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T/SP/CW/6 Part 1

SPECIFICATION FOR

THE EXTERNAL PROTECTION OF STEEL LINE PIPE


AND FITTINGS USING FUSION BONDED POWDER
AND OTHER COATING SYSTEMS
PART 1 - REQUIREMENTS FOR COATING
MATERIALS AND METHODS OF TEST

OCTOBER 2005
J229 ( Rev 03/06 )
© National Grid Gas plc 2006 - All Rights Reserved
T/SP/CW/6 Part 1

CONTENTS

Page

FOREWORD v

BRIEF HISTORY v

DISCLAIMER v

MANDATORY AND NON-MANDATORY REQUIREMENTS v

SECTION ONE- GENERAL REQUIREMENTS

1. SCOPE 1

2. REFERENCES 1

3. DEFINITIONS 1

4. COATING MATERIALS 1

4.1 Acceptable materials 1

4.2 Identification of materials 2

4.3 Production data sheets 2

4.4 Toxicity and handling 2

5. VARIENTS 2

SECTION TWO –
BASIC PROPERTIES AND TESTS FOR POWDERS AND CURED COATING

6. BASIC PROPERTIES OF THE POWDER 3

6.1 General 3

6.2 Infra-red scan 3

6.3 Gel time 3

6.4 Particle size analysis 3

6.5 Density 3

6.6 Moisture content 3

6.7 Thermal analysis 3

6.8 Stability 3

7. BASIC PROPERTIES OF THE DETACHED COATING FILM 3

7.1 General requirements 3

7.2 Micro-sectioning 4

7.3 Tensile strength 4

7.4 Elongation 4

© National Grid Gas plc 2006 - All Rights Reserved


J229 ( Rev 03/06 ) -i-
T/SP/CW/6 Part 1

Page

7.5 Dielectric strength 4

7.6 Water permeability 4

7.7 Water absorption 4

8. BASIC PROPERTIES OF THE CURED APPLIED COATING 4

8.1 Physical performance test requirements 4

8.2 Environmental test requirements 5

8.3 Thermal stability test Thermal stability test 6

9. QUALITY CONTROL REQUIREMENTS 6

10. COMPLIANCE 6

11. BASIC PROPERTIES OF UNMIXED MATERIALS 7

11.1 General 7

11.2 Total non-volatile content 7

11.3 Viscosity 7

11.4 Relative density 7

11.5 Mixing ratio 7

11.6 Pot life 7

11.7 Flash point 7

11.8 Stability 7

12. BASIC PROPERTIES OF DETACHED COATING FILM 7

12.1 General requirements 7

12.2 Micro-sectioning 8

12.3 Tensile strength 8

12.4 Elongation 8

12.5 Dielectric strength 8

12.6 Water permeability 8

12.7 Water absorption 8

13. BASIC PROPERTIES OF CURED APPLIED COATING 8

13.1 Physical performance test requirements 8

13.2 Environmental test requirements 9

13.3 Thermal stability tests 10

14. QUALITY CONTROL REQUIREMENTS 10

© National Grid Gas plc 2006 - All Rights Reserved


- ii - J229 ( Rev 03/06 )
T/SP/CW/6 Part 1

Page

15. COMPLIANCE 10

APPENDICES

A REFERENCES 11

B DEFINITIONS 12

C METHODS FOR THE EVALUATION OF THE THERMAL CHARACTERISTICS OF


POWDER AND CURED COATING 13

D FLEXIBILITY TEST 22

E HOLIDAY DETECTION OF COATINGS 25

F EVALUATION OF RESISTANCE TO IMPACT 26

G EVALUATION OF RESISTANCE TO WATER IMMERSION 29

H EVALUATION OF RESISTANCE TO CATHODIC DISBONDING 31

I STRAIN/POLARIZATION TEST 34

J EVALUATION OF RESISTANCE TO HEAT BLISTERING 35

ENDNOTE 37

© National Grid Gas plc 2006 - All Rights Reserved


J229 ( Rev 03/06 ) - iii -
T/SP/CW/6 Part 1

© National Grid Gas plc 2006 - All Rights Reserved


- iv - J229 ( Rev 03/06 )
T/SP/CW/6 Part 1

FOREWORD
This Specification was approved by Phil Brown on 21/10/04 for use by managers, engineers and
supervisors throughout National Grid Gas.

National Grid Gas documents are revised, when necessary, by the issue of new editions. Users should
ensure that they are in possession of the latest edition by referring to the Gas Documents Library
available on infonetUK (company intranet.)

Compliance with this Document does not confer immunity from prosecution for breach of statutory or
other legal obligations.

BRIEF HISTORY

First published as BGC/PS/CW6:Part 1 January 1985


Re-issued as GBE/CW6:Part1 January 1993
Editorial update to reflect demerger November 2000 June 2001
Editorial update to reflect merger October 2002 November 2002
Technical revision July 2004 November 2004
Editorial update to comply with GRM October 2004
Editorial update for National Grid re-branding October 2005

KEY CHANGES (Identify the changes from the previous version of this document)
Section Amendments

All Changes to reflect rebadging to National Grid.


Removal of Transco and substitution of National Grid.
Change of must to shall

DISCLAIMER
This document is provided for use by National Grid Gas and such of its contractors as are obliged by the
terms and conditions of their contracts to comply with this document. Where this document is used by
any other party it is the responsibility of that party to ensure that this document is correctly applied.

MANDATORY AND NON-MANDATORY REQUIREMENTS


In this document:

Shall: indicates a mandatory requirement.

Should: indicates best practice and is the preferred option. If an alternative method is used then a
suitable and sufficient risk assessment shall be completed to show that the alternative method
delivers the same, or better, level of protection.

© National Grid Gas plc 2006 - All Rights Reserved


J229 ( Rev 03/06 ) -v-
T/SP/CW/6 Part 1

© National Grid Gas plc 2006 - All Rights Reserved


- vi - J229 ( Rev 03/06 )
T/SP/CW/6 Part 1

SPECIFICATION FOR
THE EXTERNAL PROTECTION OF STEEL LINE PIPE AND
FITTINGS USING FUSION BONDED POWDER AND OTHER
COATING SYSTEMS:
PART 1 - REQUIREMENTS FOR COATING MATERIALS AND
METHODS OF TEST

SECTION ONE- GENERAL REQUIREMENTS


1. SCOPE
This National Grid Gas Technical Specification* CW6 specifies materials for use as anti-corrosion
coatings on steel line pipe and fittings (tees and bends). It deals specifically with the properties and
performance tests to establish suitability for use with Part 2 of this specification, which deals with factory
applied coatings, and for use with CW5 for certain field applied coatings.

Section One of this specification covers general requirements. Section Two covers fusion bonded
powder and Section Three covers multi-component liquid coating materials.
* Hereinafter referred to as 'this specification'.

2. REFERENCES
2.1 This Specification makes references to the documents listed in Appendix A. Unless otherwise
specified, the latest edition of the documents apply, including all amendments.

3. DEFINITIONS
3.1 The requirements and definitions applying to this Specification are listed in Appendix B.

4. COATING MATERIALS
4.1 Acceptable materials
4.1.1 Coating systems
Only coating systems conforming to this specification should be considered for application in accordance
with CW6: Part 2. Coating systems may include the use of a primer or chemical pre-treatment of the
steel surface to enhance adhesion. In such cases, the pre-treatment and coating material should be
clearly specified as a combined system.

Where recycled fusion bonded epoxy (FBE) material is used, the ratio of recycled to virgin material
should be stated. Any FBE made up with a recycled material mix should meet the requirements of this
specification. Fusion bonded powder should also meet the requirements of Part 1 of this specification
without the use of chemical pre-treatment.

4.1.2 Compliance with this specification


The Contractor should be responsible for ensuring that all coating materials and equipment comply with
all of the provisions specified in this specification and National Grid Gas may make any investigation
necessary, by way of testing, batch sampling and manufacturing inspection, to satisfy itself of compliance
by the Contractor.

4.1.3 Application of this specification


It is intended that this specification be used to encourage and stimulate the development of progressively
better external pipeline coatings. Thus, where certain minimum performance values are stated and
should future coating material test submissions yield better performance than the specified requirements

© National Grid Gas plc 2006 - All Rights Reserved


J229 ( Rev 03/06 ) -1-
T/SP/CW/6 Part 1

then, after economic evaluation, these new values may be adopted as the minimum requirements and
the specification would be up-graded accordingly.

4.1.4 Supply of data


The Contractor shall furnish, on request and in confidence, such details as may be required by National
Grid Gas, which may include formulations, typical physical constants, manufacturing tolerances and
application data associated with the coating materials being used. National Grid Gas also reserve the
right of direct communication with the Manufacturer should the need arise.

