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....................... (1)
where C
P
= specific heat of sample at the temperature of interest.
H
r
= heating rate.
m = sample mass.
Equation (1) is derived from another equation (2), which relates the heat release (or absorption) to the area of
the event on the thermogram, i.e.:
H =
M
A
(B E q
s
) ....................... (2)
where H = heat released.
A = area of the exotherm.
B = time base setting (see A.2.5.3 e)).
The heat release is a function of the specific heat of the test material and equal to:
H =
Y
1
AB H C
r P
....................... (3)
Therefore, if this is substituted in equation (2) and transposed, we arrive at the equation for E.
Alternatively, the cell constant may be determined by relating the latent heat fusion of the pure material
(e.g. iridium) to the area produced from the melting endotherm.
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J229b ( Rev 08/98) - 15 -
A.2.3.3 Method for determining the cell coefficient E
A.2.3.3.1 Place two empty pans in the DSC cell and run a temperature programme between ambient
temperature and 300
0
C. If the trace is not almost horizontal, the baseline slope control shall be adjusted until
the best line is achieved. A typical temperature calibration chart is shown in Figure A.1.
A.2.3.3.2 Load the sample pan with a weighed sapphire disc for a second run. Heat the pan up to the initial
ambient temperature and hold until equilibrium is obtained. This shall be achieved by setting the starting
temperature to ambient temperature and running in isothermal mode.
A.2.3.3.3 Run a second trace using the same final temperature as is used in A.2.3.3.1.
A.2.3.3.4 Measure several values for Y, the vertical difference between the traces, to calculate E values at
these points. The average of E over the range of interest shall be used.
A.2.4 Sampling
When it is necessary to sample large amounts of powder from the sample batch (e.g. several kilogram boxes),
take representative amounts (approximately 50 g) from each container, mix together and sample by coning
and quartering. Analyse different batches separately.
Take a final sample (approximately 250 g) and store it in an airtight container, at a temperature not higher
than 0
0
C, in case subsequent testing is required. When the cold sample is taken from cold storage, allow at
least 30 min in its closed container to reach ambient temperature. Take powder for DSC tests directly from the
250 g sample.
When amounts of powder less than 1 kg are involved, coning and quartering or riffle sampling is not
necessary.
Record the following information for each sample:
a) Date.
b) Time.
c) Powder lot number/batch number.
A.2.5 Test procedure
A.2.5.1 Instrument setting
The test procedure and instrument settings depend upon the design of equipment employed. However, there
are certain essential features in the test method which shall be followed if consistent and comparable results
are to be obtained.
Where applicable, select a baseline slope setting which gives a virtually horizontal line when the reference
and sample pans are loaded identically. This is normally carried out with empty pans.
A.2.5.2 Preparation of test samples
Weigh out accurately between 10 mg and 15 mg of powder into an aluminium sample pan. Heavier weights
(up to 25 mg) may be used, if needed, to give adequate sensitivity. The accuracy of weighing shall be
0.1 mg.
A.2.5.3 Standard air test
Carry out the standard air test under the following conditions:
a) Use open pans throughout.
b) Use an empty aluminium pan for the reference.
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c) No purge gas is employed; carry out the test in static air at atmospheric pressure.
d) Appropriate experimental data recording conditions.
e) If exothermal areas are to be recorded accurately, it may be necessary with some instruments
to change from a temperature base on the abscissa to one of time before the onset of cure.
f) Heat the sample from ambient temperature to 280
0
C at a rate of 20
0
C/min and record the
trace. Rapidly cool the sample to ambient temperature. Repeat this procedure for the second
run, except that this run may be terminated at approximately 20
0
C in excess of the second run
glass transition temperature (Tg
2
).
The test temperature of 280
0
C may be subject to change depending on the type of coating material under test.
It should be advised by the powder manufacturer.
A.2.5.4 Inert gas test
Carry out the inert gas test as for the standard air test (see A.2.5.3), using an inert gas purge instead of static
air throughout the test. A flow rate of 40 ml/min shall be used.
A.2.5.5 Measuring the glass transition temperature
The glass transition temperature (Tg) is defined as that temperature (or temperature range) at which the
coating polymer is transformed from a hard and often brittle material (the glass) into a tough, rubber-like
material.
