Ethanol as a blending component for gasoline - Determination of water content - Karl Fischer potentiometric titration method

This European standard specifies a method for the direct determination of water in ethanol to be used in gasoline blends. It is applicable in the range 0,05 % (m/m) to 0,54 % (m/m).
NOTE   For the purposes of this European Standard, the term “% (m/m)” is used to represent the mass fraction.

Ethanol zur Verwendung als Blendkomponente in Ottokraftstoff - Bestimmung des Wassergehaltes - Potentiometrische Titration nach Karl Fischer

Dieses Dokument legt ein direktes Bestimmungsverfahren für den Wassergehalt von Ethanol zur Verwendung als Blendkomponente in Ottokraftstoff sowie in Ethanolkraftstoff (E85) fest.
Dieses Verfahren ist anwendbar im Bereich von 0,05 % (m/m) bis 0,54 % (m/m).
ANMERKUNG Für die Zwecke dieses Dokuments wird zur Angabe des Massenanteils 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, geeignete Maßnahmen für die Sicherheit und den Gesundheitsschutz zu ergreifen und vor der Anwendung die Geltung behördlicher Einschränkungen zu prüfen.

Ethanol comme base de mélange à l'essence - Détermination de la teneur en eau - Méthode de Karl Fischer par titrage potentiométrique

Le présent document prescrit une méthode de détermination directe de la teneur en eau dans l’éthanol utilisé comme constituant d’essence pour automobiles, ainsi que dans le carburant éthanol (E85).
Cette méthode s’applique à une plage de teneur en eau comprise entre 0,05 % (m/m) et 0,54 % (m/m).
NOTE Pour les besoins du présent document, le terme “% (m/m) ” représente la fraction massique.
AVERTISSEMENT — L'utilisation du présent document peut impliquer l'intervention de produits, d'opérations et d'équipements à caractère dangereux. Le présent document n'est pas censé aborder tous
les problèmes de sécurité concernés par son usage. Il est de la responsabilité de l'utilisateur de ce document de consulter et d'établir des règles de sécurité et d'hygiène appropriées et de déterminer l'applicabilité des restrictions réglementaires avant utilisation.

Etanol kot komponenta za dodajanje motornemu bencinu - Določevanje vode - Metoda potenciometrične titracije po Karlu Fischerju

General Information

Status
Published
Public Enquiry End Date
01-Nov-2020
Publication Date
29-Aug-2021
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
02-Aug-2021
Due Date
07-Oct-2021
Completion Date
30-Aug-2021

RELATIONS

Buy Standard

Standard
SIST EN 15692:2021
English language
10 pages
sale 10% off
Preview
sale 10% off
Preview

e-Library read for
1 day
Draft
oSIST prEN 15692:2020
English language
9 pages
sale 10% off
Preview
sale 10% off
Preview

e-Library read for
1 day

Standards Content (sample)

SLOVENSKI STANDARD
SIST EN 15692:2021
01-oktober-2021
Nadomešča:
SIST EN 15692:2009
Etanol kot komponenta za dodajanje motornemu bencinu - Določevanje vode -
Metoda potenciometrične titracije po Karlu Fischerju

Ethanol as a blending component for gasoline - Determination of water content - Karl

Fischer potentiometric titration method
Ethanol zur Verwendung als Blendkomponente in Ottokraftstoff - Bestimmung des
Wassergehaltes - Potentiometrische Titration nach Karl Fischer
Ethanol comme base de mélange à l'essence - Détermination de la teneur en eau -
Méthode de Karl Fischer par titrage potentiométrique
Ta slovenski standard je istoveten z: EN 15692:2021
ICS:
71.080.60 Alkoholi. Etri Alcohols. Ethers
75.160.20 Tekoča goriva Liquid fuels
SIST EN 15692:2021 en,fr,de

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

---------------------- Page: 1 ----------------------
SIST EN 15692:2021
---------------------- Page: 2 ----------------------
SIST EN 15692:2021
EN 15692
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2021
EUROPÄISCHE NORM
ICS 75.160.20 Supersedes EN 15692:2009
English Version
Ethanol as a blending component for gasoline -
Determination of water content - Karl Fischer
potentiometric titration method

Ethanol comme base de mélange à l'essence - Ethanol zur Verwendung als Blendkomponente in

Détermination de la teneur en eau - Méthode de Karl Ottokraftstoff - Bestimmung des Wassergehaltes -

