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DRAFT MALAYSIAN 14H003R1STANDARD

STAGE : PUBLIC COMMENT (40.20) DATE : 01/06/2014 31/07/2014

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

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STANDARDS MALAYSIA 2014 - All rights reserved i

Contents

Page Committee representation .......................................................................................................... ii Foreword .................................................................................................................................... iii 1 Scope ............................................................................................................................. 1 2 Normative references .................................................................................................... 1 3 Definition ........................................................................................................................ 1 4 Sampling ........................................................................................................................ 1 5 Pump marking ............................................................................................................... 1 6 Requirements and test methods.................................................................................... 2 Tables 1 General applicable requirements and test methods ...................................................... 3 2 Reference test methods ................................................................................................ 5 B1 Precision data from interlaboratory test programme ..................................................... 9 Annexes A Normative references .................................................................................................... 6 B Details of interlaboratory test programme ..................................................................... 9 C Correction factor for calculation of density of FAME ................................................... 10 Bibliography .............................................................................................................................. 11

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ii STANDARDS MALAYSIA 2014 - All rights reserved

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: 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: 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)

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STANDARDS MALAYSIA 2014 - All rights reserved iii

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; c) an update of the specification in the perspective of blending at up to 10% (v/v) of PME in

automotive diesel fuel; d) deletion of the requirement on carbon residue as it is no longer considered necessary; e) an increase of oxidation stability requirement from 6 h minimum to 10 h minimum; f) 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; 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;

i) updating of test methods on esters, (mono) glycerides, polyunsaturated fatty acids and

stability characteristics of PME; and j) a re-evaluation of Table B1. 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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STANDARDS MALAYSIA 2014 - All rights reserved 1

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. NOTE. For the purposes of this Malaysian Standard, the term % (m/m) is used to represent the mass fraction. 2 Normative references The documents and publications referred to in this standard are listed in Annex A. Refer to Annex A. 3 Definition For the purposes of this standard, the following definition applies. 3.1 Palm methyl ester (PME) Methyl ester derived from palm oil and palm oil products. 4 Sampling 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. 5 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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2 STANDARDS MALAYSIA 2014 - All rights reserved

6 Requirements and test methods 6.1 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. 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 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-4-hydroxytoluene (BHT). 6.2.3 Non-PME Components 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. 6.3 Generally applicable requirements and related test methods 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 Test methodsa

Minimum Maximum FAME content % (m/m) 96.5b - EN 14103 Density at 15 Cc kg/m3 860 900 ISO 3675d

ISO 12185 ASTM D 4052 ASTM D 1298

Viscosity at 40 C mm2/s 3.50 5.00 ISO 3104d

ASTM D 445 Flash pointe C 120 - ISO 2719d

ISO 3679f ASTM D 93

Sulfur content mg/kg - 10.0 ISO 20846d

ISO 20884 ISO 13032

ASTM D 5453 Cetane numbere,g 51.0 - ISO 5165d

ASTM D 613 ASTM D 6890

Sulfated ash content % (m/m) - 0.02 ISO 3987d

ASTM D 874 Water content mg/kg - 500 ISO 12937d

ASTM E 203 ASTM D 6304

Total contamination mg/kg - 24 EN 12662h Copper strip corrosion (3 h at 50 C)

rating Class 1 ISO 2160d

ASTM D 130 Oxidation stability, 110 C hours 10.0 - EN 14112d

EN 15751 Acid value mg

KOH/g - 0.50 EN 14104d

ASTM D 664 Iodine value g iodine/

100 g - 110 EN 14111d

EN 16300 Linolenic acid methyl ester % (m/m) - 12.0 EN 14103

Polyunsaturated (4 double bonds) methyl esters

% (m/m) - 1 EN 15779

Methanol content % (m/m) - 0.20 EN 14110 Monoglyceride content % (m/m) - 0.70 EN 14105d

ASTM D 6584

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

Property Unit Limits Test methodsa

Minimum Maximum Diglyceride content % (m/m) - 0.20 EN 14105d

ASTM D 6584 Triglyceride content % (m/m) - 0.20 EN 14105d

ASTM D 6584 Free glycerol % (m/m) - 0.02 EN 14105d

EN 14106 ASTM D 6584

Total glycerol % (m/m) - 0.25 EN 14105d

ASTM D 6584 Group I metal (Na + K) f

mg/kg

- 5.0

EN 14108d

EN 14109 EN 14538

Group II metals (Ca + Mg) mg/kg 5.0 EN 14538 Phosphorus content mg/kg - 4.0 EN 14107d

ASTM D 4951 CFPP C - 15 EN 116 a 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.

6.4 Precision and dispute 6.4.1 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

Property

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

Acid value EN 14104

Monoglyceride content

EN 14105

Diglyceride content

Triglyceride content

Free glycerol

Total glycerol

Phosphorus content EN 14107

Oxidation stability EN 15751

Iodine value EN 14111

Group I metals (Na+K) EN 14538

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 ISO 2160, Petroleum products Corrosiveness to copper Copper strip test ISO 2719, Determination of flash point - Pensky-Martens closed cup method 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 ISO 3675, Crude petroleum and liquid petroleum products Laboratory determination of density Hydrometer method ISO 3679, Determination of flash point Rapid equilibrium closed cup method ISO 3987, Petroleum products Lubricating oils and additives Determination of sulfated ash 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 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 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 EN 14109, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of potassium content by atomic absorption spectrometry EN 14110, Fat and oil derivatives Fatty Acid Methyl Esters (FAME) Determination of methanol content 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 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 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 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 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 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 Test method Unit CEN/TC 19 data for pure FAME

Flash point ISO 2719 C r = 2.4 R = 11.4

Cetane number ISO 5165 r = 2.4 R = 5.0

Sum of Na + K EN 14108 EN 14109

mg/kg r = -0.017 X + 0.512 R = 0.305 X 1.980

where,

r is the repeatablity (ISO 4259);

R is the reproducibility (ISO 4259); and

X 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]. 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:

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

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STANDARDS MALAYSIA 2014 - All rights reserved

Acknowledgements Members of Technical Committee on Petroleum Fuels Name OrganisationProf 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 BerhadMr Ahmed Ismail Amin Automobile Association of Malaysia Mr Tan Kwang Weng Boustead Petroleum Marketing Sdn Bhd Mr Philip Chee Caltex Oil (M) LimitedMr Ryan Ooi/ Department of EnvironmentMr 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 Mr Chew Choy/ Mr Teh Hock Xiong

PETRON Malaysia Refining and Marketing Berhad

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 Co-opted members Mr Klaus Laudhaeusser/ Mr Frank Mccluskey

EU-Malaysia Chamber of Commerce and Industry

Ms Aiman Najati Akmar Rahman/ Malaysian Biodiesel Association Ms Chan Yuen Teng Mr Mohd Rizal Osman PETRON Malaysia Refining and Marketing

Berhad (Refinery)

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