The glass transition temperature of the cured material is visible on the DSC trace as a baseline shift, resulting
from a marked step-like change in specific heat at Tg, the step usually covering several degrees. It is
conventional to take Tg as the point of intersection of the extrapolated baseline at the low temperature end and
the tangent of the curve at the inflection point (see Figure A.2). For raw powders, the Tg usually takes the
form of a baseline shift with a superimposed endothermic peak (see Figure A. 3).
A.2.5.6 Measuring the heat released during cure
It is necessary to measure the area under the curing exotherm either in the determination of thermal stability,
or when the quality of oversprayed powder is in question.
There are several ways of measuring the exothermal area which vary in their accuracy. These are:
a) Electronic integration using a computer or a dedicated integrator.
b) Planimeter.
c) Cut out the exothermal area marked on the chart paper, weigh it and compare it with the
weight of a known area of the same paper.
d) Count the squares within the exothermal area marked on the chart paper.
One of these, or a similar method, shall be selected for use with the DSC.
The points at which the cure exotherm commences and ends are used to calculate the heat release. They are
usually determined by drawing in the baseline to the exotherm using a rule. Care must be taken to distinguish
between the onset of cure (T
oc
) and the onset of flow (T
of
) and to commence the baseline at T
oc
(see Figure A. 3).
A.3 MEASUREMENT OF DEGREE OF CURE OF POWDER COATING
A.3.1 Principle
The method of assessment of the cure of the powder coating film cure by measurement of its glass transition
temperature consists of heating a ground coating sample at a constant rate in a DSC. A first trace is made
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which records thermal changes in the sample between ambient temperature and some point after full cure as
defined by the powder manufacturer. The sample is cooled to ambient temperature and a second run carried
out. The glass transition temperatures before and after heating are determined and are used to assess the
degree of cure. It is essential that samples are initially pretreated in the calorimeter to remove moisture and to
confer a uniform thermal history.
A.3.2 Apparatus
The apparatus used shall be a DSC with sufficient calorimetric sensitivity to respond to the glass transition
temperature of the materials under test (the thermal analysis curve should display the heat flow rate at a
sensitivity of cm / W 400 minimum). Additionally, the following accessories will be required:
a) Aluminium sample pans.
b) Quench cooling accessory.
c) Analytical balance capable of weighing to an accuracy of 0.1 mg.
d) Liquid nitrogen or other cooling fluid. Alternatively, a DSC with a built-in cooling device is
acceptable provided it can cool the sample rapidly at the rate required in the method.
e) Hammer and cold chisel.
f) Microhammer mill or equivalent.
A.3.3 Temperature axis calibration
The method to be used for checking the temperature axis calibration is as follows:
a) Calibrate the upper temperature scale of the DSC using samples of pure indium, tin and lead
which have melting points of 156.6
0
C, 231.9
0
C and 327.4
0
C respectively.
b) Melt the samples in open pans in either static air or under an inert gas purge, depending on the
test procedure being followed.
c) Take the melting point as the intersection of the leading edge of the fusion endotherm with the
projected baseline.
The results obtained are influenced by the scan rate, therefore adjust the instrument such that these values are
correct at the scanning rate employed in the test, i.e. 20
0
C/min.
In practice, melting points are usually within 2
0
C to 3
0
C of the true values when determined at a
20
0
C/min scan rate and this is found to be adequate for Tg measurements of the coating film. When the
temperature deviation is higher than this, it is necessary to adjust the sample thermocouple reference junction.
If adjustment has been necessary to bring within limits, carry out a further calibration to demonstrate that the
instrument is calibrated accurately.
A.3.4 Sampling
Remove coating film samples from the coated component using a hammer and cold chisel. This produces
furled coating flakes. Care should be taken to remove samples of full film thickness, but at the same time
avoid the inclusion of steel debris.
Sample a component at several points along its length and around its circumference. Take samples from test
panels in a similar manner.
Collect the coating flakes in a plastics bag and identify. Grind the flakes to pieces small enough to pass
through a 2.8 mm aperture sieve in a microhammer mill. Record the following information for each sample:
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a) Date.
b) Time.
c) Component number.
d) Sequence number.
e) Powder lot number/batch number.
f) Location of sample on component.
A.3.5 Test procedure
A.3.5.1 Instrument setting
The test procedure and instrument settings used depends upon the design of equipment involved. However,
there are certain essential features in the test method which shall be followed if consistent and comparable
results are to be obtained.
Where applicable, select a baseline slope setting which gives a virtually horizontal line when the reference
and sample pans are loaded identically. This is normally carried out with empty pans.
