Petroleum and natural gas industries - Evaluation and testing of thread compounds for use with casing, tubing, line pipe and drill stem elements (ISO 13678:2009)

ISO 13678:2009 provides requirements, recommendations and methods for the testing of thread compounds intended for use on ISO/API thread forms, as well as proprietary casing, tubing, line pipe and drill stem elements with rotary shouldered connections. The tests outlined are used to evaluate the critical performance properties and physical and chemical characteristics of thread compounds under laboratory conditions.
These test methods are primarily intended for thread compounds formulated with a lubricating base grease and are not applicable to some materials used for lubricating and/or sealing thread connection. It is recognized that many areas can have environmental requirements for products of this type. ISO 13678:2009 does not include requirements for environmental compliance.

Erdöl- und Erdgasindustrie - Beurteilung und Prüfung von Gewindefetten zur Verwendung an Futter-, Steig- und Leitungsrohren und an Bohrgestängeteilen (ISO 13678:2009)

Industries du pétrole et du gaz naturel - Évaluation et essais des graisses pour filetage utilisées pour les tubes de cuvelage, les tubes de production, les tubes de conduites et les éléments de garnitures de forage (ISO 13678:2009)

L'ISO 13678:2009 fournit des exigences, des recommandations et des méthodes pour les essais des graisses pour filetage à utiliser sur des formes de filetage ISO/API aussi bien que pour des spécialités de tubes de cuvelage, tubes de production, tubes de conduites et éléments de garnitures de forage à connexions rotatives à épaulement. Les essais décrits dans la présente Norme internationale sont utilisés pour évaluer les caractéristiques de performance critiques des graisses pour filetage et leurs caractéristiques physicochimiques dans des conditions de laboratoire.
Ces méthodes d'essai sont principalement indiquées pour les graisses pour filetage formulées à partir d'une graisse lubrifiante de base et peuvent ne pas être applicables à certains produits utilisés pour la lubrification et/ou l'étanchéité des connexions filetées. Il est admis que beaucoup de zones d'exploitation peuvent avoir des exigences environnementales pour ce type de produits. L'ISO 13678:2009 ne comprend pas d'exigences pour la mise en conformité environnementale.

Industrija za predelavo nafte in zemeljskega plina - Ovrednotenje in preskušanje navojnih spojev za uporabo pri zaščitnih, proizvodnih (dvižnih) in vrtalnih elementih (ISO 13678:2009)

General Information

Status
Withdrawn
Publication Date
14-May-2009
Withdrawal Date
17-Jan-2012
Current Stage
9960 - Withdrawal effective - Withdrawal
Due Date
18-Jan-2012
Completion Date
18-Jan-2012

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Erdöl- und Erdgasindustrie - Beurteilung und Prüfung von Gewindefetten zur Verwendung an Futter-, Steig- und Leitungsrohren und an Bohrgestängeteilen (ISO 13678:2009)Industries du pétrole et du gaz naturel - Évaluation et essais des graisses pour filetage utilisées pour les tubes de cuvelage, les tubes de production, les tubes de conduites et les éléments de garnitures de forage (ISO 13678:2009)Petroleum and natural gas industries - Evaluation and testing of thread compounds for use with casing, tubing, line pipe and drill stem elements (ISO 13678:2009)75.180.10Oprema za raziskovanje in odkopavanjeExploratory and extraction equipmentICS:Ta slovenski standard je istoveten z:EN ISO 13678:2009SIST EN ISO 13678:2009en,fr01-julij-2009SIST EN ISO 13678:2009SLOVENSKI

STANDARD
SIST EN ISO 13678:2009

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN ISO 13678May 2009ICS 75.180.10 English VersionPetroleum and natural gas industries - Evaluation and testing ofthread compounds for use with casing, tubing, line pipe and drillstem elements (ISO 13678:2009)Industries du pétrole et du gaz naturel - Évaluation etessais des graisses pour filetage utilisées pour les tubes decuvelage, les tubes de production, les tubes de conduiteset les éléments de garnitures de forage (ISO 13678:2009)Erdöl- und Erdgasindustrie - Beurteilung und Prüfung vonGewindefetten zur Verwendung an Futter-, Steig- undLeitungsrohren und an Bohrgestängeteilen (ISO13678:2009)This European Standard was approved by CEN on 30 April 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre:

Avenue Marnix 17,

B-1000 Brussels© 2009 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 13678:2009: ESIST EN ISO 13678:2009

