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le : 19/03/2013 à 07:54
Afnor, Saga Web pour: TOTAL SA le 19/03/2013 à 07:54 NF A49-711:1992-11 (Annulé le 2012-06-16)
ISSN 0335-3931
NF A 49-711
November 1992
Steel tubes
External three-layer
polypropylene-based coating
Application by extrusion
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ill +-' French standard certified by the General Director of AFNOR on October 20,
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correspondence At the date of publication of this standard, there is no ISO or European
f--'i5J standard on the same subject.
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a analysis This standard relates to steel tubes with an external three-layer,
polypropylene-based coating applied by extrusion. This type of coated tube
can be used for the construction of pipelines, the working temperature of
which is between - 20 °e and + 110 °e.
modifications
corrections
Published and distributed by I'Association Fran«aise de Normalisation (AFNOR). Tour Europe 92049 Paris La Defense Cedex - Tel. : (1) 0142915555
AFNOR 1992
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BNCF
UNM
M AUZEL SEMT PIELSTICK
MME BARACAT HIMONT FRANCE
M CAVALIE GTS ISOPIPE
M DENIS ESSO
M DUTEN ALYNOX
M FALLOUEY VALLOUREC
M GAILLARD COFIDEP
MME GUILLOU GDF DEPT/ST
M HENRY EUROPIPE FRANCE
M HENGSEN EXMA
M LEMAIRE VALLOUREC
M LOPPINET TOTAL
M MATHIEU LE CARBONE LORRAINE
M MOCQUET TROUVAY ET CAUVIN
M MONTAGNE ELF AQUITAINE
M PETIT SOCOMO ET SOCOTUB
REUNIES
M PIELUCHA BNPE
M PIERRE LE CENTRE DU ZINC
M PROVOU BNS
M RENAUD VALEXY
M ROCHE BNS/BNTA
M ROULEAU GDF DEPT/CTO
M SCHIMA SNCT
M SIOUR ELFATOCHEM
M TURCAS COFIDEP
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-3- NF A 49-711
Contents
Page
1 Scope ................................................................................................................................................. 5
2 Normative references ... .... ............ ........ ... ........ ........... ...... ... ............... ....... ....... ......... ............ ........... 5
3 Symbols ............................................................................................................................................. 5
4 Designation .................................................................................. .......................................... ........... 6
5 Inspection documents ...................................................................................................................... 6
5.1 General conditions ............................................................................................................................ 6
5.2 Specific conditions ............................................................................................................................ 6
6 Description of the coating ....... ....... ........ ............... ... ............. ....... ...... .......... .......... .... ..... ........... ..... 6
7 Basic materials .................................................................................................................................. 6
7.1 Composition of the coating ................................. ~ ............................................................................ 6
7.2 Technical documents ........................................................................................................................ 7
9 Properties of the applied coating ........ ................ ............ ........... ... ...... ..... .......... ...... ........ .... ...... ..... 9
9.1 Polymerization or hardening of layer 1 ......................................................................................... 10
9.2 Appearance and constitution of the coating ................................................................................. 10
9.3 Thickness on the body .................................................................................................................... 10
9.4 Cut back at the ends ........................................................................................................................ 11
9.5 Electrical non-porosity .................................................................................................................... 11
9.6 Impact resistance ............................................................................................................................ 11
9.7 Peel strength ................................................................................................................................... 11
9.8 Indentation resistance under punch load ..................................................................................... 11
9.9 Electrical insulation resistance ....................................................................................................... 12
9.10 Ultimate elongation ........................................................................................................................ 12
9.11 Resistance to ultraviolet rays ......................................................................................................... 12
9.12 Thermal stability ............................................................................................................................. 12
9.13 Resistance to cathodic disbonding under negative polarization ................................................ 12
9.14 Stress cracking resistance .............................................................................................................. 13
9.15 Resistance to micro-organisms ..................................................................................................... 13
9.16 Bendability ....................................................................................................................................... 13
11 Repairs ............................................................................................................................................. 15
12 Marking ............................................................................................................................................ 15
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NF A 49-711 -4-
Contents (end)
Page
Annex A (normative) Test for assessing the degree of cure of the epoxy powder layer ........................ 17
-5- NF A 49-711
1 Scope
The purpose of this standard is to define the external polypropylene-based coatings applied in the factory
by extrusion on two binder coats and intended to protect the external surface of the tubes used as pipeline
components. It also defines their application conditions.
In particular, this type of coating is used for protecting buried or submerged pipelines conveying fluids at
working temperatures between - 20°C and + 110°C inclusive. For other working temperatures, additional
requirements may be defined between Purchaser and Coater.
The coatings covered by this standard are applicable to longitudinally or spirally welded steel tubes and
to seamless tubes used for the construction of pipelines conveying fluids, liquids or gases.
2 Normative references
This French Standard incorporates by dated or undated reference, provisions from other publications.
