EN ISO 13678:2012

Petroleum and natural gas industries - Evaluation and testing of thread compounds for use with casing, tubing, line pipe and drill stem elements (ISO 13678:2010)

ISO 13678:2010 provides requirements, recommendations and methods for the testing of thread compounds intended for use on threaded casing, tubing, and line pipe connections; and for thread compounds intended for use on 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. ISO 13678:2010 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.

Erdöl- und Erdgasindustrie - Beurteilung und Prüfung von Gewindefetten zur Verwendung an Futter-, Steig- und Leitungsrohren und an Bohrgestängeteilen (ISO 13678:2010)

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 13678:2010)

L'ISO 13678:2010 fournit des exigences, des recommandations et des méthodes pour les essais des graisses pour filetage à utiliser sur des connexions filetées de tubes de cuvelage, de tubes de production et de tubes de conduites, ainsi que pour les graisses pour filetage à utiliser sur des connexions rotatives à épaulement. Les essais décrits dans l'ISO 13678:2010 sont utilisés pour évaluer les caractéristiques de performance critiques des graisses pour filetage et leurs caractéristiques physico-chimiques 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 ne sont pas 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 13678:2010 ne comprend pas d'exigences pour mise en conformité environnementale. Il est de la responsabilité de l'utilisateur final d'examiner ces exigences et de sélectionner, d'utiliser et de détruire les graisses pour filetage et les déchets associés en fonction de celles-ci.

Industrija za predelavo nafte in zemeljskega plina - Ovrednotenje in preskušanje navojnih spojev za uporabo pri zaščitnih, proizvodnih (dvižnih) in vrtalnih elementih (ISO 13678:2010)

Ta mednarodni standard določa zahteve, priporočila in metode za preskušanje navojnih spojev za uporabo pri navojnih zaščitnih in proizvodnih zvez ter za navojne spoje za uporabo na vrtečih vijačnih zvezah. Predstavljeni preskusi se uporabljajo za vrednotenje kritičnih lastnosti delovanja ter fizičnih in kemičnih lastnosti navojnih spojev pod laboratorijskimi pogoji. Te preskusne metode so namenjene predvsem za navojne spoje, oblikovane z mastjo za mazalno osnovo, in se ne uporabljajo za nekatere materiale za mazanje in/ali tesnjenje navojnih spojev. Znano je, da lahko imajo številna območja okoljske zahteve za izdelke te vrste. Ta mednarodni standard ne vključuje zahtev za okoljsko skladnost. Končni uporabnik je odgovoren, da te zahteve razišče ter skladno z njimi izbere, uporabi in zavrže navojne spoje ter povezane odpadne materiale.

General Information

• Status: Published
• Publication Date: 17-Jan-2012
• Withdrawal Date: 30-Jul-2012
• ICS: 75.100 - Lubricants, industrial oils and related products
• ICS: 75.180.10 - Exploratory, drilling and extraction equipment
• Technical Committee: CEN/TC 12 - Materials, equipment and offshore structures for petroleum and natural gas industries
• Drafting Committee: CEN/TC 12 - Materials, equipment and offshore structures for petroleum and natural gas industries
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 18-Jan-2012
• Due Date: 13-Nov-2012
• Completion Date: 18-Jan-2012
• Ref Project: SIST EN ISO 13678:2012 - Petroleum and natural gas industries - Evaluation and testing of thread compounds for use with casing, tubing, line pipe and drill stem elements (ISO 13678:2010)

Relations

• Replaces: EN 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)
• Effective Date: 17-Jul-2010

Overview

EN ISO 13678:2012 (ISO 13678:2010) applies to the petroleum and natural gas industries and specifies requirements, recommendations and laboratory test methods for thread compounds used on threaded casing, tubing, line pipe and drill stem / rotary shouldered connections. The standard focuses on evaluating critical performance properties and physical/chemical characteristics of primarily grease-based thread compounds under controlled conditions. It does not address environmental compliance - users are responsible for local regulatory requirements and safe disposal.

Key topics and technical requirements

The standard defines test methods and acceptance considerations for core performance areas, including:

• Frictional properties - consistent makeup and breakout torque to ensure reliable connection engagement.
• Galling (extreme surface contact pressure) resistance - lubrication adequacy to prevent metal damage during make-up/breakout.
• Fluid sealing properties - effectiveness for thread-type seals and compatibility with non-thread seals (metal-to-metal, PTFE, etc.).
• Physical and chemical characteristics - penetration, oil separation, evaporation, gas evolution, water leaching and stability.
• Application and adherence - how compounds apply and remain on connection surfaces in expected service conditions.
• Quality assurance and marking - batch control, labelling and traceability requirements.

