DRAFT

MALAYSIAN
STANDARD

14H003R1

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STAGE : PUBLIC COMMENT (40.20)

DATE : 01/06/2014 31/07/2014

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Automotive fuels - Palm Methyl Esters (PME)

for diesel engines - Requirements and test
methods
(First revision)

OFFICER/SUPPORT STAFF: (ZB/DN)

ICS: 76.160.20
Descriptors: automotive fuels, palm methyl esters(PME), diesel engines, requirements, test methods

Copyright 2014
DEPARTMENT OF STANDARDS MALAYSIA

14H003R1

Contents
Page

Committee representation .......................................................................................................... ii

Foreword.................................................................................................................................... iii

Scope.............................................................................................................................1

Normative references ....................................................................................................1

Definition ........................................................................................................................1

Sampling ........................................................................................................................1

Pump marking ...............................................................................................................1

Requirements and test methods....................................................................................2

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Tables

General applicable requirements and test methods ......................................................3

Reference test methods ................................................................................................5

B1

Precision data from interlaboratory test programme .....................................................9

Annexes

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Normative references ....................................................................................................6

Details of interlaboratory test programme .....................................................................9

Correction factor for calculation of density of FAME ...................................................10

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Bibliography ..............................................................................................................................11

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14H003R1

Committee representation
The Industry Standards Committee on Petroleum and Gas (ISC H) under whose authority this Malaysian Standard
was developed, comprises representatives from the following organisations:

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Association of Consulting Engineers Malaysia

Association of Malaysian Oil and Gas Engineering Consultants
Department of Occupational Safety and Health Malaysia
Department of Standards Malaysia
Federation of Malaysian Manufacturers - Malaysian Industrial Gases Manufacturers Group
Jabatan Bomba dan Penyelamat Malaysia
Jabatan Pengangkutan Jalan Malaysia
Kastam Diraja Malaysia
Malaysian Gas Association
Malaysian Palm Oil Board
Malaysian Plastics Manufacturers Association
Ministry of Domestic Trade, Co-operatives and Consumerism
Ministry of International Trade and Industry
Petroliam Nasional Berhad
PETRON Malaysia Refining and Marketing Berhad
PETRONAS Group Technology Solutions
Shell Malaysia Trading Sdn Bhd
SIRIM Berhad (Secretariat)
Suruhanjaya Tenaga
The Institution of Engineers, Malaysia
Universiti Teknologi Malaysia
Universiti Teknologi PETRONAS

The Technical Committee on Petroleum Fuels which developed this Malaysian Standard consists of representatives
from the following organisations:

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Automobile Association of Malaysia

Boustead Petroleum Marketing Sdn Bhd
Caltex Oil (M) Limited
Department of Environment
Department of Occupational Safety and Health Malaysia
Jabatan Pengangkutan Jalan Malaysia
Malaysian Automotive Association
Malaysian Palm Oil Board
Ministry of Domestic Trade, Co-operatives and Consumerism
Petroliam Nasional Berhad
PETRON Malaysia Refining and Marketing Berhad
PETRONAS Dagangan Berhad
PETRONAS Group Technical Solution
Science and Technology Research Institute for Defence
Shell Global Solutions Malaysia
Shell (M) Trading Sdn Bhd
Shell Refining Company (FOM) Berhad
SIRIM Berhad (Secretariat)
Universiti Kebangsaan Malaysia
Universiti Teknologi Malaysia
Co-opted members:

EU-Malaysia Chamber of Commerce and Industry

Malaysian Biodiesel Association
PETRON Malaysia Refining and Marketing Berhad (Refinery)

ii

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14H003R1

Foreword
This Malaysian Standard was developed by the Technical Committee on Petroleum Fuels
under the authority of the Industry Standards Committee on Petroleum and Gas.
In the preparation of this standard, reference was made to EN 14214:2012, Liquid petroleum
products - Fatty acid methyl esters (FAME) for use in diesel engines and heating applications
- Requirements and test methods.
Major modifications in this revision are as follows:
a) definition of PME has been introduced;
b) background information for national climate grades selection has been removed;
an update of the specification in the perspective of blending at up to 10% (v/v) of PME in
automotive diesel fuel;

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c)

d) deletion of the requirement on carbon residue as it is no longer considered necessary;

f)

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e) an increase of oxidation stability requirement from 6 h minimum to 10 h minimum;

a decrease of the monoglycerides content from 0.8 % (m/m) to 0.7 % (m/m);

g) a decrease of the phosphorus content from 10 mg/kg maximum to 4 mg/kg maximum;

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h) introduction of additionally developed test methods for flash point, oxidation stability,
iodine value and sulfur content, ISO 2719, EN 15751, EN 16300 and ISO 13032,
respectively. Plus updating toward revised sulfur and sulfated ash content determination
test methods;
updating of test methods on esters, (mono) glycerides, polyunsaturated fatty acids and
stability characteristics of PME; and

j)

a re-evaluation of Table B1.

