CEN/TR 15160:2005

SLOVENSKI STANDARD
01-oktober-2005
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Petroleum and related products - Applicability of diesel fuel test methods for Fatty Acid
Methyl Esters (FAME) - Information and results on round robin tests
Mineralölerzeugnisse und verwandte Produkte - Anwendbarkeit von Prüfverfahren für
Diesel-Kraftstoffe auf Fettsäure-Methylester (FAME) - Informationen und Ergebnisse aus
Ringversuchen
Produits pétroliers et produits connexes - Applicabilité des méthodes d'essai des
carburants diesel (gazoles) aux esters méthyliques d'acides gras (EMAG) - Information
et résultats relatifs aux essais circulaires
Ta slovenski standard je istoveten z: CEN/TR 15160:2005
ICS:
75.160.20 7HNRþDJRULYD Liquid fuels
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL REPORT
CEN/TR 15160
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
August 2005
ICS 75.160.20
English Version
Petroleum and related products - Applicability of diesel fuel test
methods for Fatty Acid Methyl Esters (FAME) - Information and
results on round robin tests
Produits pétroliers et produits relié - Application des Mineralölerzeugnisse und verwandte Produkte -
méthodes d'examination de gazole en Methyl Acides Graz Anwendbarkeit von Prüfverfahren für Diesel-Kraftstoffe auf
(UMAG) - Information ét résultats d'examination inter- Fettsäure-Methylester (FAME) - Informationen und
laboratoir Ergebnisse aus Ringversuchen
This Technical Report was approved by CEN on 18 June 2005. It has been drawn up by the Technical Committee CEN/TC 19.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2005 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 15160:2005: E
worldwide for CEN national Members.

Contents Page
Foreword .3
Introduction.4
1 Summary.5
2 Background.5
3 Basis of the work .6
4 Details of the round robin.7
5 Results.7
6 Conclusion .10
Annex A (informative) List of participants in working group 26 activities .11
Annex B (informative) Report of the result of the round robin on 'determination of flash point using
the rapid equilibrium close cup method' (prEN ISO/DIS 3679).13
Annex C (informative) Report of the result of the round robin series on 'distillation of petroleum
products at reduced pressure' (ASTM D 1160).20
Annex D (informative) Preliminary study on applicability of 'distillation of petroleum products at
atmospheric pressure' (EN ISO 3405) on blends of FAME in diesel fuel.25
Annex E (informative) Report of the results of the round robin on 'determination of carbon residue via
the micro method' (EN ISO 10370).29
Annex F (informative) Report of the result of the round robin series on 'corrosiveness to copper via
the copper strip test' (EN ISO 2160).33
Annex G (informative) Report of the result of the round robin series on 'determination of fatty acid
methyl esters (FAME) in middle distillates via infrared spectroscopy' (prEN 14078).36
Annex H (informative) Influence of FAME origin on the measure of FAME content in mineral oil using
prEN 14078 ('Determination of fatty acid methyl esters (FAME) in middle distillates via infrared
spectroscopy method').40