Any change of formulation, or manufacturing supply route, of a material may be proposed for
consideration as a variant by National Grid Gas and supply of the modified material shall not be
implemented until such time as the revised procedure qualification trials have been completed and the
results accepted in writing by National Grid Gas.

4.2 Identification of materials


All materials supplied for coating operations should be suitably marked giving the following information:

a) Manufacturer's name, initials or identification mark.


b) Name of material.
c) Batch number.
d) Date of manufacture and 'use by' date.
e) Storage temperature limits.
f) Safety data sheet (included with delivery).

Containers and any associated packaging should, where appropriate, be marked in accordance with the
Chemicals (Hazard Information and Packaging for Supply) Regulations 2002.

The Contractor shall require the Manufacturer to supply certificates confirming that tests specified in this
specification have been carried out on the batches supplied and that the materials meet the specified
requirements. These certificates shall be made available for examination by National Grid Gas on
request.

4.3 Production data sheets


The Contractor should be responsible for obtaining data sheets from the Manufacturer which shall
include values for all the basic properties of the material as specified in the 'Basic properties' clause in
the appropriate Section of this specification.

4.4 Toxicity and handling


Any hazard including toxic, corrosive and fire risks, associated with coating materials offered for use to
meet the requirements of this specification shall be specified by the Manufacturer, together with his
recommendations for safe handling in accordance with the requirements of the Health and Safety at
Work etc. Act 1974 and the COSHH Regulations 2002.

Containers and associated packages should be marked with their weights and, where appropriate, be
provided with handling points, e.g. handles or hand holes.

The manufacturer shall also provide information to cover the environmental aspects of the coating
materials to include:

a) Identification of the environmental risks associated with the use of the materials.
b) Identification of suitable control measures to prevent environmental damage.
c) Identification of suitable methods of disposal of waste materials and contaminated items.

5. VARIENTS
A contractor should only propose variants to this specification where the text indicates that variants
would be considered by National Grid Gas.

© National Grid Gas plc 2006 - All Rights Reserved


-2- J229 ( Rev 03/06 )
T/SP/CW/6 Part 1

SECTION TWO – BASIC PROPERTIES AND TESTS FOR POWDERS AND CURED COATING
6. BASIC PROPERTIES OF THE POWDER
6.1 General
The Contractor should obtain from the Manufacturer the specified and qualified ranges of values for all
properties listed in 6.2 to 6.8 inclusive that will ensure an acceptable coating. The frequency of testing
should be in accordance with 9.2.

6.2 Infra-red scan


An infra-red spectrogram, preferably made by using a standard potassium bromide (KBr) disc, should be
obtained from the batch of the powder used for approval testing. This should subsequently be used for
comparison with type spectrograms and future production batches.

6.3 Gel time


A hot plate technique should be used to obtain values of the gel time, and the values obtained of each
batch should be used for comparison with values originally quoted.

6.4 Particle size analysis


The particle size distribution of the powder should be the optimum to suit the particular method of
application.

Particle size range should be quoted in the production data sheet. Each batch should be checked for
conformity with the values originally quoted.

6.5 Density
The density of the powder should be measured for all batches produced, and the values should conform
with the value originally specified.

6.6 Moisture content


The moisture content of the powder shall be less than 0.5% by weight and should be checked for every
batch.

6.7 Thermal analysis


Thermal analysis data for each batch should be made available showing, by use of a Differential
Scanning Calorimeter (DSC), the glass transition of the raw powder and also the enthalpy of the curing
powder. The glass transition temperature of the fully cured powder should also be quoted. The reference
curve should be provided as part of the production data sheet (see 4.3). The limiting values of ΔH , Tg1
and Tg2 (see Appendix C) should be identified by the Manufacturer.

6.8 Stability
After ageing for 120 days at 25 ±1 °C in a sealed container, the powder should not exhibit any significant
change from the properties identified in 6.2 to 6.7 inclusive.

7. BASIC PROPERTIES OF THE DETACHED COATING FILM


7.1 General requirements
The Contractor should ensure that the tests specified in 7.2 to 7.7 inclusive are carried out by the
Manufacturer in accordance with 9.4. The tests should be carried out on detached coating samples,
400µm to 450µm thick, which have been prepared by application on to polished steel plates, 6 mm thick,
previously coated with polytetrafluoroethylene (PTFE).

© National Grid Gas plc 2006 - All Rights Reserved


J229 ( Rev 03/06 ) -3-
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7.2 Micro-sectioning
A cross-section of the cured film should be examined at a magnification of X100 and should be seen to
be homogeneous and essentially free of voids, foaming or other defects.

7.3 Tensile strength


Test specimens of detached coatings should be tested at an extension rate of 1 mm/min. Values for
tensile strength should be quoted in MN/m² as maximum strength and strength at break.

7.4 Elongation
When tested in accordance with 7.3, the elongations at 'yield' and 'break' should be quoted by the
Manufacturer.

7.5 Dielectric strength


The dielectric strength of the cured material should be quoted by the Manufacturer as kV/mm together
with the method of test.

7.6 Water permeability


The water permeability of the cured material, expressed as g/24 h m²/mm thickness should be specified
by the Manufacturer together with the method of test.

7.7 Water absorption


The quantity of water absorbed after three months immersion at 20 °C should be quoted by the
Manufacturer.

8. BASIC PROPERTIES OF THE CURED APPLIED COATING


8.1 Physical performance test requirements
8.1.1 General requirements
The Contractor should ensure that the tests specified in 8.1.2 to 8.1.9 inclusive are carried out in
duplicate by the Manufacturer in accordance with 9.3 and results of the tests, demonstrating compliance,
made available to National Grid Gas.

The tests should be carried out on sections of 6 mm thick laboratory coated standard steel plate, as
appropriate to the test requirement. Prior to coating, the steel surface should be blast cleaned using G34
grit to ISO 8501 Sa 3 quality and surface profile of between 50µm and 100µm peak to trough height. The
coating thickness should be in the range 400µm to 450µm. A destructive film thickness test should be
carried out to verify the accuracy of the coating thickness measurement technique employed.

8.1.2 Cissing and pinholing test


The coating should not show signs of cissing or pinholing when applied to a prepared steel panel.

8.1.3 Blistering and appearance test


The coating should not show signs of blistering and should exhibit uniform appearance.

8.1.4 Sagging test


The coating should not exhibit sagging when applied to a steel panel in the vertical plane prepared in
accordance with 8.1.1.

8.1.5 Thermal analysis - coating cure test


Thermal analysis should be carried out, in accordance with Appendix C, on samples taken from
laboratory prepared panels which are to be used for subsequent performance testing.

The values of Tg1 and Tg2 specified by the Manufacturer should be in a range to ensure the coating is
adequately cured to meet subsequent performance tests.

© National Grid Gas plc 2006 - All Rights Reserved


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T/SP/CW/6 Part 1

The Contractor should obtain complete results of all thermal analyses from the Manufacturer for record
purposes. National Grid Gas should have the right to examine the results on request.

8.1.6 Flexibility test


Steel plates, 50 mm x 300 mm x 6 mm thick, should be coated to a film thickness of 400µm to 450µm
and be cured to represent the extremes of ΔTg specified by the manufacturer. After bending in
accordance with Appendix D (at a deflection rate of 25 mm/min) over appropriate sized mandrels, the
coating shall not crack, disbond or pinhole and shall pass a holiday test in accordance with Appendix E.

8.1.7 Impact resistance test


Impact resistance should be determined in accordance with Appendix F using plate specimens. The
method of statistical analysis described in ASTM G14-77 should also apply.

The coating shall withstand a minimum mean impact value of 1.5 J without resulting in a breakdown or
loss of adhesion of the coating.

8.1.8 Adhesion test


The adhesion test procedure should be as specified in clauses G.5 and G.6 and the results assessed in
accordance with clause G.7.

8.1.9 Hardness test


The Manufacturer should specify the method used to test coating hardness and should quote the values
obtained.

8.2 Environmental test requirements


8.2.1 General requirements
The Contractor should ensure that the tests specified in 8.2.2 to 8.2.8 inclusive are carried out in
duplicate by the Manufacturer and the results of the tests, demonstrating compliance, made available.

The Contractor should be responsible for ensuring that the range of values for any material under
consideration will be capable of providing a finished product in compliance with the relevant Sections of
T/SP/CW/6: Part 2.

All tests should be carried out on coatings properly cured and in the thickness range 400µm to 450µm.

8.2.2 Cathodic disbondment test


Sample panels should be tested by the procedure specified in Appendix H. The coating, when subjected
to an impressed current at a negative voltage of 1500 mV at 20 °C, shall not disbond for greater than 5
mm radius from the edge of the coating pre-damage after 28 days.