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i)

This standard is to read in conjunction with MS 123-1 and MS 123-2.

This Malaysian Standard cancels and replaces MS 2008:2008, Automotive fuels - Palm
Methyl esters (PME) for diesel engines - Requirements and test methods.
Compliance with a Malaysian Standard does not of itself confer immunity from legal
obligations.

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iii

14H003R1

Automotive fuels - Palm Methyl Esters (PME) for diesel engines Requirements and test methods (First revision)
1

Scope

This Malaysian Standard specifies requirements and test methods for marketed and delivered
Palm methyl esters (PME) to be used either as automotive fuel for diesel engines at 100 %
concentration, or as an extender for automotive fuel for diesel engines in accordance with the
requirements of MS 123. At 100 % concentration it is applicable to fuel for use in diesel
engine vehicles designed or subsequently adapted to run on 100 % PME. The standard is
meant for domestic consumption and automotive application only. The methyl ester is NOT to
be derived from used oil.

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NOTE. For the purposes of this Malaysian Standard, the term % (m/m) is used to represent the mass fraction.

Normative references

The documents and publications referred to in this standard are listed in Annex A.

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Refer to Annex A.

Definition

Palm methyl ester (PME)

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For the purposes of this standard, the following definition applies.

Sampling

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Methyl ester derived from palm oil and palm oil products.

Samples shall be taken as described in ISO 3170 or ISO 3171 and ISO 5555 and/or in
accordance with the requirements of regulations for the sampling of automotive diesel fuel.
In view of the sensitivity of some of the test methods referred to in Table 1, particular attention
shall be paid to compliance with any guidance on sampling containers, which is included in
the test method standards.

Pump marking

Information to be marked on dispensing pumps used for delivering PME diesel fuel and the
dimensions of the mark shall be in accordance with the requirements of regulations for the
marking of pumps for automotive diesel fuel.

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6
6.1

Requirements and test methods

Dyes and markers

The use of dyes or markers is allowed.

6.2

Additives

6.2.1 General
In order to improve the performance quality, the use of additives is allowed. Suitable fuel
additives without known harmful side effects are recommended in the appropriate amount, to
help to avoid deterioration of driveability and emissions control durability. Other technical
means with equivalent effect may also be used.

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NOTE. Deposit forming tendency test methods suitable for routine control purposes have not yet been identified and
developed.

6.2.3 Oxidation stability enhancing additives

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In order to improve the oxidation stability of PME, it is recommended to add oxidation stability
enhancing additives to PME at the production stage and before storage, providing an
oxidation stability similar to that obtained with 1 000 mg/kg of 2,6-di-tert-butyl-4hydroxytoluene (BHT).
6.2.3 Non-PME Components

Generally applicable requirements and related test methods

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The addition of non-PME components (other than additives) such as diesel or other
hydrocarbons prior to testing PME for compliance with the MS 2008 specification is not
permitted.

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6.3.1
When tested by the methods indicated in Table 1, PME shall be in accordance with
the limits specified in Table 1. The test methods listed in Table 1 have been shown to be
applicable to PME in an interlaboratory test programme. Precision data from this programme
are given in Annex B, where these were found to be different from the precision data given in
the test methods for petroleum products.
6.3.2
In case of a need for identification of PME, a recommended method based on
separation and characterisation PME by LC/GC is EN 14331 [1].
6.3.3
PME shall be free from any adulterant or contaminant that may render the fuel
unacceptable for use in diesel engine vehicles.

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Table 1. General applicable requirements and test methods

Property

Unit

Limits
Minimum
Maximum
b
96.5
860
900

% (m/m)
kg/m3

Total contamination
Copper strip corrosion (3 h at
50 C)

mg/kg
rating

Oxidation stability, 110 C

hours

10.0

mg
KOH/g

0.50

g iodine/
100 g
% (m/m)

110

12.0

EN 14103
ISO 3675d
ISO 12185
ASTM D 4052
ASTM D 1298
ISO 3104d
ASTM D 445
ISO 2719d
ISO 3679f
ASTM D 93
ISO 20846d
ISO 20884
ISO 13032
ASTM D 5453
ISO 5165d
ASTM D 613
ASTM D 6890
ISO 3987d
ASTM D 874
ISO 12937d
ASTM E 203
ASTM D 6304
EN 12662h
ISO 2160d
ASTM D 130
EN 14112d
EN 15751
EN 14104d
ASTM D 664
EN 14111d
EN 16300
EN 14103