A.3.5.2 Preparation of test samples
Weigh out accurately between 10 mg and 15 mg of ground coating into an aluminium sample pan. Heavier
weights (up to 25 mg) may be used, if needed, to give adequate sensitivity. The accuracy of weighing shall
be 0.1 mg.
A.3.5.3 Standard air test
Carry out the standard air test under the following conditions:
a) Use open pans to assist the release of moisture from the sample during pretreatment.
b) Use an empty aluminium pan for the reference.
c) No purge gas is employed; carry out the test in static air at atmospheric pressure.
d) Appropriate experimental data recording conditions.
e) It will normally be necessary to subject the coating sample to thermal pretreatment before
assessment of its degree of cure. Pretreatment is designed to remove any absorbed moisture
from the coating because moisture is known to influence glass transition temperature
measurements. Such pretreatment shall not significantly advance the cure of the coating
sample.
The powder Manufacturer should specify the thermal pretreatment required for the product.
This will typically require heating the sample in the DSC cell from ambient temperature
(i.e. 20
0
C to 25
0
C) to some defined temperature higher than 100
0
C, probably in the range
100
0
C to 150
0
C. This required temperature will typically be attained within 120 s and held
for a period up to 60 s. Immediately cool the sample to ambient temperature with liquid
nitrogen or a suitable cooling fluid; alternatively, a DSC with a built-in cooling device is
acceptable provided it can cool the sample rapidly at the rate required in the method.
Make a suitable record of the pretreatment run.
f) Heat the sample from ambient temperature to a temperature specified by the Manufacturer, at
a rate of 20
0
C/min, so that the sample achieves full cure, but avoids significant degradation.
Rapidly cool the sample to ambient temperature using liquid nitrogen or a suitable cooling
fluid. This establishes the first glass transition temperature (Tg
1
).
Repeat the procedure for the second run, except that this run may be terminated at
approximately 20
0
C higher than the second glass transition temperature (Tg
2
).
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Make pen records of both (Tg
1
) and (Tg
2
) runs.
A.3.5.4 Inert gas test
Carry out the inert gas test as for the standard air test (see A.3.5.3), using an inert gas purge instead of static
air throughout the test. Use a flow rate of 40 ml/min throughout the test.
A.3.5.5 Measuring the glass transition temperature
The glass transition temperature (Tg) is defined as that temperature (or temperature range) at which the
coating polymer is transformed from a hard and brittle material (the glass) into a tough, rubber-like material.
The glass transition temperature is visible on the DSC trace as a baseline shift, resulting from a marked
step-like change in specific heat at Tg, the step usually covering several degrees. It is conventional to take Tg
as the point of intersection of the extrapolated baseline at the low temperature end and the tangent of the curve
at the inflection point (see Figure A.2).
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FIGURE A.1 - Typical temperature calibration
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FIGURE A.2 - Typical DSC traces - Glass transition temperature
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FIGURE A.3 - Typical DSC traces - Enthalpy H
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APPENDIX B
FLEXIBILITY TEST
B.1 LABORATORY PREPARED TEST PANELS
B. 1.1 Apply the coating to steel plates 50 mm x 300 mm x 6 mm thick and properly cure. Bend (at a
deflection rate of 25 mm/min) over appropriate sized mandrels (see B. 1.2) at two substrate test temperatures
(5
0
C and 20
0
C). After bending, the coating shall not crack, disbond or pinhole when holiday tested in
accordance with Appendix C. Inspect plates immediately after bending and again after 24 h at 20
0
C.
B.1.2 Select mandrel sizes according to the following formula:
D =
S
S t ) 1 (
where D = mandrel diameter, in mm (see Figure B.1).
t = plate thickness, in mm.
S = one of the values in clause B.3 depending on the intended coating application and
the temperature of the test.
The arc length of the mandrel shall be fixed at 225 25 mm.
B.1 .3 Set the panel support gap set according to the following formula:
Support gap = M + 2t + 4 mm
where M = chord length across the mandrel arc, in mm (see Figure B.1).
t = plate thickness, in mm.
Bend the panel until it makes contact with the entire surface area of the mandrel.
B.1 .4 During bending, peaking (point at which a gap occurs between the mandrel and the panel) may be
observed at the centre of the panel. In this case, the area of the panel where the gap exceeds 0.254 mm
(0.010 in.) shall be disregarded in evaluating the test results. This area shall not exceed 25% of the mandrel
surface area.
