CEN/TR 15160:2005

Petroleum and related products - Applicability of diesel fuel test methods for Fatty Acid Methyl Esters (FAME) - Information and results on round robin tests

(no Scope)
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.

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

Dans le cadre du mandat européen M/245, le CEN/TC 19 a été chargé d'étudier l'applicabilité aux esters méthyliques d'acides gras (EMAG) des méthodes d'essai normalisées pour les produits pétroliers. A cette fin, le CEN/TC 19 a créé un groupe de travail spécial, le CEN/TC 19/WG 26. Celui-ci a réalisé des essais circulaires qui ont permis de valider 24 méthodes, parmi lesquelles certaines sont des développements nouveaux.
Le travail du CEN/TC 19/WG 26 a visé à la rédaction d'amendements aux méthodes ISO existantes (avec des méthodes destinées aux fuels fossiles). Ces amendements comprennent l'extension du domaine d'application des normes aux biocarburants et biocombustibles ainsi que de nouvelles données de fidélité pour ces produits. L'établissement de ces nouvelles données de fidélité (répétabilité et reproductibilité) a nécessité de la part du WG 26 un très gros travail sur toutes les méthodes pertinentes qui ont été désignées par les Task Forces spécialisées des CEN/TC 19/WG 24 et CEN/TC 19/WG 25 consacrés aux spécifications.

Naftni in sorodni proizvodi – Uporabnost preskusnih metod dizelskega goriva za metil estre maščobnih kislin (FAME) – Informacije in rezultati »round robin« preskusov

General Information

• Status: Published
• Publication Date: 02-Aug-2005
• ICS: 75.160.20 - Liquid fuels
• ICS: 75.160.40 - Biofuels
• Technical Committee: CEN/TC 19 - Petroleum products, lubricants and related products
• Drafting Committee: CEN/TC 19/WG 24 - Specification for automotive diesel
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 03-Aug-2005
• Completion Date: 03-Aug-2005
• Ref Project: SIST-TP CEN/TR 15160:2005 - Petroleum and related products - Applicability of diesel fuel test methods for Fatty Acid Methyl Esters (FAME) - Information and results on round robin tests

Standards Content (Sample)

SLOVENSKI STANDARD
SIST-TP CEN/TR 15160:2005
01-oktober-2005
1DIWQLLQVRURGQLSURL]YRGL±8SRUDEQRVWSUHVNXVQLKPHWRGGL]HOVNHJDJRULYD]D
PHWLOHVWUHPDãþREQLKNLVOLQ)$0(±,QIRUPDFLMHLQUH]XOWDWLªURXQGURELQ©
SUHVNXVRY

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
SIST-TP CEN/TR 15160:2005 en

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

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SIST-TP CEN/TR 15160:2005
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SIST-TP CEN/TR 15160:2005
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.
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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

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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.
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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.
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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.
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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)

 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)
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 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 of participating laboratories changed with each standard, going from 7 to 15. There was a

variety in countries but from France, Italy, Austria and Germany there were always laboratories participating.

Samples from actual FAME products from different feed-stocks were supplied by ITERG, France. Distribution of the

samples, together with the correct protocol, was organised by WG 26. All data received from the labs were

statistically treated according to EN ISO 4259.

For pure FAME, inter-laboratory testing has been completed for the following determination methods : density

(EN ISO 3675 and EN ISO 12185), viscosity (EN ISO 3104), flash point (prEN ISO/DIS 3679), sulfur content

(EN ISO 20846), carbon residue (EN ISO 10370), cetane number (EN ISO 5165), ash content (ISO 3987), water

content (EN ISO 12937), copper corrosion (EN ISO 2160), acid number (EN 12634). For 5 % blends of FAME in

diesel fuel only testing on determination of alkyl nitrate content (EN ISO 13759) has been done by WG 26. For

sulfur content (five methods) and cetane number (one 5 % blend sample tested among four petroleum type

samples) studies have been done by other CEN/TC 19 groups, while they were conducting their round robin

investigations.
5 Results

All results are compiled in Table 1 and Table 2. The conclusions on applicability, repeatability and reproducibility

are given for pure FAME and one for blends of 5 % in diesel. The results of the sulfur study on the blends have

been left out of the table, as this is part of the report of WG 27. However, their results have been incorporated in

the drafting of the two FAME specification standards.

Detailed reports on studies on flash point, distillation, carbon residue, corrosiveness to copper and the FAME

detection method are given in Annex B to Annex H. Other short reports are not available.

