Paper No.

10003 2010

STUDY OF A DELAMINATION FAILURE IN A THREE LAYER COATING OF A 24” GAS

PIPELINE IN VERACRUZ, SOUTH EAST MEXICO.

Francisco Fernandez Lagos,1 Carlos Sanchez Magaña,1 Miguel Angel Lopez,1

PEMEX DCO. Torre Ejecutiva, Marina Nacional 329, Col. Huasteca, México, Distrito
Federal, C.P. 11311.

Jose Padilla,2 Jorge Canto,2 William Villamizar,2 Lorenzo M. Martinez-de la-Escalera,2

Corrosion y Proteccion Ingeneria, S.C. Rio Nazas 6. Cuernavaca, Morelos. Mexico. 62290.

Jorge A. Ascencio3, and Lorenzo Martínez3*

Instituto de Ciencias Físicas, Universidad Nacional Autonoma de Mexico, Universidad 1001,

Chamilpa, Cuernavaca, Morelos. 62210. Also at Corrosion y Proteccion Ingenieria SC

ABSTRACT

The three layer pipeline coating system is one of the fastest growing and more accepted
systems in the world, in great part due to the combination of the excellent adhesion
properties of the FBE, and the excellent water impermeability and mechanical resistance of
the HDPE. We report a case study of a disbondment failure occurred at a 24” gas pipeline
and the steps taken to try to determine the root cause of the failure.

KEY WORDS.- Fusion bonded epoxy, three layer pipeline coating system, cathodic protection
shielding, material characterization.

©2010 by NACE International. Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to NACE
International, Publications Division, 1440 South Creek Drive, Houston, Texas 77084. The material presented and the views expressed in this paper are
solely those of the author(s) and are not necessarily endorsed by the Association.

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 INTRODUCTION

Corrosion in metallic underground pipelines is an electrochemical process, caused by the

anodic and cathodic sites generation on the pipeline surface with the consequent
continuous current flux between those areas. On anodic sites, electrons from the metal
dissolution are generated. Those electrons travel through the metallic substrate to the
cathodic zones, where they are used during reduction reactions (oxidation); and the electric
circuit is completed by means of the ionic flux in the land between the cathodic and the
anodic sites (electrolyte), this involves the media where the structure is located in the
electrochemical cell. Because external corrosion is one of the mayor causes of leaks in
buried pipelines, the pipes are protected against these effects by means of a combination of
dielectric coatings and cathodic protection systems.

The dielectric coatings are the first line of defense against the external corrosion. Even
when the coatings generally induce an excellent protection, most of them suffer damage
after a period of time. Examples include water absorption, soil stress, abrasion with rocks,
bacterial attack and loss of protective properties due to aging. Those damages allow
corrosion to occur in sites where there is contact between the corrosive media and the steel
surface by the coating defects. If these conditions remain, corrosion will cause metal loss
and eventual product leaks. For this reason, CP is an important component of the corrosion
protection system.

The region of the Gulf of Mexico has a tremendous importance in the hydrocarbon
extraction and transportation, Veracruz State has an important amount of pipelines and
consequently there are continuous programs to inspect them by in-line methods. During the
routine program of indirect inspections of the gas pipeline operator (PEMEX), the report of
the in-line inspection indicated three anomalies localized in a section of approximately 7 Km
in length, on the 610 mm. (24’’) Ø ERG Playuela – EMC Playuela gas pipeline with five
years in operation.

This motivated the operator to perform a direct inspection in the three indicated points by
the instrumented tool (Km. 11+500, 19+273 and 23+372); when the coating was being
removed to make the wall measurements, a massive adhesion loss of the three layer
coating system was detected, leaving the pipe surface totally exposed (Figure 1a and 1b).

The PEMEX authorities (sub-direction of the transportation by pipelines coordination –

Direction of Corporative Operations) in collaboration with corrosion specialists took the
initiative of identifying the cause of the failures observed in the three layer coating system of
the gas pipeline. Consequently, a specialized inspection to perform a failure analysis
resulted in a deep study of the three-layer coating system that suffered the adhesion failure.