These normative references are cited at the appropriate places in the text and the publications are listed
hereafter. For dated references, subsequent amendments to or revisions of any ofthese publications apply
to this French Standard only when incorpored in it by amendment or revision. For undated references the
latest editon of the publication referred to applies.
NF EN 10021 General Technical Delivery requirements for steel and steel product (classification index:
A 00-100).
NF EN 10204 Steel and iron and steel products -Inspection documents (classification index: A 00-001).
NF T 30-052 Paints - Identation Bucholz test.
NF T 51-016 Plastics - Determination of the melt flow rate of thermoplastics.
NF T 51-034 Plastics - Determination of tensile properties.
NF T 51-056 Plastics - Method of exposure to a xenon arc lamp.
NF T 51-063 Methods for determining the density of products of non-cellular plastics.
NF X 41-514 Protection of plastics - Part 2 - Method for testing the strength of products manufactured
in micro-organism environment - C method.
ISO 1515 Paints and varnishes - Examination and preparation of samples for testing.
ISO 2555 Plastics - Resins in the liquid state or as emulsions or dispersions - Determination of ap-
parent viscosity by the Brookfield test method.
ISO 4287-1 Surface roughness - Terminology - Part 1 : Surface and its parameters.
ISO 8501-1 Preparation of steel substrates before application of paints and related products - Visual
assessment of surface cleanliness - Part 1 : Rust grades and preparation grades of uncoat-
ed steel substrates and of steel subtrates after overall removal of previous coatings.
3 Symbols
Rz roughness parameter (Roughness depth average of 5 successive evaluation areas) - ISO 4287-1.
HR relative humidity of the ambient air, in percentage.
Tg glass transition temperature, in degrees Celsius.
~ Tg variation of the glass transition temperature, in degrees Celsius.
Rs specific electrical resistance, in ohms square metres, (Q m 2 )
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NF A 49-711 -6-
4 Designation
The tubes coated in accordance with this standard shall be designated by the type of coating, the reference
to this standard followed by the thickness class of the coating. If applicable, the reference to the standard
for the tube to which the coating is applied shall be added to this designation.
EXAMPLE:
5000 meters oftubes-NF A 49-150 of 406,4-4,0-
external coating NF A 49-711 Class 1, and lining coating NF A 49-701
with an end shaped according to figure 2 of Annex A of NF A 49-150
5 Inspection documents
5.1 General conditions
The coater shall provide a certificate of compliance with the order (type "2.1" of standard NF EN 10204).
On specific request at the time of the enquiry or order, another type of inspection document may be pro-
vided according to NF EN 10204. The type of inspection document required shall be specified at the time
of enquiry and order.
7 Basic materials
7.1 Composition of the coating
7.1.1 Layer 1
This shall be formed by a film of powder or liquid epoxy resin, of minimum thickness 50 Jlm.
7.1.2 Layer 2
This shall be formed by a polymer intended to provide adhesion between layers 1 and 3. It can be applied
by extrusion or as a powder. It shall have all the compatibility properties. Its thickness shall be uniform and
its minimum value shall be of 150 Jlm.
7.1.3 Layer 3
This shall be formed by the polypropylene coating having the basic product properties indicated in Table 1.
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Pigments and additives can be added to the basic polypropylene, provided that they make it possible to
obtain all the required properties of the coating.
Moreover, they shall be dispersed uniformly.
These documents (technical data sheet and analysis certificate) shall contain the items required in Table 2.
References layer 1
Elements layer 2 layer 3
to test standards Powder Liquid
Date of issue +0 +0 +0 +0
Name of product manufacturer +0 +0 +0 +0
Origin factory 0 0 0 0
Shelf life 0 0 + +
Delivery form of the product + + + +
Conditioning + + + +
Storage conditions + + + +
Sieve analysis or viscosity 0 0 0 0
Spec. grav. +0 +0 +0 +0
NF T 51-016
Melt index +0 +0
condition no. 12
ISO 787/1
Bucholz hardness of crosslinked film +0 +0
NF T 30-052
Gel time +0
f, Tg of crosslinked film + +
NF A 49-711 -8-
The coating application and repair procedure carried out on pipes in the coating mill shall be supplied to
the Purchaser beforehand at his request.
For the application of the coating, the steel surface to be coated shall be dry and free from any impurities
(such as old coating, paint and non-adhesive particles, grease, oil, etc.) detrimental to the tube coating
quality.
The method for preparing the surfaces shall be given in the document defining the application and repair
procedure.
In particular, it shall take account of sub-clauses 8.2.1 to 8.2.4.
8.2.1 Oils, greases or other contaminants shall be removed prior to shot-blasting using a suitable sol-
vent, which will not be spread over the whole surface of the tube.
For tubes subject to surface contamination, the contaminants shall be removed by any means and suitable
products compatible with the coating to be applied.
