nitrogen as carrier gas is
not possible on all configurations. Contact the equipment manufacturer for specific information or
instructions on the use of nitrogen.
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oSIST prEN ISO 22854:2020
ISO/DIS 22854:2020(E)
5.1.3 Compressed air.
5.2 Vials, airtight and inert, e.g. with rubber-membrane caps covered with self-sealing polytetra-
fluoroethylene (PTFE).
5.3 Reference solutions, finished automotive motor gasoline(s) used as reference and which contain
components and concentration levels comparable to those of the test sample.
The composition of the reference solution should have been determined in a round robin or by other
methods.
DANGER — Flammable. Harmful if inhaled.
5.4 Diluting solvent, used in Procedure B, shall not interfere with any other component in gasoline
being analysed. Dodecane (C H ) or tridecane (C H ) are recommended solvents.
12 26 13 28
6 Apparatus
6.1 Gas chromatograph, computer-controlled, multidimensional GC equipment, injector, FID, suitable
columns, traps and hydrogenation catalysts, of which an example is given in Annex A.
6.2 Switching valves, suitable switching valves that are used for the transfer of compounds from one
column to the other in the gas chromatograph.
They shall have a chemically inactive surface and a small dead volume.
6.3 Traps, suitable short columns (see Annex A for an example) used for retaining certain selected
chemical groups of the automotive motor gasoline using temperature control.
The absorption of the trapped compounds shall be reversible.
EXAMPLE A typical sequence is the following:
— The alcohols and higher-boiling aromatics are absorbed in a trap (sulfate column I). The remaining aromatics
are separated from the other components by means of a polar column (for example, OV 275).
— The ethers are separated from the remaining fraction by means of another trap (sulfate column II).
— The olefins are separated from the saturates by the olefin trap (for example, silver salt) in two steps. This is
necessary due to the limited capacity of such traps to retain high amounts of butene or total olefins. If the
trap capacity is sufficient for the olefin concentration, the separation may be performed in one step.
— The remaining saturated hydrocarbons are separated into paraffins and naphthenes according to their
carbon number using a 13X molecular sieve column.
— The ethers are then eluted from the trap (sulfate column II) and separated and detected according to
boiling point.
— The olefins are desorbed from the olefin trap and hydrogenated in the Pt-column. They are separated and
detected as the corresponding saturated compounds using a 13X molecular sieve.
— The alcohols and higher-boiling aromatics are eluted from the polar column and the trap (sulfate column I),
separated using a non-polar column (for example, OV 101 methyl silicone) and detected according to
boiling point.
Examples of typical chromatograms with this order of elution of the hydrocarbon fractions are shown
in Figures B.1 and B.2. Specifically for Procedure B, a typical chromatogram is shown in Figure B.6.
IMPORTANT — Sulfur-containing compounds are irreversibly adsorbed in the olefins trap and
can reduce its capacity to retain olefins. Sulfur can also be adsorbed in the alcohol and ether-
4 © ISO 2020 – All rights reserved
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oSIST prEN ISO 22854:2020
ISO/DIS 22854:2020(E)
alcohol-aromatic traps. Although the effect of low amounts of sulfur components on the various
traps or columns is very small, it is important to exercise care with automotive motor gasoline
samples with high levels of sulfur.
7 Sampling
Unless otherwise required by national fuel specification standards or by the regulations for the
sampling of automotive motor gasoline, samples shall be taken in accordance with ISO 3170 for manual
sampling or in accordance with ISO 3171 for automatic pipeline sampling.
8 Procedure
8.1 Conditioning
Condition the apparatus according to the manufacturer’s instructions after shutdowns.
8.2 Sample preparation
8.2.1 Procedure B only − Sample dilution
The procedure as described in this subclause is used to analyse gasoline samples containing higher
amounts of ethanol such as ethanol (E85) automotive fuel with ethanol content between 50 % (V/V)
and 85 % (V/V).
As the sulfate column I trap (see Table A.1) cannot trap high amounts of ethanol, the sample shall be
diluted. The selected dilutant (5.4) shall not interfere with the analysis. The level of dilution should be
chosen in such a way that the final amount of ethanol does not exceed 20 % (V/V). If the ethanol content
is unknown, it is advised to use a dilution ratio of 4:1 when analysing the sample.
8.2.2 Procedure A and B − Sample cooling
Cool the test sample to prevent loss by evaporation. Transfer a sufficient portion of the test sample to a
vial (5.2) and immediately tightly close and seal it using the self-sealing PTFE cap (see 5.2). It is advised
to cool the test sample to a temperature between 0 °C and 5 °C.
8.3 Test sample injection volume
Size the injection volume of the test sample in such a way that the capacity of the columns is not
exceeded and that the linearity of the detector is valid.
NOTE An injection volume of 0,1 µl has proven to be satisfactory.
8.4 Verification of the apparatus and test conditions
Run the reference solution (5.3) and check for correct instrument parameters, cutting times and
grouping times. If they are not correct, adjust the apparatus to the manufacturer’s recommendations
and rerun the reference solution.
Attention should be paid to components, such as benzene, olefins and oxygenates, that are near the
boundaries of separation on the group-selective columns. Care should be taken to accurately identify
the oxygen-containing compounds. It is recommended to verify
...
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