EN ISO 13678:2009 (E) 2 Contents Page Foreword ..............................................................................................................................................................3 SIST EN ISO 13678:2009

EN ISO 13678:2009 (E) 3 Foreword This document (EN ISO 13678:2009) has been prepared by Technical Committee ISO/TC 67 "Materials, equipment and offshore structures for petroleum and natural gas industries" in collaboration with Technical Committee CEN/TC 12 “Materials, equipment and offshore structures for petroleum, petrochemical and natural gas industries” the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by November 2009, and conflicting national standards shall be withdrawn at the latest by November 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 13678:2009 has been approved by CEN as a EN ISO 13678:2009 without any modification.

SIST EN ISO 13678:2009
SIST EN ISO 13678:2009
Reference numberISO 13678:2009(E)© ISO 2009

INTERNATIONAL STANDARD ISO13678Second edition2009-05-15Petroleum and natural gas industries — Evaluation and testing of thread compounds for use with casing, tubing, line pipe and drill stem elements Industries du pétrole et du gaz naturel — Évaluation et essais des graisses pour filetage utilisées pour les tubes de cuvelage, les tubes de production, les tubes de conduites et les éléments de garnitures de forage

SIST EN ISO 13678:2009

ISO 13678:2009(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.

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ISO 2009 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO's member body in the country of the requester. ISO copyright office Case postale 56 • CH-1211 Geneva 20 Tel.

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ii © ISO 2009 – All rights reserved
SIST EN ISO 13678:2009

ISO 13678:2009(E) © ISO 2009 – All rights reserved iiiContents Page Foreword............................................................................................................................................................iv Introduction........................................................................................................................................................v 1 Scope......................................................................................................................................................1 2 Conformance..........................................................................................................................................1 2.1 Dual citing of normative references.....................................................................................................1 2.2 Units of measurement...........................................................................................................................1 3 Normative references............................................................................................................................2 4 Terms and definitions...........................................................................................................................3 5 Thread compound characteristics.......................................................................................................4 5.1 Product characteristics.........................................................................................................................4 5.2 Physical and chemical characteristics................................................................................................5 6 Thread compound performance properties........................................................................................9 6.1 Small-scale test......................................................................................................................................9 6.2 Frictional properties..............................................................................................................................9 6.3 Extreme surface-contact pressure (gall resistance) properties for casing, tubing and line pipe........................................................................................................................................................10 6.4 Fluid sealing properties for casing, tubing and line pipe................................................................11 7 Quality assurance and control...........................................................................................................11 8 Marking requirements.........................................................................................................................12 8.1 Marking.................................................................................................................................................12 8.2 Labelling...............................................................................................................................................12 Annex A (informative)

API modified thread compound.................................................................................13 Annex B (normative)

Casing, tubing and line pipe reference standard formulation.................................17 Annex C (normative)

Penetration test.............................................................................................................19 Annex D (normative)

Evaporation test............................................................................................................20 Annex E (normative)

Oil separation test.........................................................................................................21 Annex F (normative)

Application/adherence test..........................................................................................22 Annex G (normative)

Gas evolution test.........................................................................................................23 Annex H (normative)

Water leaching test.......................................................................................................27 Annex I (informative)

Frictional properties test.............................................................................................30 Annex J (informative)

Extreme surface-contact pressure (galling) test for casing, tubing and line pipe........................................................................................................................................................40 Annex K (informative)

Fluid sealing test for casing, tubing and line pipe..................................................41 Annex L (informative)

Corrosion inhibition tests...........................................................................................44 Annex M (informative)

Compound high-temperature stability test..............................................................45 Bibliography......................................................................................................................................................46

SIST EN ISO 13678:2009

ISO 13678:2009(E) iv © ISO 2009 – All rights reserved Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 13678 was prepared by Technical Committee ISO/TC 67, Materials, equipment and offshore structures for petroleum, petrochemical and natural gas industries, Subcommittee SC 5, Casing, tubing and drill pipe. This second edition cancels and replaces the first edition (ISO 13678:2000), which has been technically revised. It is the intent of ISO/TC 67 that the first and second editions of ISO 13678 both be applicable, at the option of the purchaser, for a period of six months from the first day of the calendar quarter immediately following the date of publication of this second edition, after which period the first edition will no longer be applicable. SIST EN ISO 13678:2009