Fischer par titrage potentiométrique Potentiometrische Titration nach Karl Fischer

This European Standard was approved by CEN on 14 June 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 15692:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN 15692:2021
EN 15692:2021 (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 and sample handling ........................................................................................................ 6

8 Procedure ................................................................................................................................................ 6

8.1 Standardization of the Karl Fischer reagent ............................................................................... 6

8.2 Analysis .................................................................................................................................................... 7

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

10 Expression of results ........................................................................................................................... 8

11 Precision .................................................................................................................................................. 8

11.1 General...................................................................................................................................................... 8

11.2 Repeatability, r ...................................................................................................................................... 8

11.3 Reproducibility, R ................................................................................................................................. 8

12 Test report ............................................................................................................................................... 9

Bibliography ....................................................................................................................................................... 10

---------------------- Page: 4 ----------------------
SIST EN 15692:2021
EN 15692:2021 (E)
European foreword

This document (EN 15692:2021) 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 January 2022, and conflicting national standards shall

be withdrawn at the latest by January 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 15692:2009.

In comparison with the previous edition, the following technical modifications have been made:

— The original document was prepared by CEN/TC 19’s Ethanol Task Force under its Working Group

21 and is based on ISO 760 [1]. It is developed as an alternative to EN 15489 [2], delivering a method

more widely used in the alcohol and beverage industry environment.

— The test method has been revised in terms of its precision and scope. A second interlaboratory study

(ILS) in 2010 [5] confirmed the application to automotive ethanol (E85) fuel. Use of the method over

time, especially in proficiency testing programmes, gave questions around whether the precision in

the original document. When CEN/TC 19/WG 36 was requested to study the ILS reports, the

recalculated precision results did not reflect the published precision.

— The newly calculated precision is lower than the one published and the statistics allow introducing a

constant reproducibility for the determination of water content in ethanol. The test method lower

limit could remain at 0,05 % (whereas the lowest sample mean was 0,02 %). So the scope range has

not been changed, but the precision calculations have.

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, Turkey and the United

Kingdom.
---------------------- Page: 5 ----------------------
SIST EN 15692:2021
EN 15692:2021 (E)
1 Scope

This document specifies a method for the direct determination of water in ethanol to be used as a

blending component for petrol, as well as in automotive ethanol (E85) fuel.
This method is applicable in the range 0,05 % (m/m) to 0,54 % (m/m).

NOTE For the purposes of this document, the term “% (m/m)” is used to represent 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 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)

3 Terms and definitions
For the purposes of this document, the following term and definition apply.

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
3.1
water content

content of water determined by potentiometric Karl Fischer procedure as given in this document

4 Principle

A weighed test portion is injected into the titration vessel of a potentiometric Karl Fischer apparatus. The

water present is titrated to a potentiometric end point using Karl Fischer reagent. Iodine (I ), with

presence of anhydride sulfur (SO ), of methanol (CH OH) and of an appropriate nitrogen base (RN), is

2 3

introduced for the Karl Fischer reaction. Based on the stoichiometry of the reaction, one mole of iodine

reacts with one mole of water.
The reaction can be expressed as follows:
CH OH + SO + RN → [RNH]SO CH
3 2 3 3
H O +I + [RNH]SO CH + 2RN → [RNH]SO CH +2[RNH]I
2 2 3 3 4 3
---------------------- Page: 6 ----------------------
SIST EN 15692:2021
EN 15692:2021 (E)
5 Reagents and materials
Use only chemic
...

SLOVENSKI STANDARD
oSIST prEN 15692:2020
01-oktober-2020
Etanol kot komponenta za dodajanje motornemu bencinu - Določevanje vode -
Metoda potenciometrične titracije po Karlu Fischerju

Ethanol as a blending component for petrol - Determination of water content - Karl

Fischer potentiometric titration method
Ethanol zur Verwendung als Blendkomponente in Ottokraftstoff - Bestimmung des
Wassergehaltes - Potentiometrische Titration nach Karl Fischer
Ethanol comme base de mélange à l'essence - Détermination de la teneur en eau -
Méthode de titrage potentiométrique Karl Fischer
Ta slovenski standard je istoveten z: prEN 15692
ICS:
71.080.60 Alkoholi. Etri Alcohols. Ethers
75.160.20 Tekoča goriva Liquid fuels
oSIST prEN 15692:2020 en,fr,de

