EN ISO 13678:2009

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
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

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
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ii © ISO 2009 – All rights reserved
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
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
I
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. 5.2.4 Gas evolution The gas evolution test indicates a thread compound’s chemical stability at elevated temperatures. When evaluated in accordance with the test method in Annex G, the volume of gas evolution shall not exceed 20 cm3. 5.2.5 Oil separation The oil separation test indicates a compound’s physical and chemical stability at elevated temperatures, which is related to the base grease/oil. 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, oil separation loss shall be measured as a percentage volume fraction. In order to meet current requirements for high-temperature service, the maximum oil separation loss when evaluated in accordance with the test method in Annex E shall be 10,0 % volume fraction. 5.2.6 Penetration The penetration test measures the consistency, i.e. “thickness” or “stiffness” of a lubricating grease and relates to the ease of application or “brushability” of a thread compound. The compound manufacturer shall measure and record the penetration of each production batch of thread compound and report the mean value for that specific compound. When evaluated in accordance with the test method in Annex C, the penetration acceptability range (minimum to maximum) at 25 °C (77 °F) shall not be greater than 30 cone penetration points. An acceptability range for penetrations is used because thread compounds with penetrations between 265 and 385 can be used for different applications. For information purposes, cold temperature penetration, at −7 °C (19 °F), is reported as a typical value. Mass density affects the values obtained from this procedure. Therefore, it is not a useful measurement for relative comparisons of materials with widely varying mass densities. NOTE Brookfield viscosity (ASTM D2196 [19]) is not substantially affected by material mass density and therefore can provide a closer correlation to brushability than the cone penetration. The range below was determined using several different supplier samples of API modified thread compound as well as proprietary thread compounds used currently with casing, tubing and line pipe connections. It is appropriate that a specific spindle size, rotational frequency and test temperature be utilized to develop viscosity data for comparison. The Brookfield viscosity range, as measured with a #7 Spindle, at 10 r/min and 25 °C, was 200 000 mPa⋅s to 400 000 mPa⋅s. A typical value for API modified thread compounds could range from 200 000 mPa⋅s to 240 000 mPa⋅s. SIST EN ISO 13678:2009

ISO 13678:2009(E) 8 © ISO 2009 – All rights reserved The SI unit of viscosity is the pascal second (Pa·s). The pascal second is rarely used in scientific and technical publications today. The most common unit of viscosity is the dyne second per square centimetre (dyne·s/cm2), which is given the name poise (P) after the French physiologist Jean Louis Poiseuille (1799-1869). Ten poise equal one pascal second (Pa·s) making the centipoise (cP) and millipascal second (mPa·s) identical. 1 pascal second = 10 poise = 1 000 millipascal second 1 centipoise = 1 millipascal second 5.2.7 Mass density The mass density test result of a thread compound depends on the type and quantity of the constituents utilized in the formulation. The range of mass density between production batches for a particular thread compound is an indication of the consistency of manufacture. The compound manufacturer shall measure and record the mass density of each production batch of thread compound and report the mean value for that specific compound. The mass density of a particular thread compound batch shall not vary more than 5,0 % from the manufacturer's established mean value. 5.2.8 Water leaching The water leaching test indicates the physical and chemical stability of compounds when exposed to water at elevated temperatures. When evaluated in accordance with the test method in Annex H, the compound mass loss shall not exceed 5,0 %. 5.2.9 Application and adherence properties Thread compounds should be applied in a manner consistent with the compound manufacturer and thread manufacturer’s recommendations and in sufficient quantity to provide effective lubrication and/or sealing characteristics for threaded connections. The thread compound shall be brushable and capable of adherence over a temperature range of −7 °C (19 °F) to 66 °C (151 °F) without either agglomerating or sliding off the connector. Laboratory tests for determining the thread compound application and adherence properties shall be performed and recorded. The laboratory test methods described in Annex F are intended to provide a means for comparing thread compound performance, but it is possible for them not to be representative of field service. 5.2.10 Corrosion inhibition and protection properties Thread compounds are often utilized to provide shipping and storage corrosion protection on threaded connections, as well as lubrication and sealing properties. Certain field exposure conditions, particularly on offshore platforms and in-service conditions such as sour gas environments, require corrosion protection and inhibition. Therefore, the thread compounds with corrosion protection shall provide an effective barrier against (and not contribute to) corrosive attack of connection threads and seals. The corrosion-inhibition properties of thread compounds depend on application variables such as the following: ⎯ compound additive types and treatment levels; ⎯ type and condition of threading process fluids and residue remaining on thread surfaces; ⎯ compound application method and equipment utilized; ⎯ type of thread protector and application method (“knock-on” or “screw-on”); ⎯ specific user application procedures and environmental conditions; ⎯ compatibility with thread storage compound; ⎯ galvanic differences between compound components, environment and connector material. SIST EN ISO 13678:2009