ISO 13678:2009(E) © ISO 2009 – All rights reserved vIntroduction This International Standard is based on API RP 5A3 [5], second edition, July 2003, with errata and inclusion of all clauses of API RP 7A11) [6], first edition, November 1992, incorporated into Annex I. This International Standard specifies requirements and gives recommendations for the manufacture, testing and selection of thread compounds for use on casing, tubing, line pipe and drill stem elements based on the current industry consensus of good engineering practice. It is intended that the words casing and tubing apply to the service application, rather than to the diameter of the pipe. The performance requirements of thread compounds for use with casing, tubing, line pipe, premium connections and rotary shouldered connections include: ⎯ consistent frictional properties that allow both proper and uniform connection engagement; ⎯ adequate lubrication properties to resist galling or damage of connection contact surfaces during make-up and breakout; ⎯ adequate sealing properties for thread-type seal connections and/or not inhibiting the sealing properties of non-thread sealing connections (e.g. metal-to-metal seals, polytetrafluoroethylene (PTFE) seals, etc.) depending upon service requirements; ⎯ physical and chemical stability both in service and in expected compound storage conditions; ⎯ properties that allow effective application to the connection contact surfaces in expected service conditions and environment. In addition, compounds for rotary shouldered connections provide: ⎯ lubrication of the connection members during make-up to achieve the proper axial bearing stress; ⎯ an effective seal between connection shoulders to prevent wash-out by drilling fluids; ⎯ more uniform distribution of circumferential bearing stress if shoulders are not parallel; ⎯ resistance to additional make-up down hole. When evaluating the suitability of a thread compound, the user can define the service conditions and then consider field trials and field service experience in addition to laboratory test results. Appropriate supplementary tests can be utilized for specific applications which are not evaluated by the tests herein. The user and manufacturer are encouraged to discuss service applications and limitations of the compound being considered. Representatives of users and/or other third party personnel are encouraged to monitor tests wherever possible. Interpolation and extrapolation of test results to other products, even of similar chemical composition, is not recommended.

1) Obsolete. Incorporated into this International Standard. SIST EN ISO 13678:2009

ISO 13678:2009(E) vi © ISO 2009 – All rights reserved Testing in compliance with this International Standard does not in and of itself ensure adequate thread compound/connection system performance in field service. The user has the responsibility of evaluating the results obtained from the recommended procedures and test protocols and determining whether the thread compound/connection system in question meets the anticipated requirements of that particular field service application. SIST EN ISO 13678:2009

INTERNATIONAL STANDARD ISO 13678:2009(E) © ISO 2009 – All rights reserved 1Petroleum and natural gas industries — Evaluation and testing of thread compounds for use with casing, tubing, line pipe and drill stem elements 1 Scope This International Standard provides requirements, recommendations and methods for the testing of thread compounds intended for use on ISO/API thread forms, as well as proprietary casing, tubing, line pipe and drill stem elements with rotary shouldered connections. The tests outlined are used to evaluate the critical performance properties and physical and chemical characteristics of thread compounds under laboratory conditions. These test methods are primarily intended for thread compounds formulated with a lubricating base grease and are not applicable to some materials used for lubricating and/or sealing thread connections. It is recognized that many areas can have environmental requirements for products of this type. This International Standard does not include requirements for environmental compliance. It is the responsibility of the end user to investigate these requirements and to select, use and dispose of the thread compounds and related waste materials accordingly. 2 Conformance 2.1 Dual citing of normative references In the interests of world-wide application of this International Standard, Technical Committee ISO/TC 67 has decided, after detailed technical analysis, that certain of the normative documents listed in Clause 3 and prepared by ISO/TC 67 or another ISO Technical Committee are interchangeable in the context of the relevant requirement with the relevant document prepared by the American Petroleum Institute (API), the American Society for Testing and Materials (ASTM) and the American National Standards Institute (ANSI). These latter documents are cited in the running text following the ISO reference and preceded by “or”, for example “ISO XXXX or API YYYY”. Application of an alternative normative document cited in this manner will lead to technical results different from the use of the preceding ISO reference. However, both results are acceptable and these documents are thus considered interchangeable in practice. 2.2 Units of measurement In this International Standard, data are expressed in both the International System (SI) of units and the United States Customary (USC) system of units. For a specific order item, it is intended that only one system of units be used, without combining data expressed in the other system. Products manufactured to specifications expressed in either of these unit systems shall be considered equivalent and totally interchangeable. Consequently, compliance with the requirements of this International Standard as expressed in one system provides compliance with requirements expressed in the other system. For data expressed in the SI system, a comma is used as the decimal separator and a space as the thousands separator. For data expressed in the USC system, a dot (on the line) is used as the decimal separator and a space as the thousands separator. In the text, data in SI units are followed by data in USC units in parentheses. SIST EN ISO 13678:2009

