Coating Procedure PE

DOCUMENT DESCRIPTION

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COATING PROCEDURE

DOCUMENT No.

CP 0110-01-00-PE

REV.

Issue Date

SHEET

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The Petroleum Projects & Technical Consultations Co. ( PETROJET )

CLIENT : AQP

PROJECT: NEW 16” SEALINE JOINING NAQP-2 PLATFORM

COATING PROCEDURE FOR EXTERNAL PROTECTION OF STEEL PIPELINES USING SIDE-EXTRUSION POLYETHYLENE THREE LAYER SYSTEM

0

27/12/2011

Issued for Construction

A

20/11/2011

Issued for client comment

A.Elsamahy

S.Rezk

E.Eisa

REV.

DATE

DESCRIPTION

BY

CH'D

APPR.

THIS DOCUMENT IS CONFIDENTIAL AND THE SOLE PROPERTY OF PETROJET


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TABLE OF CONTENTS 1.

INTRODUCTION

4

2.

DEFINITIONS AND ABBREVIATIONS

5

2.1 Definitions 2.2 Abbreviations

5 6

3.

REFERENCE STANDARDS AND CODES

7

4.

RECEIVING, HANDLING, STORAGE AND LOUD OUT

5. 6.

COATING MATERIALS PROPERTIES/VENDORS PRODUCTION TESTING AND INSPECTION

9 11

6.1 6.2 6.3 6.4

11 12 12 13

7.

7.

Inspection and Tests Sampling Re-tests Nature and Frequency of Testing At Regular Production

25

REQUIREMENTS OF THE APPLIED COATING

14

7.1 Pipe Surface Preparation 7.2 Cut Back 7.3 Visual Inspection 7.4 Coating Thickness 7.5 Pre-Heating Temperature 7.6 Coating Continuity ( Holiday Detection ) 7.7 Adhesion ( Peel-Off ) Test 7.8 Impact Resistance Test 7.9 Indentation Resistance Test 7.10 Tensile Strength and Ultimate Elongation Test 7.11 Durometer Hardness – Shore D 7.12 Melt Flow Rate 7.13 Entrapment Assessment 7.14 Degree of Cure Of Fusion Bonded Epoxy Primer 7.15 Flexibility Test 7.16 Cathodic Disbonding Resistance Test 7.17 Hot Water Immersion Resistance Test

14 15 15 15 15 16 16 16 16 17 17 17 17 17 18 18 18

SURFACE PREPARATION FOR CONCRETE COATING ( Anti-

20

Slip Finish on Coating ) Surface )

8. 9.

REPAIR OF COATING STRIPPING OF COATING


21 22


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10. 11. 12.


PIPE MARKING PROCEDURE QUALIFICATION TRAIL ( PQT ) DOCUMENTATION

24 27 29

APPENDIXES Appendix A

VERIFICATION OF PIPE SURFACE PREPARATION

Appendix B

TEST FOR ASSESSING THE DEGREE OF CURE OF THE FUSION BONDED EPOXY POWDER COATING

30

33

Appendix C

INSPECTION OF THE COATING THICKNESS

36

Appendix D

HOLIDAY DETECTION TEST

37

Appendix E

IMPACT RESISTANCE TEST

38

Appendix F

PEEL -OFF RESISTANCE TEST

39

Appendix G

DETERMINATION OF ADHESION OF COATINGS

37

Appendix H

INDENTATION RESISTANCE TEST

39

Appendix I

TENSILE AND ELONGATION TEST

40

Appendix K

CATHODIC DISBONDMENT TEST

44

Appendix L

DETERMINATION OF HOT-WATER IMMERSION RESISTANCE

46

Appendix M

DETERMINATION OF FLEXIBILITY OF COATINGS

47

Appendix N

DETERMINATION AIR ENTRAPMENT IN COATINGS

48

Appendix O

DETERMINATION OF HARDNESS OF COATINGS

50

Appendix P

DETERMINATION OF MELT FLOW RATE OF POLYMERS

51



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INTRODUCTION

This procedure describes the process of the application, testing and repair of workshop side-extruded Polyethylene coatings ( 3 layer system ) which shall be applied on the external surface of AQP NEW 16" SEALINE JOINING NAQP-2 PLATFORM The coating covered by this procedure is to comply the requirements of NF A 49-710 and DIN 30 670 standards and Company spec. DOC. No. 4222-430-630-03 Rev.1 Where conflict occures between requirement of company specification and referenced codes and standards; the requirements of specification shall apply The coating system shall consist of three layers and shall be applied in accordance with this procedure, the composition of the three layers is : 1) Layer of Fusion bonded epoxy powder. 2) Layer of Polyethylene polymeric adhesive . 3) Layer of Polyethylene top coat . 4) Layer of Polyethylene Powder (Rough Coat)



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DEFINITIONS AND ABBREVIATIONS

Within the application of this procedure the following definitions and abbreviations shall be apply:

2.1 DEFINITIONS • Coating system The coating technique or process system consisting of the same type of coating

material . • Side extrusion Coating process whereby a hot extruded films of coating materials are wrapped

around the pipe in layers. The pipe is moved past the extrusion head in a spiral motion. The extruded coating films are fused together to form a continuous adherent sheath around the pipe . • Three layer system Coating system consists of three layers which are epoxy primer, adhesive and

outer layer. • Procedure qualification trial PQT application of a coating and subsequent inspection/testing to confirm that the coating system is adequate to produce a coating with the specified properties, carried out prior to the start of production. • Epoxy primer The first coating layer ( the anti-corrosion layer )

which applied directly onto the preheated pipe to improve the final adhesion of the final coating to the pipe surface .

• Adhesive The intermediate coating layer to improve the adhesion between the primer and the outer

layer . • Outer layer The Polyethylene ( PE ) layer . • Coating thickness Understood to be the average thickness of the coating system ( summation of

average thickness for the applied top coat, adhesive and primer layers ) . • Unit of production Set of pipes have the same DN and coated with the same coating system and

the same type of material . • Coating cycle

Any production process have the same DN and coated with the same coating system, and not interrupted more than 3 days .

• Test ring

Test sample from a coated pipe.

• Day

Production run and shall not more than 24 hrs.

• Shift

Production run and shall not more than 12 hrs.

• Batch No. Quantity of coating material not more than 50 tons and have the same source and grade.



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2.2 ABREVIATIONS • DN • FBE

• PE • RH • Tg • ∆Tg • J • UV • DSC • MEK • M.D.S • FIFO

Pipe nominal diameter Fusion Bonded Epoxy ( epoxy primer ) Polyethylene Relative humidity % Glass transition temperature, expressed in °C. Variation of the glass transition temperature ( Tg2 – Tg1 ), expressed in °C. Impact energy in joules. Ultra Violet . Differential Scanning Calorimetry Methyl Ethyl Ketone Material Data Sheet First in first out



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3- REFERENCE INTERNATIONAL CODES AND STANDARDS . This specification makes reference to the documents listed below, where relevant, all work shall be carried out in accordance with the latest editions of these documents, including all revisions and addenda . Where conflict occurs between the requirements of this procedure and reference codes and standards, the requirements of this procedure shall apply .

European Committee for Standardization PrEN 10285

.. (

Steel Tubes and Fittings for On and Off-shore Pipelines – External Three Layer Extruded Polyethylene Based Coatings.

L’Asaociation Francaise de Normalisation NF A 49-710

CEN )

.. (

AFNOR )

Steel Tubes External Triple-Layer Polyethylene Based Coatings Application By Extrusion.

Deutsche Institute fur Normung

.. (

DIN )

DIN 53 505

Testing of Rubber, Elastometer and Plastics; Shore Hardness A and D Testing.

DIN 53 455

Testing Of Plastics; Tensile Test .

DIN 30 670

Polyethylene Coatings For Steel Pipes and Fittings, Requirements and Testing

American Society for Testing and Materials

.. (

ASTM )

ASTM D 543

Standard Practices for Evaluating The Resistance of Plastics to Chemical Reagents .

ASTM D 638

Standard Test Method For Tensile Test Of Plastics .

ASTM D 1238 ASTM D 2240

Standard Test Method For Flow Rates Of Thermoplastics Extrusion Plastometer

ASTM D 3359

Standard Test Method For Measuring Adhesion By Tape Test

ASTM D 4752 ASTM D 5402 ASTM G 42

Standard Test Method For Rubber Property- Durometer Hardness . Standard Test Method For Measuring MEK Resistance of Ethyl Silicate ( Inorganic) Zinc-Rich Primers by Solvent Rub . Standard Test Method For Assessing the Resistance of Organic Coatings using Solvent Rubs . Standard Test Method For Cathodic Disbonding Of Pipe Lines Coatings Subjected to Elevated Temperatures. .

National American Of Corrosion Engineering NACE RP 0394

.. ( NACE ) Standard Recommended Practice - Application, Performance, and Quality Control Of Plant-Applied, Fusion Bonded Epoxy External Pipe Coating .