Foreword
This document (CEN/TR 15160:2005) 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 has been prepared under a mandate given to CEN by the European Commission and the European
Free Trade Association.
Introduction
This Technical Report gives the results of the round robin series of tests to evaluate different test methods on their
compatibility on FAME which are referred to in:
• EN 14213: Heating fuels – Fatty acid methyl esters (FAME) – Requirements and test methods, and
• EN 14214: Automotive fuels – Fatty acid methyl esters (FAME) for diesel engines – Requirements and test
methods.
CEN/TC 19 acknowledges Mrs. M.F. Benassy from Total, all project leaders of each test method as indicated in the
annexes and all other participants in CEN/TC 19/WG 26 "FAME related fuel test methods" (see Annex A) for their
contribution to this report.
1 Summary
One task under the European Mandate M/245 was to investigate the applicability of existing petroleum test method
standards for fatty acid methyl esters (FAME). For this task CEN/TC 19 has founded a separate working group 26,
which has validated 24 methods via round robins, including the development of new test methods.
The work of CEN/TC 19/WG 26 was aimed at the drafting of amendments for existing ISO standards (with test
methods for fossil fuels). These amendments include the extension of the scope of the standards to biodiesel as
well as the new precision data for biodiesel. To get these new precision data (repeatability & reproducibility),
WG 26 has done a major effort to validate all relevant test methods on request of the Task Force of WG 24 and
WG 25 dealing with the specifications.
2 Background
CEN has been asked by the Commission (Mandate M/245) to elaborate standards for fatty acid methyl esters
(FAME) to be used as sole fuel for heating and diesel engines and as an additive to mineral oil based fuels. This
work has been divided amongst two Technical Committees, of which CEN/TC 19 was responsible for determining
the applicability of already existing petroleum type test method standards to both pure FAME and to blends. This
included comparing precision data, generating new reproducibility and repeatability figures and developing new test
method standards if necessary.
For this task CEN/TC 19 has founded a separate working group with the following task: “Verification of applicability
to biodiesel (for use in diesel engines as well as for use as heating oil) of existing test methods (to be validated via
round robins) and development of new test methods, if necessary”. The convenor of this WG 26 was Mrs. Benassy
of Total (former ELF Antar), France. For a list of participants in this WG, see Annex A.
The work of WG 26 was aimed at the drafting of amendments for existing ISO standards (with test methods for
fossil fuels). These amendments include the extension of the scope of the standards to biodiesel as well as the new
precision data for biodiesel. To get these new precision data (repeatability & reproducibility), WG 26 has organised
several round robin studies. Besides that it had several consultations with other WG's responsible for existing or
revising of test methods and with the WG 24 (automotive diesel) and WG 25 (heating fuels) dealing with the
specifications.
Scope of the work was investigating the applicability of each test method towards FAME as 100 % diesel fuel. The
repeatability and reproducibility were determined if the test method was applicable. Furthermore, it was determined
whether the method was also applicable to blends of FAME and diesel fuel.
This Technical Report gives an overview of the work of WG 26 and of the results in relation to applicability of each
test method and the determined precision data, giving the basic conclusions and data. A full report with all data per
test method has been presented within CEN/TC 19. This report is the basis of two standards:
1. EN 14213:2003, Heating fuels — Fatty acid methyl esters (FAME) — Requirements and test methods
2. EN 14214:2003, Automotive fuels — Fatty acid methyl esters (FAME) for diesel engines — Requirements and
test methods
Moreover, the results of the study by WG 26 have been input in the revision of the automotive diesel fuel
specification standard (EN 590).
NOTE For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent respectively the mass
fraction and the volume fraction.
3 Basis of the work
The following list of standards has been investigated in the period 1999 until 2002:
 EN 116:1997, Diesel and domestic heating fuels – Determination of cold filter plugging point
 EN 590: 1998, Automotive fuels – Diesel – Requirements and test methods
 EN 12662:1998, Liquid petroleum products – Determination of contamination in middle distillates
 EN 12634:1998, Petroleum products and lubricants – Determination of acid number – Non-aqueous
potentiometric titration method
 prEN 14078:2001, Liquid petroleum products – Determination of fatty acid methyl esters (FAME) in middle
distillates – Infrared spectroscopy method
 EN 22719:1993, Petroleum products and lubricants – Determination of flash point - Pensky-Martens closed
cup method (ISO 2719:1988)
 EN 23015:1994, Petroleum products – Determination of cloud point (ISO 3015:1992)
 EN ISO 2160:1998, Petroleum products – Corrosiveness to copper – Copper strip test (ISO 2160:1998)
 EN ISO 3104:1998/C2:1999, Petroleum products – Transparent and opaque liquids – Determination of
kinematic viscosity and calculation of dynamic viscosity (ISO 3104:1997)
 EN ISO 3405:2000, Petroleum products – Determination of distillation characteristics at atmospheric pressure
(ISO 3405:2000)
 EN ISO 3675:1998, Crude petroleum and liquid petroleum products – Laboratory determination of density –
Hydrometer method (ISO 3675:1998)
2)
 prEN ISO/DIS 3679:2001 , Petroleum products - Determination of flash point - Rapid equilibrium closed cup
method
 EN ISO 4259:1995, Petroleum products – Determination and application of precision data in relation to
methods of test (ISO 4259:1992/Cor.1: 1993)
 EN ISO 5165:1998, Petroleum products – Determination of ignition quality of diesel fuels – Cetane engine
method (ISO 5165:1998)
 EN ISO 10370:1995, Petroleum products – Determination of carbon residue – Micro method (ISO 10370:
1993)
 EN ISO 12185:1996, Crude petroleum and petroleum products – Determination of density – Oscillating U-tube
method (ISO 12185:1996)
 EN ISO 12205:1996, Petroleum products – Determination of the oxidation stability of middle distillate fuels
(ISO 12205:1995)
 EN ISO 12937:2000, Petroleum products – Determination of water – Coulometric Karl Fisher titration method
(ISO 12937:2000)
These standards are referred to in the document as either the EN ISO or the ISO number (given in brackets), but here the
correct reference of the actual, updated standard is given.
2 Succeeded by EN ISO 3679:2004, Petroleum products - Determination of flash point - Rapid equilibrium closed cup method
(ISO 3679:2004)
 EN ISO 13759:1996, Petroleum products – Determination of alkyl nitrate in diesel fuels – Spectrometric
method (ISO 13759:1996)
 EN ISO 14596:1998/C1:1999, Petroleum products – Determination of sulfur content – Wavelength-dispersive
X-ray fluorescence spectrometry (ISO 14596:1998/C1:1999)
 prEN ISO/DIS 20846:2002, Petroleum products – Determination of total sulfur content of liquid petroleum
products – Ultraviolet Fluorescence Method
 ISO 3016:1994, Petroleum products – Determination of pour point
 ISO 3987:1994, Petroleum products – Lubricating oils and additives – Determination of sulfated ash.
 ISO 6245:2001, Petroleum products – Determination of ash
 ISO 12156-1:1997, Diesel fuels – Assessment of lubricity using the high-frequency reproducing rig (HFRR) –
Part 1: Test method (including Cor. 1:1998)
 ASTM D 1160:99, Distillation of Petroleum Products at Reduced Pressure
4 Details of the round robin
After having considered all existing (statistical) data in the standards, WG 26 has decided for which test methods
an inter-laboratory study was necessary. For some methods the data were sufficient, for others the decision on
applicability was made after internal discussions.
For each of the remaining test methods a round robin study was initiated and a project leader from WG 26 was
assigned. The number
...