ISO 13678:2009(E) 2 © ISO 2009 – All rights reserved 3 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 2137, Petroleum products and lubricants — Determination of cone penetration of lubricating greases and petrolatum ISO 2176, Petroleum products — Lubricating grease — Determination of dropping point ISO/TR 10400, Petroleum and natural gas industries — Equations and calculations for the properties of casing, tubing, drill pipe and line pipe used as casing or tubing ISO 10405, Petroleum and natural gas industries — Care and use of casing and tubing ISO 13679, Petroleum and natural gas industries — Procedures for testing casing and tubing connections ANSI/API BUL 5C3, Bulletin on formulas and calculations for casing, tubing, drill pipe, and line pipe properties API RP 5C1, Recommended practice for care and use of casing and tubing API RP 5C5, Recommended practice on procedures for testing casing and tubing connections API RP 7G, Recommended practice for drill stem design and operating limits

ASTM D217, Standard Test Methods for Cone Penetration of Lubricating Grease

ASTM D2265, Standard Test Method for Dropping Point of Lubricating Grease over Wide Temperature Range ASTM D4048, Standard Test Method for Detection of Copper Corrosion from Lubricating Grease SIST EN ISO 13678:2009

ISO 13678:2009(E) © ISO 2009 – All rights reserved 34 Terms and definitions For the purposes of this document, the following terms and definitions apply. 4.1 API connection pipe assembly consisting of two external threaded connectors (pins) and a coupling with two internal threaded connectors (box) or one pin and an integral box manufactured in accordance with ISO/API specifications 4.2 API modified thread compound compound designated as “modified thread compound” in API BUL 5A2

NOTE API BUL 5A2 [4] is obsolete and has been replaced by API RP 5A3 [5]. 4.3 box connector with internal threads 4.4 CT and LP casing, tubing and line pipe production and delivery tubulars

4.5 drill stem elements

components of the drilling assembly from the swivel or top drive to the bit, composed of the kelly, drill string, subs, drill collars and other down hole tools such as stabilizers and reamers, also commonly referred to as rotary shouldered connections 4.6 pin connector with external threads 4.7 premium connection connection with or without metal-to-metal seal(s) that can provide greater clearance and/or higher performance properties when compared to the API connections 4.8 proprietary connection connection, without published specifications, made and marketed by companies with exclusive rights to manufacture and/or sell

4.9 reference standard formulation 〈casing, tubing and line pipe (CT and LP)〉 thread compound formulated in accordance with the requirements of Annex B, to include the limitations and tolerances in Tables B.1, B.2 and B.3 4.10 reference standard formulation 〈rotary shouldered connection〉=thread compound formulated in accordance with the requirements of I.4.2.3 NOTE The reference standard formulations are not intended for general field service. 4.11 rotary shouldered connection RSC connection used on drill stem elements, which has threads and sealing shoulders SIST EN ISO 13678:2009

ISO 13678:2009(E) 4 © ISO 2009 – All rights reserved 4.12 seal barrier resisting the passage of fluids, gases and liquids 4.13 storage compound substance applied to threaded pipe connections for protection against corrosion, during shipment and/or storage only, that is not used for connection make-up 4.14 thread compound substance applied to threaded pipe connections prior to make-up for lubrication during assembly and disassembly and for assistance in sealing internal and external pressures NOTE Some thread compounds can also contain substances that provide storage compound properties. 4.15 thread compound/connection system system consisting of the various critical threaded pipe connection components, including the specific connection geometry and the individual connection materials and coatings combined with the thread compound 4.16 tool joint threaded connector used to join sections of drill pipe 5 Thread compound characteristics 5.1 Product characteristics This International Standard outlines tests to characterize the performance of thread compounds under service conditions, rather than specifying the formulation. Thus, the purchaser and the manufacturer should agree on the product characteristics to be provided, such as: Thickener type Rheological properties Fluid type Compound/copper reaction Appearance Extreme-pressure properties Dropping point Fluid sealing properties Mass density Frictional properties Oil separation Corrosion inhibition Flash point Brushing/Adherence Water-absorption resistance Service applications Gas evolution Storage and service life limitations The thread compound manufacturer shall revise product bulletins when any modification in formulation is implemented which would result in a change of any critical performance characteristics. All documentation shall provide data which are representative of a typical production batch. Test and inspection records generated under this International Standard shall be retained by the manufacturer and shall be available to the purchaser for a minimum of three years after the date of manufacture. SIST EN ISO 13678:2009