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Gas Business Engineering .. ( GBE ) GBE/CW6 : part 1

Technical Specification For The External Protection Of Steel Line Pipe and Fittings Using Fusion Bonded Powder and Associated Coating Systems ( Part 1 : Requirements For Coat materials and Methods Of Test .

International Standard ISO 8501-1

.. (

ISO )

Pictorial Surface Preparation Standards For Painting Steel Surfaces .

( SIS 05 59 00 )

ISO 8502-1

Field Test for Soluble Iron Corrosion Products .

ISO 8502-3

Field Test for The Determination Of Dust Contamination

ISO 8502-4

Guidance on the Estimation of the Probability of Condensation Prior to Paint Application . Extraction of Soluble Contaminants for Analysis – The Bresle method

ISO 8502-6 ISO 1133 ISO 21809-1

Plastics - Determination of the Melt Mass-Flow Rate ( MFR ) and Melt VolumeFlow Rate ( MVR ) of Thermoplastics . Petroleum and natural gas industries — External coatings for buried or submerged pipelines used in pipeline transportation systems — Part 1:Polyolefin coatings (3-layer PE and 3-layer PP)



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4- RECEIVING, HANDLING, STORAGE AND LOUD OUT 4.1 RECEIVING 4.1.1 PIPE RECEIVING 4.1.1.1 Received pipes shall be checked ( 100% ) for the following : - Dents. - Damaged bevels. - Pipe interior and exterior “ Rust grade “ in accordance with ISO 8501 Part 1. - Manufacturers mill identification marks ( heat and pipe number ) . - Pipe diameter and wall thickness. - Quantity of pipes. 4.1.1.2 Only Pipes of Rust grade in conditions A&B in accordance with ISO 8501 Part 1. shall be accepted for coating. 4.1.1.3 Pipes of Rust grade in conditions C or D in accordance with ISO 8501 Part shall be rejected. 41.1.4 Contaminated pipes that would result in additional pre-cleaning process shall be rejected. 4.1.1.5 Rejected pipes or that dose not comply with the shipping documents shall be segregated from acceptable pipes and reviewed by client Rep. 4.1.1.6 Pipes that comply with the shipping documents but is damaged or contaminated shall be segregated until reviewed by client Rep. and the proposed action is agreed and approved. 4.1.1.7 Only approved pipe shall be coated in accordance to the approved procedure . 4.1.2 COATING RAW MATERIALS 4.1.2.1 The received materials shall be inspected for the following : - correct material type ( as per Petrojet order ) - correct components ( as per material data sheet ) - correct labeling on each package, unit or container ( as per material data sheet ). 4.1.2.2 All accepted materials shall be entered onto the material inventory and stored in the proper warehouse . 4.1.2.3 All unacceptable materials shall be segregated from acceptable materials .

4.2 HANDLING 4.2.1 COATING RAW MATERIALS/ANODES 4.2.1.1 All material shall be carefully handled in the way not damage the material or the packing. 4.2.1.2 Old received material shall be used before new received material ( FIFO). 4.2.2 PIPE HANDLING 4.2.2.1 BARE PIPE 4.2.2.1.1 Bare pipe shall be carefully removed from the truck using a crane and stacked on concrete or sand beams. 4.2.2.1.2 Fork lift shall carefully remove the pipe from the storage yard and with equal care place the pipe on the blast machine incoming rack.



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4.2.2.2 COATED PIPE 4.2.2.2.1 A properly prepared fork lift shall be used to transport the coated pipes to the storage area provided they have padded forks.

4.3 STORAGE/STACKING 4.3.1 Storage of Coating Materials 4.3.2.1.1 Periodically, the visual inspection shall be performed in order to verify that the coating materials have been stored in conditions as recommended by the material Manufacturer. 4.3.2 Pipe Storage/Stacking ( Bare and Coated ) 4.3.2.1 Pipe shall be stacked in such a manner that prevents damage to the pipe or coating. 4.3.2..2 The pipes (bare and coated) shall be stacked on a leveled ground, free from foreign materials, stones. Pipes shall be suitably spaced from the soil (minimum 150mm) to prevent any contact with the ground and to prevent surface water from entering during the entire storage period. 3.3.2.3 The pipes shall be stacked off ground on well prepared beams. 4.3.2.4 Stacks of pipes of different type shall be clearly separated. 4.3.2.5 For safety reasons for pipes of any diameter the maximum height for stacking pipes shall not exceeds the maximum number of layers shown in the following table and for any reason the allowed height of any stack shall be not exceeds 3.5 meters. Pipe Dia.

Permissible No. of Layers

16”

4 Layers for bare pipes

16"

2 Layers for coated pipes

4.4 LOAD-OUT 4.4.1 Only accepted pipes shall be loaded onto trucks from the storage area. 4.4.2 Pipes shall not be stacked onto the truck any higher than 2.5 meters or any higher than the law permits or is safe. 4.4.3 The loaded pipes shall not exceed the maximum allowable weight for the truck or by law or is safe. 4.4.4 The loaded pipes shall be tied down using Nylon straps or other means to avoid damage to the coating during transportation .



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5- COATING MATERIALS PROPERTIES/VENDORS. 5.1 GENERAL PROPERTIES OF THE COATING MATERIALS The coating materials used in this project shall be have the following general properties: 5.1.1 PROPERTIES OF EPOXY PRIMER

1- Powder epoxy primer, applied as anti-corrosion layer for coating of carbon steel pipe line by polyethylene 3 layer system . 2- Possess good similarity and compatibility with the polymeric adhesive, and react with it, so that the reciprocal anchorage is increased. 3- Show high capability to minimize cathodic disbondment when steel pipe is subjected to negative polarization as per ASTM G 8 standard [ the maximum radius of disbonding ≤ 5 mm. ] .

PROPERTY

UNIT 3

Specific Gravity

g / cm

Sieve Analysis

% ( retained ) 250 μm mesh % ( retained ) 150 μm mesh

TEST METHOD

VALUE

CSA Z 245.20 CSA Z 245.20

1.3 - 1.6 0.5 % max.

CSA Z 245.20

3.0 % max.

Sec.

CSA Z 245.20

10 – 50

Thermal Characteristics ( Tg2 )

°C

CSA Z 245.20

≥ 100

Glass transition temperature

°C

CSA Z 245.20

≥ 100

Moisture Content

%

CSA Z 245.20

max. 0.3

Radius( mm )

EN 10288

≤5

Gel Time ( at 200 c° )

Cathodic Disbonding - @ 65 c° , 2 days

5.1.2

PROPERTIES OF ADHESIVE

1- Ethylene adhesive suitable for 3 layer coating system . 2- Be suitably stabilized against aging at its maximum application temperature and free from volatile or other unstable substances at maximum application temperature ( application temperature indicated by the manufacturer ) . 3- Show high affinity and strong bond with polyethylene layer (top coat layer), high affinity and strong bond with primer layer, and assure a strong bond with primer (equal to or higher than that with PE).



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4- Possess the following properties ...

PROPERTY

UNIT g / cm3

Density

g / 10 min.

Melt Flow Index

190 °c / 2.16 Kg

TEST METHOD ASTM D 1505

VALUE 0.910 - 0.940

ASTM D 1238

0.5 – 6

Vicat softening point

°c

ASTM D 1525

>100

Melting point

°c

ASTM D 2117

≥ 110

Tensile Strength at Break

Mpa

ASTM D 638

≥ 17

%

ASTM D 638

≥ 400

Elongation at Break

5.1.3

PROPERTIES OF POLYETHYLENE

1- Fully stabilized PE, in granular state, contains additives for stability and resistance to weather conditions and its combined action of oxygen, sunlight and temperature. 2- Designed for coating of steel pipe, three layer system, where it is side-extruded directly in multiple wraps to build-up the requested thickness. 3- Possess the following properties...

PROPERTY Density, compound Melt Flow Index Carbon Black

UNIT

TEST METHOD

g / cm3

ASTM D 1505

0.948 – 0.955

ASTM D 1238

0.15 – 1.0

ASTM D 1603

2–3

ASTM D 2240

≥ 50

g / 10 min. 190 °c / 2.16 Kg

%

Durometer Hardness

shore D

VALUE

Brittleness Point

°C

ASTM D 746

≤ - 70

ESCR

hr

ASTM D 1693

> 1000

Vicat Softening Point

°c

ASTM D 1525

>115

ASTM D 2117

>120

Kg/cm2

ASTM D 638

≥ 150

%

ASTM D 638

> 400

°c

Melting point Tensile Strength at Break Elongation at Break



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6- PRODUCTION TESTING AND INSPECTION . The inspection testing during coating application ( needed to ensure that the coating is being applied in accordance with the approved specification ) shall be carried out as following:

6.1 INSPECTION S AND TESTS 6.1.1 PIPE SURFACE PREPARATION

The surface preparation operation and prevailing parameters shall be measured in accordance with ISO 8501 and at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix A. - Ambient conditions ( prevailing temperature, relative humidity, dew point ). - Pipe Surface Temperature ( before blast). - Surface cleanliness. - Surface profile. - Surface salt contamination . - Dust control . 6.1.2 PRE-HEATING TEMPERATURE

The preheating temperature of the coating materials shall be measured at the frequencies indicated in para. 6.4 to insure that the application is comply with the manufacturer recommendation. - Pipe temperature . - PE temperature . - Adhesive temperature . 6.1.3 COATING SYSTEM THICKNESS

The coating thickness of the system shall be measured at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix B. - Thickness of primer layer - Thickness of adhesive layer - Total coating thickness 6.1.4 COATING CONTINUITY ( HOLIDAY DETECTION )

The coated pipes shall be holiday detected 100 % at voltage set at 10 Kv per millimeter of nominal thickness of coating and not exceeding 25 Kv. The holiday detection shall be performed in accordance with the method defined in Appendix C. 6.1.5 IMPACT RESISTANCE TEST

The impact resistance of the coating system shall be measured at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix D . 6.1.6 ADHESION ( PEEL OFF ) TEST

The peel-off resistance of the coating system shall be measured at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix E . 6.1.7 MELT FLOW RATE

The melt flow rate of the PE and adhesive for the new and extruded material shall be measured at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix P.



