Liquid petroleum products - Unleaded petrol - Determination of benzene content by gas chromatography

This document specifies a column switching gas chromatographic method for the quantitative determination of benzene content in the range 0,05 % (V/V) to 6 % (V/V) in unleaded petrol having a final boiling point not greater than 220 °C.
The method described in this document is suitable for determining benzene in petrol, including petrol containing oxygenates up to E10 (up to 3,7 % (m/m) oxygen content), in line with the relevant EC Directives [1].
NOTE   For the purposes of this document, the terms "% (V/V)" and "% (m/m)" are used to represent respectively the volume fraction and the mass fraction.
WARNING - Use of this document might involve hazardous materials, operations and equipment. This document does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this document to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

Flüssige Mineralölerzeugnisse - Unverbleiter Ottokraftstoff - Bestimmung des Benzolgehaltes mittels Gaschromatographie

Dieses Dokument legt ein gaschromatographisches Verfahren mit Säulenschaltung zur quantitativen Bestimmung des Benzolgehaltes im Bereich von 0,05 % (V/V) bis 6 % (V/V) in unverbleitem Ottokraftstoff, dessen Siedeende nicht höher ist als 220 °C, fest.
Das in diesem Dokument beschriebene Verfahren ist zur Bestimmung von Benzol in Ottokraftstoffen, einschließlich Ottokraftstoffen, die sauerstoffhaltige Verbindungen bis zu E10 (Sauerstoffgehalt bis zu 3,7 % (m/m)) enthalten, in Übereinstimmung mit den einschlägigen EG-Richtlinien [1] geeignet.
ANMERKUNG   Für die Zwecke dieses Dokuments wird zur Angabe des Volumenanteils einer Substanz der Ausdruck „% (V/V)“ und für den Massenanteil einer Substanz der Ausdruck "% (m/m)" verwendet.
WARNUNG - Die Anwendung dieses Dokuments kann die Anwendung gefährlicher Stoffe, Arbeitsgänge und Geräte mit sich bringen. Dieses Dokument beansprucht nicht, alle damit verbundenen Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung des Anwenders dieses Dokuments, vor der Anwendung geeignete Maßnahmen für die Sicherheit und den Gesundheitsschutz zu ergreifen, und die Geltung weiterer diesbezüglicher Auflagen zu prüfen.

Produits pétroliers liquides - Essence sans plomb - Détermination de la teneur en benzène par chromatographie en phase gazeuse

Le présent document spécifie une méthode de chromatographie en phase gazeuse à commutation de colonne pour la détermination quantitative de la teneur en benzène dans la plage de 0,05 % (V/V) à 6 % (V/V) dans l'essence sans plomb dont le point d'ébullition final n'est pas supérieur à 220 °C.
La méthode décrite dans ce document est adaptée à la détermination du benzène dans l'essence, y compris l'essence contenant des composés oxygénés jusqu'à E10 (jusqu'à 3,7 % (m/m) de teneur en oxygène), conformément aux directives CE pertinentes [1].
NOTE   Pour les besoins du présent document, les termes "% (V/V)" et "% (m/m)" sont utilisés pour représenter respectivement la fraction volumique et la fraction massique.
AVERTISSEMENT — L'utilisation de ce document peut impliquer des matériaux, des opérations et des équipements dangereux. Ce document n'a pas la prétention de traiter tous les problèmes de sécurité liés à son utilisation. Il incombe à l'utilisateur de ce document d'établir des pratiques appropriées en matière de sécurité et de santé et de déterminer l'applicabilité des restrictions réglementaires avant de l'utiliser.

Tekoči naftni proizvodi - Neosvinčeni motorni bencini - Določevanje benzena s plinsko kromatografijo

General Information

Status
Published
Publication Date
01-Nov-2022
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
02-Nov-2022
Due Date
03-Jan-2023
Completion Date
02-Nov-2022

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SLOVENSKI STANDARD
SIST EN 12177:2023
01-januar-2023
Nadomešča:
SIST EN 12177:1999
SIST EN 12177:1999/AC:2001
Tekoči naftni proizvodi - Neosvinčeni motorni bencini - Določevanje benzena s
plinsko kromatografijo

Liquid petroleum products - Unleaded petrol - Determination of benzene content by gas

chromatography
Flüssige Mineralölerzeugnisse - Unverbleite Ottokraftstoffe - Bestimmung des
Benzolgehaltes mittels Gaschromatographie

Produits pétroliers liquides - Essence sans plomb - Détermination de la teneur en

benzène par chromatographie en phase gazeuse
Ta slovenski standard je istoveten z: EN 12177:2022
ICS:
75.160.20 Tekoča goriva Liquid fuels
SIST EN 12177:2023 en,fr,de