The tube shall be dried before shot-blasting when its temperature is equal to, or greater than, 3 °C above
the dew point.
8.2.2 The tubes to be coated shall be shot-blasted. The abrasive spraying treatment shall be carried out
so as to obtain a surface texture corresponding at least to the degree of surface preparation Sa 2,5 - as
defined by ISO 8501-1.
The shot-blasted surface shall have a roughness Rz between 40 J.1m and 80 J.1m inclusive. It shall be meas-
ured in accordance with a method given in the procedure for applying and repairing the coating (see 8.1).
8.2.3 After shot-blasting, the surface of the tubes shall be inspected. All slivers, scales, weld drops, sur-
face imperfections made visible by the shot-blasting and detrimental to the coating procedure quality shall
be removed.
After removal of these defects, the residual thickness of the tube shall satisfy the minimum tolerance re-
quirements as specified by the tube standard.
All repaired areas of a surface greater than 10 cm 2 shall have a roughness profile making it possible to sat-
isfy the provisions of sub-clause 8.2.2.
8.2.4 If after preparation of the surface of the tube to be coated, this surface is contaminated or covered
with rust, the tube shall undergo, partially or completely, further shot-blasting in order to make it possible
to apply the coating satisfying the provisions of this standard in every point.
The shot-blasting will also be resumed if the production process is interrupted for time intervals greater
than those given below:
• 2 h for a relative humidity RH > 80 %
• 3 h for a relative humidity 70 % < RH ~ 80 %
• 4 h for a relative humidity RH ~ 70 %
In all cases, the tube shall be at least 3 °C above the dew point temperature.
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8.2.5 Any residue of abrasive by a process given in the procedure for applying and repairing the coating
will be removed from the surface of the tube before application of the coating.
A chemical treatment of the steel can complete the surface preparation after Purchaser's agreement.
8.3.2 The coating in the factory shall be applied in accordance with the established and approved pro-
cedure.
8.3.3 The temperature holding time ofthe tube shall not result in oxidation of its surface, detrimental to
the good quality and adhesion of the coating.
At the time of application, the temperature range at the surface of the tube to be coated shall be in con.
formity with the application conditions as given on the product data sheet.
The temperature of the tube shall be monitored using suitable means in order to make sure that the appli-
cation conditions are fully satisfied.
NF A 49-711 -10-
9.1.2 The degree of polymerization of layer 1 (epoxy powder) shall be determined by differential thermal
analysis.
The check shall be carried out in accordance with the provisions of Annex A.
The acceptance criteria are based on the value of f). Tg as given by the product Manufacturer.
9.1.3 The degree of hardening (liquid epoxy) shall be determined using the method in NF T 30-052.
Thickness classes 1)
Tube diameter D (inmm)
(in mm)
1 2
0::; 114,3 1,2 1,2
Different thickness can be defined by agreement between the Purchaser and the Coater.
The thickness check shall be carried out in accordance with the criteria defined in Annex B.
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Unless otherwise specified in the enquiry and the order, the coating shape of the cut back is a bevel form-
ing an angle less than 30°. The length shall be 100 mm ± 20 mm.
In particular, in case the coating is removed, it shall be checked that the tube surface is not damaged.
The coating shall be free from porosity which can be detected by the method defined in Annex C.
The applied tension is 10 kV mm of coated thickness.
The minimum impact energy, in joules, ajustable to within 5 % and determined in accordance with the
method described in Annex D, shall correspond to 10 <1>. Joules per millimetre of coating thickness. The <I>
factor permits to take into account the influence of the curvature of the tube wall (Table 4).
Tube diameter D
<1>
(in mm)
This property can be determined in accordance with 3 methods, as defined in Annex E. The choice between
Method E 1 (measurement of the peel speed) and Method E 2 and E 3 (measurement of the peel force) shall
be made by agreement between the Purchaser and the Coater.
According to the method chosen, the requirements shall be as follows:
Method e 1 : The average coating peel speed over an arc of 45° shall not be more than 10 mm/min.
Methods e 2 and e 3 : The minimal peel force as measured by the method given in Annex E shall be:
• 15 N/mm for the room temperature of 23°C ± 2 °c
• 4 N/mm for the test temperature of 110°C ± 2 °C
9.7.2 Other values can be agreed upon between the Purchaser and the Coater.
As measured in accordance with the method defined in Annex F, the penetration shall not exceed:
• 0,1 mm during the test performed at 20°C ± 2°C
• 0,4 mm during the test performed at 110°C ± 2°C
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NF A 49-711 -12-
The electrical resistance of the coating, Rs' as measured in accordance with the method described in Annex
G, after being immersed for 100 days in a 0,1 M solution of NaCI shall satisfy the criterion:
Rs (100 days)
The ratio Rs (70 days) shall in addition be greater than 0,8 ; with a coefficient down grade (a) of the
02
a< 30 Rgr (55 days)
where Rgr (55 days) is the electric resistance calculated at the 55 th day according to the equation of the
linear regression line.