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6.1.8 INDENTATION RESISTANCE TEST

The indentation resistance of the PE shall be measured at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix G. 6.1.9 TENSILE STRENGTH and ULTIMATE ELONGATION

The tensile strength at yield and at break and the ultimate elongation of the PE shall be measured at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix H. 6.1.10 DUROMETER HARDNESS - SHORE D

The hardness shore D of the PE shall be measured at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix O. 6.1.11 DEGREE OF CURE OF PWODER EPOXY

The degree of cure of the F.B.E layer shall be measured at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix A. 6.1.12

FLEXIBILITY

The flexibility of the coating shall be performed at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix M. 6.1.13

AIR ENTRAPMENT ASSESSMENT

The air entrapment in the coating shall be measured at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix N . 6.1.14 CATHODIC DISBONDING TEST

The cathodic disbonding test for the coating shall be performed at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix K . 6.1.15 HOT WATER IMMERSION TEST

The Hot water immersion test for the coating shall be performed at the frequencies indicated in para. 6.4 and in accordance with the method defined in Appendix L .

6.2 Sampling Petrojet QC representative or the Client representative shall select, on random bases, the pipes on which the specified tests shall be carried out. To minimize repair of coating, all destructive testing shall be carried out on the ends of the pipes ( cut back area ).



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6.3 Re-tests In the event that a production coated pipes fails to meet the acceptance criteria of a specified test or if the no. of holidays detected is excessive the pipe length shall be rejected unless approval is given by the company to accept said pipe. The preceding and following pipe lengths in the same production run shall then be similarly tested and if both are accepted, than the remainder of the pipe length shall provide a test schedule for company approval this schedule shall determine which pipes may be defective since the last passing test pipe.

6.4 Nature and Frequency of Testing At Regular Production Properties Surface condition ( before blast cleaning ) Ambient temperature Relative humidity Dew point Pipe surface temperature ( before blast cleaning ) Surface cleanliness ( after blast cleaning ) Roughness of the blast surface Surface salt contamination Cleanliness of blast surface for dust Abrasive Check For Contamination Cut back Visual Inspection Thickness of FBE primer layer Thickness of adhesive layer Total coating thickness of the system Pipe surface temperature ( before FBE application ) PE / Adhesive temperature Continuity-holiday- control Peel-off test Impact test Indentation Resistance Tensile strength at Yield and Break Ultimate elongation Hardness, Shore D Melt Flow rate Entrapment Assessment Degree of Cure of FBE ( DSC ) Degree of Cure of FBE ( MEK ) Flexibility, 3º PD @ -10 °c Cathodic disbonding test Hot water immersion test

Subclause 7.1 7.1 7.1 7.1 7.1 7.1 7.1 7.1 7.1 7.2 7.3 7.4.1 7.4.2 7.4.3 7.5.1 7.5.2 7.6 7.7 7.8 7.9 7.10 7.10 7.11 7.12 7.13 7.14 7.14 7.15 7.16 7.17

Reference Test method Appendix A Appendix A Appendix A Appendix A Appendix A Appendix A Appendix B Appendix B Appendix B M.D.S M.D.S Appendix C Appendix E Appendix D Appendix G Appendix H Appendix H Appendix O Appendix P Appendix N Appendix A Appendix A Appendix M Appendix K Appendix L

Frequency At Regular Production Every pipe test / hr test / hr test / hr test / hr Every pipe First 5/1 tests Every 30pipe First 5/1 tests Every 30pipe First 5/1 tests Every 30pipe test/shift Every pipe Every pipe test / day test / day 1 pipe out 20 pipes test/hr test/hr Every pipe First pipe / 1 test per shift. Test/ PE batch No. Test/ PE batch No. Test/ PE batch No. Test/ PE batch No. Test/ PE batch No. test / day test / shift. test / day test / shift. 1st. pipe 1st. pipe 1st. pipe



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7- REQUIREMENTS OF THE APPLIED COATING . 7.1 PIPE SURFACE PREPARATION 7.1.1 Before blast cleaning, the pipe exterior surface shall inspect from a corrosion standpoint in accordance with ISO 8501 Part 1. Pipes in conditions A&B only shall be accepted and any pipe in conditions C or D shall be rejected and brought to the attention of client representative. 7.1.2 Before blast cleaning the pipe surface shall be free of all surface contaminants…. 7.1.2.1 Oil, grease and other contaminants shall be removed wiping the contaminated area by suitable solvent, detergent or potable water. 7.1.2.2 Temporary protective coating layer which can't be removed easily be normal blasting and will effect the quality of coating, An additional pre-cleaning will be necessary to remove the protective layer. 7.1.3 The pipe surface temperature should be at least 3 °c above the dew point temperature prior to coating. All pipes should be visually checked for moisture, if the pipe looks damp, the pipe must be preheated to eliminate the moisture. 7.1.4 The pipe surface shall be cleaned by shot/grit blast cleaning technique to achieve the requirements of SA 2 ½ Very thorough blast cleaning in accordance with ISO 8501-1 Part 1. and shall be checked in accordance with the method defined in Appendix A. 7.1.5 The pipe Surface profile ( peak-to-valley ) shall be in the range of 40 μm -100 μm and shall be checked using testex tape (or equivalent ) and shall be measured in accordance with the method defined in Appendix A. 7.1.6 The salt contamination for the blasted pipe surface shall be verified to insure that the salt level ≤ 10 mg/m2 , the test shall be measured in accordance with the method defined in Appendix A. 7.1.7 The dust contamination level for the blasted pipe surface shall be verified to insure the dust level is ≤ rating 2 in accordance with ISO 8502-3 standard and the test shall be checked in accordance with the method defined in Appendix A. 7.1.8 The blasted pipes shall be inspected for all surface imperfections ( slivers, scabs, dents, ..etc ) which shall be marked and shall be checked in accordance with the method defined in Appendix A. 7.1.9 The abrasive material in the blasting machine shall be checked for absence of foreign particles and oil contamination and shall be checked in accordance with the method defined in Appendix A. 7.1.10 Prior to induction heater, the pipe surface shall be cleaned from all dust and abrasives which still remain on the exterior surface of the pipe using mechanical nylon brush supplemented with vacuum system. 7.1.11 Any blasted pipes shall be coated within the following maximum times and any pipe delayed beyond this period shall be re-blasted and re-inspected. % RH 85 80 70

TIME 0.50 hr 1.00 hr 1.50 hrs.

60

1.75 hrs.

50

2.00 hrs.



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7.2 CUT BACK The coating, at pipe ends shall be cut back over length of 120mm +20/- 0mm and beveled at angle of 30 ° to 45 °, at cut backs the PE and Adhesive layers shall be removed.

7.3 VISUAL INSPECTION The coating shall be inspected100 % to insure that … 1- The coating free from blisters , wrinkles, voids and disbondment. 2- Pipe temperature after cooling shall be ≤ 65 °c.

7.4 COATING THICKNESS 7.4.1 Epoxy Primer Thickness : The thickness shall be 200 -400 μm. 7.4.2 Adhesive Thickness : The thickness shall be 250-350 μm. 7.4.3 Total Coating Thickness : Pipe Dia. 16”

at weld Min 2.5 mm

at body Min 3 mm

The average total thickness is the summation of the thickness of individual layers, The coating thickness shall be measured in accordance with the method defined in Appendix C.

7.5 PRE-HEATING TEMPERATURE The pre-heating temperature of the pipe and the coating materials as following.. 7.5.1 Pipe temperature The pipe surface temperature should be between 175 °C - 220 °C using the TEMPIL STICK temperature indicating crayons. 7.5.2 Polyethylene & Adhesive temperature The temperature of both extruded PE should be less then 260 °C and adhesive material should be less then 240°C, or as per recommended material data sheet and shall be measured using optical pyrometer.

7.6 COATING CONTINUITY ( holiday detection ) The coating system shall be holiday detected 100 % in accordance with the method defined in Appendix D, the test voltage shall be set at 10 Kv. per millimeter of nominal thickness of coating and not exceeding 25 Kv. The maximum number of allowed holidays is 5 localized or scattered holidays per coated pipe.