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

---------------------- Page: 1 ----------------------
SIST EN 12177:2023
---------------------- Page: 2 ----------------------
SIST EN 12177:2023
EN 12177
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2022
EUROPÄISCHE NORM
ICS 75.160.20 Supersedes EN 12177:1998
English Version
Liquid petroleum products - Unleaded petrol -
Determination of benzene content by gas chromatography

Produits pétroliers liquides - Essence sans plomb - Flüssige Mineralölerzeugnisse - Unverbleiter

Détermination de la teneur en benzène par Ottokraftstoff - Bestimmung des Benzolgehaltes mittels

chromatographie en phase gazeuse Gaschromatographie
This European Standard was approved by CEN on 16 October 2022.

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, Türkiye 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

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 12177:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN 12177:2023
EN 12177:2022 (E)
Contents Page

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

1 Scope .......................................................................................................................................................... 4

2 Normative references .......................................................................................................................... 4

3 Terms and definitions ......................................................................................................................... 4

4 Principle ................................................................................................................................................... 4

5 Reagents and materials ...................................................................................................................... 5

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

6.1 Gas chromatographic assembly ...................................................................................................... 5

7 Sampling ................................................................................................................................................... 6

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

8.1 Setup of the apparatus ........................................................................................................................ 7

8.1.1 General...................................................................................................................................................... 7

8.1.2 Carrier gas .............................................................................................................................................. 7

8.2 Calibration ............................................................................................................................................... 7

8.3 Determination of density ................................................................................................................... 7

8.4 Preparation of test sample ............................................................................................................... 7

8.5 Introduction of test portion ............................................................................................................ 8

8.6 Examination of the chromatogram ................................................................................................. 8

9 Calculation ............................................................................................................................................... 8

9.1 Calculation of mass of benzene in the test sample ............................................................... 8

9.2 Calculation of volume of benzene in the test sample ............................................................... 8

9.3 Calculation of volume of test sample ......................................................................................... 8

9.4 Calculation of benzene content as % (V/V) ............................................................................. 9

10 Expression of results ........................................................................................................................... 9

11 Precision .................................................................................................................................................. 9

11.1 General...................................................................................................................................................... 9

11.2 Repeatability, r ...................................................................................................................................... 9

11.3 Reproducibility, R ................................................................................................................................. 9

12 Test report ............................................................................................................................................. 10

Annex A (informative) Guidance on the column switching technique ........................................... 11

A.1 Introduction .......................................................................................................................................... 11

A.2 General apparatus parameters for the flow switching technique .................................... 12

A.3 Gas chromatogram ............................................................................................................................. 12

Bibliography ....................................................................................................................................................... 15

---------------------- Page: 4 ----------------------
SIST EN 12177:2023
EN 12177:2022 (E)
European foreword

This document (EN 12177:2022) has been prepared by 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 May 2023, and conflicting national standards shall be

withdrawn at the latest by May 2023.

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 12177:1998.

At the time of the development of the test method, the ethanol content of gasoline was limited to

5 % (V/V) which was reflected in the scope of the test method. Since several years, fuels containing up to

10 % of ethanol (3,7 % (m/m)) are common in the European market. This revision is meant to extend the

scope of the test methods to those fuels, thus reflecting market needs.

Any feedback and questions on this document should be directed to the users’ national standards body.

A complete listing of these bodies can be found on the CEN website.

According to the CEN-CENELEC Internal Regulations, the national standards organisations 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, Türkiye and the United

Kingdom.
---------------------- Page: 5 ----------------------
SIST EN 12177:2023
EN 12177:2022 (E)
1 Scope

This document specifies a column switching gas chromatographic method for the quantitative

determination of benzene content in the range 0,05 % (V/V) to 6 % (V/V) in unleaded petrol having a

final boiling point not greater than 220 °C.

The method described in this document is suitable for determining benzene in petrol, including petrol

containing oxygenates up to E10 (up to 3,7 % (m/m) oxygen content), in line with the relevant EC

Directives [1].

NOTE For the purposes of this document, the terms "% (V/V)" and "% (m/m)" are used to represent

respectively the volume fraction and the mass fraction.

WARNING — Use of this document might involve hazardous materials, operations and equipment. This

document does not purport to address all of the safety problems associated with its use. It is the

responsibility of the user of this document to establish appropriate safety and health practices and

determine the applicability of regulatory limitations prior to use.
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.