This test shall be performed in accordance with the method defined in Annex H. The value of the ultimate
elongation at break shall be at least 400 %.
9.13.1 This test shall be carried out in accordance with the method defined in Annex K.
9.13.2 The peel ratio shall be assessed as being the radius starting from the previously damaged edge
and from which the coating peels easily, flaking off the metal surface.
9.13.3 The average radius of disbondment shall be determined over 6 measurements. The average radius
of disbondment shall be equal to or less than 7 mm after:
• 2 days at 65°C ± 2°C,
• 7 days at 40°C ± 2°C,
• 28 days at 23°C ± 2°C.
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-13- NF A 49-711
The resistance of the coating to cracking under stress as determined in accordance with the method
described in the American Standard ASTM 0 1693 shall be such that after 1 000 h of the coating being
immersed in the active solution, maintained at 50°C, no test piece shall crack. The active solution used is
10% by weight of nonylphenoxy poly(ethyleneoxy) ethanol in water. It shall be kept in a closed container,
made of metal or glass because of its hygroscopic properties.
After 6 months of burying tests, in accordance with NF X 41-514 method C, the loss of adhesion, as deter-
mined in accordance with the method described in Annex E.2 shall not be less than 80 % of the initial val-
ues on the circumference of the tube. No defect shall be longer than 20 mm.
A strip of 5 cm in width shall be cut radially to the metal on each test piece prior to burying.
9.16 Bendability
The coating shall be able to withstand bending with a radius of curvature equal to 20 times the diameter
of the tube, without visible damage (visible crack) or reduction in its initial properties (adhesion, electrical
insulation).
The inspection of the coating provided by the competent services of the coater consists of 4 types of
operations.
The results of these inspection operations shall be recorded by the Coater in a register made available to
any coater's inspection representative or any purchaser's representative.
10.2 Sampling
The Purchaser's representative or the Coater's inspection representative shall select the tubes on which
the specified tests (10.4) shall be ca rried out.
The test pieces for destructive testing shall be taken, if possible, from the ends of the tubes. Samples and
the test tubes shall be marked in order to be able to be identified.
Unless otherwise specified, a unit of production is composed of a set of tubes coated under the following
conditions:
- the same type of manufacturing technique and the same production line;
- the same outside diameter and the same thickness of tube;
- the same production run;
- the same production batch of material for the three layers.
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NF A 49-711 -14-
10.5 Retests
10.5.1 This does not take into account the unsatisfactory results of tests which are not attributable to the
quality of the coating but result:
-15- NF A 49-711
11 Repairs
The tubes with localized defects (porosities, surface, stripping) as well as those which have been subjected
to the control tests may be repaired.
The coating materials that can be used for repairing defects shall satisfy two conditions:
- be suitable for protecting on- and offshore pipelines in the required service conditions (working tem-
perature in particular) ;
- be compatible with the polypropylene previously applied coating.
The application conditions shall be those defined in the specifications for the corresponding materials, or,
failing this, those agreed between the parties involved (manufacturers of the polypropylene coating and
material suppliers).
The repair shall meet the values specified in the manufacturer's technical data sheet.
12 Marking
The necessary marking shall be agreed upon between the parties.
Each tube shall be marked with the following, as a minimum:
- code or name of the Producer of the coated steel tube,
- Coater code, if it differs from the preceding code,
- reference to the steel standard,
- reference to this standard followed by the thickness class.
The marking shall be made using a suitable method such as stencil painting or printing making legible and
indelible identification possible, using durable materials compatible with the subsequent use of the
equipment.
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NF A 49-711 -16-
13.3 Storage
Storage shall be carried out so that the coating does not undergo any deterioration. In particular, the stacks
of tubes which are intended or prolonged'storage shall be protected from the action of ultraviolet
radiation.
13.4.2 Generally, the Coater's responsibility for the supply ofthe correct coated tube is complete as long
as the tube is at this plant and, in the case of accidental damage to the coating, the repairs and inspection
operations shall be his responsibility.
13.4.3 The duration of the tests specified in 7.1.4 shall not delay dispatch of the tubes.
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-17- NF A 49-711
AnnexA
(normative)
A.1 General
The purpose of the test is to assess the thermal properties of the cured layer 1 (powder epoxy) by differ-
ential thermal analysis by:
- assessing the cure of the epoxy film by measurement of the glass transition temperature,
- calibration of the temperature of the thermal analysis equipment.
A.2 Principle
After removing layer 3, the method consists in raising the temperature of a sample of film at a constant
speed in a differential thermal calorimeter.
It is essential that the samples are pretreated to remove moisture and to provide a uniform thermal devel-
opment.
The first plot records the thermal changes in the sample from room temperature up to a point located be-
yond the complete cure. The sample shall be cooled down to room temperature. A second heating cycle
identical to the first cycle shall then be carried out.