Viscosity at 40 C

mm2/s

3.50

5.00

120

mg/kg

10.0

% (m/m)

EN 15779

% (m/m)
% (m/m)

0.20
0.70

EN 14110
EN 14105d
ASTM D 6584

Sulfur content

Cetane numbere,g

Sulfated ash content

% (m/m)
mg/kg

Acid value

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Water content

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51.0

Iodine value
Linolenic acid methyl ester
Polyunsaturated (4 double
bonds) methyl esters
Methanol content
Monoglyceride content

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Flash pointe

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FAME content
Density at 15 Cc

Test methodsa

0.02

500

24
Class 1

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Table 1. General applicable requirements and test methods (continued)

Property

Unit

Limits
Minimum
Maximum

% (m/m)

0.20

Triglyceride content

% (m/m)

0.20

Free glycerol

% (m/m)

0.02

Total glycerol

% (m/m)

0.25

Group I metal (Na + K) f

mg/kg

5.0

Group II metals (Ca + Mg)

Phosphorus content

mg/kg
mg/kg
C

5.0
4.0

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CFPP

EN 14105d
ASTM D 6584
EN 14105d
ASTM D 6584
EN 14105d
EN 14106
ASTM D 6584
EN 14105d
ASTM D 6584
EN 14108d
EN 14109
EN 14538
EN 14538
EN 14107d
ASTM D 4951
EN 116

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Diglyceride content

Test methodsa

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6.4.1

Precision and dispute

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See 6.4.1
b
The addition of non-PME components other than additives is not allowed, see 6.2.
c
Density may be measured by ISO 3675 over a range of temperatures from 20 C to 60 C. Temperature
correction shall be made according to the formula given in Annex C.
d
See 6.4.2.
e
See Annex B for precision data.
f
A 2 ml sample and apparatus equipped with a thermal detection device shall be used.
g
See 6.4.3.
h
This test method developed for diesel fuel may show analytical problem when applied to PME. A more suitable
test method in under development by CEN.

Precision and dispute

All test methods referred to Table 1 include a precision statement according to ISO 4259. In
cases of dispute, the procedures described in ISO 4259 shall be used for resolving the
dispute, and interpretation of the results based on the test method precision, or, where
precision data is known to be different for PME as listed in Annex C, precision data from
Annex B, shall be used.
6.4.2 In cases of dispute concerning properties in Table 1, the Table 2 below indicates
reference test method shall apply.

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Table 2. Reference test methods

Reference test method

Density

ASTM D 4052

Viscosity

ASTM D 445

Flash point

ASTM D 93

Sulfur content

ASTM D 5453

Cetane number

ASTM D 613

Sulfated ash content

ASTM D 874

Water content

ISO 12937

Copper strip corrosion

ASTM D 130

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Property

EN 14104

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Acid value
Monoglyceride content

Triglyceride content

EN 14105

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Free glycerol

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Diglyceride content

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Total glycerol

EN 14107

Oxidation stability

EN 15751

Iodine value

EN 14111

Group I metals (Na+K)

EN 14538

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Phosphorus content

6.4.3
For the determination of cetane number alternative methods may also be used in
cases of dispute, provided that these methods originate from a recognised method series,
and have a valid precision statement, derived in accordance with ISO 4259, which
demonstrates precision at least equal to that of the referenced method. The test result, when
using an alternative method, shall also have a demonstrable relationship to the result
obtained when using the reference method.

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Annex A
(normative)
Normative references
The following normative references are indispensable for the application of this standard. For
dated references, only the edition cited applies. For undated references, the latest editions of
the normative references (including any amendments) apply:
MS 123-1, Diesel fuel - Specification - Part 1: Euro 2M
MS 123-2, Diesel fuel - Specification - Part 2: Euro 4M

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ISO 2160, Petroleum products Corrosiveness to copper Copper strip test

ISO 2719, Determination of flash point - Pensky-Martens closed cup method

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ISO 3104, Cor 1, Petroleum products Transparent and opaque liquids Determination of
kinematic viscosity and calculation of dynamic viscosity
ISO 3170, Petroleum liquids Manual sampling

ISO 3171, Petroleum liquids Automatic pipeline sampling

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ISO 3675, Crude petroleum and liquid petroleum products Laboratory determination of
density Hydrometer method

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ISO 3679, Determination of flash point Rapid equilibrium closed cup method