8.2.3 Strain/polarization cracking test


The sample panels should be subjected to a bend strain at 20 °C and then predamaged, polarized and
tested as specified in Appendix I with the test area selected on the minimum radius of the bend, i.e. area
of maximum strain.

8.2.4 Water immersion test


The sample panels should be subjected to a water immersion test as specified in Appendix G. The test
shall not show loss of adhesion greater than 3 mm after 28 days.

8.2.5 Humidity resistance test


Coated steel test plates should be exposed for 2000 h in accordance with ISO 6270. The coating shall
not lose adhesion when tested in accordance with Appendix G.6.2 and no underfilm corrosion or
blistering of the film shall occur.

© National Grid Gas plc 2006 - All Rights Reserved


J229 ( Rev 03/06 ) -5-
T/SP/CW/6 Part 1

8.2.6 Salt spray resistance test


Coated steel test plates should be cross-cut and exposed for 2000 h to continuous salt spray conditions
in accordance with BS 3900: Part F4. The coating shall not lose adhesion when tested in accordance
with Appendix G.6.2 , and no underfilm corrosion or blistering of the film shall occur.

8.2.7 Artificial weathering test


Coated steel test plates should be exposed for 2000 h to artificial weathering, in accordance with
ISO 11507, and should show no signs of deterioration, apart from superficial chalking. UVA lamps should
be employed and the test cycle should consist of 4h UV and 4h condensation, both at a temperature of
50 °C.

8.2.8 Heat blister test


Coated steel test plates should be subjected to a heat blister test as specified in Appendix J. The test
shall not show blistering after 3 days immersion.

8.3 Thermal stability test Thermal stability test


8.3.1 General requirements
The Contractor should ensure that the test specified in 8.3.2 is carried out in duplicate by the
Manufacturer and the results of the test, demonstrating compliance, made available.

8.3.2 Test conditions


Coated steel test plates should be exposed to dry heat at 50 °C for three months to determine thermal
stability and shall still meet the full requirements of 8.1.6 to 8.1.8 and 8.2.2 to 8.2.6.

The coating colour and appearance should be uniform and free from runs, sags, blistering, roughness,
foaming and general film defects.

9. QUALITY CONTROL REQUIREMENTS


9.1 Before dispatch from the factory, the Manufacturer should carry out sampling and testing of the
manufactured material covered by this specification in accordance with 9.2, 9.3 and 9.4.

9.2 During the production of each separate batch of powder or twice every 8 h of continuous
production (whichever is the more frequent), the tests specified in 6.2 to 6.7 inclusive should be carried
out.

9.3 At least once every 8 h of continuous production, the tests specified in 8.1.2 to 8.1.9 inclusive
should be carried out.

9.4 The tests specified in 7.2 to 7.7 inclusive, 8.2.2 to 8.2.4 inclusive, 8.2.8 and the requirements
of 6.8 should be carried out once per year.

9.5 Any time a production, source, process or formulation change is made to the coating system,
the tests specified in 7.2 to 7.7 inclusive, 8.2.2 to 8.2.8 inclusive and the requirements of 6.8 should be
carried out.

10. COMPLIANCE
The coating material shall not be dispatched until it has been demonstrated that the Manufacturers
inspection and testing complies with the requirements of this specification.

© National Grid Gas plc 2006 - All Rights Reserved


-6- J229 ( Rev 03/06 )
T/SP/CW/6 Part 1

SECTION THREE – BASIC PROPERTIES AND TESTS OF MULTI-COMPONENT LIQUID COATING


MATERIALS AND CURED COATINGS
11. BASIC PROPERTIES OF UNMIXED MATERIALS
11.1 General
This Section Three covers multi-component liquid systems suitable for both spraying and brush
application.

The Contractor shall obtain, from the Manufacturer, specified and qualified ranges of values for all
properties, listed in 11.2 to 11.8 inclusive, that will ensure an acceptable coating. The frequency of
testing should be in accordance with 14.2.

11.2 Total non-volatile content


The total non-volatile content should be specified by the Manufacturer for each individual material
component as supplied. The method of test should be in accordance with the method given in ISO 3251.

11.3 Viscosity
The viscosity of each material component as supplied, and that of the mixture when prepared for use in
the correct ratio, should be specified by the Manufacturer, together with the method of test.

11.4 Relative density


The relative density of each material component as supplied, and that of the mixture when prepared for
use in the correct ratio, should be specified by the Manufacturer, together with the method of test.

11.5 Mixing ratio


The mixing ratio of material components should be specified by the Manufacturer, both by weight and by
volume.

11.6 Pot life


The pot life measured in accordance with the definitions contained in BS 2015 should be quoted by the
Manufacturer.

11.7 Flash point


The flash point of each material component as supplied, and that of the mixture when prepared for use,
should be specified by the Manufacturer.

11.8 Stability
The separate material components when stored at 20 °C to 25 °C for a period of 6 months should:

a) Show no signs of hard settlement.


b) Show no deterioration in application properties.
c) Show no deterioration in curing properties.

The separate material components, when stored in closed containers approximately 75 mm diameter x
75 mm high, two-thirds full at 20 °C to 25 ° for 24 h, shall not show signs of skinning or other
deterioration.

12. BASIC PROPERTIES OF DETACHED COATING FILM


12.1 General requirements
The Contractor should ensure that the tests specified in 12.2 to 12.7 inclusive are carried out by the
Manufacturer at the frequency specified in 14.4. The tests should be carried out on detached coating
samples which have been prepared by application on to polished steel plates, 6 mm thick, previously
coated with PTFE. The coating should be applied to give a minimum dry film thickness of 1.5 mm and

© National Grid Gas plc 2006 - All Rights Reserved


J229 ( Rev 03/06 ) -7-
T/SP/CW/6 Part 1

allowed to cure at 20 °C to 25 °C and 60% to 70% relative humidity for a period of seven days to achieve
optimum properties before test. Samples should be of uniform thickness for all tests.

12.2 Micro-sectioning
A cross-section of the cured film should be examined at a magnification of X100 and should be seen to
be homogeneous and essentially free of voids or other defects.

12.3 Tensile strength


Test specimens of detached coatings should be tested at an extension rate of 1 mm/min. Values for
tensile strength should be quoted in MN/m² as maximum strength and strength at break.

12.4 Elongation
When tested in accordance with 12.3, the elongations at 'yield' and 'break' should be quoted by the
Manufacturer.

12.4 Dielectric strength


The dielectric strength of the cured material should be quoted by the Manufacturer as kV/mm together
with the method of test.

12.6 Water permeability


The water permeability of the cured material, expressed as g/24 h m²/mm thickness should be specified
by the Manufacturer together with the method of test.

12.7 Water absorption


The quantity of water absorbed after three months immersion at 20 °C should be quoted by the
Manufacturer.

13. BASIC PROPERTIES OF CURED APPLIED COATING


13.1 Physical performance test requirements
13.1.1 General requirements
Coating materials should develop adequate handling properties within 24 h of application to suit factory
or field conditions.

The Contractor should ensure that the tests specified in 13.1.2 to 13.1.8 inclusive are carried out in
duplicate by the Manufacturer in accordance with 14.3 and the results of the tests, demonstrating
compliance, made available.

The tests should normally be carried out on standard steel surfaces which have been blast cleaned,
using G34 grit, to ISO 8501, Sa 3 quality to produce a profile of between 50µm and 50µm peak to trough
height. Coating application should normally be by a suitable technique with pre-heating of components,
where necessary. The coating should be applied to give a dry film thickness of not less than 1.5 mm and
allowed to cure at 20 °C to 25 °C and 60% to 70% relative humidity for a period of 24 h to achieve
optimum properties before test.

Testing of applied coatings should be carried out seven days after the coating application.

13.1.2 Cissing and pinholing test


The coating should show no signs of cissing or pinholing when applied to a prepared steel panel. In
cases of doubt, a further test may be carried out by applying the coating to a grit roughened glass panel
and examining it by viewing over a bright light source.

13.1.3 Blistering and appearance test


The coating should show no signs of blistering and should exhibit uniform appearance when examined
by either of the tests specified in 13.1.2.

© National Grid Gas plc 2006 - All Rights Reserved


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T/SP/CW/6 Part 1

13.1.4 Sagging test


The coating should not exhibit sagging when applied to a steel panel in the vertical plane prepared and
coated in accordance with 13.1.1 and which, immediately subsequent to coating, has been placed in a
vertical position and has remained in that position until the coating is dry.

13.1.5 Flexibility test


Steel plates, 50 mm x 300 mm x 6 mm thick, should be coated in accordance with 13.1.1 and be properly
cured. After bending in accordance with clause D.1 (at a deflection rate of 25 mm/min) over appropriate
sized mandrels, the coating shall not crack, disbond or pinhole and shall pass a holiday test in
accordance with Appendix E.