ISO 13678:2009(E) © ISO 2009 – All rights reserved 9A laboratory test shall be performed and recorded to determine whether potentially corrosive components are present in the thread compound. A copper corrosion test should be carried out in accordance with the procedures in ASTM D4048 or equivalent. Although copper is not typically utilized (other than as a thread surface plating) in production connections, it more readily reacts in the presence of reactive materials such as sulfur and chlorine, which can also damage steel. Thread compounds should provide a level 1B or better by this method. For RSCs, if thread compounds with metallic zinc are used, it is recommended that active sulfur be limited to less than 0,3 %. A laboratory test for determining the thread compound corrosion-inhibition properties should be performed and recorded. Thread compounds vary as to the existence and treatment level of corrosion inhibition. It is, therefore, the purchaser's/user's responsibility to outline the necessary requirements with the compound manufacturer for products being utilized for storage or corrosive field applications. The methods listed in Annex L are generally accepted and utilized by lubricant test laboratories and users. They are intended to provide a means for the relative comparison of thread compound properties. 5.2.11 Compound stability properties Thread compound stability, both in storage and in service, is a property essential to adequate sealing performance within an assembled connection. Instability in the form of excessive softening and separation can result in the development of leak passages over time or with changes in temperature. Excessive hardening in storage can adversely affect brushability and proper application of the compound onto the pipe thread surfaces. The compound manufacturer shall keep production batch samples and evaluate them periodically for storage stability. Thread compound storage stability over a minimum of 12 months is adequate to resist softening or hardening of more than 30 cone penetration points at 25 °C (77 °F), when evaluated in accordance with the test method in Annex C. Stratification or oil separation should not be greater than 10,0 % volume fraction over a minimum period of 12 months. The test described in Annex M should also be performed and is intended to provide a means for the relative comparison of thread compound high-temperature stability. Thread compound stability test results shall be available in a product bulletin. 6 Thread compound performance properties 6.1 Small-scale test The small-scale (bench top) test described in I.4 compares the friction properties of a test compound to a lead-based reference compound formulated for laboratory use. There is a possibility that small-scale tests might not correlate directly with full-scale connection tests or be truly representative of field service. Annex I [formerly API RP 7A1 [6] (obsolete)] covers a small-scale test procedure that was developed and validated utilizing the metal-based RSC compounds that were commonly used in field applications in the early 1990s. Subsequent industry test programmes utilizing non-metallic RSC compounds have shown limited correlation of small-scale test frictional properties with full-scale test results. Therefore, this test method has limited usefulness for determining friction factors for non-metallic compounds for use on any type of connection.
6.2 Frictional properties A thread compound acts as a lubricant during make-up and breakout and provides consistent and repeatable frictional properties between the mating members of a threaded connection. For a given amount of connection engagement (a specific number of engaged threads), the torque required varies in direct proportion to the apparent coefficient of friction of the thread compound/connection system. The frictional properties of the thread compound/connection system affect the following torque values: ⎯ the torque required to make up the connection; SIST EN ISO 13678:2009

ISO 13678:2009(E) 10 © ISO 2009 – All rights reserved ⎯ the torque required to cause further make-up; ⎯ the torque required to break out the connection. The frictional properties of a thread compound in a connection also depend on several factors external to the compound. These external factors include connection geometry, machined surface finish, coating of the contact surfaces, relative surface speed (make-up revolutions per minute) of the connection members during make-up, compound film thickness and surface contact pressure. Each of these parameters should be taken into account when designing a test to determine frictional properties and when using a compound in the field. A laboratory test, such as described in Annex I, for determining the thread compound frictional properties should be performed and recorded. The laboratory test methods described in Annex I are intended to provide a means of comparing thread compounds with the specified reference standard formulations. In the case of casing, tubing and line pipe, if different thread compounds are applied to opposite ends of a coupling, frictional differences can occur between the mill end connection and the field end connection and can result in excessive movement and engagement of the mill end prior to adequate engagement of the field end. The field torque required for proper assembly of API-type connections should be determined in accordance with the procedures described in ISO 10405 or as recommended by the connection manufacturer. 6.3 Extreme surface-contact pressure (gall resistance) properties for casing, tubing and line pipe A thread compound provides resistance to adhesive wear (metal galling) of the mating connection surfaces subjected to extreme surface-contact pressure. High surface-contact pressure in threaded connections can occur as a result of various factors during manufacturing and in field service. Manufacturing factors include product variations, such as geometric characteristics (thread length, pipe and coupling thicknesses) and process variations, such as machining (thread taper, lead and flank angles), surface finishing and coating. Field service factors include handling damage, contact-surface contamination, inadequate or inconsistent application of thread compound, misalignment during assembly and improper torque application. An important consideration is the greater tendency of some materials towards connection galling than others. Galling tendency increases between two smooth metal surfaces with increasing similarities of composition, similarities of relative hardness and decreasing actual hardness. For OCTG (Oil Country Tubular Goods), the composition and hardness of each component of the mating pair is virtually the same. Consequently, OCTG are relatively prone to galling. Therefore, a coating for one of the connection members, such as zinc phosphate and manganese phosphate and API modified thread compound, has traditionally been utilized to provide adequate galling resistance. The increasing use of quench-hardened alloys and the significantly greater tendency of martensitic chromium steels, duplex stainless steels and nickel-based alloys to galling requires that all possible care be applied to every aspect of surface preparation: coating, thread compound selection and application, handling and connection assembly to achieve connection galling resistance. A laboratory test such as described in Annex J for determining the total thread compound/connection system extreme surface-contact pressure properties (gall resistance) should be performed and the results recorded. The laboratory test methods described in Annex J are intended to provide a means for comparing thread compounds with the reference standard, described in Annex B. For specific service applications, the total thread compound connection system should be evaluated for galling resistance. This requires repeated assembly and disassembly tests on full-scale connections, preferably in the vertical mode, to simulate rig assemblies, with minimum and maximum amounts of thread compound. Such tests should be performed in accordance with the industry test methods referenced in Annex J. Connections with inadequate surface preparation can not resist galling, regardless of handling or assembly technique. Conversely, connections with adequate surface preparation can be galled with inadequate handling or assembly technique. Each activity should be controlled to achieve repeatable extreme pressure properties. SIST EN ISO 13678:2009

ISO 13678:2009(E) © ISO 2009 – All rights reserved 11The combination of proper surface preparation, connection coating and thread compound selection and application should be established for each type of connection and material combination, based on their tendency to gall, during both assembly and disassembly following service. 6.4 Fluid sealing properties for casing, tubing and line pipe When used on thread-seal
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