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ISO 3987, Petroleum products Lubricating oils and additives Determination of sulfated ash

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ISO 4259, Petroleum products Determination and application of precision data in relation to
methods of test
ISO 5165, Petroleum products Diesel fuels Determination of the ignition quality of diesel
fuels Cetane engine method
ISO 5555, Animal and vegetable fats and oils Sampling
ISO 12185, Cor 1, Crude petroleum and petroleum products Determination of density
Oscillating U-tube method
ISO 12937, Petroleum products Determination of water Coulometric Karl Fisher titration
method
ISO 13032, Petroleum products - Determination of low concentration of sulfur in automotive
fuels - Energy-dispersive X-ray fluorescence spectrometric method

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ISO 20846, Petroleum products Determination of the sulfur content of automotive fuels
Ultraviolet X-ray fluorescence method
ISO 20884, Petroleum products Determination of sulfur content of automotive fuels
Wavelength-dispersive X-ray fluorescence spectrometry
EN 116, Diesel and domestic heating fuels Determination of cold filter plugging point
EN 12662, Liquid petroleum products Determination of contamination in middle distillates
EN 14103, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of ester
and linolenic acid methyl ester contents
EN 14104, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of acid
value

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EN 14105, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of free
and total glycerol and mono-, di- and triglyceride content - (Reference method)

EN 14106, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of free
glycerol content

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EN 14107, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of
phosphorus content by inductively coupled plasma (ICP) emission spectrometry
EN 14108, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of
sodium content by atomic absorption spectrometry

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EN 14109, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of
potassium content by atomic absorption spectrometry

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EN 14110, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of
methanol content

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EN 14111, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of
iodine value
EN 14112, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of
oxidation stability (accelerated oxidation test)
EN 14538, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of Ca
K, Mg and Na content by optical emission spectral analysis with inductively coupled plasma
(ICP OES)
EN 15751, Automotive fuels - Fatty acid methyl ester (FAME) fuel and blends with diesel fuel
- Determination of oxidation stability by accelerated oxidation method
EN 15779, Petroleum products and fat and oil derivates - Fatty acid methyl esters (FAME) for
diesel engines - Determination of polyunsaturated (4 double bonds) fatty acid methyl esters
(PUFA) by gas chromatography
EN 16300, Automotive fuels - Determination of iodine value in fatty acid methyl esters (FAME)
- Calculation method from gas chromatographic data
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ASTM D 93, Test method for flash-point by Pensky-Martens closed cup tester
ASTM D 130, Test method for corrosiveness to copper from petroleum products by copper
strip test
ASTM E 203, Standard test method for water using volumetric Karl Fischer titration
ASTM D 445, Test method for kinematic viscosity of transparent and opque (and the
calculation of dynamic viscosity)
ASTM D 613, Test method for cetane number of diesel fuel oil
ASTM D 664, Test method for acid number of petroleum products by potentiometric titration
ASTM D 874, Standard test method for sulfated ash from lubricating oils and additives

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ASTM D 4052, Standard test method for density and relative density of liquids by digital
density meter

ASTM D 5453, Standard test method for determination of total sulfur in light hydrocarbons,
spark ignition engine fuel, diesel engine fuel, and engine oil by ultraviolet fluorescence

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ASTM D 6584, Standard test method for determination of free and total glycerin in B-100
biodiesel methyl esters by gas chromatography
ASTM D 4951, Standard test method for determination of additive elements in lubricating oils
by inductively coupled plasma atomic emission spectrometry

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ASTM D 6890, Standard test method for determination of ignition delay and derived Cetane
Number (DCN) of diesel fuel oils by combustion in a constant volume chamber

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ASTM D 1298, Standard test method for density, relative density (Specific gravity), or API
gravity of crude petroleum and liquid petroleum products by hydrometer method

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ASTM D 6304, Standard test method for determination of water in petroleum products,
lubricating oils, and additives by Coulometric Karl Fischer Titration

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Annex B
(normative)
The precision data given in Table B1 apply in the case of fatty acid methyl esters (FAME), as
far as not already indicated in the standard. In Table B1 only those data for requirements from
standardised test methods that differ from ISO/TC 28 or ASTM precision data are given. More
details are available in the interlaboratory test report [5].
Table B1. Precision data from interlaboratory test programme
Property
Flash point

Test method

CEN/TC 19 data for pure

FAME

Unit

ISO 2719

r = 2.4
R = 11.4

ISO 5165

r = 2.4

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Cetane number

R = 5.0
EN 14108

mg/kg

r = -0.017 X + 0.512

Sum of Na + K

R = 0.305 X 1.980

where,

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EN 14109

is the repeatablity (ISO 4259);

is the reproducibility (ISO 4259); and

is the mean of two results being compared.