EN ISO 3170, Petroleum liquids — Manual sampling (ISO 3170)
EN ISO 3171, Petroleum liquids — Automatic pipeline sampling (ISO 3171)

EN ISO 3675, Crude petroleum and liquid petroleum products — Laboratory determination of density —

Hydrometer method (ISO 3675)

EN ISO 3838, Crude petroleum and liquid or solid petroleum products — Determination of density or

relative density — Capillary-stoppered pyknometer and graduated bicapillary pyknometer methods (ISO

3838)

EN ISO 12185, Crude petroleum and petroleum products — Determination of density — Oscillating U-tube

method (ISO 12185)
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp/
4 Principle

The benzene-containing fraction is isolated from the sample using a capillary column and, in a second

capillary column, the benzene is separated and detected using a flame ionization detector.

NOTE 1 Some oxygenates are known to interfere with the determination of benzene using a single column gas

chromatographic method.
NOTE 2 Guidance on the column switching technique is given in Annex A.
---------------------- Page: 6 ----------------------
SIST EN 12177:2023
EN 12177:2022 (E)
5 Reagents and materials
Use only chemicals and reagents of recognized analytical grade.
5.1 Gases

5.1.1 Carrier gas, helium, nitrogen or hydrogen, of at least 99,999 % (V/V) purity. Any oxygen

present is removed by a chemical resin filter.
5.1.2 Hydrogen, grade suitable for flame ionization detectors.
5.1.3 Compressed air regulated for flame ionization detectors.

WARNING - Hydrogen is explosive in mixtures with air at concentrations of hydrogen ranging

approximately from 4 % (V/V) to 75 % (V/V). All joints and lines carrying hydrogen shall be made gas

tight to prevent leakage of hydrogen into a confined space.
5.2 Reagents for the preparation of calibration samples
NOTE Calibration samples will normally be combinations of benzene, solvent and a
...

SLOVENSKI STANDARD
oSIST prEN 12177:2022
01-januar-2022
Tekoči naftni proizvodi - Neosvinčeni motorni bencini - Določevanje benzena s
plinsko kromatografijo

Liquid petroleum products - Unleaded petrol - Determination of benzene content by gas

chromatography
Flüssige Mineralölerzeugnisse - Unverbleite Ottokraftstoffe - Bestimmung des
Benzolgehaltes mittels Gaschromatographie

Produits pétroliers liquides - Essence sans plomb - Détermination de la teneur en

benzène par chromatographie en phase gazeuse
Ta slovenski standard je istoveten z: prEN 12177
ICS:
75.160.20 Tekoča goriva Liquid fuels
oSIST prEN 12177:2022 en

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

---------------------- Page: 1 ----------------------
oSIST prEN 12177:2022
---------------------- Page: 2 ----------------------
oSIST prEN 12177:2022
DRAFT
EUROPEAN STANDARD
prEN 12177
NORME EUROPÉENNE
EUROPÄISCHE NORM
January 2022
ICS 75.160.20 Will supersede EN 12177:1998
English Version
Liquid petroleum products - Unleaded petrol -
Determination of benzene content by gas chromatography

Produits pétroliers liquides - Essence sans plomb - Flüssige Mineralölerzeugnisse - Unverbleite

Détermination de la teneur en benzène par Ottokraftstoffe - Bestimmung des Benzolgehaltes

chromatographie en phase gazeuse mittels Gaschromatographie

This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee

CEN/TC 19.

If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations

which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.

This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other

language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC

Management Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, 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.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

aware and to provide supporting documentation.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without

notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 12177:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN 12177:2022
prEN 12177:2022 (E)
Contents Page

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

1 Scope .......................................................................................................................................................... 4

2 Normative references .......................................................................................................................... 4

3 Terms and definitions ......................................................................................................................... 4

4 Principle ................................................................................................................................................... 4

5 Reagents and materials ...................................................................................................................... 5

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

7 Sampling ................................................................................................................................................... 6

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

8.1 Setup of the apparatus ........................................................................................................................ 7

8.1.1 General...................................................................................................................................................... 7

8.1.2 Carrier gas ............................................................................................................................................... 7

8.2 Calibration ............................................................................................................................................... 7

8.3 Determination of density ................................................................................................................... 7

8.4 Preparation of test sample ................................................................................................................ 7

8.5 Introduction of test portion .............................................................................................................. 8

8.6 Examination of the chromatogram ................................................................................................. 8

9 Calculation ............................................................................................................................................... 8

9.1 Calculation of mass of benzene in the test sample.................................................................... 8

9.2 Calculation of volume of benzene in the test sample ............................................................... 8

9.3 Calculation of volume of test sample ............................................................................................. 8