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

---------------------- Page: 1 ----------------------
oSIST prEN 15692:2020
---------------------- Page: 2 ----------------------
oSIST prEN 15692:2020
DRAFT
EUROPEAN STANDARD
prEN 15692
NORME EUROPÉENNE
EUROPÄISCHE NORM
October 2020
ICS 75.160.20 Will supersede EN 15692:2009
English Version
Ethanol as a blending component for petrol -
Determination of water content - Karl Fischer
potentiometric titration method

Ethanol comme base de mélange à l'essence - Ethanol zur Verwendung als Blendkomponente in

Détermination de la teneur en eau - Méthode de titrage Ottokraftstoff - Bestimmung des Wassergehaltes -

potentiométrique Karl Fischer Potentiometrische Titration nach Karl Fischer

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

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15692:2020 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
oSIST prEN 15692:2020
prEN 15692:2020 (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 and sample handling ........................................................................................................ 6

8 Procedure ................................................................................................................................................ 6

8.1 Standardization of the Karl Fischer reagent ............................................................................... 6

8.2 Analysis .................................................................................................................................................... 7

9 Calculation ............................................................................................................................................... 7

10 Expression of results ........................................................................................................................... 8

11 Precision .................................................................................................................................................. 8

11.1 General...................................................................................................................................................... 8

11.2 Repeatability, r ...................................................................................................................................... 8

11.3 Reproducibility, R ................................................................................................................................. 8

12 Test report ............................................................................................................................................... 8

Bibliography ......................................................................................................................................................... 9

---------------------- Page: 4 ----------------------
oSIST prEN 15692:2020
prEN 15692:2020 (E)
European foreword

This document (prEN 15692:2020) 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 15692:2009.

In comparison with the previous edition, the following technical modifications have been made:

— The original document was prepared by CEN/TC 19’s Ethanol Task Force under its Working Group

21 and is based on ISO 760 [1]. It is developed as an alternative to EN 15489 [2], delivering a method

more widely used in the alcohol and beverage industry environment.

— The test method has been revised in terms of its precision and scope. A second interlaboratory study

(ILS) in 2010 [5] confirmed the application to automotive ethanol (E85) fuel. Use of the method over

time, especially in proficiency testing programmes, gave questions around whether the precision in

the original document. When CEN/TC 19/WG 36 was requested to study the ILS reports, the

recalculated precision results did not reflect the published precision.

— The newly calculated precision is lower than the one published and the statistics allow introducing a

constant reproducibility for the determination of water content in ethanol. The test method lower

limit could remain at 0,05 % (whereas the lowest sample mean was 0,02 %). So the scope range has

not been changed, but the precision calculations have.
---------------------- Page: 5 ----------------------
oSIST prEN 15692:2020
prEN 15692:2020 (E)
1 Scope

This document specifies a method for the direct determination of water in ethanol to be used as a

blending component for petrol, as well as in automotive ethanol (E85) fuel.
This method is applicable in the range 0,05 % (m/m) to 0,54 % (m/m).

NOTE For the purposes of this document, the term “% (m/m)” is used to represent 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 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)

3 Terms and definitions
For the purposes of this document, the following term and definition apply.

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

• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp
3.1
water content

content of water determined by potentiometric Karl Fischer procedure as given in this document

4 Principle

A weighed test portion is injected into the titration vessel of a potentiometric Karl Fischer apparatus. The

water present is titrated to a potentiometric end point using Karl Fischer reagent. Iodine (I ), with

presence of anhydride sulfur (SO ), of methanol (CH OH) and of an appropriate nitrogen base (RN), is

2 3

introduced for the Karl Fischer reaction. Based on the stoichiometry of the reaction, one mole of iodine

reacts with one mole of water.
The reaction can be expressed as follows:
CH OH + SO + RN → [RNH]SO CH
3 2 3 3
H O +I + [RNH]SO CH + 2RN → [RNH]SO CH +2[RNH]I
2 2 3 3 4 3
---------------------- Page: 6 ----------------------
oSIST prEN 15692:2020
prEN 15692:2020 (E)
5 Reagents and materials
Use only chemicals and reagents of recognized analytical grade.

5.1 Karl Fischer reagent, pyridine-free Karl Fischer reagent, containing iodine, sulfur dioxide and an

odourless amine and with a nominal water equivalent content of either 2 mg or 5 mg

...

Questions, Comments and Discussion

Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.