A.3 Apparatus
The apparatus used for this test shall be a differential thermal calorimeter with a sufficient calorimetric sen-
sitivity to assess the glass transition of the epoxy products.
Moreover, the following accessories are necessary:
- laboratory scales accurate to the nearest 0,1 mg,
- hammer and firmer chisel,
- small hammer pulverizer or equivalent.
A.4 Sampling
Samples of epoxy film shall be taken from the coated tube without adhesive, immediately after application,
using a hammer and a firmer chisel, which provides rolled coating chips. Care shall be taken to remove
samples from the whole thickness of the film and, atthe same time, to avoid the inclusion of steel fragments.
The chips of film shall be inserted in a plastic box and identified. Samples may be taken at various points
along the length and around the circumference of a tube. The chips shall be separated into small pieces.
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NF A 49-711 -18-
Accurately weigh between 10 mg and 15 mg of product in an aluminium sample pan. Larger quantities,
but not exceeding 25 mg, can be used if necessary for obtaining the required sensitivity.
A.S.2 Method
A.5.2.1 Use of the differential thermal calorimeter
The sample shall be heated up to 240°C 1) at the rate of 20°C per min and the curve shall be recorded. The
sample shall then be cooled to room temperature. This procedure shall be repeated for the second cycle.
However, the latter cycle may be stopped approximately 20 °C above the (glass) transition which deter-
mines Tg.
-19- NF A 49-711
A.6 Results
A completely cured coating will give an identical glass temperature during 2 successive tests. On the other
hand, an incompletely cured coating will give a difference in glass transition temperature. This difference
shall be less than that communicated by the Manufacturer of the powder product (see 9.1).
u
E
....
OJ Glass-transition temperature
.c
..... 1st run
o
x
w
u Glass-transition temperature
"E.... 2nd run
OJ
..c
.....
o
"C
C
W
Temperature °C
NF A 49-711 -20-
Annex B
(normative)
Thickness inspection
B.1 General
The test consists in measuring, by means of a non-destructive process, the thickness ofthe applied coating.
B.2 Apparatus
Magnetic or electromagnetic measuring instrument or any other non-destructive method with ± 5 % accu-
racy.
This instrument shall be calibrated with respect to the metal on which the coating is applied in the range
of thickness of the coating to be tested. It shall be recalibrated frequently in order to as certain its correct
working order and its precision.
B.3 Procedure
On each tube to be tested, carry out at least 12 measurements distributed along 4 longitudinal generating
lines located at 90° from each other and at a distance of at least 200 mm from the end of the coating. Thus 3
measurements shall be made along each generating line: one close to each end and one in the middle of
the tube.
NOTE: In case of dispute on the result at one point, a recalibration of the instrument is made and 5
measurements at this point are carried out again.
The arithmetical mean of the result of the 5 measurements is taken into account.
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Annex C
(normative)
C.1 General
The test consists in looking for any porosity in the coating using a scanning electrode energized by a high
d.c. voltage source.
Porosity shall be detected by a spark occuring between the steel ofthe tube and the electrode atthe defec-
tive location, and by a sound or light signal provided by the holiday detector.
C.2 Apparatus
Adjustable high-voltage holiday detector, equipped with a sound or light signal.
Converted scanning electrode in the form of a metal brush or coil spring with continuous spirals or con-
ductive rubbers according to the diameter of the tubes.
Conductors which are used for connecting the tube to an earth electrode.
C.3 Procedure
Only carry out this test on a coating free from surface moisture.
At the time of the test, set the voltage at 10 kV/mm of nominal thickness of coating, with a maximum
of 25 kV.
Connect the instrument and the coated tube to earth.
Switch on the electrode and move it continuously in contact with the surface of the coating to be
inspected; the relative holiday detector/coating movement shall be less than 0,3 m/s.
NF A 49-711 -22-
Annex 0
(normative)
Impact test
D.1 General
The test consists of verifying the strength of the coating by the impact of a punch of defined shape falling
directly onto the coating from a fixed height and at a fixed temperature. This test shall not be carried out
on tubes of diameter less than 50 mm.
0.2 Apparatus
A drop weight testing machine comprising:
- a straight tubular guide provided with levelling devices (for example, two spirit levels for the hori-
zontal plane and a plumb line for the vertical plane) and a graduated rod which makes it possible to
assess the drop height with an accuracy of 5 mm.
- a hard steel punch, with a polished hemispherical head, with a diameter of 25 mm ; the mass of
which shall be known to ± 5 g.
- a sufficient number of additional weights; the mass of which shall be known with an accuracy
of± 5 g.
D.3 Procedure
The test shall be carried out at the temperature of 15°C to 25 °C. If provision has been made to perform
this test at different temperatures, the method described shall be adapted, after agreement, if necessary,
between Coater and Purchaser.