In brackets the documents which have been used as a basis for the lab-protocol are given. After the study these standards

might have been updated.
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Table 1 - Details of inter-laboratory test programme
Methods for pure FAME
Standard Applicable Precision Repeatability Reproducibility Comments
similar to
std
3 3
EN ISO 3675 Yes Yes 0,000 5 g/cm 0,001 2 g/cm Conversion tables
Density at 15 ºC applicable
3 3
EN ISO 12185 Yes Yes 0,2 kg/m 0,5 kg/m Conversion tables not
Density at 15 ºC applicable
EN ISO 3104 Yes Yes 0,11 % 1,8 %
Viscosity at 40 ºC
EN 22719 No
Flash point (Pensky-
Martens)
0,9
prEN ISO/DIS 3679 Yes r: Yes 0,022X °C 15 °C - Electronic detection
Flash point R: No - 2ml test portion
(equilibrium)
EN ISO 20846 Yes Yes 0,028 5 X + 2 0,108 8 X + 2
Sulfur content (X in mg/kg) (X in mg/kg)
2/3 2/3
EN ISO 10370 Yes Yes 0,077 X 0,245 X 10% residue obtained
Carbon residue (X in %) (X in %) by ASTM D1160 run
at 10 mmHg
EN ISO 5165 Yes r: No 2,4 5
Cetane number R: Yes
0,85 0,.85
ISO 3987 Yes Yes 0,06 X 0,142 X
Ash content
(sulphated)
0,5 0,5
EN ISO 12937 Yes Yes 0,0187 4 X 0,0687 7 X
Water content (X in %) (X in %)
EN ISO 2160 Yes No value Not a numerical result
Copper corrosion
EN ISO 3405 No
Distillation
ASTM D 1160 Yes Yes 2 °C 3 °C run at 10mmHg
Distillation (90% distilled) (90% distilled)
ISO 3016 Yes
Pour point
EN 116 Yes As stated by
CFPP CEN/TC19/WG14
EN 12662 Wait for method
Total contamination revision
EN 12634 Yes r: Yes 0,05 X 0,065+ 0,281 X
(X in mg KOH/g) (X in mg KOH/g)
Acid number R: No

if YES: repeatability and reproducibility quoted are the one of the reference standard,

if NO: repeatability and reproducibility quoted are the one obtained during the inter-laboratory testing

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Table 2 - Details of inter-laboratory test programme
Methods for blends of FAME, (up to 5 % volume)
Standard Applicable Precision Repeatability Reproducibility Comments
similar to std
3 3
EN ISO 3675 Yes Yes 0,000 5 g/cm 0,001 2 g/cm No inter-lab. test
Density at 15 ºC
3 3
EN ISO 12185 Yes Yes 0,2 kg/m 0,5 kg/m No inter-lab. test
Density at 15 ºC
EN ISO 3104 Yes Yes 0,11% 1,8% No inter-lab. test
Viscosity at 40 ºC
EN 22719 Yes Yes 2 °C 3,5 °C Procedure A.
Flash point (P.M.) (at 101°C) (at 101°C) Decision made after
short study
EN ISO 14596 Yes Yes 0,037 X + 1,9 0,063 X + 3,2
Sulfur content (mg/kg) (mg/kg)
2/3 2/3
EN ISO 10370 Yes Yes 0,077 X 0,245 X No inter-lab. test
Carbon residue (X in %) (X in %)
EN ISO 5165 Yes Yes 0,9 4,3
Cetane number at 52 at 52
ISO 6245 Yes Yes Decision made after
Ash content short study
0,5 0,5
EN ISO 12937 Yes Yes 0,0187 4 X 0,068 77 X No inter-lab. test
Water content (X in %) (X in %)
EN ISO 2160 Yes No value Decision made after
Copper corrosion short study
EN ISO 13759 Yes Yes Decision made after
Alkyl nitrate short study
ISO 12156-1 Yes
Lubricity
EN ISO 3405 Yes Yes Decision made after
Distillation short study
EN ISO 12205 Yes Yes No inter-lab. test
Oxidation stability
ISO 3016 Yes Yes As advised by
Pour point CEN/TC19/WG14
EN 23015 Yes Yes As advised by
Cloud point CEN/TC19/WG14
EN 116 Yes Yes As advised by
CFPP CEN/TC19/WG14
EN 12662 Wait for method
Total contamination revision
EN 14078 Yes r = 2,5 g/l X = 100 g/l
Fame content by IR R = 7,7 g/l
X > 100 g/l
R = 12,7 g/l

if YES: repeatability and reproducibility quoted are the one of the reference standard,

if NO: repeatability and reproducibility quoted are the one obtained during the inter-laboratory testing

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6 Conclusion
6.1 Pure FAME

Flash point by EN 22719 and distillation by EN ISO 3405 where found to be not applicable to FAME samples after

an internal study.