13.1.6 Impact resistance test


Coated steel plates should be tested in accordance with Appendix F.

The coating shall withstand a minimum impact of 5 J without resulting in a breakdown or loss of adhesion
of the coating.

13.1.7 Adhesion test


The adhesion test procedure should be as specified in clauses G.5 and G.6 and the results assessed in
accordance with clause G.7.

13.1.8 Hardness and cure of coating


The hardness and degree of cure of the coating should be determined and the Manufacturer should
specify the hardness range, and the temperature at which hardness values were conducted, to indicate
the correct degree of cure of the coating.

13.2 Environmental test requirements


13.2.1 General
The Contractor should ensure that the tests specified in 13.2.2, 13.2.3 and 13.2.4 are carried out in
duplicate by the Manufacturer in accordance with 14.4 and the results of the tests, demonstrating
compliance, made available.

The tests specified in 13.2.5 to 13.2.7 inclusive should be carried out once to provide evidence of
satisfactory long term performance.

13.2.2 Cathodic disbondment test


Sample panels should be tested by the procedure specified in Appendix H. The coating, when subjected
to an impressed current at a negative voltage of 1500 mV at 20 °C, shall not disbond for greater than 5
mm radius from the edge of the coating pre-damage after 28 days.

13.2.3 Strain/polarization cracking test


The sample panels should be subjected to a bend strain at 20 °C and then predamaged, polarized and
tested as specified in Appendix I with the test area selected on the minimum radius of the bend, i.e. area
of maximum strain.

13.2.4 Water immersion test


The sample panels should be subjected to a water immersion test as specified in Appendix G. The test
shall show no loss of adhesion greater than 3 mm after 28 days.

13.2.5 Humidity resistance test


Coated steel test plates should be exposed for 2000 h in accordance with ISO 6270. The coating shall
not lose adhesion when tested in accordance with Appendix G.6 and no underfilm corrosion or blistering
of the film shall occur.

© National Grid Gas plc 2006 - All Rights Reserved


J229 ( Rev 03/06 ) -9-
T/SP/CW/6 Part 1

13.2.6 Salt spray resistance test


Coated steel test plates should be cross-cut across diagonal corners and exposed for 2000 h to
continuous salt spray conditions in accordance with BS 3900: Part F4. The coating shall not lose
adhesion when tested in accordance with Appendix G.6 and no underfilm corrosion or blistering of the
film shall occur.

13.2.7 Artificial weathering test


Coated steel test plates should be exposed for 2000 h to artificial weathering, in accordance with
ISO 11507, and should show no signs of deterioration, apart from superficial chalking. UVA lamps should
be employed and the test cycle should consist of 4h UV and 4h condensation, both at a temperature of
50 °C.

13.3 Thermal stability tests


13.3.1 General
The Contractor should ensure that the test specified in 13.3.2 is carried out in duplicate by the
Manufacturer and the results of the test, demonstrating compliance, made available.

13.3.2 Test conditions


Coated steel test plates should be exposed to dry heat at 50 °C for three months to determine thermal
stability and shall still meet the full requirements of 13.1.5 to 13.1.7 inclusive and 13.2.2 to 13.2.6
inclusive.

14. QUALITY CONTROL REQUIREMENTS


14.1 Before dispatch from the factory, the Manufacturer should carry out sampling and testing of the
manufactured material covered by this specification in accordance with 14.2, 14.3 and 14.4.

14.2 During the production of each separate batch or twice every 8 h of continuous production
(whichever is the more frequent), the tests specified in 11.2, 11.3 and 11.4 should be carried out. The
requirements of 11.5 to 11.7 inclusive shall also be met.

14.3 At least once every 8 h of continuous production, the tests specified in 13.1.2 to 13.1.8
inclusive should be carried out.

14.4 The tests specified in 12.2 to 12.7 inclusive and in 13.2.2, 13.2.3 and 13.2.4 (considered as
type tests) and the requirements of 11.8 should be carried out once per year or at any time a production,
source, process or formulation change is made to the coating system.

15. COMPLIANCE
The coating material shall not be dispatched until it has been demonstrated that the Manufacturers
inspection and testing complies with the requirements of this specification.

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APPENDIX A
REFERENCES
This Specification makes reference to the documents listed below.

A.1 Statutes and Regulations


- Control of Substances Hazardous to Health (COSHH)
Regulations (2002).
- The Health and Safety at Work etc. Act 1974.
- Management of Health and Safety at Work Regulations (1999).
- Chemicals (Hazards Information and Packaging for Supply)
Regulations (2002).
- Environmental Protection Act (1990).
- Environmental Protection (Duty of Care) Regulations (1991).
- Special Waste Regulations (1996).

A.2 British Standards


BS 1357 - Specification for screwed and socketed steel tubes and tubulars
and plain end steel tubes suitable for welding or for screwing to
BS21 pipe threads.
BS 2015 - Glossary of paint terms.
BS 3900 - Methods of test for paints: PartF4: Resistance to continuous salt
spray.
ISO 3251 - Determination of volatile matter and non-volatile matter.
ISO 6270 - Determination of resistance to humidity (cyclic condensation).
ISO 8501 - Preparation of steel surfaces before application of paints and
related products.
ISO 9000 - Quality Systems.
ISO 11507 - Paints and varnishes:Exposure of coatings to artificial
weathering.

A.3 American Society for Testing and Materials


ASTM G14-77 - Test for impact resistance of pipeline coatings - (Falling weight
test).

A.4 National Grid Gas Documents


T/SP/CM/2 - Specification for internal coating materials for steel line pipe and
fittings.
T/SP/CW/5 - Technical specification for field applied external coatings for
buried pipework and systems.
T/SP/CW/6 - Technical specification for the external protection of steel line
Part 2 pipe and fittings using fusion bonded powder and other coating
systems.
Part 2 -Factory applied coatings.

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APPENDIX B
DEFINITIONS
The definitions applying to this specification are given below.

National Grid Gas - National Grid Gas - a part of National Grid plc.

National Grid Gas - The person appointed from time to time by National Grid Gas and notified in
representative writing to the Contractor to act as National Grid Gas representative for the
purposes of the Contract.

Contractor - The person, firm or company with whom National Grid Gas enters into a
contract to which this specification applies, including the Contractor's personal
representatives, successors and permitted assigns.

Manufacturer - The producer of the coating material or his appointed agents or assigns.

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APPENDIX C
METHODS FOR THE EVALUATION OF THE THERMAL CHARACTERISTICS OF POWDER AND
CURED COATING
C.1 INTRODUCTION
This appendix details methods by which the thermal characteristics of a powder (see clause C.2) and the
thermal characteristics of cured coating (see clause C.3) can be evaluated.

C.2 EVALUATION OF THERMAL CHARACTERISTICS OF POWDER


C.2.1 Principle
The method for the determination of powder reactivity and glass transition temperatures of powder
consists of heating the powder at a constant rate in a differential scanning calorimeter (DSC). A first trace
is made which records thermal changes in the sample between ambient temperature and some point
after full cure. When full cure is achieved, the sample is cooled rapidly to ambient temperature and a
second DSC run is carried out. Values for glass transition temperature and heat of cure can be derived
from the trace. The accuracy of both axes, should be confirmed by calibration before powder testing is
carried out.

C.2.2 Apparatus
The apparatus used should be a DSC∗ with sufficient calorimetric sensitivity to respond to the glass
transition temperature of the powder (the thermal analysis curve should be capable of displaying the heat
flow rate at a sensitivity of not less than 400µW/cm). Additionally, the following accessories will be
required:

a) Aluminium sample pans.


b) Quench cooling accessory.
c) Analytical balance capable of weighing to an accuracy of 0.1 mg.
d) Liquid nitrogen or other cooling fluid. Alternatively, a DSC with a built-in cooling device is
acceptable provided it can cool the sample rapidly at the rate required in the method.
A further device is required to measure the area under the cure exotherm (see C.2.5.6).

C.2.3 Calibration of the Differential Scanning Calorimeter


C.2.3.1 Temperature axis calibration
A method suitable for checking the temperature axis calibration is as follows:

a) Calibrate the upper temperature scale of the DSC using samples of pure indium, tin and
lead which have melting points of 156.6 °C, 231.9 °C and 327.4 °C respectively.
b) Melt the metal samples in open pans in either static air or under inert gas purge,
depending on the test procedure being followed.
c) Take the melting point as the intersection of the leading edge of the fusion endotherm with
the projected baseline.

The results obtained are influenced by the scan rate, therefore adjust the instrument such that these
values are correct at the scanning rate employed in the test, i.e. 20 °C/min.