ISO 13678:2009(E) © ISO 2009 – All rights reserved 55.2 Physical and chemical characteristics 5.2.1 General The physical and chemical characteristics of performance-based thread compounds are specified in Table 1. These properties can vary widely and the formulation of many of the available compounds is proprietary. Therefore, the user should consider the performance properties and recommendations given by the compound manufacturers, in addition to the physical and chemical characteristics outlined in Table 1. SIST EN ISO 13678:2009

ISO 13678:2009(E) 6 © ISO 2009 – All rights reserved Table 1 — Thread compound physical and chemical characteristics tests Property a Test method Performance value b Dropping point, °C (°F) M ISO 2176 or ASTM D2265 138 (280) min. S Evaporation, % volume fraction loss M See Annex D

24 h at 100 °C (212 °F)
3,75 max. S Gas evolution, cm3 M See Annex G
120 h at 66 °C (151 °F)
20 max. S Oil separation, % volume fraction M See Annex E
24 h at 100 °C (212 °F) (nickel gauze cone)
10,0 max. S Penetration, mm × 10−1 M See Annex C
Worked, 60 strokes at 25 °C (77 °F)
Production acceptability range (min. to max.)
± 15 max. S Worked, 60 strokes at −7 °C (19 °F)
Report typical R Mass density, % variance M Manufacturer’s controls
From production mean value
± 5,0 max. S Water leaching, % mass fraction loss M See Annex H
2 h at 66 °C (151 °F)
5,0 max. S Application and adherence M See Annex F
S Cold application
Applies at −7 °C (19 °F) R Adherence at 66 °C (151 °F), % mass fraction loss
25 max. R Copper corrosion M ASTM D4048
Specified corrosion level
1B or better R Corrosion inhibition, % area corrosion I See Annex L
500 h at 38 °C (100 °F)
< 1,0 R Compound stability, 12 months storage M Manufacturer’s controls
Penetration change, mm × 10−1
See Annex C ± 30 max. R Oil separation, % volume fraction
See Annex E 10,0 max. R Compound stability, field service
I See Annex M
24 h at 138 °C (280 °F), % volume fraction loss

25,0 max. R NOTE The values in this table are not intended to be consistent with Table A.3, which presents the original values and requirements of API BUL 5A2 (obsolete, replaced by API RP 5A3). They have been revised to take into account the high-temperature requirements of current field operating conditions and the mass density variations between different proprietary thread compound formulations. a M mandatory

informative b S specification

R recommendation 5.2.2 Dropping point The dropping point test measures the tendency of grease to soften and flow when hot. Results of the dropping point test may be used as an indication of the maximum temperature to which a grease can be exposed without liquefaction or oil separation, for indication of the type of grease and for establishment of manufacturing or quality control limits for this characteristic. Results are not considered as having any direct bearing on service performance unless such correlation has been established. SIST EN ISO 13678:2009

ISO 13678:2009(E) © ISO 2009 – All rights reserved 7In the case of a thread compound, the dropping point is considered to be an indicator of the thermal stability of the base grease and other lubricant additives. Poor thermal stability could adversely affect thread compound performance in high-temperature field service. In order to meet present-day requirements for high temperature service, the minimum dropping point temperature shall be 138 °C (280 °F), as measured in accordance with ISO 2176 or ASTM D2265. NOTE Extreme-temperature field-service conditions can require a higher performance limit. 5.2.3 Evaporation The evaporation test indicates a thread compound’s physical and chemical stability at elevated temperatures, which is related to the base grease/oil or other additives. Due to the wide variation in mass density of thread compounds currently in service, percentage mass fraction does not provide a reliable basis for comparison; therefore, evaporation loss shall be measured as a percentage volume fraction. The evaporative loss, when evaluated in accordance with the test method in Annex D for a 24 h duration at a temperature of 100 °C (212 °F), shall not exceed 3,75 % volume fraction.

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