B.2 TESTS ON PIPE SPECIMENS
B.2.1 Cold cut test specimens 356 mm long x 50 mm wide from a pipe section with the long axis in the
circumferential direction. Where seamless pipe is being tested, select specimens which show a minimal
variation in pipe wall thickness, particularly within the test area (i.e. middle 75 mm to 100 mm of specimen).
Bend the test specimens over appropriate sized mandrels at two substrate test temperatures (5
0
C
and 20
0
C). After bending, the coating shall not exhibit visible signs of cracks, disbonding or pinholes and
shall pass a holiday detection test when tested in accordance with Appendix C. Inspect specimens immediately
after bending and again after 24 h at 20
0
C.
B.2.2 Select mandrel sizes according to the following formula:
D
1
= t
t D
1
t
S
1
o
+
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where D
1
=
mandrel diameter, in mm.
D
o
=
original specified pipe outside diameter, in mm.
t = pipe wall nominal thickness, in mm.
S = one of the values specified in clause B.3 depending on the intended coating
application and the temperature of the test.
B.2.3 The arc length of the mandrel shall be fixed at 225 25 mm.
B.2.4 For specimens from pipes having an outside diameter in the range 406 mm to 1219 mm, set the
panel support gap according to the following formula:
Support gap = M + 2t + 4 mm
where M = chord length across the mandrel arc, in mm (see Figure B.1).
t = plate thickness, in mm.
Bend the specimen until contact is made with 75 10% of the mandrel area.
B.2.5 For specimens from pipes having an outside diameter in the range 305 mm to 405 mm, set the panel
support gap according to the following formula:
Support gap = M + 2t + 29mm
where M = chord length across the mandrel arc, in mm (see Figure B.1).
t = plate thickness, in mm.
Bend the specimen until it makes contact with the entire surface area of the mandrel.
Test specimens from pipes having an outside diameter below 305 mm by an appropriate method.
B.2.6 During bending, peaking (point at which a gap occurs between the mandrel and the panel) may be
observed at the centre of the panel. In this case, the area of the panel where the gap exceeds 0.254 mm
(0.010 in.) shall be disregarded in evaluating the test results. This area shall not exceed 25% of the mandrel
surface area.
B.3 S VALUES
B.3.1 For coatings intended for use on fittings, the following S values shall apply:
S = 0.005 at a temperature of 5
0
C.
S = 0.01 at a temperature of 20
0
C.
B.3.2 For coatings intended for use on line pipe, the following S values shall, apply:
S = 0.02 at a temperature of 5
0
C.
S = 0.03 at a temperature of 20
0
C.
B.4 TESTING AT 5 C
0
Testing at 5
0
C may be carried out by pre-cooling the panel in a refrigerator to a temperature slightly lower
than 5
0
C and carrying out the bending operation when the panel temperature reaches 5 2
0
C.
Alternatively, an environmental chamber which controls the temperature in the bending apparatus may be
used. The test specimens shall not be immersed in any liquefied coolant to achieve the test temperature.
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FIGURE B.1 - Typical mandrel for flexibility tests
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APPENDIX C
HOLIDAY DETECTION OF COATINGS
C.1 EQUIPMENT
Holiday detection shall be carried out using dc, non-pulsing holiday detection equipment on surfaces at
temperatures below 90
0
C and free from moisture.
C.2 OPERATING VOLTAGE
The operating voltage shall be 125 V per m 25 of coating thickness.
The rate of travel of the probe over the surface shall not exceed 300 mm/s.
C.3 ELECTRODE TYPE
For all coating systems the wire brush type of electrode shall be used, suitably curved to conform to the
contour of the coated surface of pipe. For fittings, a suitable procedure shall be agreed with the coating
applicator and shall normally be the one that is approved within the procedure qualification.
C.4 IDENTIFICATION METHOD
All holidays shall be identified with a waterproof marker.
C.5 EQUIPMENT CALIBRATION
All holiday detectors shall be calibrated at the beginning of every working day and, additionally, when
requested by Transco.
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APPENDIX D
EVALUATION OF RESISTANCE TO IMPACT
D.1 GENERAL
The procedures specified in clauses D.2 to D.6 inclusive serve to assess the comparative resistance of
coatings to impact damage.