In practice, melting points are usually within 2 °C to 3 °C of the accepted values when determined at a 20
°C/min scan rate and this is found to be adequate for Tg measurements of the coating film. If the
measured value differs from the true value by more than 2 °C to 3 °C, recalibrate the temperature axis.


There are a number of DSC machines available and correlation should be demonstrated

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C.2.3.2 Theory of calorimetric calibration


The mV signal which drives the pen of the recorder in the Y direction is a measure of the rate of heat
absorbed or evolved and is derived from the following equation:

dh
= K1 δY
dt

where δY = difference in Y-axis deflection between the sample and empty pan curves at the
temperature of interest, measured in units of length (centimetres, inches, etc.).

K1 = proportionality constant, made up of:

a) The signal attenuation setting on the Y-axis, i.e. q s (Y axis range in mW or equivalent).
b) The cell calibration coefficient E (dimensionless).

The cell calibration coefficient E can be determined at any given temperature through the use of a
material of known specific heat (e.g. sapphire (A12O3)) using the following equation:

CpHrm
E= (1)
q sδ Y

where Cp = specific heat of sample at the temperature of interest.

Hr = heating rate.

m = sample mass.

Equation (1) is derived from another equation (2), which relates the heat release (or absorption) to the
area of the event on the thermogram, i.e.:

A
H= (B E qs) (2)
M

where H = heat released.

A = area of the exotherm.

B = time base setting (see A.2.5.3 e).

The heat release is a function of the specific heat of the test material and equal to:

1
H = CpHrAB (3)
δY

Therefore, if this is substituted in equation (2) and transposed, we arrive at the equation for E.

Alternatively, the cell constant may be determined by relating the latent heat fusion of the pure material
(e.g. indium) to the area produced from the melting endotherm.

C.2.3.3 Method for determining the cell coefficient E


C.2.3.3.1 Place two empty pans in the DSC cell and run a temperature programme between ambient
temperature and 300 °C. If the trace is not almost horizontal, the baseline slope control should
be adjusted until the best line is achieved. A typical temperature calibration chart is shown in
Figure C.1.

C.2.3.3.2 Load the sample pan with a weighed sapphire disc for a second run. Heat the pan up to the
initial ambient temperature and hold until equilibrium is obtained. This should be achieved by
setting the starting temperature to ambient temperature and running in isothermal mode.

C.2.3.3.3 Run a second trace using the same final temperature as is used in C.2.3.3.1.

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C.2.3.3.4 Measure several values for δ Y, the vertical difference between the traces, to calculate E
values at these points. The average of E over the range of interest should be used.

C.2.4 Sampling
When it is necessary to sample large amounts of powder from the sample batch (e.g. several kilogram
boxes), take representative amounts (approximately 50 g) from each container, mix together and sample
by coning and quartering. Analyse different batches separately.

Take a final sample (approximately 250 g) and store it in an airtight container, at a temperature not
higher than 0 °C, in case subsequent testing is required. When the cold sample is taken from cold
storage, allow at least 30 min in its closed container to reach ambient temperature. Take powder for DSC
tests directly from the 250 g sample.

When amounts of powder less than 1 kg are involved, coning and quartering or riffle sampling is not
necessary.

Record the following information for each sample:

a) Date.
b) Time.
c) Powder lot number/batch number.

C.2.5 Test procedure


C.2.5.1 Instrument setting
The test procedure and instrument settings depend upon the design of equipment employed. However,
there are certain essential features in the test method which should be followed if consistent and
comparable results are to be obtained.

Where applicable, select a baseline slope setting which gives a virtually horizontal line when the
reference and sample pans are loaded identically. This is normally carried out with empty pans.

C.2.5.2 Preparation of test samples


Weigh out accurately between 10 mg and 15 mg of powder into an aluminium sample pan. Heavier
weights (up to 25 mg) may be used, if needed, to give adequate sensitivity. The accuracy of weighing
should be ±0.1 mg.

C.2.5.3 Standard air test


Carry out the standard air test under the following conditions:

a) Use open pans throughout.


b) Use an empty aluminium pan for the reference.
c) No purge gas is employed; carry out the test in static air at atmospheric pressure.
d) Appropriate data sampling and recording rate.
e) If exothermal areas are to be recorded accurately, it may be necessary with some
instruments to change from a temperature base on the abscissa to one of time before the
onset of cure.
f) Heat the sample from ambient temperature to 280 °C at a rate of 20 °C/min and record the
trace. Rapidly cool the sample to ambient temperature. Repeat this procedure for the
second run, except that this run may be terminated at approximately 20 °C in excess of the
second run glass transition temperature (Tg2).
The test temperature of 280 °C may be subject to change depending on the type of coating material
under test. It should be advised by the powder manufacturer.

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C.2.5.4 Inert gas test


Carry out the inert gas test as for the standard air test (see C.2.5.3), using an inert gas purge instead of
static air throughout the test. A flow rate of 40 ml/min should be used.

C.2.5.5 Measuring the glass transition temperature


The glass transition temperature (Tg) is defined as that temperature (or temperature range) at which the
coating polymer is transformed from a hard and often brittle material (the glass) into a tough, rubber-like
material.

The glass transition temperature of the cured material is visible on the DSC trace as a baseline shift,
resulting from a marked step-like change in specific heat at Tg, the step usually covering several
degrees. It is conventional to take Tg as the point of intersection of the extrapolated baseline at the low
temperature end and the tangent of the curve at the inflection point (see Figure C.2). For raw powders,
the Tg usually takes the form of a baseline shift with a superimposed endothermic peak (see Figure C.3).

C.2.5.6 Measuring the heat released during cure


It is necessary to measure the area under the curing exotherm either in the determination of thermal
stability, or when the quality of oversprayed powder is in question.

There are several ways of measuring the exothermal area which vary in their accuracy. These are:

a) Electronic integration using a computer or a dedicated integrator.


b) Planimeter.
c) Cut out the exothermal area marked on the chart paper, weigh it and compare it with the
weight of a known area of the same paper.
d) Count the squares within the exothermal area marked on the chart paper.

One of these, or a similar method, should be selected for use with the DSC.

The points at which the cure exotherm commences and ends are used to calculate the heat release.
They are usually determined by drawing in the baseline to the exotherm using a rule. Care shall be taken
to distinguish between the onset of cure (Toc) and the onset of flow (Tof) and to commence the baseline at
Toc (see Figure C. 3).

C.3 MEASUREMENT OF DEGREE OF CURE OF POWDER COATING


C.3.1 Principle
The method of assessment of the cure of the powder coating film cure by measurement of its glass
transition temperature consists of heating a ground coating sample at a constant rate in a DSC. A first
trace is made which records thermal changes in the sample between ambient temperature and some
point after full cure as defined by the powder manufacturer. The sample is cooled to ambient temperature
and a second run carried out. The glass transition temperatures before and after heating are determined
and are used to assess the degree of cure. It is essential that samples are initially pretreated in the
calorimeter to remove moisture and to confer a uniform thermal history.

C.3.2 Apparatus
The apparatus used should be a DSC with sufficient calorimetric sensitivity to respond to the glass
transition temperature of the materials under test (the thermal analysis curve should display the heat flow
rate at a sensitivity of 400µW/cm minimum). Additionally, the following accessories will be required:

a) Aluminium sample pans.


b) Quench cooling accessory.
c) Analytical balance capable of weighing to an accuracy of 0.1 mg.
d) Liquid nitrogen or other cooling fluid. Alternatively, a DSC with a built-in cooling device is
acceptable provided it can cool the sample rapidly at the rate required in the method.
e) Hammer and cold chisel.

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f) Microhammer mill or equivalent.

C.3.3 Temperature axis calibration


The method to be used for checking the temperature axis calibration is as follows:

a) Calibrate the upper temperature scale of the DSC using samples of pure indium, tin and
lead which have melting points of 156.6 °C, 231.9 °C and 327.4 °C respectively.
b) Melt the samples in open pans in either static air or under an inert gas purge, depending
on the test procedure being followed.
c) Take the melting point as the intersection of the leading edge of the fusion endotherm with
the projected baseline.

The results obtained are influenced by the scan rate, therefore adjust the instrument such that these
values are correct at the scanning rate employed in the test, i.e. 20 °C /min.

In practice, melting points are usually within 2 °C to 3 °C of the true values when determined at a
20 °C/min scan rate and this is found to be adequate for Tg measurements of the coating film. When the
temperature deviation is higher than this, it is necessary to adjust the sample thermocouple reference
junction.

If adjustment has been necessary to bring within limits, carry out a further calibration to demonstrate that
the instrument is calibrated accurately.

C.3.4 Sampling
Remove coating film samples from the coated component using a hammer and cold chisel. This
produces furled coating flakes. Care should be taken to remove samples of full film thickness, but at the
same time avoid the inclusion of steel debris.