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7.7 ADHESION ( PEEL-OFF ) TEST The adhesion of the coating shall be determined by measuring the peel-off resistance in accordance with DIN 30 670 standard and the method defined in Appendix F. The minimum force required to lift the coating shall be as indicated in the table below … @ 23 °C ± 3 °C

@ 80 °C ± 5 °C

150 N / 10mm

40 N / 10mm

7.8 IMPACT RESISTANCE TEST The impact resistance of the PE coating system shall be tested at Temperature ( 23 ± 3 °C ) in accordance with DIN 30 670 ,NF A 49-710 standards and the method defined in Appendix E. The coating shall have a minimum impact resistance ≥ E= ( 5 x ϕ ) J per mm of coating thickness.

7.9 INDENTATION RESISTANCE TEST The indentation resistance of the PE material shall be tested in accordance with DIN 30 670 and NF A 49-710 standards and the method defined in Appendix H. The maximum indentation resistance shall be as following … @ 23 °C ± 3 °C

@ 80 °C ± 3 °C

0.2 mm

0.3 mm

7.10 TENSILE STRENGTH AND ULTIMATE ELONGATION TEST The tensile strength and ultimate elongation ( elongation at break ) of the PE material in accordance with DIN 30 670,NF A 49-710, ASTM D 638 standards and the method defined in Appendix I. The PE material should show the following values : Tensile Strength ( Yield )

Tensile Strength ( Break)

Ultimat Elongation

≥ 126 Kg/cm2

≥ 170 Kg/cm2

≥ 400 %



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7.11 DUROMETER HARDNESS – SHORE D The hardness shore D of the PE material shall tested in accordance with ASTM D 2240 and DIN 53 505 standards and the method defined in Appendix P. The PE material should show Hardness ≥ 50 shore D.

7.12 MELT FLOW RATE The melt flow rate ( MFR ) of the PE and adhesive materials shall be tested in accordance with ASTM D 1238 and the method defined in Appendix Q. 6.12.1 New MFR = shall be within ± 15 % of the material certificate of analysis or material data sheet. 6.12.2 Extruded MFR = shall be within ± 20 % of the New MFR .

7.13 AIR ENTRAPMENT ASSESSMENT The degree of presence of air entrapment between coating layers in accordance with the method defined in Appendix O. A strip of coating from the adhesion test shall be used to determine the level of air entrapment on the body of the pipe or in the saw weld, The coating should show Not more than 10% of the observed area contains air entrapment, bubble size in the PE layer shall be limited to less than 1/2 the thickness of the PE layer in height or circumference and not linked together.

7.14 DEGREE OF CURE OF FUSION BONDED EPOXY PRIMER The degree of cure of the FBE coating shall be tested in accordance with the method defined in Appendix B, the acceptance criteria shall be: 7.14.1 MEK Rub method The degree of cure of the F.B.E when tested using MEK ( Methyl-Ethyl Ketone ) double rubs according with ASTM D 5402 standard, The curing of the coating shall be ≤ rating 2 . 7.14.2 Glass Transition Temperature method ( ∆Tg ) The degree of cure of the F.B.E when tested using Differential Scanning Calorimetry ( DSC ) shall be between -2 oC and +3 oC.

7.15 FLEXIBILITY TEST The degree of flexibility of the coating shall be tested in accordance with CAN/CSA Z 245.20-M92 standard and the method defined in Appendix N. The test ring shall be bent over a mandrel at -10 °c, The coating shall satisfy the requirements when no visible cracks is shown in the coating system when bending performed to 3º PD.



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7.16 CATHODIC DISBONDING RESISTANCE TEST The degree of coating to resistance cathodic disbondment shall be tested in accordance with ASTM G 8, NF A 49-710 standards and the method defined in Appendix L. The coating should show good resistance to cathodic disbondment when subjected to a potential of – 1.5 V, in a 3% NaCl electrolyte solution at the following test conditions …

Test Duration Max. Disbonding Radius

@ 60 °C ± 2 °C 2 days ≤ 7 mm

7.17 HOT WATER IMMERSION RESISTANCE TEST The degree of coating to resistance disbondment due to hot water immersion shall be tested in accordance with as per GBE/CW6:part 1 standards and the method defined in Appendix M. The coating shall show good resistance to disbondment when immersed potable water at the following test conditions … @ 80 °C ± 2 °C 7 days Test Duration Max. Disbonding Radius

≤ 2 mm



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SUMMARY OF THE REQUIREMENTS OF THE COATING Properties Surface cleanliness Surface profile Surface salt contamination Pipe Temperature After Blasting Cleanliness Of Blast Cleaned Surface For Dust Thickness of primer layer Thickness of adhesive layer Total coating thickness. Peel-off resistance Continuity-holiday- control Cut back Impact resistance Indentation resistance Ultimate elongation Tensile strength Hardness, Shore D Air entrapment Degree of Cure Flexibility Cathodic disbondment Hot water immersion

Requirements min SA 2 ½ 40 -100 μm max 10 mg/ m2 ≥ 3°c above dew point ≤ Rating 2 200 -400 μm. 250-350μm at weld at body min 2.5mm min 3mm @ 80 oC @ 23 oC 150 N/10mm 40 N/10mm max. 5 holidays / pipe @ 25 Kv 120mm +20/- 0mm ≥ 5 J per mm coating thickness @ 80 oC @ 23 oC ≤ 0.2 mm ≤ 0.3 mm ≥ 400 @ Yield @ break ≥ 126 Kg/cm2 ≥ 170 Kg/cm2 ≥ 50 ≤ 20% MEK DSC ≤ rating 2 between -2 oC and +3 oC no visible cracks @ 60 °C/2 days ≤ 7 mm @ 80 °C/7 days ≤ 2 mm


Subclause 7.1 7.1 7.1 7.1 7.1 7.4 7.4 @ 50 oC 7.7 7.6 7.3 7.8 7.9 7.10 7.10 7.11 7.13 7.14 7.15 7.16 7.17


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7. SURFACE PREPARATION FOR CONCRETE COATING ( Anti-Slip Finish on Coating Surface )

In Case of Off-shore pipe lines: Following the extrusion of the polyethylene layer and before cooling, the surface of polyethylene shall be finished in a way that will improve the friction coefficient and enhance the bonding of concrete coating to prevent slipping of concrete weight coatings. The external surface of the coating system shall be roughened by applying polyethylene powder. The maximum length allowed for missing of rough finish per coated pipe ≤ 1 meter. The shear strength required between the concrete and the anti-corrosion protection coating is to be higher than 3 Mpa (at ambient temperature).



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8- REPAIR OF COATING In theory, no coating defect or damage should ever be found during the coating process, but at practical level it can not however be excluded, so .. some defects may occasionally show up in pipe coating . Taking the above into consideration , the following repair methods are applied for in plant damaged coated pipe . 8.1 For local defects ( scratches, cuts, dents, … etc. ) of any dimension and any quantity where the defect not reach the metal surface ( the remaining coating thickness is not less than 80% of the specified thickness ), no repair is required . 8.2 For same defect mentioned above, where the remaining coating thickness is less than 80% of the specified thickness, OR where the defect reach the metal surface, No single defect shall exceeded a pipe area of 625mm2 , all defects exceeding this value shall be cause for rejection of the coating. These defects could be repaired using Spot Patch Method : 8.2.1 Remove rust or other contaminants, if any, with a hand brush . 8.2.2 Preheat the steel surface of the damaged part . 8.2.3 Apply a piece of sealant material smaller than the size of the damage on the steel surface . 8.2.4 Heat the sealant then extending the hot sealant with trowel and Apply a piece of sealant material more and more to mold the damaged part with a sealant more or less thicker than the polyethylene coating . 8.2.5 Cut a piece of the patch sheet larger by 5 cm than the damaged part, cut the corner of the patch piece . 8.2.6 Apply the patch piece centering in the damaged part and heat from the center to each edge. 8.2.7 Tapping from the center to the edge to drive away the trapped air and heat again and tapping again . 8.2.8 Immediately after heating the repair patch, press all the edges by finger to get an adequate adhesive strength . 8.3 The maximum level for repair of coating ( exclude repair due to QC tests ) is 5 repairs . 8.4 External coating damages and the relevant repair are not allowed at the cutback area where the coating has been beveled (at the coating bevel angle). 8.5 The quality of the repair shall be examined and tested for appearance and holidays. Each repair shall be inspected for … - Visual inspection 100% of repaired coating, the repaired coating shall be smooth, and free of folds or bubbles . - Holiday detection shall be performed on each repair using a voltage of 25 Kv.