D.2 TEST EQUIPMENT
The following test equipment will be required:
a) A variable impact tester (ASTM G14-77, paragraph 4.2 or equivalent) with punch hammer
type indentor modified as shown in Figure D.1 to accommodate a 14.3 mm diameter ball
bearing and equipped with a minimum impact mass of 1 kg.
b) A sufficient supply of 14.3 mm diameter ball bearings manufactured from EN31 steel with a
Vickers hardness of 800 to 930.
c) A holiday detector (see Appendix C).
d) A thickness gauge.
e) Repair materials.
D.3 TEST PROCEDURE ON COMPONENTS
D.3.1 Check the test site to ensure that it is free from holidays with the holiday detector set at the required
voltage for the particular coating film (see clause C.2).
D.3.2 Position the impact tester on a holiday free site 300 50 mm from one end of the component.
D.3.3 Drop the impact weight from a height calculated to impart the specified impact energy to the
coating. The impact height may be calculated using the following formula:
H =
W 81 . 9
J
where H = impactor height, in m.
W = impactor mass, in kg.
J = impact energy, in joules.
D.3.4 Retest the impact area for holidays using the detector set at the required operating voltage
D.3.5. Repeat D.3.2, D.3.3 and D.3.4 at four more locations evenly spaced over the surface of the
component.
D.3.6 Rotate the ball bearing after each impact.
D.3.7 After every 20 impacts fit a new ball bearing.
D.3.8 If a holiday is caused by the impact test, check the coating thickness in the test area using a
thickness gauge.
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D.4 REPAIR PROCEDURE FOR COMPONENTS
Repair any holiday caused by impact testing using repair materials.
D.5 TEST PROCEDURE ON PANELS
D.5.1 Test sample panels (300 mm x 50 mm x 6 mm) and test panels (300 mm x 50 mm) cold cut from
component in the longitudinal direction according to the procedure detailed in ASTM G14-77, paragraphs
6 to 9, using the apparatus detailed in clause D.2 a). The additional modifications to the ASTM procedure
specified in D.5.2 to D.5.6 inclusive shall apply.
D.5.2 Test impact areas for failure using the holiday detector set at a voltage of 125 V per m 25 of
coating thickness (this relates to coating thickness before impact damage).
D.5.3 The minimum spacing between impacts along the centre line of the specimen shall be 25 mm.
D.5.4 Rotate the ball bearing after each impact.
D.5.5 After every 20 impacts fit a new ball bearing.
D.5.6 Increase the height by an increment of 10 mm between impacts.
D.5.7 There shall be no disbonding at the minimum impact energy. Verify this by testing in accordance
with clause E.6 and report in accordance with clause E.7.
D.6 REPORTING RESULTS
D.6. 1 If the coating withstands the specified impact energy without forming a holiday, the test shall be
recorded as a 'Pass'. If a holiday is formed at the specified impact energy, the test shall be reported as 'Fail at
thickness of...' and the measured coating thickness shall be recorded.
D.6.2 The impact strength shall be converted to impact energy in joules and this value shall be reported.
(A typical calculation is shown in Figure D.1).
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FIGURE D.1 - Impactor and typical calculation
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APPENDIX E
EVALUATION OF RESISTANCE TO WATER IMMERSION
E.1 GENERAL
The equipment and procedure detailed in clauses E.2 to E.7 inclusive shall be used to assess the comparative
resistance of coatings applied to components (free of holidays) to loss of adhesion due to water absorption.
E.2 EQUIPMENT
The following equipment will be required:
a) A water bath which shall be maintained at a temperature of 50 2
0
C.
b) A holiday detector.
c) Internal pipe coating material (complying with CM2).
d) 6 mm diameter twist drill.
e) Pointed sharp knife, e.g. Stanley type or similar.
f) 5 mm diameter steel rod 450 mm long.
g) Elastomeric adhesive for repairing test areas, e.g. Silastic silicone-rubber, grades RTV 738 or
RTV 732 or equivalent.
E.3 SAMPLE PREPARATION
E.3.1 Laboratory prepared specimens
Prepare 300 mm x 50 mm x 6 mm panels under conditions of application and cure similar to those for a
coated component.
E.3.2 Specimens taken from components
Cold cut 300 mm x 50 mm specimens from a sample pipe or, in the case of a fitting, from the pipe pup which
has been coated as a test piece.
E.4 PREPARATION OF TEST AREA
E.4.1 To ensure freedom from holidays, test the prepared panels for holidays with the holiday detector set
at the required voltage (see clause C.2).
E.4.2 Drill a 6 mm diameter hole through the test panel within 25 mm of one end.