Sample a component at several points along its length and around its circumference. Take samples from
test panels in a similar manner.

Collect the coating flakes in a plastics bag and identify. Grind the flakes to pieces small enough to pass
through a 2.8 mm aperture sieve in a microhammer mill. Record the following information for each
sample:

a) Date.
b) Time.
c) Component number.
d) Sequence number.
e) Powder lot number/batch number.
f) Location of sample on component.

C.3.5 Test procedure


C.3.5.1 Instrument setting
The test procedure and instrument settings used depends upon the design of equipment involved.
However, there are certain essential features in the test method which should be followed if consistent
and comparable results are to be obtained.

Where applicable, select a baseline slope setting which gives a virtually horizontal line when the
reference and sample pans are loaded identically. This is normally carried out with empty pans.

C.3.5.2 Preparation of test samples


Weigh out accurately between 10 mg and 15 mg of ground coating into an aluminium sample pan.
Heavier weights (up to 25 mg) may be used, if needed, to give adequate sensitivity. The accuracy of
weighing should be ±0.1 mg.

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C.3.5.3 Standard air test


Carry out the standard air test under the following conditions:

a) Use open pans to assist the release of moisture from the sample during pre-treatment.
b) Use an empty aluminium pan for the reference.
c) No purge gas is employed; carry out the test in static air at atmospheric pressure.
d) Appropriate experimental data recording conditions.
e) It will normally be necessary to subject the coating sample to thermal pre-treatment before
assessment of its degree of cure. Pre-treatment is designed to remove any absorbed
moisture from the coating because moisture is known to influence glass transition
temperature measurements. Such pre-treatment should not significantly advance the cure
of the coating sample.

The powder Manufacturer should specify the thermal pre-treatment required for the
product. This will typically require heating the sample in the DSC cell from ambient
temperature
(i.e. 20 °C to 25 °C) to some defined temperature higher than 100 °C, probably in the
range 100 °C to 150 °C. This required temperature will typically be attained within 120 s
and held for a period up to 60 s. Immediately cool the sample to ambient temperature with
liquid nitrogen or a suitable cooling fluid; alternatively, a DSC with a built-in cooling device
is acceptable provided it can cool the sample rapidly at the rate required in the method.

Make a suitable record of the pre-treatment run.


f) Heat the sample from ambient temperature to a temperature specified by the
Manufacturer, at a rate of 20 °C /min, so that the sample achieves full cure, but avoids
significant degradation. Rapidly cool the sample to ambient temperature using liquid
nitrogen or a suitable cooling fluid. This establishes the first glass transition temperature
(Tg1).
Repeat the procedure for the second run, except that this run may be terminated at
approximately 20 °C higher than the second glass transition temperature (Tg2).
Record both (Tg1) and (Tg2) runs as a hard copy.

C.3.5.4 Inert gas test


Carry out the inert gas test as for the standard air test (see C.3.5.3), using an inert gas purge instead of
static air throughout the test. Use a flow rate of 40 ml/min throughout the test.

C.3.5.5 Measuring the glass transition temperature


The glass transition temperature (Tg) is defined as that temperature (or temperature range) at which the
coating polymer is transformed from a hard and brittle material (the glass) into a tough, rubber-like
material.

The glass transition temperature is visible on the DSC trace as a baseline shift, resulting from a marked
step-like change in specific heat at Tg, the step usually covering several degrees. It is conventional to
take Tg as the point of intersection of the extrapolated baseline at the low temperature end and the
tangent of the curve at the inflection point (see Figure C.2).

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FIGURE C.1 - Typical temperature calibration

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FIGURE C.2 - Typical DSC traces - Glass transition temperature

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FIGURE C.3 - Typical DSC traces - Enthalpy H

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APPENDIX D
FLEXIBILITY TEST
D.1 LABORATORY PREPARED TEST PANELS
D.1.1 Apply the coating to steel plates 50 mm x 300 mm x 6 mm thick and properly cure. Bend (at a
deflection rate of 25 mm/min) over appropriate sized mandrels (see D. 1.2) at two substrate
test temperatures (5 °C and 20 °C). After bending, the coating shall not crack, disbond or
pinhole when holiday tested in accordance with Appendix E. Inspect plates immediately after
bending and again after 24 h at 20 °C.

D.1.2 Select mandrel sizes according to the following formula:

t(1-S)
D=
S

where D = mandrel diameter, in mm (see Figure D.1).

t = plate thickness, in mm.

S = one of the values in clause D.3 depending on the intended coating


application and the temperature of the test.

The arc length of the mandrel should be fixed at 225 ±25 mm.

D.1.3 Set the panel support gap according to the following formula:

Support gap = M + 2t + 4 mm

where M = chord length across the mandrel arc, in mm (see Figure D.1).

t = plate thickness, in mm.

Bend the panel until it makes contact with the entire surface area of the mandrel.

D.1.4 During bending, peaking (point at which a gap occurs between the mandrel and the panel)
may be observed at the centre of the panel. In this case, the area of the panel where the gap
exceeds 0.254 mm (0.010 in.) should be disregarded in evaluating the test results. This area
should not exceed 25% of the mandrel surface area.

D.2 TESTS ON PIPE SPECIMENS


D.2.1 Cold cut test specimens 356 mm long x 50 mm wide from a pipe section with the long axis in
the circumferential direction. Where seamless pipe is being tested, select specimens which
show a minimal variation in pipe wall thickness, particularly within the test area (i.e. middle 75
mm to 100 mm of specimen). Bend the test specimens over appropriate sized mandrels at two
substrate test temperatures (5 °C and 20 °C). After bending, the coating shall not exhibit visible
signs of cracks, disbonding or pinholes and shall pass a holiday detection test when tested in
accordance with Appendix E. Inspect specimens immediately after bending and again after 24
h at 20 °C.

D.2.2 Select mandrel sizes according to the following formula:

1
D1 = -t
S 1
+
t D0 - t

where D1 = mandrel diameter, in mm.

D0 = original specified pipe outside diameter, in mm.

t = pipe wall nominal thickness, in mm.

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S = one of the values specified in clause D.3 depending on the


intended coating application and the temperature of the test.

D.2.3 The arc length of the mandrel should be fixed at 225 ± 25 mm.

D.2.4 For specimens from pipes having an outside diameter in the range 406 mm to 1219 mm, set
the panel support gap according to the following formula:

Support gap = M + 2t + 4 mm
where M = chord length across the mandrel arc, in mm (see Figure D.1).
t = plate thickness, in mm.

Bend the specimen until contact is made with 75 ± 10% of the mandrel area.

D.2.5 For specimens from pipes having an outside diameter in the range 305 mm to 405 mm set the
panel support gap according to the following formula:

Support gap = M + 2t + 29mm


where M = chord length across the mandrel arc, in mm (see Figure D.1).
t = plate thickness, in mm.

Bend the specimen until it makes contact with the entire surface area of the mandrel.
Test specimens from pipes having an outside diameter below 305 mm by an appropriate
method.

D.2.6 During bending, peaking (point at which a gap occurs between the mandrel and the panel)
may be observed at the centre of the panel. In this case, the area of the panel where the gap
exceeds 0.254 mm (0.010 in.) should be disregarded in evaluating the test results. This area
should not exceed 25% of the mandrel surface area.

D.3 S VALUES
D.3.1 For coatings intended for use on fittings, the following S values should apply:

S = 0.005 at a temperature of 5 °C.

S = 0.01 at a temperature of 20 °C.

D.3.2 For coatings intended for use on line pipe, the following S values should, apply:

S = 0.02 at a temperature of 5 °C.

S = 0.03 at a temperature of 20 °C.

D.4 TESTING AT 5 °C
Testing at 5 °C may be carried out by pre-cooling the panel in a refrigerator to a temperature slightly
lower than 5 °C and carrying out the bending operation when the panel temperature reaches 5 ±2 °C.
Alternatively, an environmental chamber that controls the temperature of the bending apparatus may be
used. The test specimens should not be immersed in any liquefied coolant to achieve the test
temperature.

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FIGURE D.1 - Typical mandrel for flexibility tests

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APPENDIX E
HOLIDAY DETECTION OF COATINGS

E.1 EQUIPMENT
Holiday detection should be carried out using dc, non-pulsing holiday detection equipment on surfaces at
temperatures below 90 °C and free from moisture.

E.2 OPERATING VOLTAGE


The operating voltage should be 125 V per 25 µm of coating thickness.

The rate of travel of the probe over the surface should not exceed 300 mm/s.

E.3 ELECTRODE TYPE


For all coating systems the wire brush type of electrode should be used, suitably curved to conform to
the contour of the coated surface of pipe. For fittings, a suitable procedure should be agreed with the
coating applicator and should normally be the one that is approved within the procedure qualification.
The brush should be maintained in such a condition that a full contact is assured over the full length of
the brush.