Place the coated tube on a rigid, and stable, horizontal support and, if necessary, stiffen the tube interior
to reduce its elastic response.
Beforehand, carry out the holiday detection test (see Annex C) and identify the defective points to avoid
making the impact atthese locations; ifthe numberoffaults found istoo high, take another coated test piece.
For each point of impact, arrange the drop weight testing machine perpendicular to the coating surface so
that the loaded punch can fall freely without friction or resistance.
Carry out 10 impacts allowing the weight corresponding to the energy laid down in 9.6 to fall from a height
of one metre. The points of impact shall be selected so as to avoid, as much as possible, any protuberant
welds. Furthermore, the distance from the points of impact to the end of the tube shall be at least 1,5 D
(D=outside diametre of the tube in millimetres) and at least 50 mm between the axes of the impacts.
Then carry out the holiday detection test at each location (see Annex C).
Depending on the result obtained (number of perforations obtained from the 10 impacts made), carry out
a new test series of 10 impacts increasing or reducing the additional weights, so as to be able to plot a
curve of the number of perforations with respect to the impact energy, at the very least on that part of the
curve corresponding to a rapid increase in the number of perforations (in practice 5 or 6 well distributed
test series are adequate, i.e. 50 or 60 impacts to be made).
The hard steel punch shall be checked every 30 impacts. It is changed in case of deterioration.
-23- NF A 49-711
Annex E
(normative)
The method consists in measuring the average speed for tearing off the coating from its metal substrate.
E.1.2 Apparatus
E.1.3 Procedure
The test shall be performed at the temperature of 15°C to 25 °C. If it is intended to perform this test at dif-
ferent temperatures, the method described shall be adapted, if necessary, after agreement, between the
Coater and Purchaser.
Isolate a coating strip, 50 mm wide, perpendicular to the axis of the tube.
Cut this strip along one generating line.
Separate the strip over a sufficient sector to make it possible to attach the mass.
Arrange the tube in accordance with the diagram in Figure E.1 and fix a mass of 40 kg to the end of the
separated strip.
Measure the period (time in minutes) required to peel off the coating over an arc of 45° ending at the lower
generating line.
E.2 Measurement of the peel strength (on coated sample) (Figure E.2)
E.2.1 General
The method consists in measuring the average force required for peeling off the coating from its metal
substrate at a constant pull rate.
E.2.2 Apparatus
A tensile testing machine which makes it possible to record the peeling force and which can operate at a
pulling rate of 10 mm/min.
A cutting tool (knife for example).
A test piece holder which makes it possible for the tube to rotate without friction about its axis and which
can be fitted in the jaws of the tensile testing machine.
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NF A 49-711 -24-
E.2.3 Procedure
The test shall be performed at the temperature of 23°C ± 2°C and/or 110°C ± 2°C. The method described
shall be adapted after agreement, if necessary, between the Coater and Purchaser if different temperatures
are selected.
From the coated tube, cut a sample of a minimum length of 100 mm. On this sample isolate a strip of coat-
ing, 50 mm wide, perpendicular to the axis of the tube.
Cut this strip along one generating line.
Separate the strip over a circumferential length of approximately 20 mm.
Arrange the tube on its support and secure the latter to one of the gripping jaws of the testing machine.
Grip the separated part ofthe coating in the other jaw and verify that the tensile force is applied in the plane
passing through the axis of rotation of the support.
Graphically record the peeling force along the whole circumference of the tube, the constant peeling rate
being set at 10 mm/min.
Record the average peeling force, in newtons, calculated over the whole circumference of the tube in steps
of 20 mm, disregarding the results obtained from the first 20 and last 20 millimetres of the peeling length.
Record the minimum peeling force corresponding to the lowest value of the average forces calculated for
peeling distances of 20 mm.
The method consists in measuring the averqge force required for peeling off the coating from its metal
substrate at a constant pull rate.
E.3.2 Apparatus
A portable tensile test machine, fixed directly on the tube which makes it possible to record the peeling
force on a minimum strip length of 100 mm and which can operate at a pulling rate of 10 mm/min.
A cutting tool (knife for example).
E.3.3 Procedure
The test shall be performed at the temperature of 23°C ± 2 °C and/or 110°C ± 2°C. If it is intended to per-
form this test at different temperatures, the method described shall be adapted after agreement, if neces-
sary, between the Coater and Purchaser.
From the sample isolate a strip of coating, 50 mm wide, perpendicular to the axis of the tube.
Cut this strip along one generating line.
Separate the strip over a circumferential length of approximately 20 mm.
Put the tensile test machine on the tube and fix the polypropylene strip to the gripping jaws. Verify that the
tensile force is applied in the plane passing through the axis.
Graphically record the peeling force over 100 mm minimum, the constant pulling rate being set
at 10 mm/min.