Such failures were detected approximately after five years in service of the gas pipeline. In
nine of the inspected trenches a complete disbondment of the three-layer systems was
observed, whereas in just one of the trenches (Km. 23+327) a delamination of the adhesive
copolymer layer and the HDPE top coat was observed, while the FBE remained very well
adhered to the steel structure (see Figure 2a). Figure 1c shows the location of the
inspected trenches along the gas pipeline path. The red dots indicate the zones where the
study of DCVG identified sections with exposed metal.

It must pointed out that during the course of this investigation, the quality control reports
from the applicator or the results of their routine lab tests were not available. They would
have provided more data to reach a more assured root cause of the failure.

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 a c
Gas pipeline
Detected failures
by DCVG
Trenches

Inspection sites by dates

30, 31/March/ 2009

19/June/ 2009
4,11/June/ 2009

Figure 1. a) and b) Details of the delamination failure; c) a scheme of the sites where failures
were found over the length of the gas pipeline.

THE THREE-LAYER COATING SYSTEM.-

The use of coatings for pipeline protection is well sustained in the own properties of the
materials, because of the requirements for mechanical and chemical resistance to reduce
corrosion related problems or other types of damages to the structure; in fact, the
confidence about pipelines is related to the confidence in the coating system. The use of
the three layer coating system has been vastly accepted in many countries around the
world, where they account for between 65 and 90% of new coatings use; with the exception
of Africa and the Middle East, where the use is between 45 and 50%, and USA, Canada
and the UK, where they only account for 15% of new coatings as it was reported
previously.(1) This is due to its ability to combine the properties of two different coatings,
which individually have been successfully on their own. This coating system combines the
excellent adhesion and oxygen impermeability of FBE, with the good abrasion resistance
and excellent impermeability to water provided by the polyolefin.

The three layer system consists of the application of a first coat of FBE, that can be applied
from 50 to 100 μm (2 to 4 mils). Today, it is more common to find systems with more than
150 μm (6 mils) thickness of this coat, with the premise that the higher the FBE thickness,
the better the impact and cathodic disbondment resistance.

After the application of the FBE, and just before its gel stage concludes, a layer of polyolefin
copolymer adhesive is applied, usually between 150 to 250 μm (6 to 10 mils). This layer
provides the necessary adhesion between the final polyolefin layer with the FBE. The final
layer is an extruded polyolefin (polyethylene or polypropylene, depending on the service
conditions) to reach the final thickness between 2 and 4.5 mm.(2) A scheme of this system is
illustrated in figure 2b, where all of the individual layers can be visualized.

In particular, the use of FBE has proved to be a reliable coating because of its capability to
adhere to the metal substrate. Consequently FBE is commonly used as a standalone
coating and there are not many reports in the literature about failures of this type of coating.
Based on that, the use of this type of coating is a good solution, and the singular cases
where failure occurs requires a deep analysis to recognize the reasons and the conditions
that caused it. Following this tradition, we are reporting the results of field and laboratory

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evaluations to the materials that presented the generalized disbondment failure on the
coating system of the above mentioned gas pipeline.

c d

Figure 2. a) Adhesive copolymer layer and the HDPE top coat delamination, with the FBE
showing excellent adhesion to the pipeline b) Three layer coating system scheme, and
procedures of c) CIS and d) DCVG.

PIPELINE CONSTRUCTION AND COATING APPLICATION PARAMETERS.-

The construction parameters are listed in Table 1, which are common in gas transportation
pipelines, and particularly the three layer coating system is well accepted for the protection
of these metal pipelines.

TABLE 1
PIPELINE CONSTRUCTION SPECIFICATIONS
Steel type API X5L
Pipe thickness 16.7 mm. (0.659’’)
Pipe diameter 610 mm. (24”)
Pipeline length 24 Km. (14.9 miles)
Product Sweet gas
Coating operations First semester of 2003
Three layer:
- FBE
Coating system
- Copolymer Adhesive
- HDPE
Complete coating thickness 3.5 mm. (average)
Time in service 5 years

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However the gas pipeline operator contracted the procurement and construction to a third
party; project specifications were not issued, neither an independent inspection was hired
by the operator during the application and lay down operations. The operator subcontracted
a company to certify the coating and lay down process of the pipeline, but the visits made
by this company to the application plant during this stage of the project were scarce and
simply were limited to support the written reports from the applicator without any verification.
This motivated an evaluation to try to identify the root cause of the problem and also the
real extension of the failure.