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9- STRIPPING OF COATING In the event of pipes failing to meet the requirements of sections 6 and 7, the coating of these pipes shall be stripped and the pipes shall be recoated and re-inspected. The coating removal shall be performed using any of the following methods:

9.1 ON LINE STRIPPING 9.1.1 The pipe stripping temperature will be verified by the following method: An uncoated test pipe (of the same diameter/wall thickness as the pipe to be stripped) shall be run through the induction coils in the pipe coating plant, and heated to 275°C. 9.1.2 The coating conveyor speed and induction system settings shall be noted and recorded. These settings shall be used for all subsequent stripping operations for a given pipe diameter and wall thickness. 9.1.3 The pipe to be stripped is moved from the storage yard using a forklift and carefully placed on the incoming racks. The pipe tally information shall be recorded in order to identify pipes which pass through the stripping process. 9.1.4 The pipe is moved through the plant to the coating conveyor where it is heated by the induction system to a temperature of 275°C. The induction system and line-speed settings shall be set to the values established on the bare pipe test, and carefully monitored. The pipe temperature shall not exceed 275°C. 9.1.5 A spiral cut will be made by hand through the PE coating using a cutting knife. The knife cuts will be at a pitch of approx. 10 -20 cm. Care will be taken to ensure that there is no damage to the steel. 9.1.6 The PE topcoat shall then be manually peeled off the pipe, and removed in strips. 9.1.7 The pipe will be cooled in the quench. 9.1.8 The pipe is then returned to the coating conveyer and the steps described in points 2 through 3 are repeated to heat the pipe to 275°C. The pipe temperature shall not exceed 275°C. 9.1.9 The residual FBE and copolymer coating materials shall then be removed by means of a scraper. This shall be a mild steel plate with a 45° blade held axially on the pipe surface. Care will be taken to ensure that there is no damage to the steel. 9.1.10 The pipe will be cooled in the quench. 9.1.11 The pipe shall then be moved to the shot/grit blast machine conveyor to blast the pipe and remove any residual coating materials. 9.1.12 The pipe shall be visually checked after blasting to ensure that all coating materials are removed, and that there is no damage to the steel from the stripping process. Any pipes with major steel damage/defects caused by the stripping process shall be quarantined. These pipes shall be subject to further inspection.



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9.2 OFF- LINE STRIPPING ( manual stripping ) 9.2.1 The pipe to be stripped is moved from the storage yard using a forklift and carefully placed on the stripping rack. The pipe tally information shall be recorded in order to identify pipes which pass through the stripping process. 9.2.2 The interior surface of the pipe to be stripped shall be heated using Propane torch, pipe is heated to a temperature of 250°C, and carefully monitored to sure that the pipe temperature shall not exceed 260°C. 9.2.3 A spiral cut will be made by hand through the PE coating using a cutting knife. The knife cuts will be at a pitch of approx. 10 -20 cm. Care will be taken to ensure that there is no damage to the steel. 9.2.4 The PE topcoat shall then be manually peeled off the pipe and removed in strips. 9.2.5 The residual FBE and copolymer coating materials shall then be removed by means of manual scraper. 9.2.6 After the pipe is cooled down, the pipe shall be moved to the shot/grit blast machine conveyor to blast the pipe and remove any residual coating materials. 9.2.7 The pipe shall be visually checked after blasting to ensure that all coating materials are removed, and that there is no damage to the steel from the stripping process. Any pipes with major steel damage/defects caused by the stripping process shall be quarantined. These pipes shall be subject to further inspection.



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10- PIPE MARKING 10.1 All mill identification data ( Heat Number, Pipe Number and Pipe Length ), if available, shall recorded before surface preparation . 10.2 After coating process pipe number, pipe length and PETROJET coating serial number shall be recorded on the external surface of the pipe . 10.3 All mill identification data ( heat number, pipe number, pipe length) and PETROJET coating serial number ) shall be recorded on the daily pipe tally sheet . 10.4 In case of any of mill ID data is not clear, The PETROJET coating serial number shall be consider as official ID for the pipes . 10.5 For pipes have the same DN but differ in wall thickness, each wall thickness shall marked with special code color .



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11.


PROCEDURE QUALIFICATION TRAIL ( PQT )

Prior to the commencement of production a Qualification trial shall be performed to determine the working parameters and to verify that the final coating meet the requirements of the specification. PETROJET has the right to commence the coating production before the final evaluation of the PQT results. Test Reference

Acceptance Criteria

Surface condition ( before blast cleaning )

Appendix A

Surface cleanliness of the blast surface Roughness of the blast surface Surface salt contamination ( after blast ) Cleanliness of blast surface for dust

Appendix Appendix Appendix Appendix

No contaminations No surface defects min SA 2 ½ 40 - 100 μm max 10 mg/ m2 ≤ Rating 2

Thickness of primer layer( FBE)

Appendix C

200 -400 μm.

Thickness of adhesive layer

Appendix C

250 - 350 μm.

Total coating thickness

Appendix C

Test

A A A A

conditions A&B

at weld

Visual Inspection for full coated pipe

Subclause 6.3

Continuity-holiday- control

Appendix D

Adhesion test for FBE

Appendix G

Adhesion test for complete system

Appendix F

Impact Resistance test

Appendix E

Hardness, Shore D

Appendix P

No. of Test Samples

at body

min min 3mm 2.5 mm Uniform appearance, no coating imperification ( flat, spots,dents,air bubbles,... etc. Verified with a holiday detector Pass at 25 kv. ≤ Rating 2 @ 20 °c ± 5°c ≥ 150N/cm @ 80 °c ± 5°c ≥ 40N/cm ≥ 5 j / mm coating Temperature range 23 °c -2°c /+10°c (no holiday at 25 kv)

10 pipes. 10 pipes. 10 pipes. 10 pipes. 10 pipes. Partially 1 pipe coated with FBE. - 12 measurements. Partially 1 pipe coated with adhesive. - 12 measurements. 10 fully coated pipes. - 12 on pipe body - 12 on weld seem.

10 fully coated pipes

10 fully coated pipes Partially 1 pipe coated with FBE. - 3 measurements. 5 fully coated pipes - .2 Tests/pipe/test condition 5 fully coated pipes. - 50 impacts/pipe

≥ 50


2 samples


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Test Degree of Cure of primer, DSC Degree of Cure of primer, MEK Tensile strength at Yield Tensile strength at Break Ultimate elongation

Test Reference Appendix B Appendix B Appendix I Appendix I Appendix I

Indentation Resistance

Appendix H

Air Entrapment

Appendix O

Flexibility

Appendix N

Hot water Immersion @ 80 °c, 7 days Cathodic disbonding @ 60 °c, 2 days

Appendix M Appendix L

Acceptance Criteria between -2 oC and +3 oC ≤ rating 2

No. of Test Samples 3 samples 3 samples 3 samples 3 samples 3 samples

2

≥ 126 Kg/cm ≥ 170 Kg/cm2 ≥ 400 Max.0.1 mm at 20°C±5°c Max.0.3 mm at 80°C±2°c

No air entrapment No cracking ,no disbondment ≤ 2 mm ≤ 7 mm

1 sample 3 samples 1 samples 1 sample 2 pipes (first and last pipes)



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12. DOCUMENTATION Prior to the start of Production Operations, the following documentation, written in the English Language, shall be submitted to the client for review. 1.

Coating and Testing Procedures;

2.

Pipe Handling Equipment Description and Procedures;

3.

Pipe Stacking Arrangements;

4.

Inspection Test Plan;

5.

Repair Procedure;

6.

Procedures for all PQT and Production Tests;

7.

Certification/Calibration Certificates for all Testing Equipment;

8.

Coating Material data sheet, test certificate and MSDS;

9.

Forms of daily Inspection, Test Records and production tally sheet.



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Appendix A – VERIFICATION OF PIPE SURFACE PREPARATION A-1 General This test method covers the procedure of verification and testes performed on pipe surface before and after surface preparation to check the quality of the blasted pipe.

A-2 Standard ISO 8501-1 Pictorial Surface Preparation Standards For Painting Steel Surfaces. ( SIS 05 59 00 )

ISO 8502-1 Field Test for Soluble Iron Corrosion Products. ISO 8502-3 Field Test for The Determination Of Dust Contamination ISO 8502-4 Guidance on the Estimation of the Probability of Condensation Prior to Paint Application. A-3 Apparatus - Digital Hygrometer or equivelant. - Digital Thermometer. - Dial Micrometer. - Salt Contamination Meter.

A-4 Measurement of the Ambient Conditions The ambient conditions shall be measured before the start of the pipe surface blast cleaning - Ambient temperature - Ambient Relative humidity - Ambient dew point The pipe surface temperature shall be measured before the blast cleaning on the incoming rack of the blast station, the steel surface temperature shall be minimum 3°c above the ambient dew point.

A-5 Check of The Blast Cleaning Abrasive Material The cleanliness of the blast abrasive material in the blast machine shall be checked as follows: 1- Small quantity of the abrasive material shall be poured in transparent plastic container filled with clean water, then the container is closed and shacked. Once the abrasive material deposited at the bottom of the container, The water within the container does not contain foreign particles. 2- Small quantity of the abrasive material shall be put on a clean white paper, another clean white paper is put on the top of the blast abrasive sample and rubes against them. After wards, both pieces of paper shall be examined that they do not contain any trace of oil, grease contaminants.