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-25- NF A 49-711
Record the average peeling force, in newtons, calculated over the whole peeling length, in steps of 20 mm,
disregarding the results obtained from the first 20 mm.
Record the minimum peeling force corresponding to the lowest value of the average forces calculated for
peeling distances of 20 mm.
Figure E.3
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NF A 49-711 -26-
Annex F
(normative)
F.1 General
The test consists in measuring the indentation of a punch in the coating under fixed conditions of temper-
ature and load.
F.2 Apparatus
A chamber thermostatically controlled to ± 2,oC.
A penetrometer comprising:
- a cylindrical punch of diameter 1,8 mm (cross-sectional area 2,5 mm 2 ) on the top of which is moun-
ted a weight. The assembly, punch plus weight, has a mass equal to 2,5 kg.
- a dial gauge or any other measurement system accurate to 1/100 mm.
F.3 Procedure
The test shall be performed 3 times on one coated tube sample.
Place the test piece equipped with the penetrometer in the thermostatically controlled chamber, set to the
test temperature and wait for 1 h.
Read the indication on the dial gauge (a).
Load the punch regularly with the mass giving 2,5 kg in total.
Wait for 1 h.
Read the indication of the dial gauge (b).
NOTE: When sampling ofthe test piece is impossible (case of large diameter tube), the test shall be
carried out directly on the coated tube, in air, provided that:
-27- NF A 49-711
Annex G
(normative)
G.1 General
The test consists in measuring, at regular intervals, the specific electrical insulation resistance of the coat-
ing of a tube sample immersed continuously in a saline solution, for a fixed time.
G.2 Apparatus
Tank filled with demineralized water added with sodium chloride in order to form a solution of
NaCI = 0,1 moliL. The tank shall be realized with an electrical insulating material.
Backplate electrode made of copper.
Direct current supply.
Suitable megohmmeter of voltmeter and micro-ampermeter.
Conductors which make it possible to connect the test piece and the backplate electrode to the current
supply.
Material for insulating the tank from the sample.
G.3 Procedure
The test shall be carried out at the temperature of 23°C ± 2 °C ; if it is intended to perform this test at
different temperatures, the method described shall be adapted, after agreement, if necessary, between
Coater and Purchaser.
Use a cylindrical section of tube coated for more than 24 h and proceed according to figure G.1 a or G.1 b
in order to have an immersed test surface of a least 0,03 m 2 .
R = U xS
5 I
where:
S (expressed in square metres) represents the immersed area at the time of the measurement, then draw
the curve as a fonction of the time;
U is the applied voltage in volts between the backplate electrode and steel piece of tube;
is the current intensity in amperes passing between the back electrode and the steel tube.
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NF A 49-711 -28-
/
./
. . . . . -- _1_1- -;/
1 I ~_ _ _ _ Tank made of
insulating material
I
Insulating coating
/
/'
-
/
Steel tube
Figure G.1
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-29- NF A 49-711
- =1= =""""'"
1
I I
- -1- \...,L
insulating coating
Steel tube
NF A 49-711 -30-
Annex H
(normative)
Elongation at break
H.1 General
The test consists in measuring the value of the elongation at break of a polypropylene sample taken from
a tube in accordance with the requirements of standard NF T.51-034.
H.2 Apparatus
Tensile testing machine which makes it possible to record the peeling force and which can operate at a
constant peeling rate of 100 mm/min.
H.3 Sampling
The test is carried out on a sample of polypropylene taken from a tube.
The polypropylene is applied without adhesive in order to make sampling easier.
H.4 Procedure
Take a piece of coating from the tube.
The size of the sample to be taken shall make it possible to make up 5 bar-bell test pieces of type H1 or H2
(see NF T 51-034).
Measure the elongation at break between the gauge length of the 5 test pieces, the peeling rate between
jaws being 100 mm/min.
L,- Lo
- L - x 100
o
where:
Lo is the initial gauge length;
-31- NF A 49-711
Annex J
(normative)
The test consists in subjecting polypropylene test pieces, taken from the coating, to the continuous irradi-
ation of a xenon lamp under fixed temperature and humidity conditions.
The change in the polypropylene shall be assessed by the variation in its elongation at break or in its melt
index.
J.1.2 Apparatus
J.1.3 Sampling
The test is carried out on a sample of polypropylene taken from the tube.
The polypropylene is applied without adhesive in order to make sampling easier.
J.1.4 Procedure
L, - La
- L - x100
a
where:
La is the initial gauge length;
L, is the gauge distance at the breaking time.
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NF A 49-711 -32-
Take the arithmetical mean of the results obtained (A,) and calculate the variation in elongation at break
in percent with respect to the initial elongation, using the equation:
(A, - Ao)
A x 100
o
where:
Aa is the initial elongation (see Annex H)
Alternative: On a sample before and after irradiation taken in the conditions defined above, carry
out 3 melt index measurements in accordance with NF T 51-016. Calculate the arithmetical mean of the
results obtained IF, and the variation of the melt flow index with respect to the initial value IFa as
calculated from the test before irradiation.