Normative and informative annexes describe specific laboratory procedures (e.g., penetration, evaporation, oil separation, frictional tests, galling and fluid sealing tests, corrosion inhibition and high-temperature stability).

Practical applications

EN ISO 13678:2012 is used to:

• Evaluate and qualify thread compounds during product development.
• Establish quality control and acceptance testing for manufacturing batches.
• Compare competing thread compounds for selection in drilling, completion and production operations.
• Support procurement specifications and supplier audits for casing, tubing and line pipe projects.
• Guide field trial planning by providing laboratory-based performance benchmarks.

Using the tests in the standard helps reduce connection failures caused by improper lubrication, galling or poor sealing, improving operational reliability in wells and pipelines.

Who should use this standard

• Thread compound manufacturers and R&D teams
• Oil & gas operators and drilling/completions engineers
• Test laboratories and quality assurance personnel
• Procurement specialists and specification writers
• Standards and compliance teams in upstream industry

Related standards

• ISO 13678 is based on and incorporates elements from API RP 5A3 and API RP 7A1 (historical references).
• Adopted as a European standard: EN ISO 13678:2012 (CEN).

Keywords: ISO 13678, EN ISO 13678:2012, thread compounds, casing, tubing, line pipe, rotary shouldered connections, galling resistance, frictional properties, fluid sealing, oilfield testing, petroleum industry.

Standards Content (Sample)

SLOVENSKI STANDARD
01-marec-2012
1DGRPHãþD
SIST EN ISO 13678:2009
,QGXVWULMD]DSUHGHODYRQDIWHLQ]HPHOMVNHJDSOLQD2YUHGQRWHQMHLQSUHVNXãDQMH
QDYRMQLKVSRMHY]DXSRUDERSUL]DãþLWQLKSURL]YRGQLKGYLåQLKLQYUWDOQLK
HOHPHQWLK,62
Petroleum and natural gas industries - Evaluation and testing of thread compounds for
use with casing, tubing, line pipe and drill stem elements (ISO 13678:2010)
Erdöl- und Erdgasindustrie - Beurteilung und Prüfung von Gewindefetten zur
Verwendung an Futter-, Steig- und Leitungsrohren und an Bohrgestängeteilen (ISO
13678:2010)
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 13678:2010)
Ta slovenski standard je istoveten z: EN ISO 13678:2012
ICS:
75.180.10 Oprema za raziskovanje in Exploratory and extraction
odkopavanje equipment
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 13678
NORME EUROPÉENNE
EUROPÄISCHE NORM
January 2012
ICS 75.180.10 Supersedes EN ISO 13678:2009
English Version
Petroleum and natural gas industries - Evaluation and testing of
thread compounds for use with casing, tubing, line pipe and drill
stem elements (ISO 13678:2010)
Industries du pétrole et du gaz naturel - Évaluation et Erdöl- und Erdgasindustrie - Beurteilung und Prüfung von
essais des graisses pour filetage utilisées pour les tubes de Gewindefetten zur Verwendung an Futter-, Steig- und
cuvelage, les tubes de production, les tubes de conduites Leitungsrohren und an Bohrgestängeteilen (ISO
et les éléments de garnitures de forage (ISO 13678:2010) 13678:2010)
This European Standard was approved by CEN on 3 December 2011.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the CEN-CENELEC 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 translation
under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same
status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, 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, Turkey and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 13678:2012: E
worldwide for CEN national Members.

Contents Page
Foreword .3

Foreword
The text of ISO 13678:2010 has been prepared by Technical Committee ISO/TC 67 “Materials, equipment
and offshore structures for petroleum, petrochemical and natural gas industries” of the International
Organization for Standardization (ISO) and has been taken over as EN ISO 13678:2012 by 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 July 2012, and conflicting national standards shall be withdrawn at the
latest by July 2012.
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.
This document supersedes EN ISO 13678:2009.
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, Croatia, 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, Turkey and the United Kingdom.
Endorsement notice
The text of ISO 13678:2010 has been approved by CEN as a EN ISO 13678:2012 without any modification.