E.4.3 Protect the bare metal of the panel with internal coating material (see clause E.2 c)).
E.5 INITIAL TEST PROCEDURE
E.5.1 Carry out an initial adhesion test as described in clause E.6.
E.5.2 Using the steel rod fitted through the 6 mm diameter hole, suspend the specimen panel in the water
bath immersing all but the top 50 mm of the panel.
E.5.3 At intervals of 24 h, remove the panel from the water bath and allow it to cool to ambient
temperature.
E.5.4 Test the coating adhesion as specified in clause E.6.
E.5.5 Repair the test area using elastomeric adhesive.
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E.5.6 Return the panel to the water bath immediately.
E.5.7 If, after seven days immersion, the coating is retested and is found to be satisfactory, return the
panel to the water bath and repeat the adhesion test at intervals of seven days up to a total immersion time of
28 days.
E.6 INVESTIGATION PROCEDURE
E.6.1 Use one or other of the following procedures (E.6.2, E.6.3) as appropriate.
E.6.2 For all coated components and coatings on panels equal to or less than m 600 thickness, use the
following procedure:
a) Using a sharp pointed knife (e.g. Stanley knife or similar), make two incisions approximately
13 mm long through to the metal surface to form a V with an angle of approximately 30
0
at
the intersection point.
b) Starting at the point of intersection force the coating from the steel substrate using the sharp
pointed knife. Take care to protect the eyes and hands when carrying out this operation.
E.6.3 For laboratory panels with coatings greater than m 600 thickness use the following procedure:
a) Using a small hacksaw blade (e.g. 'Junior' type or similar) make two incisions through to the
metal surface to form an X with an angle of approximately 30
0
at the point of intersection.
b) Draw a sharp knife along the cut lines to ensure that the hacksaw blade has reached the metal
surface.
c) Starting at the point of intersection, force the coating from the steel substrate using the sharp
pointed knife. Take care to protect the eyes and hands when carrying out this operation.
E.7 REPORTING RESULTS
Refusal of the coating to peel or a cohesive failure within the coating shall be recorded as a 'Pass'.
Cohesive failure, caused by voids leaving a honeycomb structure on the specimen surface, shall constitute a
'Fail' condition.
For the purpose of this test, cohesive failure will be recorded where some coating material remains on the
metal surface and where difficulty in coating removal has been experienced.
The extent of the adhesive failure between the coating and the metal substrate shall be recorded.
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APPENDIX F
EVALUATION OF RESISTANCE TO CATHODIC DISBONDING
F.1 GENERAL
The procedures detailed in clauses F.2 to F.8 inclusive serve to assess the comparative resistance of damaged
pipe coatings to disbonding when exposed to cathodic protection in potentially corrosive soils.
F.2 TEST REQUIREMENT
F.2.1 Apparatus
The following apparatus will be required:
a) A stabilized dc power unit having a voltage output of 12 V and a capability to supply 20 mA
simultaneously to each test area in circuit. A suitable circuit is shown in Figure F.1 a).
b) Digital voltmeter, range 1.999 V (3.5 digit), input impedance 10
3
M. Accuracy of 0.1% 1
digit at 20 1
0
C.
c) Variable resistor, range 1 k 10%, 1 W (one required for each specimen).
d) 75 mm length of 0.8 mm diameter platinum wire, or similar length of 6 mm wide, 1.5 mm thick
platinized titanium strip (one required for each test area).
e) Holiday detection equipment.
f) Reference electrode of the saturated calomel type, constructed from glass or plastics with
porous plug. The diameter should be not greater than 10 mm.
g) 6 mm diameter twist drill with included cutting angle of 160
0
.
h) Equipment for maintaining the temperature of the specimens and test area
at 20 2
0
C.
i) A length of rigid plastics pipe per test area to be used as a solution container (approximate
dimensions 60 mm long x 50 mm nominal bore).
j) Elastomeric adhesive for fixing the plastics pipe to the test surface, e.g. a silastic silicone
rubber grade RTV 738 or RTV 732 or equivalent material.
k) Fixed resistor, 1 2%, 1 W (one required for each test area).
F.2.2 Reagent
An electrolyte comprising a sodium chloride (NaCl) solution, (3% W/V). 30 g of NaCl should be dissolved in
distilled water and made up to 1 litre.
F.3 PREPARATION OF TEST PANELS
F.3.1 Laboratory prepared specimens
Sample panels 300 mm x 50 mm x 6 mm shall be prepared simulating the conditions of application for a
factory coated pipe.