All other methods were found applicable to FAME samples with similar precision data as for petroleum products,

except for:
- Cetane number: r is significantly higher
- Acid number: R is significantly higher
- Flash point (prEN ISO/DIS 3679): R is significantly higher

No improvement of these methods could be expected in the time given by the Mandate, but information has been

given to the different method working groups for possible future work.

No inter-laboratory test has been conducted on cold properties (EN 116), following advice of CEN/TC19/WG14.

Pour point and cloud point methods where considered to be applicable.
6.2 5 % blends of FAME in diesel fuel

Considering the work done on pure FAME and the known method on diesel fuel, the experts agreed on the fact that

the following methods where applicable with the same precision data than already stated in the standard, without

running an inter-laboratory testing:
 density (EN ISO 3675 and EN ISO 12185),
 viscosity (EN ISO 3104),
 flash point (EN 22719),
 carbon residue (EN ISO 10370),
 cetane number (EN ISO 5165),
 ash content (ISO 6245),
 water content (EN ISO 12937),
 copper corrosion (EN ISO 2160),
 distillation (EN ISO 3405),
 pour point (ISO 3016),
 cloud point (EN 23015),
 lubricity (ISO 12156-1), and
 oxidation stability (EN ISO 12205).

EN ISO 13759 (determination of alkyl nitrate content) was tested and found adequate to be used on products

containing FAME. Cetane number was tested by another WG and found adequate, too.
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Annex A
(informative)
List of participants in working group 26 activities

The following people have been active in WG 26 "FAME related fuel test methods" and in the underlying laboratory

work.
Name Company
Mrs. M.F. BENASSY TOTALFINAELF (Convenor)
P. FERRARI EURON
Dr. T. FEUERHELM DIN/FAM
Dr. Ing. J CONNEMANN OELMUEHLE LEER CONNEMANN GmbH Co
Dipl. Ing. B. BLAICH Robert BOSCH GmbH FV/FLA
Dr. J. FISCHER AG QM Biodiesel e.V.
Dr. Ing. K. SCHARMER GET - Gesellschaft Für Entwicklungstechnik
Dr. Ing. TH. GOTTSCHAU FNR
X. MONTAGNE IFP
Mrs. N. DAVIAS RENAULT Technocentre
Ms. U. KIISKI FORTUM Oil and Gas OY, Technology Centre
D. KARNER OMV
Dr. F. van DIEVOET BfB Oil Research
Dott. P. TITTARELLI Stazione Sperimentale Combustibili
Dott. M. VIGO UNIONE PETROLIFERA
M.L. DAANE SHELL Research and Technology Centre
J. WOLDENDORP SHELL Research and Technology Centre
Dr. M. HUTTER IMU
B. DUFRENOY NOVAOL
Ms. F. LACOSTE ITERG
A. FRASER NOVAOL
R.W. HOOKS Shell Research Ltd. / R.W. HOOKS consultancy
F. TORT TOTALFINAELF
Ing. U. JANISCH OELMUEHLE LEER CONNEMANN GmbH Co
W. DORMER ARAL AG
J. PHIPPS INSTITUTE OF PETROLEUM
L. BURMAN SGS SWEDEN AB
U. OSTAN SAYBOLT SWEDEN AB
J. BERG SWEDISH Farmer Supply and Crop Marketing Association
D. MEHLIS PETRO LAB GmbH
T. WILHARM ASG
B. CAHILL PSA CITROEN/PEUGEOT
F. MORDRET ITERG
F. HEGER OMV
A. PHILIPPSEN OELMUEHLE LEER CONNEMANN GmbH Co
J. MUELLER_BELAU Deutsche Shell AG
11
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Dr. J. BOSSE VOLKSWAGEN AG
T.J. BERRYMAN TIM-BER Support
S. PAGLIANTI NOVOAL Srl
M. MARCHI IES Raffineria di Mantova
G. ARALDI TAMOIL
S. CATALANO SGS Redwood
G. LO BAIDO Esso Technical Services
G. PINELLI Stazione Sperimentale Combustibili
F. AVELLA Stazione Sperimentale Combustibili
E. COLOMBO SARPOM
Mrs. C. PUEL ELF ANTAR / TOTALFINAELF
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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)
B.1 Scope

In this round robin the applicability of test method EN ISO 3679 "Determination of flash point - Rapid equilibrium

close cup method" towards FAME as 100 % diesel fuel is investigated. The precision, repeatability and

reproducibility, for this product versus the stated precision for petroleum products were also investigated.