INTERNATIONAL ISO
STANDARD 13678
Third edition
2010-12-01
Petroleum 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
Reference number
ISO 13678:2010(E)
©
ISO 2010
ISO 13678:2010(E)
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All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
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Published in Switzerland
ii © ISO 2010 – All rights reserved

ISO 13678:2010(E)
Contents 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 .2
5 Thread compound characteristics.3
5.1 Product characteristics.3
5.2 Physical and chemical characteristics.4
6 Thread compound performance properties.8
6.1 Small-scale test .8
6.2 Frictional properties.8
6.3 Extreme surface contact pressure (gall resistance) properties for casing, tubing and line
pipe .9
6.4 Fluid sealing properties for casing, tubing and line pipe .10
7 Quality assurance and control.10
8 Marking requirements.11
8.1 Marking.11
8.2 Labelling.11
Annex A (informative) API modified thread compound .12
Annex B (normative) Casing, tubing and line pipe reference standard formulation.16
Annex C (normative) Penetration test .18
Annex D (normative) Evaporation test .19
Annex E (normative) Oil separation test .20
Annex F (normative) Application/adherence test.21
Annex G (normative) Gas evolution test .22
Annex H (normative) Water leaching test.26
Annex I (informative) Frictional properties test .29
Annex J (informative) Extreme surface contact pressure (galling) test for casing, tubing and line
pipe .39
Annex K (informative) Fluid sealing test for casing, tubing and line pipe.40
Annex L (informative) Corrosion inhibition tests .43
Annex M (informative) Compound high-temperature stability test.44
Bibliography.45

ISO 13678:2010(E)
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 third edition cancels and replaces the second edition (ISO 13678:2009), of which it constitutes a minor
revision.
It is the intent of ISO/TC 67 that the second and third 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 third edition, after which period the second edition will no longer be applicable.
iv © ISO 2010 – All rights reserved

ISO 13678:2010(E)
Introduction
[9]
This International Standard is based on API RP 5A3 , second edition, July 2003, with errata and inclusion of
1)[13]
all clauses of API RP 7A1 , 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:
a) consistent frictional properties that allow both proper and uniform connection engagement;
b) adequate lubrication properties to resist galling or damage of connection contact surfaces during make-up
and breakout;
c) 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 seals, etc.)
depending upon service requirements;
d) physical and chemical stability both in service and in expected compound storage conditions;
e) 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,
are not recommended.
1) Obsolete. Incorporated into this International Standard.
ISO 13678:2010(E)
Testing in compliance with this International Standard does not in 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.
vi © ISO 2010 – All rights reserved

INTERNATIONAL STANDARD ISO 13678:2010(E)

Petroleum 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 threaded casing, tubing, and line pipe connections; and for thread compounds
intended for use on 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 interest 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 those obtained 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.
ISO 13678:2010(E)
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
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
4 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
[8]
compound designated as “modified thread compound” in API BUL 5A2
[9]
NOTE API BUL 5A2 is obsolete and has been replaced by API RP 5A3 .
4.3
box
connector with internal threads
4.4
casing, tubing and line pipe
CT and LP
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
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
2 © ISO 2010 – All rights reserved

ISO 13678:2010(E)
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〉 thread compound formulated, in accordance with the requirements of Annex B,
to include the limitations and tolerances specified 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
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 the following:
⎯ thickener type;
⎯ fluid type;
ISO 13678:2010(E)
⎯ appearance;
⎯ dropping point;
⎯ mass density;
⎯ oil separation;
⎯ flash point;
⎯ water-absorption resistance;
⎯ gas evolution;
⎯ rheological properties;
⎯ compound/copper reaction;
⎯ extreme-pressure properties;
⎯ fluid sealing properties;
⎯ frictional properties;
⎯ corrosion inhibition;
⎯ brushing/adherence;
⎯ service applications;
⎯ 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.
5.2 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.
4 © ISO 2010 – All rights reserved

ISO 13678:2010(E)
Table 1 — Thread compound physical and chemical characteristics tests
a b
Property Test method Performance value
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, cm 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
−1
Penetration, mm × 10 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  Applicable at −7 °C R
(19 °F)
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
−1
Penetration change, mm × 10 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
[8] [9]
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.
ISO 13678:2010(E)
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, as a means of determining the type of grease and establishing
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.
In 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 24 h at a temperature of 100 °C (212 °F), shall
not exceed a 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 cm .
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 a 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.
[27]
NOTE 1 Brookfield viscosity (ASTM D2196 ) is not substantially affected by material mass density and can therefore
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.
6 © ISO 2010 – All rights reserved

ISO 13678:2010(E)
NOTE 2 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/cm ), 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 densities 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 by 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.
ISO 13678:2010(E)
A 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/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
[13]
[formerly API RP 7A1 (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;
8 © ISO 2010 – All rights reserved

ISO 13678:2010(E)
⎯ 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 connections should be determined in accordance with
[2] [10]
or API RP 5C1 or as recommended by the connection
the procedures described in ISO 10405
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 Oil Country Tubular Goods (OCTG), 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 such as zinc phosphate and manganese phosphate and
API modified thread compound, for one of the connection members, 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: coati
...