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Annex C
(normative)
Correction factor for calculation of density of FAME
The conversion factor for the correction of density, determined by ISO 3675 over a range of
temperatures from 20 C to 60 C, to density at 15 C is based on data published at the
International Conference on Standardization and Analysis of Biodiesel, Vienna, November
1995 [6].

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The density of seven samples of FAME was measured by pyknometer at 6 temperatures over
the range 20 C to 60 C. The mean correction factor over the range was calculated as 0.723
kg/(m3 C), with a standard deviation of 1.2 %. The average density of the FAME samples at
15 C was calculated as 886.5 kg/m3.

The following formula shall be used for the calculation of density of FAME at 15 C ((15),
given in kg/m3), using the density ((T)) at a certain temperature (T), determined by ISO 3675
over the range of temperatures from 20 C to 60 C:

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(15) = (T) + 0.723(T 15)

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Bibliography
[1] EN 14331, Liquid petroleum products - Separation and characterisation of fatty acid
methyl esters (FAME) from middle distillates - Liquid chromatography (LC)/gas
chromatography (GC) method
[2] CEN/TR 15367-1, Petroleum products - Guide for good housekeeping - Part 1:
Automotive diesel fuels
[3] EN 16091:2011, Liquid petroleum products - Middle distillates and fatty acid methyl ester
(FAME) fuels and blends - Determination of oxidation stability by rapid small scale oxidation
method

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[4] Guidelines for handling and blending of FAME, CONCAWE report 9/09, available from
Concawe, Brussels, Belgium (www.concawe.org)

[5] 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

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[6] J. Rathbauer & A. Bachler, Physical Properties of Vegetable Oil Methyl Esters,
International Conference on Standardization and Analysis of Biodiesel, November 6th 7th,
1995, Vienna
[7] S. Schober, I. Seidl and M. Mittelbach, Ester content evaluation in biodiesel from animal
fats and lauric oils, Eur. J. Lipid Sci. Technol. 108 (2006) 309314

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[8] EN ISO 13759:1996, Petroleum products - Determination of alkyl nitrate in diesel fuels Spectrometric method (ISO 13759:1996)

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Acknowledgements

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Co-opted members

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Members of Technical Committee on Petroleum Fuels

Name
Organisation
Prof Dr Abu Bakar Mohamad (Chairman)
Universiti Kebangsaan Malaysia
Mr Chan Keng Sam (Deputy Chairman)
Science and Technology Research Institute
for Defence
Ms Zuraidah Baba (Secretary)
SIRIM Berhad
Mr Ahmed Ismail Amin
Automobile Association of Malaysia
Mr Tan Kwang Weng
Boustead Petroleum Marketing Sdn Bhd
Mr Philip Chee
Caltex Oil (M) Limited
Department of Environment
Mr Ryan Ooi/
Mr Nur Mizhuari Haji Abdul Samat
Mr Ahamad Yani Mohamad
Department of Occupational Safety and Health
Malaysia
Mr Azizul Abdul Aziz
Jabatan Pengangkutan Jalan Malaysia
Mr Liew Wei Jye
Malaysian Automotive Association
Datuk Dr Choo Yuen May/
Malaysian Palm Oil Board
Mr Yung Chee Liang/
Dr Harrison Lau Lik Nang
Ms Masturah Abd Aziz
Ministry of Domestic Trade, Co-operatives and
Consumerism
Mr Fazil Mat Isa
Petroliam Nasional Berhad
PETRON Malaysia Refining and Marketing
Mr Chew Choy/
Berhad
Mr Teh Hock Xiong
Ms Ramona Nazreen Abdul Rahman/
PETRONAS Dagangan Berhad
Mr Mohamad Hafiz Abd Aziz
Mr Abd Rahim Othman
PETRONAS Group Technical Solution
Ir Loke Ean Bee/
Shell Global Solutions Malaysia
Mr Colin Chin
Mr Ho Meng Tuck
Shell (M) Trading Sdn Bhd
Mr Peter Law
Shell Refining Company (FOM) Berhad
Assoc Prof Dr Normah Mulop
Universiti Teknologi Malaysia

Mr Klaus Laudhaeusser/
Mr Frank Mccluskey
Ms Aiman Najati Akmar Rahman/
Ms Chan Yuen Teng
Mr Mohd Rizal Osman

EU-Malaysia Chamber of Commerce and

Industry
Malaysian Biodiesel Association
PETRON Malaysia Refining and Marketing
Berhad (Refinery)

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