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A-6 Visual Inspection of Pipe Surface Before Blast Cleaning The visual inspection shall be carried out on the incoming rack of the blast station in order to verify that the pipe surface is not contaminated with salt, oil, grease or any other similar contaminant. Salt, oil, grease and other contaminants –if any- shall be removed from the pipe surface by washing the contaminated area with a solvent or washing method suitable to completely remove the contaminant. The pipe surface shall be checked to ensure that there is no moisture present on the pipe surface, if the pipe looks damp shall be pre-heated up to eliminate the moisture, the pipe surface should be at least 3 °c above the dew point Temperature prior to coating . The pipe surface shall be checked to ensure that there is no major steel defects.

A-7 Visual Inspection of The Blast Cleaned Surface A-7.1 The blast cleaned surface shall be visually inspected after the blast cleaning in order to determine the steel surface cleanliness degree. The degree of pipe surface cleanliness shall be determined by visual comparison with photographs in SIS 05 59 00 standard, allowance must be made for the fact that differences in color can occur due to the type of grit used, spherical grit, for example, results in a slightly darker surface than that in the photographs in SIS 05 59 00 standard ). The acceptance criteria: The minimum surface cleanliness grade shall be SA 2 ½ Very thorough blast cleaning in accordance with ISO 8501-1 (SIS 05 59 00) standard. A-7.2 The blasted pipes shall be inspected for all surface imperfections ( silvers, scabs, dents, ..etc ) which shall be marked . - All marked defects shall be brought to the attention of client representative to approve the action shall be taken by Petrojet or to provide the corrective action. - Only light cosmetic i.e. superficial grinding may be performed. This shall be limited to approx. 0.1-0.2 mm in depth, in general the grinding shall not reduce the pipe wall thickness below the client requirements or API 5L standard ( all grinding exceeding the light cosmetic definition shall be followed by a measurement and recording of the wall thickness at the ground area). - For repaired area more than 100 cm2 the pipe shall be re-blasted and re-inspected.

A-8 Surface Profile Measurement After Blast Cleaning The pipe Surface profile ( peak-to-valley ) of the blasted surface shall be measured after the blast cleaning using testex tape ( or equivalent ) in accordance with the following procedure : - Zero the dial micrometer ensuring the flat contact points are clean. - Remove paper backing from Testex tape and stick Testex tape to the surface to be measured. - Rub the Testex tape paste into the troughs using a blunt instrument, until the peaks can be seen butting up to the transparent plastic . - Remove the Testex tape from the surface and measure the overall thickness with the dial micrometer. - Deduct 50 μm for the plastic from the reading to obtain the amplitude ( surface profile ) . The acceptance criteria: 40 µm - 100 µm.



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A-9 Salt Contamination Level After Blast Cleaning The salt contamination level of the blast cleaned surface shall be measured after the blast cleaning using the Bresle method. The salt contamination level shall be checked at the cut back area on one pipe end. The acceptance criteria shall be ≤ 10 mg/ m2.

A-10 Dust Contamination Level After Blast Cleaning The dust contamination level of the blast cleaned surface shall be checked after the blast cleaning at the cut back area on one pipe end using the transparent adhesive tape in accordance with ISO 85023 standard. The acceptance criteria shall be ≤ Rating 2.



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CLIENT : AQP Appendix B –

PROJECT: NEW 16” SEALINE JOINING NAQP-2 PLATFORM TEST FOR ASSESSING THE DEGREE OF CURE OF THE FUSION BONDED EPOXY POWDER COATING

B-1 General This test method covers the procedure of determination of the degree of cure of the FBE epoxy film, the test shall be performed on a test specimen taken from the coated pipe or carried out on the coated pipe .

B-2 METHOD I ( Measurement of glass transitions temperature ( Tg ) ) B-2.1 Standard CAN/CSA Z 245.20-M92: External Fusion Bond Epoxy Coating For Steel Pipe. NACE RP 0394: Standard Recommended Practice - Application, Performance, and Quality Control of Plant-Applied, Fusion Bonded Epoxy External Pipe Coating.

B-2.2 Apparatus The apparatus used for this test is a differential scanning calorimeter with sufficient calorimetric sensitivity to determine the glass transition temperature of the epoxy products . Moreover the following accessories are necessary : - laboratory scale, accurate to the nearest 0.1 mg. - sharp tool. - Sample crucible.

B-2.3 Sampling Immediately after application , a sample of the epoxy film shall be taken from the coated pipe without adhesive by using a sharp tool to provide flakes of the coating care shall be taken to remove the sample from the whole thickness of the film while , at the same time , the inclusion of steel fragments shall be avoided. the sample may be taken at be broken into small pieces . Accurately weight sample between 10 mg and 15 mg, sample of weight not exceeding 25 mg , can be used if necessary for obtaining the required sensitivity.

B-2.4

procedure

The test procedure and the setting up of the instruments may differ according to the equipment used .however , the main characteristics of the test method shall be satisfied in order to obtain valid and comparable results. 1- An empty aluminum pan shall be used as a reference . 2- Weight the sample, put on lid and seal in sample press. 3- Place the sample crucible in the DSC cell together with an empty reference crucible.



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4- Start the temperature program. - The method consists of raising the temperature of a sample of epoxy coating (layer 1) at constant rate in a differential thermal calorimeter . - The samples shall be pre-treated to remove moisture and to provide a uniform thermal state. - The first plot records the thermal changes in the sample between room temperature and point located beyond complete polymerization. - Then the sample shall be cooled down to room temperature - .A second identical heating cycle identical to the first cycle shall then be carried out .

B-2.5 RESULTS : The glass transition temperature is defined as being the temperature ( or range of temperatures ) at which the polymer passes from a hard and often brittle state ( glass ) to a rubbery type . The transition of the polymer product is visible in the form of a jump in the baseline giving a marked variation in the steps of the specific heat at Tg . this step usually represents several degrees. By convention , temperature shall be taken as the point of inflection of the curve . The curing of the coating is acceptable when variation of the glass transition temperature ∆Tg ( Tg2 – Tg1 ) between -2 oC and +3 oC.

B-3 METHOD II ( Determination of FBE curing using MEK ) B-3.1 Standard ASTM D 4752: ASTM D 5402:

Standard Test Method For Measuring MEK Resistance of Ethyl Silicate ( Inorganic) Zinc-Rich Primers by Solvent Rub . Standard Test Method For Assessing the Resistance of Organic Coatings Using Solvent Rubs .

B-3.2 Apparatus - MEK Methyl-Ethyl Ketone. - Cotton Cloth

B-3.3

procedure

1-Place the forefinger in a cotton cloth in such a manner that the forefinger is covered by the cloth. 2-Saturate the cloth with MEK and rub the coating with the forefinger using back and forth motion, the length of the stroke is to be approximately 2 inches. 3-Sufficient pressure is to be exerted by the finger to ensure good contact to the film. 4-Rub 30 double rubs ( 30 rubs in each direction ), if the cloth become dry during the test, re-saturate with MEK .



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B-3.4 RESULTS : The degree of cure of the FBE coating tested using MEK double rubs shall be ≤ rating 2 after 30 double rubs . Rating

Criteria

0

No change of gloss, No softening ( no scratch by finger nail )

1

Slight loss of gloss, No softening ( no scratch by finger nail )

2

Slight loss of gloss, Slight softening ( can be scratched by finger nail )

3

Strong reduction in gloss, Complete softening ( easily scratched by finger nail )

4

Strong reduction in gloss, Complete softening ( coating partially removed )

5

Removal of coating



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CLIENT : AQP Appendix C –

PROJECT: NEW 16” SEALINE JOINING NAQP-2 PLATFORM INSPECTION OF THE COATING THICKNESS

C- 1 General This test method covers the procedure of determination of the dry film thickness ( DFT ) of applied coatings on magnetic steel substrates .

C- 2 Apparatus 1- Electronic thickness gauge. 2- Standardized calibration foils.

C- 3 Procedure 1- Before thickness measurements are carried out the instrument shall be adjusted and verified using a calibrated shim of the same thickness range as the coating as follows: - The coating thickness meter shall be calibrated on a clean steel plate and the display value must be 0.00 mm. - In case any other value is displayed, the instrument shall be calibrated manually until 0.00 mm value is obtained. - Choose a calibration plate of a thickness close to the thickness you expect to fined. - At least measurements shall be taken and each displayed value is within the range specified by the instrument's manufacturer. - If the displayed value is within the range is not specified the following acceptance criteria shall be apply: Displayed value = Nominal value of the calibration plate ± 5%. 2- A series of 12 individual measurements shall be carried out on each pipe to be inspected, the measurements shall be regularly distributed along 3 transverse sections of the tested pipe . 3- At each section the thickness shall be measured at 4 positions, equally spaced around the circumference of the pipe and at a distance of at least 200 mm from the end of the coating . 4- When a weld seam is visible, one measurement per section shall be executed on the top of the weld seam .

C- 4 Results A calculation of the arithmetic mean of the series of 12 individual measurements shall be made and shall be ≥ the specified thickness . NOTE : In case of dispute of results , recalibration of the instrument should be undertaken and five measurements at this pipe should be carried out again . The arithmetic mean of the result of the five measurements should be calculated.