NOTE This study has been supervised by Mr. M.L. Daane and Mr. J. Woldendorp.
B.2 Assessed standard documents

EN 22719:1993, Petroleum products and lubricants – Determination of flash point – Pensky-Martens closed cup

method (ISO 2719:1988)

prEN ISO/DIS 3679:2002 – Determination of flash point - Rapid equilibrium closed cup method (ISO/DIS

3679:2002)

EN ISO 4259:1995, Petroleum products – Determination and application of precision data in relation to methods of

test (ISO 4259:1992, including Cor.1: 1993).
B.3 Background

The actual test method at the date of investigation for flash point for EN 590 diesel was EN 22719, the Pensky-

Martens closed cup test method . The applicability of this test method for 100 % FAME has been studied and

found unsuitable for two reasons.

1) the precision of this method for products containing trace amounts of highly flammable material in relatively

high flash point material is very poor;

NOTE The flash point for fatty acid methyl esters is high (> 160 °C). Methanol is used for the manufacturing of FAME.

Methanol is to a large extent removed from the final product, but remnants may still be present. The current specification for

100 % FAME allows 0,2 % (m/m) methanol max. Methanol as such has a flash point of 11 °C. The use of non-equilibrium test

methods for the determination of flash point for products containing trace amounts of highly flammable material (i.e. like FAME

containing methanol) give poor repeatable test results due to
i) non homogeneous heat transfer conditions, and
ii) unfavourable V/L (Vapour/Liquid) conditions in the test cup.

2) optical detection is unsuitable, because methanol burns (and flashes) with a colourless, invisible flame.

NOTE The flash point of FAME is caused by methanol, which gives a colourless, invisible flame. Even experienced

operators have difficulties to detect this flame using their eyes.

4 At the date of publication of this document a revision (EN ISO 2719) has been published in November 2002.

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SIST-TP CEN/TR 15160:2005
CEN/TR 15160:2005 (E)

Both procedures A and B of EN 22719 were tested (see Table B.1). Procedure A gave repeatable results for FAME

A, giving a greenish flame, caused by the FAME itself, i.e. all methanol is evaporated during the test without giving

a flash. Procedure A gave poorly repeatable results for FAME B. Procedure B gave poorly repeatable results for

FAME A and B. These results clearly demonstrated that EN 22719 is not applicable for 100 % FAME.

Based on the above, the most suitable test method is an equilibrium test method with a mandatory non-optical flash

detection. According to state of the art, EN ISO 3679 test method was considered to be most appropriate to run a

round robin with.
Table B.1 — Flash point determinations of 100 % FAME by EN 22719
FAME A FAME B
Procedure A Procedure B Procedure A Procedure B
166 (134 ) 160 (118 ) 126 116
a a
166 (132 ) 154 (122 ) 126 120
b
168 (120 ) 156 (118 ) 124 122
b a
(122 ) 160 (126 ) 128 124
140 130
134 134
148
very weak flash observed, flame blown out, no flame observed
flame blown out (sucked into the cup)
B.4 Pre-study for round robin with prEN ISO/DIS 3679
B.4.1 Set-up

The suitability of prEN ISO/DIS 3679 was initially tested at SRTCA. For this purpose a flash point tester was got on

loan. The first tests showed that repeatable flashpoints results for FAME, containing methanol at several

concentrations, can be achieved using this apparatus (see Figure B.1, flash point App. 1, 2 ml). Therefore SRTCA

decided to get possession of such a flash point tester. The samples, tested on apparatus 1, were also tested on

this new apparatus (see Figure B.1, flash point App. 2, 2 ml). It was noted that the flashpoints were somewhat

lower on apparatus 2. The curve through the flashpoints is S-shaped; the left end site is limited by the flash point of

FAME without methanol, the right end site is asymptotically limited by the flash point of methanol, the steep middle

of the curve is around the methanol concentration of 0,2 % (m/m) (i.e. the current FAME specification).

According to prEN ISO/DIS 3679, a specified volume is introduced into the test cup, which is maintained at the

temperature of the estimated flash point of the material under test. After a specified time, a test flame is applied and

the presence or absence of a flash observed. For flashpoints up to and including 100 °C, the specified test portion

is 2 ml and the specified time is 1 minute; for flashpoints above 100 °C the specified test portion is 4 ml and the

specified time is 2 min.
When 4
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