The test consists in subjecting a polypropylene test piece to the effect of the dry heat of a thermostatically
controlled oven.
The change in the polypropylene shall be assessed by the variation in its melt index.
J.2.2 Apparatus
A thermostatically controlled chamber with pulsed air which can maintain a test temperature with an ac-
curacy of : ± 2°C.
J.2.3 Sampling
The test is carried out on a sample of polypropylene taken from the tube. The polypropylene is applied
without adhesive in order to make sampling easier.
J.2.4 Procedure
Express the variation of the melt index as a percentage, after a stay in the oven of 300 or 1 000 h using the
equation.
IF,-IFa
IF x 100
a
where:
IF1 is the melt index measured after the stay in the oven;
-33- NF A 49-711
Annex K
(normative)
K.1 Principle
The test consists in assessing the comparative resistance of the coating under negative polarization.
This test shall be carried out using a coated test piece, previously subjected to holiday detection and in
which an artificial defect has been drilled.
The method is applicable to coatings with a thickness:::; 5 mm. It can be adapted to thicker coatings by
agreement between Coater and Purchaser.
K.2 Apparatus
K.2.1 Potentiostat
The main characteristics are as follows:
- an output voltage of 20 V max;
- intensity: 200 rnA max;
- voltage adjustable by potentiometer by ± 5 V ;
- 3-functions switch permitting to display:
- intensity
- "E" potential of the working electrode with regard to the refer~nce electrode
- 'V" difference in potential between the working electrode and the auxiliary electrode.
K.2.3 Electrodes
K.2.3.1 Reference electrode
Saturated calomel type, placed in an electrode holder terminated by a sintered glass plug containing the
electrolyte.
NF A 49-711 -34-
NOTE: The auxiliary electrode is fixed perpendicularly to and at 10 mm from the hole. The reference
electrode is located at 10 mm from the coating and at 20 mm from the auxiliary electrode (see
Figure K2).
K.2.4 Electrolyte
K.2.4.1 3 % NaCI solution, chemically pure (99,5 % minimum) in distilled or deionized water.
See 9.13.3.
In order to reach the testing temperature for the sample, the whole electrolyte equipment shall be placed
on a regulated sand bath.
The sample temperature is checked on the artificial defect (see § K.3.5) with an appropriate means (for in-
stance: a measurement probe).
The tested steel shall be at the required temperature and the electrolyte temperature shall be brought
down to a temperature of 30 DC ± 5 DC. Cooling is achieved using a coil made of neutral glass containing a
coolant.
K.3 Sampling
K.3.1 Samples taken from an industrially coated tube have a minimum size of: 80 h x 80 h x thickness
in mm.
K.3.2 The test on tube or fitting shall be carried out on samples taken outside of the welded zone, in
case of pieces manufactured by welding.
K.3.3 The wall thickness of the coating is checked by measuring the tube at 10 places over the surface
to be tested.
The mean value shall be used as the reference wall thickness for the test.
K.3.4 The samples shall be submitted to a holiday detection test in accordance with the Annex C.
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-35- NF A 49-711
K.3.5 At the centre of the sample, a 6 mm diameter flat-bottom hole is drilled with a flat-ended drill bit,
through the coating up to the steel (see Figure K.1). The depth of the drilled hole shall not exceed 0,5 mm.
It shall be checked that all the test surface is uncoated.
K.3.6 This area shall be degreased rapidly using a detergent and immediately dried after rinsing.
K.4.2 By means of the potentiostat a voltage of - 1 500 mV is applied between the calomel reference
electrode and the working electrode (see Figure K.2) with an accuracy of ± 10 mY.
The temperature in the tested area shall be of 20°C ± 3 °C ; it shall be maintained during the whole test
period according to the clause K.2.6.
K.4.4 For tests at temperatures higher than 23°C, the test duration shall be determined after agreement
between the Coater and the Purchaser.
b) for thermoplastic coatings: 2 parallel cuts of 50 mm, centered on the initial defect are made through
the coating down to the steel using a sharp knife. The sample shall be placed in a air drying oven in
order to reach the necessary temperature for easy peeling of the 3rd layer.
NF A 49-711 -36-
Coating
Figure K.1
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-37- NF A 49-711
Reference electrode
Platinum wire
(Anode)
Plexiglass cover
.....
- ...
Plexiglass tube
Cooling coil 1oE---- ¢ 50
¢ ..:...8-----I-----+1--=~:
Working electrode o
(Cathode)
Coating
¢ 6
Isolation
Figure K.2
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NF A 49-711 -38-
m2 is the mass of the tracing paper of the surface S2 in milligrams per square millimetre;
Disbonded surface
S1 G--S
m,
5, = -
x S2
Figure K.3
Figure K.4