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Appendix D –

HOLIDAY DETECTION TEST

D-1 General This test method covers the procedure of determination of the degree of porosity present in the coating using a scanning electrode energized by a high arc voltage. The Porosity shall be detected by a spark occurring between the steel of the pipe and the electrode of the detector .

D-2 Standard : DIN 30 670:

Polyethylene Coatings For Steel Pipes and Fittings, Requirements and Testing.

NF A 49-710:

Steel Tubes External Triple-Layer Polyethylene Based Coatings Application By Extrusion

D-3 Apparatus -

Holiday detector 0 – 30 Kv. Coating thickness gauge. Scanning electrode in the form of a metal brush, or conductive rubber conforming to the shape of the pipes. Conductors which are used to connect the pipe to the holiday detector.

D-4 Procedure : 1- Calibrate the holiday detector as following : • A series of 5 holes of around 1 mm diameter shall be made in the coating, down to the pipe metal, with a needle; these holes shall be spaced by about 10 cm . • The detector is switched on, the voltage shall be set at 10 Kv per millimeter of nominal thickness of coating and not exceeding 25 Kv and the electrode is set to pass the test holes . • A spark discharge must be correspondence with every hole . 2- Adjust the test voltage to 25 Kv . 3- The conductive scanning electrode ( brush or ring ) shall be maintained in good contact to the tested pipe. 4- The coating system shall be holiday detected 100 % .. 5- The maximum number of holidays is 5 per pipe .



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Appendix E – IMPACT RESISTANCE TEST E-1 General : This test method covers the procedure of determination of the strength of the coating by the impact of a punch of defined shape falling directly onto the coating from a fixed height at a fixed temperature.

E-2 Standard : DIN 30 670:


NF A 49-710:


E-3 Apparatus : - Heavy duty impact tester 25 mm spherical end. - Holiday detector 0 – 30 Kv. - Coating thickness gauge.

E-4 Procedure : 1- The impact resistance of the coating shall be tested at temperature 25 ± 5 °C. 2- A minimum of 30 points shall be selected on the surface of the test pipe/ring, the distance between each two impact points shall be at least 30 mm . 3- Drop the impact weight with hemispherical steel head with diameter of 25 mm from approximately 1 meter height. 4- the weight required to produce the specified energy to the coating is calculated using the following formula : H = J / 9.81 * W Where H = impact height, m. W = impact mass, Kg. J = Impact energy, joules.

E-5 Results : 1-This described body shall produce an impact energy, E, equal to ( 5 x ϕ ) J per mm of coating thickness 2- The impacted coating shall not crack or disbond at the point of impact and shall inspected for failure using holiday detector set at 25 Kv ( see Appendix C ) .



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Appendix F - PEEL -OFF RESISTANCE TEST F-1 General This test method covers the procedure of determination of the adhesion of applied 3LPE coatings on steel substrates using peel off machine method.

F-2 Standard : DIN 30 670:


NF A 49-710:


F-3 Apparatus : -

Utility knife ( sharp cutter ) Weights

F-4 Procedure : 1- The test shall be performed at temperatures of 23 °C ±3 °C and 80 °C ± 3 °C. 2- For test at elevated temperature >23 °C, the back side of the steel shall be heated to the test temperature which shall be measured at the root the peeled strip by means of optical pyrometer . 3- A strip of coating of minimum length of 160 mm shall be cut in circumferential direction and 50 mm wide perpendicular to the axis of the pipe shall be isolated from the coated pipe. 4. Manually peel off the coating strip at an angle of 45° to the pipe surface . 5. The test weight ( see sub-clause 5.7 ) shall be suspended to the coating strip, the time ( in minutes ) required to peel off the coating with a pulling rate of 10mm/min. shall be ≥ 0.4D +20%/-10% ( where D = pipe diameter mm ).



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6- Any pipe that exhibits a peel off value below the required value, the pipe shall receive 2 additional peel tests to verify the accuracy of the first test . 6.1 If the 2 additional peel tests meet the required value, the pipe is accepted . 6.2 If the 1 out of the 2 additional peel tests is below the required value, the pipe is rejected then 5 previously coated pipes and 5 new coated pipes shall be tested, if below the required value is detected, the production line shall stopped until the defect is determined . 7- The adhesion test shall be carried out at the cut back area at both ends per test.

F-5 Results : The adhesion of the coating shall be determined by measuring the peel-off resistance and shall be calculated as following: ( 9.81 x M x 10 ) / W ( N/10mm ) where: M is the mass of the suspended weight in Kg. W is the width of the coating strip in mm The minimum force required to lift the coating shall be as indicated in the table below … Force @ 23 °C ± 3 °C 150 N / 10mm

Force @ 80 °C ± 3 °C 40 N / 10mm



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Appendix G- DETERMINATION OF ADHESION OF COATINGS G.1 General : This test method covers a procedure for determining the adhesion of applied paints or FBE coatings on steel substrates.

G.2 Standard : ASTM D 3359 : Standard Test Method For Measuring adhesion by Tape Test .

G.3 Apparatus : - Utility knife ( sharp cutter ) - Adhesive tape.

G.4 METHOD I ( X-cut test method ) G.4.1 Procedure : 1- Two 20 mm ( approximately ) long incision shall be made though the FBE to the substrate. 2- Form an ( X-cuts) with an angle of approximately 30° at the intersection point . 3- The point of the knife shall be inserted horizontally ( i.e. the flat of the blade ) under the coating at the point to intersection of the cuts that the blade point is on the metal surface. 4- Using a levering action to attempt to pries the coating off

G.4.2 Results : The adhesion of the coating shall satisfy the requirements of rating 1 or 2 When starting at the 30° Vee intersection, the blade shall be used to attempt to peel the coating from the steel . Rating

Criteria

1

No removal of coating other than that caused by insertion of the flat point of the knife blade at the intersection point ( nominally less than 1 mm ).

2

No removal of coating more than 2 mm .

3


4


5

Removal of coating more than 5 mm .



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Appendix H – INDENTATION RESISTANCE TEST H-1 General This test procedure covers the determination of the indentation ( penetration ) resistance of Polyethylene material.

H-2 Test Standard DIN 30 670:


NF A 49-710:


H-3 Apparatus : The apparatus shall consist of : 1- Chamber or a bath thermostatically to ( up to 75 °C ) 2- Penetrometer comprising: - Cylindrical punch of diameter 1.8 mm, on the top of which is mounted a weight . the assembly , punch plus weight , shall produce a force of 25 N ; - Dial gauge or any other measurement system accurate to 10 - 2 mm .

H-4 Procedure 1- A sample of PE of thickness ≤ 4 mm shall be taken from a pipe where neither the primer nor the adhesive have been applied . 2- The sample shall be subjected to an indentor with flat face and 1.8 mm diameter , The total mass of the indentor assembly shall be 25 N . 3- The indentor shall be slowly and carefully lowered on the test sample , the Zero ( T0 ) reading set at penetometer within 5 sec. then after 24 h, the final reading ( T ) of the penetometer is recorded The indentation depth is given by the following equation :Indentation ( mm ) = T - T0

H-5 Results : Indentation resistance of the PE material shall be as following … @ 23 °C ± 3 °C 0.1 mm

@ 80 °C ± 3 °C 0.3 mm



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CLIENT : AQP Appendix I-

PROJECT: NEW 16” SEALINE JOINING NAQP-2 PLATFORM TENSILE AND ELONGATION TEST

I-1 General This test procedure covers the determination of the tensile strength at yield, tensile strength at break and ultimate elongation of Polyethylene material.

I-2 Test Standard DIN 30 670:


NF A 49-710:


ASTM D 638:

Standard Test Method For Tensile Test Of Plastics .

I-3 Apparatus : -

Tensile testing machine The apparatus shall consist of a tensile testing machine which makes it possible to record the force and which can operate constant speed .

-

Micrometer

I-4 Sampling The test sample shall be free from FBE, adhesive and taken from a pipe in the extruded direction . The sample shall be of type IV in ASTM D 638.



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I-5 Test Procedure 1- A sample of PE of thickness ≈ 3mm shall be taken from a pipe where neither the primer nor the adhesive have been applied . 2 - Determine the cross-section of the test sample ( cm2 ) . 3- The sample shall be hold between the tensile grips . 4- The grips shall be moved away at constant speed = 50 mm / min. 5- Record the tensile force at the yield point, tensile force at the break point and the extension at break point .

I-6 Results : The tensile strength and ultimate elongation ( elongation at break ) of the PE material shall be as following : Tensile Strength ( Yield )

Tensile Strength ( Break)

Ultimate Elongation

≥ 126 Kg/cm2

≥ 150 Kg/cm2

≥ 400 %

-Calculation and expression of results

• Tensile strength at yield ( kg / cm2 ) = F0 /A • Tensile strength at break ( kg / cm2 ) = F/A • Elongation at break ( % ) = ΔL / L . 100 where F0 F A L ΔL

= is the tensile force at yield point ( kgf ) . = is the tensile force at break point ( kgf ) . = is the cross-section of the test sample ( cm2 ) . = is the initial gauge length of the test sample ( mm ) = is the increase in the sample length between gauge marks ( mm ) .