9.4 Calculation of benzene content as % (V/V) ................................................................................. 9

10 Expression of results ........................................................................................................................... 9

11 Precision .................................................................................................................................................. 9

11.1 General...................................................................................................................................................... 9

11.2 Repeatability, r ...................................................................................................................................... 9

11.3 Reproducibility, R ................................................................................................................................. 9

12 Test report ............................................................................................................................................. 10

Annex A (informative) Guidance on the column switching technique ......................................... 11

A.1 Introduction .......................................................................................................................................... 11

A.2 General apparatus parameters for the flow switching technique .................................... 12

A.3 Gas chromatogram ............................................................................................................................. 12

Bibliography ....................................................................................................................................................... 15

---------------------- Page: 4 ----------------------
oSIST prEN 12177:2022
prEN 12177:2022 (E)
European foreword

This document (prEN 12177:2022) has been prepared by 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 document is currently submitted to the CEN Enquiry.
This document will supersede EN 12177:1998.

At the time of the development of the test method the ethanol content of gasoline was limited to 5 % (V/V)

which was reflected in the scope of the test method. Since several years, fuels containing up to 10 % of

ethanol (3,7 % (m/m)) are common in the European market. This revision is meant to extend the scope

of the test methods to those fuels, thus reflecting market needs.
---------------------- Page: 5 ----------------------
oSIST prEN 12177:2022
prEN 12177:2022 (E)
1 Scope

This document specifies a column switching gas chromatographic method for the quantitative

determination of benzene content in the range 0,05 % (V/V) to 6 % (V/V) in unleaded petrol having a

final boiling point not greater than 220 °C.

The method described in this document is suitable for determining benzene in petrol, including petrol

containing oxygenates up to E10 (up to 3,7 % (m/m) oxygen content), in line with the relevant EC

[3]
Directives .

NOTE For the purposes of this document, the terms “% (V/V)” and “% (m/m)” are used to represent

respectively the volume fraction and the mass fraction.

WARNING — Use of this document might involve hazardous materials, operations and equipment. This

document does not purport to address all of the safety problems associated with its use. It is the

responsibility of the user of this document to establish appropriate safety and health practices and

determine the applicability of regulatory limitations prior to use.
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.

EN ISO 3170, Petroleum liquids - Manual sampling (ISO 3170)
EN ISO 3171, Petroleum liquids - Automatic pipeline sampling (ISO 3171)

EN ISO 3675, Crude petroleum and liquid petroleum products - Laboratory determination of density -

Hydrometer method (ISO 3675)

EN ISO 3838, Crude petroleum and liquid or solid petroleum products - Determination of density or relative

density - Capillary-stoppered pyknometer and graduated bicapillary pyknometer methods (ISO 3838)

EN ISO 12185, Crude petroleum and petroleum products - Determination of density - Oscillating U-tube

method (ISO 12185)
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

• IEC Electropedia: available at https://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp
4 Principle

The benzene-containing fraction is isolated from the sample using a capillary column and, in a second

capillary column, the benzene is separated and detected using a flame ionization detector.

NOTE 1 Some oxygenates are known to interfere with the determination of benzene using a single column gas

chromatographic method.
NOTE 2 Guidance on the column switching technique is given in Annex A.
---------------------- Page: 6 ----------------------
oSIST prEN 12177:2022
prEN 12177:2022 (E)
5 Reagents and materials
Use only chemicals and reagents of recognized analytical grade.
5.1 Carrier gas

5.2 Carrier gas, helium, nitrogen or hydrogen, of at least 99,999 % (V/V) purity. Any oxygen present

is removed by a chemical resin filter.
5.3 Hydrogen, grade suitable for flame ionization detectors
5.4 Compressed air regulated for flame ionization detectors.

WARNING — Hydrogen is explosive in mixtures with air at concentrations of hydrogen ranging

approximately from 4 % (V/V) to 75 % (V/V). All joints and lines carrying hydrogen shall be made gas

tight to prevent leakage of hydrogen into a confined space.
5.5 Reagents for the preparation of calibration samples

NOTE Calibration samples will normally be combinations of benzene, solvent and an internal standard.

5.5.1 Benzene, not less than 99,0 % (m/m) pure.
WARNING — Benzene is toxic and carcinogenic.
5.5.2 Solvent, not containing benzene or internal standard, e.g. heptane.

5.6 Internal standard, reagent for which it has been established that it is not present in the sample.

NOTE Isobutyl methyl ketone is preferred as the internal standard.
6 Apparatus
Usual laboratory apparatus and glassware, together with th
...

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