E.4 IDENTIFICATION METHOD


All holidays should be identified with a waterproof marker.

E.5 EQUIPMENT CALIBRATION


All holiday detectors should be calibrated at the beginning of every working day and, additionally, when
requested by National Grid Gas.

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APPENDIX F
EVALUATION OF RESISTANCE TO IMPACT
F.1 GENERAL
The procedures specified in clauses F.2 to F.6 inclusive serve to assess the comparative resistance of
coatings to impact damage.

F.2 TEST EQUIPMENT


The following test equipment will be required:

a) A variable impact tester (ASTM G14-77, paragraph 4.2 or equivalent) with punch hammer
type indentor modified as shown in Figure F.1 to accommodate a 14.3 mm diameter ball
bearing and equipped with a minimum impact mass of 1 kg.
b) A sufficient supply of 14.3 mm diameter ball bearings manufactured from EN31 steel with
a Vickers hardness of 800 to 930.
c) A holiday detector (see Appendix E).
d) A thickness gauge.
e) Repair materials.

F.3 TEST PROCEDURE ON COMPONENTS


F.3.1 Check the test site to ensure that it is free from holidays with the holiday detector set at the
required voltage for the particular coating thickness (see clause E.2).

F.3.2 Position the impact tester on a holiday free site 300 ± 50 mm from one end of the component.

F.3.3 Drop the impact weight from a height calculated to impart the specified impact energy to the
coating. The impact height may be calculated using the following formula:

J
H =
9.81W

where H = impactor height, in m

W = impactor mass, in kg.

J = impact energy, in joules.

F.3.4 Retest the impact area for holidays using the detector set at the required operating voltage.

F.3.5. Repeat F.3.2, F.3.3 and F.3.4 at four more locations evenly spaced over the surface of the
component.

F.3.6 Rotate the ball bearing after each impact.

F.3.7 After every 20 impacts fit a new ball bearing.

F.3.8 If a holiday is caused by the impact test, check the coating thickness in the test area using a
thickness gauge.

F.4 REPAIR PROCEDURE FOR COMPONENTS


Repair any holiday caused by impact testing using repair materials.

F.5 TEST PROCEDURE ON PANELS


F.5.1 Test sample panels (300 mm x 50 mm x 6 mm) and test panels (300 mm x 50 mm) cold cut
from pipe sections in the longitudinal direction should be tested according to the procedure
detailed in ASTM G14-77, paragraphs 6 to 9, using the apparatus detailed in clause F.2 a).

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The additional modifications to the ASTM procedure specified in F.5.2 to F.5.6 inclusive should
apply.

F.5.2 Test impact areas for failure using the holiday detector set at a voltage of 125 V per 25µm of
coating thickness (this relates to coating thickness before impact damage).

F.5.3 The minimum spacing between impacts along the centre line of the specimen should be
25 mm.

F.5.4 Rotate the ball bearing after each impact.

F.5.5 After every 20 impacts fit a new ball bearing.

F.5.6 Increase the height by an increment of 10 mm between impacts.

F.5.7 There shall be no disbonding at the minimum impact energy. Verify this by testing in
accordance with clause G.6 and report in accordance with clause G.7.

F.6. REPORTING RESULTS


F.6.1 If the coating withstands the specified impact energy without forming a holiday, the test should
be recorded as a 'Pass'. If a holiday is formed at the specified impact energy, the test should
be reported as 'Fail at thickness of...' and the measured coating thickness should be recorded.

F.6.2 The impact strength should be converted to impact energy in joules and this value should be
reported. (A typical calculation is shown in Figure F.1).

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FIGURE F.1 - Impactor and typical calculation

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APPENDIX G
EVALUATION OF RESISTANCE TO WATER IMMERSION

G.1 GENERAL
The equipment and procedure detailed in clauses G.2 to G.7 inclusive should be used to assess the
comparative resistance of coatings applied to components (free of holidays) to loss of adhesion due to
water absorption.

G.2 EQUIPMENT
The following equipment will be required:

a) A water bath which should be maintained at a temperature of 50 ±2 °C.


b) A holiday detector.
c) Internal pipe coating material (complying with CM2).
d) 6 mm diameter twist drill.
e) Pointed sharp knife, e.g. Stanley type or similar.
f) 5 mm diameter steel rod 450 mm long.
g) Elastomeric adhesive for repairing test areas, e.g. Silastic silicone-rubber, grades RTV 738
or RTV 732 or equivalent.

G.3 SAMPLE PREPARATION


G.3.1 Laboratory prepared specimens
Prepare 300 mm x 50 mm x 6 mm panels under conditions of application and cure similar to
those for a coated component.

G.3.2 Specimens taken from components


Cold cut 300 mm x 50 mm specimens from a sample pipe or, in the case of a fitting, from the
pipe pup which has been coated as a test piece.

G.4 PREPARATION OF TEST AREA


G.4.1 To ensure freedom from holidays, test the prepared panels for holidays with the holiday
detector set at the required voltage (see clause E.2).

G.4.2 Drill a 6 mm diameter hole through the test panel within 25 mm of one end.

G.4.3 Protect the bare metal of the panel with internal coating material (see clause G.2 c)).

G.5 INITIAL TEST PROCEDURE


G.5.1 Carry out an initial adhesion test as described in clause G.6.

G.5.2 Using the steel rod fitted through the 6 mm diameter hole, suspend the specimen panel in the
water bath immersing all but the top 50 mm of the panel.

G.5.3 After 7 days, remove the panel from the water bath and allow it to cool to ambient temperature.
No longer than 30 minutes should be allowed between removing the test panel from the bath
and performing the adhesion test.

G.5.4 Test the coating adhesion as specified in clause G.6.

G.5.5 Repair the test area using elastomeric adhesive.

G.5.6 Return the panel to the water bath immediately.

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G.5.7 If, after seven days immersion, the coating is retested and is found to be satisfactory, return
the panel to the water bath and repeat the adhesion test at intervals of seven days up to a total
immersion time of 28 days. If the coating fails the requirements of this specification at any test
interval within the 28 days, it should be removed from test.

G.6 INVESTIGATION PROCEDURE


G.6.1 Use one or other of the following procedures (G.6.2, G.6.3) as appropriate.

G.6.2 For all coated components and coatings on panels equal to or less than 600µm thickness, use
the following procedure:

a) Using a sharp pointed knife (e.g. Stanley knife or similar), make two incisions
approximately 13 mm long through to the metal surface to form a V with an angle of
approximately 30° at the intersection point.
b) Starting at the point of intersection force the coating from the steel substrate using the
sharp pointed knife. Take care to protect the eyes and hands when carrying out this
operation.

G.6.3 For laboratory panels with coatings greater than 600µm thickness use the following procedure:

a) Using a small hacksaw blade (e.g. 'Junior' type or similar) make two incisions through to
the metal surface to form an X with an angle of approximately 30° at the point of
intersection.
b) Draw a sharp knife along the cut lines to ensure that the hacksaw blade has reached the
metal surface.
c) Starting at the point of intersection, force the coating from the steel substrate using the
sharp pointed knife. Take care to protect the eyes and hands when carrying out this
operation.

G.7 REPORTING RESULTS


Refusal of the coating to peel or a cohesive failure within the coating should be recorded as a 'Pass'.

Cohesive failure, caused by voids leaving a honeycomb structure on the specimen surface, should
constitute a failure.

For the purpose of this test, cohesive failure will be recorded where some coating material remains on
the metal surface and where difficulty in coating removal has been experienced.

The extent of the adhesive failure between the coating and the metal substrate should be recorded.
Adhesive loss greater than 3 mm shall be recorded as a 'Failure'.

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APPENDIX H
EVALUATION OF RESISTANCE TO CATHODIC DISBONDING
H.1 GENERAL
The procedures detailed in clauses H.2 to H.7 inclusive serve to assess the comparative resistance of
damaged pipe coatings to disbonding when exposed to cathodic protection in potentially corrosive soils.

H.2 TEST REQUIREMENT


H.2.1 Apparatus
The following apparatus will be required:

a) A stabilized dc power unit having a voltage output of 12 V and a capability to supply 20 mA


simultaneously to each test area in circuit. A suitable circuit is shown in Figure H.1 a).
b) Digital voltmeter, range 1.999 V (3.5 digit), input impedance 10³ M Ω. Accuracy of 0.1% ±1
digit at 20 ±1°C.
c) Variable resistor, range 1 kΩ ±10%, 1 W (one required for each specimen).
d) 75 mm length of 0.8 mm diameter platinum wire, or similar length of 6 mm wide, 1.5 mm
thick platinized titanium strip (one required for each test area).
e) Holiday detection equipment.
f) Reference electrode of the saturated calomel type, constructed from glass or plastics with
porous plug. The diameter should be not greater than 10 mm.
g) 6 mm diameter twist drill with included cutting angle of 160°.
h) Equipment for maintaining the temperature of the specimens and test area
at 20 ±2 °C.
i) A length of rigid plastic pipe per test area to be used as a solution container (approximate
dimensions 60 mm long x 50 mm nominal bore).
j) Elastomeric adhesive for fixing the plastic pipe to the test surface, e.g. a silastic silicone
rubber grade RTV 738 or RTV 732 or equivalent material.
k) Fixed resistor, 1 Ω ±2%, 1 W (one required for each test area).