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Appendix L – CATHODIC DISBONDMENT TEST This test method covers the procedure of determination of the resistance of coating to disbondment of when steel pipe is subjected to negative polarization.

L-2 Standard NF A 49-710:


ASTM G 8:

Standard Test Method For Cathodic Disbonding Of Pipe Lines Coatings.

ASTM G 42:

Standard Test Method For Cathodic Disbonding Of Pipe Lines Coatings at elevated temperature.

L-3 Apparatus - Stabilized DC power supply . - Digital voltmeter /Digital Ammeter. - Variable resistor. - Reference electrode ( saturated CuCuso4 or AgAgCl ). - Platinum anode. - Heating Equipment - Sharp knife L-4 Electrolyte L.4-1 The electrolyte shall consist of a solution of 3% NaCI concentration in potable water L-4-2 The PH of the electrolyte shall be maintained during the test period in the range of 6 to 8.5 ( at ambient temperature).

L-5 Test Temperature L.5.1 For test at elevated temperature 60 °C ± 2 °C where the cell is constructed on the pipe sample, the test sample shall be placed in a thermostatically sand or grit bath. The bath temperature shall be adjusted and controlled to maintain the required test temperature on steel surface.

L-6 Procedure : 1. Three holes of 6 mm diameter shall be drilled through the coating to the metal surface . 2. A rigid plastic container of 100 mm diameter from which the bottom is cut-out, the container is fixed to the coated sample using a silicon rubber adhesive. 3. The container filled with electrolyte, the electrolyte shall be maintained during test period at the PH as described in ( K-4-2 ) and the test temperature as per ( K-5 ). 4. A voltmeter is connected with the reference electrode , the variable resistor is adjusted until the voltmeter reads ( – 1.5V ) with respect to the calomel electrode.



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5. At intervals of 24 hr the voltmeter reading is recorded and the variable resistor is adjusted to correct any drift from the ( – 1.5V ) setting . 6. After Test period the container shall removed and the sample is dried, the degree of disbonding is evaluated as following … 6.1 A series of 2 radial cuts are made through the coating in the longitudinal direction of the pipe and 2 similar cuts shall be made in the circumferential direction. 6.2 Each pair of cuts being 5 mm apart and approx. following the tangent of the test defect, the length of the cuts shall be aprox. 20 mm each side of the defect.

6.3 Using a sharp knife, the strips of coating between the cuts shall be peeled from the pipe surface as far as possible starting at the test defect . 6.4 The distance over which the coating is detached and the metal is exposed is measured from the edge of the original test defect. 6.5 record the measurements for all directions, The result of the cathodic disbondment test is defined as the arithmetic mean value of at single values for the radial lengths in millimeters.

L-7 Results : The coating should show the a maximum disbondment as following …

Test Duration Max. Disbonding Radius

@ 60 ± 2 °c 2 days ≤ 7 mm



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Appendix M – DETERMINATION OF HOT-WATER IMMERSION RESISTANCE M.1 General: This test method covers the procedure for determination of the resistance of coating to loss of adhesion due to water absorption when subject to hot water immersion .

M.2 Standard : GBE/CW6 : part 1 : Technical Specification For The External Protection Of Steel Line Pipe and Fittings Using Fusion Bonded Powder and Associated Coating Systems ( Part 1 : Requirements For Coat materials and Methods Of Test .

M.3 Apparatus : -

Heating element, or water bath Sharp knife

M.4 Procedure : 1. Three holes having diameter ≈ 5 mm are drilled through the coating material to the metal surface . 2. A rigid plastic container of 100 mm diameter from which the bottom is cut-out, the container is fixed to the coated sample using a silicon rubber adhesive . 3. The container shall be filled with potable water . 4. Heat the test sample to 80 °C ± 2 °C in a thermostatically sand or grit bath The bath temperature shall be adjusted and controlled to maintain the required test temperature on steel surface. 5. After Test period ( 7 days ) the container shall removed and the sample is dried, the degree of disbonding is evaluated as following … 5.1 A series of 8 radial cuts are made through the coating at the area subjected to cathodic disbonding. 5.2 Using a sharp knife, the strips of coating between the cuts shall be peeled from the pipe surface as far as possible starting at the test defect . 5.3 The distance over which the coating is detached and the metal is exposed is measured from the edge of the original test defect. 5.4 record the measurements for all directions, The result of the disbondment test is defined as the arithmetic mean value of at single values for the radial lengths in millimeters.

M.5 Results : The coating shall not show disbonding greater than 2 mm or blistering ( a slight discoloration of the coating is acceptable ).



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Appendix N – DETERMINATION OF FLEXIBILITY OF COATINGS N.1 General: This test procedure covers the determination of the flexibility characteristics of applied 3 L PE coating .

N.2 Standard NF A 49-710:


CAN/CSA Z 245.20-M92:

External Fusion Bond Epoxy Coating For Steel Pipe.

N.3 Apparatus : -

Hydraulic press. Freezer Bending mandrel

N.4 Procedure : 1- Smooth the coating on the edge of the sample to remove any potential stress riser. 2- Determine the sample thickness ( t ) 3- Place the test specimen in the freezer, cool it to 0 O c or – 10 ± 3 Oc and for minimum 1 h . 4- Determine the mandrel radius that corresponds to the angle of deflection of 3O per pipe diameter length by using the following formula R = 19.6 t where : R = required mandrel radius mm t = sample thickness 5- Bend the specimen over the radius determine in the above step. The bending rate shall be such that the specimen is bent within 10 s and the dent shall be completed within 30 s of removal of specimen from the freezer 6- Warm the bent specimen to 20 ± 5 Oc and hold this temperature for a minimum of 2 hour before visual inspection.

N.5 Results : The coating shall accepted when no visible cracks is shown when bending performed to 3º PD .



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Appendix O – DETERMINATION AIR ENTRAPMENT IN COATINGS O-1 General : This test method covers the procedure for determining the amount of cross section and interface air entrapment ( foaming /porosity ) in applied 3LPE coatings on steel substrates.

O-2 Apparatus : - Knife ( sharp cutter ).

O-3 Procedure : 1- A strip of coating from the adhesion test shall be used to determine the level of air entrapment on the body of the pipe or in the saw weld. . 2- The strip shall be visually inspected. 3- Evaluate the edge of the sample and rate the cross section and interface porosity using the scale provided.

O-4 Results : The coating should show not more than 20% ( rating ≤2 ) of the observed area contains air entrapment, bubble size in the PE layer shall be limited to less than 1/2 the thickness of the PE layer in height or circumference and not linked together.



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Appendix P – DETERMINATION OF HARDNESS OF COATINGS

P.1 General : This test procedure covers the determination of the Durometer Hardness of Polyethylene material.

P.2 Standard ASTM D 2240: Standard Test Method For Rubber Property- Durometer Hardness .

P.3 Apparatus : -

SHORE D hardness meter

P.4 Procedure: - Sample of PE of thickness ≅ 3 mm shall be taken from a pipe free from FBE, adhesive. - Place the sample on the steel plates of the tester - The sample shall be subjected to a durometer dial to which total mass of 5 kg is attached. - The durometer shall be placed without shock on the sample making a firm contact with it. - The hardness SHORE D shall be read off 3 second after the presser foot of the duometer has made complete contact with the sample

P.5 Results : The hardness shore D of the PE material shall be ≥ 50 shore D



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Appendix Q – DETERMINATION OF MELT FLOW RATE Q.1 General : This test procedure covers the determination of the rate of extrusion of molten resins through a die of a specified length and diameter under constant conditions of temperature , load , and piston position in the barrel as the timed measurement is being made

Q.2 Standard ASTM D 1238: Standard Test Method For Flow Rates Of Thermoplastic By Extrusion Plastometer.

Q.3 Apparatus : -

Extrusion Plastometer. Stop watch Electronic balance

Q.4 Specimen The test specimen may be in any form that can be introduced into the bore of cylinder for example powder, granules, and strips of film

Q.5 Procedure 12345-

Heat the plastometer to 190 °c for 15 minutes. Insert the test sample ( PE or Adhesive ) in the heating barrel. Fit the piston on the sample and fit to the piston a weight 2.16 Kg ( or as recommended in M.D.S ). Each 10 minutes cut the sample extruded from bore ( minimum 5 cuts ). Weight each sample and recorded the weight.



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Q.6 Results : The melt flow rate ( MFR ), expressed in grams per 10 minutes and is given by the following equation :MFR ( θ, mnom ) = tref . m / t

Where : θ = is the test temperature, °C . mnom = is the nominal load, Kg . tref = is the reference time ( 10 minutes ), 600 sec. m = is the average mass of the cut-offs, gr. . t = is the cut-off time interval, sec. - New MFR = shall be within ± 15 % of the material certificate of analysis or material data sheet . - Extruded MFR = shall be within ± 20 % of the New MFR .


Coating Procedure PE

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