F.3.2 Specimens taken from components
Test panels 300 mm x 50 mm shall be cut from a sample production coated pipe.
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J229b ( Rev 08/98) - 33 -
F.4 PREPARATION OF TEST AREAS
F.4.1 Test the prepared panels for holidays with the holiday detector set at the required voltage
(see clause C.2).
F.4.2 Fix two lengths of rigid plastics tube perpendicular to the coated surface using a suitable
elastomeric adhesive (see Figure F.1). Place them with their centres on the centre line of the panel width and
equidistant from the panel ends and each other and leave for a period of 12 h to allow the adhesive to fully
cure.
F.4.3 Drill a 6 mm diameter hole through the coating to the metal surface in the centre of each test area
using the drill specified in F.2.1 g).
F.5 INITIAL TEST PROCEDURE
F.5.1 Fill each plastics tube with NaCl electrolyte to a depth of approximately 50 mm (see F.2.2) with the
apparatus set up as shown in Figure F.1 a). Bring the temperature of the specimens and test area
to 20 2
0
C. Maintain this temperature throughout the test period.
F.5.2 Connect a voltmeter and reference electrode to each test rig in turn as shown in Figure F.1 b) With
the tip of the calomel reference electrode positioned approximately 10 mm from the centre of the hole, adjust
the voltmeter reading to read a negative voltage of 1500 mV with respect to the calomel electrode. Carry this
out using the variable resistance shown in Figure F.1 a).
F.5.3 Record, at intervals of 24 h, the voltmeter indication for each test area and adjust the variable
resistor to correct any drift from the negative voltage setting of 1500 mV. Also record, every 24 h, the current
flow by measuring the voltage drop across the 1 fixed resistor.
F.5.4 Every 24 h check the plastics tubes for loss of electrolyte and restore the level with distilled water
as necessary.
F.6 INVESTIGATION PROCEDURE
F.6.1 After seven days, remove the electrolyte and plastics tube from one test site and remove excess
moisture.
F.6.2 Use one or other of the following procedures (F.6.3, F.6.4) as appropriate:
F.6.3 For coatings up to and including m 600 use the following procedure:
a) Using a sharp-pointed knife (e.g. Stanley type or similar), make two incisions
approximately 13 mm long through to the metal surface extending radially from the 6 mm hole
and at an angle of approximately 30
0
to each other to form a truncated V.
b) Starting at the base of the truncated V, force the coating from the steel substrate using the
sharp pointed knife. Take care to protect the eyes and hands when carrying out this operation.
F.6.4 For all coatings in excess of m 600 thickness use the following method:
a) Using a small hacksaw blade (e.g. 'Junior' type or similar), make two cuts across the 6 mm
hole at an angle of approximately 30
0
to each other to form a truncated 'X'. Make the cuts
through to the metal surface and to extend radially from the 6 mm hole.
b) To ensure that the hacksaw blade has reached the metal surface, draw the point of the sharp
knife along the cut lines.
c) Starting at the base of the truncated V, force the coating from the steel substrate using the
sharp pointed knife. Take care to protect the eyes and hands when carrying out this operation.
CW6: Part 1
- 34 - J229b ( Rev 08/98)
F.6.5 Repeat the investigation procedure at the second test site after 28 days.
F.7 REPORTING OF RESULTS
The amount of disbonding shall be quoted as the radial distance from the edge of the pre-damage to which the
coating peels easily from the metal surface.
CW6: Part 1
J229b ( Rev 08/98) - 35 -
a) Cathodic disbonding test rig
b) Voltage adjustment circuit
FIGURE F.1 - Cathodic disbonding test apparatus
CW6: Part 1
- 36 - J229b ( Rev 08/98)
APPENDIX G
STRAIN/POLARIZATION TEST
G.1 Bend the test sections in accordance with the method detailed in Appendix B using a value
of S = 0.02 for line pipe powders and S = 0.005 for fitting powders at a temperature of 20 2
0
C.
G.2 Polarize the specimens, as detailed in Appendix F, with a single test site selected on the minimum
radius of the bend, i.e. area of maximum strain. After 28 days polarization, remove the electrolyte and plastics
tube and remove excess moisture.
G.3 The area of coating exposed to the electrolyte shall not exhibit signs of cracks, disbondment or
pinholes and shall pass a holiday detection test as detailed in Appendix C.