H.2.2 Reagent
An electrolyte comprising a sodium chloride (NaCl) solution, (3% W/V). 30 g of NaCl should be dissolved
in distilled water and made up to 1 litre.

H.3 PREPARATION OF TEST PANELS


H.3.1 Laboratory prepared specimens
Sample panels 300 mm x 50 mm x 6 mm should be prepared simulating the conditions of
application for a factory coated pipe.

H.3.2 Specimens taken from components


Test panels 300 mm x 50 mm should be cut from a sample production coated pipe.

H.4 PREPARATION OF TEST AREAS


H.4.1 Test the prepared panels for holidays with the holiday detector set at the required voltage
(see clause E.2).

H.4.2 Fix two lengths of rigid plastic tube perpendicular to the coated surface using a suitable
elastomeric adhesive (see Figure H.1). Place them with their centres on the centre line of the
panel width and equidistant from the panel ends and each other and leave for a period of 12 h
to allow the adhesive to fully cure.

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H.4.3 Drill a 6 mm diameter hole through the coating to the metal surface in the centre of each test
area using the drill specified in H.2.1 g).

H.5 INITIAL TEST PROCEDURE


H.5.1 Fill each plastic tube with NaCl electrolyte to a depth of approximately 50 mm (see H.2.2) with
the apparatus set up as shown in Figure H.1 a). Bring the temperature of the specimens and
test area to 20 ±2 °C Maintain this temperature throughout the test period.

H.5.2 Connect a voltmeter and reference electrode to each test rig in turn as shown in Figure H.1 b)
With the tip of the calomel reference electrode positioned approximately 10 mm from the
centre of the hole, adjust the voltmeter reading to read a negative voltage of 1500 mV with
respect to the calomel electrode. Carry this out using the variable resistance shown in Figure
H.1 a).

H.5.3 Record, at intervals of 24 h, the voltmeter indication for each test area and adjust the variable
resistor to correct any drift from the negative voltage setting of 1500 mV. Also record, every 24
h, the current flow by measuring the voltage drop across the 1 Ω fixed resistor.

H.5.4 Every 24 h check the plastic tube for loss of electrolyte and restore the level with distilled water
as necessary.

H.6 INVESTIGATION PROCEDURE


H.6.1 After seven days, remove the electrolyte and plastic tube from one test site and remove
excess moisture.

H.6.2 Use one or other of the following procedures (H.6.3, H.6.4) as appropriate within 30 minutes of
removing the plastic tube:

H.6.3 For coatings up to and including 600µm use the following procedure:

a) Using a sharp-pointed knife (e.g. Stanley type or similar), make two incisions
approximately 13 mm long through to the metal surface extending radially from the 6 mm
hole and at an angle of approximately 30° to each other to form a truncated V.
b) Starting at the base of the truncated V, force the coating from the steel substrate using the
sharp pointed knife. Take care to protect the eyes and hands when carrying out this
operation.

H.6.4 For all coatings in excess of 600µm thickness use the following method:

a) Using a small hacksaw blade (e.g. 'Junior' type or similar), make two cuts across the 6 mm
hole at an angle of approximately 30° to each other to form a truncated 'X'. Make the cuts
through to the metal surface and to extend radially from the 6 mm hole.
b) To ensure that the hacksaw blade has reached the metal surface, draw the point of the
sharp knife along the cut lines.
c) Starting at the base of the truncated V, force the coating from the steel substrate using the
sharp pointed knife. Take care to protect the eyes and hands when carrying out this
operation.

H.6.5 Repeat the investigation procedure at the second test site after 28 days.

H.7 REPORTING OF RESULTS


The amount of disbonding should be quoted as the radial distance (from the edge of the pre-
damage) over which the coating peels easily from the metal surface.

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a) Cathodic disbonding test rig

b) Voltage adjustment circuit


FIGURE H.1 - Cathodic disbonding test apparatus

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APPENDIX I
STRAIN/POLARIZATION TEST
I.1 Bend the test sections in accordance with the method detailed in Appendix D using a value of
S = 0.02 for line pipe powders and S = 0.005 for fitting powders at a temperature of 20 ±2 °C.

I.2 Fix a length of rigid plastic tube perpendicular to the coated surface as detailed in H.4.2 with its
centre on the centre line of the panel and on the minimum radius of the bend i.e. the region of
maximum strain.

I.3 Drill a 6 mm diameter hole through the coating to the metal surface and polarize the specimen
as detailed in H.5. After 28 days polarization, remove the electrolyte and the plastic tube and
remove excess moisture from the test surface.

I.4 The area of coating exposed to the electrolyte shall not exhibit signs of cracks, disbondment in
excess of 5 mm from the edge of the predamage or pinholes, and shall pass a holiday
detection test as detailed in Appendix E.

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APPENDIX J
EVALUATION OF RESISTANCE TO HEAT BLISTERING

J.1 GENERAL
The equipment and procedures detailed in clauses J2 to J5 inclusive should be used to assess the
resistance of FBE coatings to heat blistering.

J.2 TEST REQUIREMENT


J.2.1 Equipment
The following equipment will be required:

a) A water bath which should be maintained at a temperature of 50 ±2 °C.


b) 6 mm diameter twist drill with included cutting angle of 160°.
c) A chrome/aluminium (K type) thermocouple.
d) A thermocouple welder.
e) A digital thermonmeter capable of recording and logging the response of a
chrome/aluminium electrode.
f) A hot air blower (typically 2kW).

J.3 PREPARATION OF TEST PANELS


J.3.1 Laboratory prepared specimens

Sample panels 50 mm x 50 mm x 6 mm should be prepared simulating the conditions of


application for a factory coated pipe.

J.4 INITIAL TEST PROCEDURE


J.4.1 Immerse the coated specimens in a 50 °C water bath (tap water) for a period of 24, 48 and 72
hours.

J.4.2 After each period of exposure remove the specimens from the water bath and immediately
remove excess water.

J.4.3 Drill a 6 mm diameter hole through the coating to expose the metal surface in the centre of the
panel. The thickness of the panel should not be reduced by more than 0.5 mm.

J.4.4 Attach the chrome/aluminium thermocouple to the 6 mm bare area by welding.

J.4.5 Heat the coated test panel(∗) from the back at a rate of 110 ±10 °C/minute, until the
thermocouple registers a temperature of 240 °C. No longer than 15 minutes should elapse
between removing the test panel from the water bath and commencing heating.

J.4.6 When the test plate attains a temperature of 240 °C quench the panel immediately in cold
water. Quenching will prevent blisters from deflating and will allow the size and blister density
to be recorded.

J.5 INVESTIGATIVE PROCEDURE


J.5.1 Monitor the temperature continuously during the heating process and observe the temperature
at which blistering first occurs.

J.5.2 Assess the blister size and blister intensity.


A 2kW hot air gun has proved to be suitable for this purpose. By adjusting the distance between the gun and the test panel the
heating rate can be varied. Ensure that the heating process is reproducible prior to performing the heat blister tests.

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J.6 REPORTING RESULTS


J.6.1 A graph showing the heating profile should be recorded and the temperature at which
blistering first appears marked on the graph.

J.6.2 A photographic record of the appearance of the test plate after quenching should be made.

© National Grid Gas plc 2006 - All Rights Reserved


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ENDNOTE
Comments
Comments and queries regarding the technical content of this document should be directed to:

Safety and Engineering Registrar


SHE Directorate
National Grid
National Grid House
Warwick Technology Park
Gallows Hill
Warwick
CV34 6DA

Buying documents
Contractors and other users external to National Grid Gas should direct their requests for further copies
of National Grid Gas documents to the department or group responsible for the initial issue of their
contract documentation.

Copyright National Grid Gas plc 2006 ©, all rights reserved. No part of this publication may by reproduced
in any material form (including photocopying and restoring in any medium or electronic means and
whether or not transiently or incidentally) without the written permission of National Grid plc except in
accordance with the provisions of the Copyright, Designs and Patents Act 1988.

© National Grid Gas plc 2006 - All Rights Reserved


J229 ( Rev 03/06 ) - 37 -

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