FIELD ANALYSIS

CIS/DCVG procedure for the study:

The pipeline localization was done using “RIDGY” detectors in inductive mode, which allows
a fast analysis because it does not need excavations as in the conductive mode,
particularly in zones with high concentration of metallic structures. A “Measuremark” wheel
odometer with a precision of less than 10 centimeters was also used, which allows the
identification of the line path during the Close Interval Survey (CIS) and Direct Current
Voltage Gradient (DCVG) inspection as it is shown in figure 2c.

The first stage of the CIS inspection consisted in the installation of satellite interrupters in
the rectifiers with influence on the pipe sections under study. The interrupters controlled
interruption cycles of 0.8 seconds in “on” with 0.2 seconds in “off”, receiving satellite pulses
each second to keep an exact synchronization; this right of way (ROW) has two rectifiers
that were synchronized for the study.

The studies were performed with a “MGM G1” device. In high soil resistivity or low humidity
zones the ROW is wetted to reduce measurement errors that use to happen because of
wrong contact between reference cells and the soil. The potential measurements were
performed in the exact position using the installed temporal marks during the detection of
the pipelines. The CIS cables were exchanged at each localized test station and it was
verified that they were connected to the pipeline, reducing to the minimum the typical
“staircase” effects in the “on” profiles of the CIS graphs. The reference cells were prepared
each day with saturated solutions of copper sulfate to obtain exact values for the
polarization potentials. The design of the cells avoided the influence of solar rays,
consequently eliminating erroneous readings because of the possible degeneration of the
electrode by ultraviolet radiations.

During the DCVG studies, the same interrupters used for the CIS studies were utilized for
the pulsed signal of DCVG (dV). The study was done employing the “DCVG” instruments as
in figure 2d. Temporal marks were applied over land with aerosol paint on the exact location
of the coating defects with respect to the test posts, line markers, etc., to establish fixed
references using the wheel odometer. In the localization of each defect, the potential fall
was evaluated from the epicenter of the failure to remote earth for calculating the degree
of %IR. The corrosion characteristics for each defect were examined with activated and
inactivated current to determine the cathodic protection efficiency in the exposed steel
zones. Additionally, the potential gradients around each defect were examined to determine
the type of defect (punctual or continuous).

As a result of these studies, seven additional sites were chosen where the DCVG found
coating failures, the purpose was to excavate and evaluate the behavior of the three layer
system in those sites (Km. 9+591, 9+914, 11+142, 13+106, 19+372, 22+381 and 22+600);
evaluating an additional eight pipe segments. Similar to the initial excavations, the visual

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inspection did not find coating blisters or carbonate residues (calcarious deposits) over the
coating film. In some areas, mechanical damages were found caused by the excavation
method and wrong practices during the laying of gas pipeline. It is important to mention
that at least on one of the pipes inspected; the coating system could not be removed,
showing excellent adhesion to the substrate (see Figure 3a).

Poor adhesion Weld Good adhesion

Area Area

b c

Area around a holiday

d e

Figure 3. Visual inspection of the coating over the pipeline.

In seven of the eight pipelines the same original failure was found; additionally, in two
excavations (Km. 9+591 and 22+381) there was evidence of cathodic protection shielding
(see Figures 3b, 3c and 3d); at both sites, the penetration of the electrolyte through a
holiday was observed, ultimately getting trapped under the film due to the poor adhesion of
the FBE. The high electrical resistivity of the HDPE prevented the cathodic protection
current to reach the adjacent zones around the holiday, creating corrosion under the
disbonded film with severe risks to the pipeline integrity. The observations allowed the
recognition of a generalized attack without evidence of pitting corrosion, which can be
associated to an early stage of the pitting process. Evaluation of pH is also illustrated in
figure 3e, which was considered important in the determination of the incidence of the
cathodic protection system in the failure observed over the pipeline.

The evidences found (shown in figure 3) denote an important presence of generalized

corrosion under the film, with the corresponding risk to the integrity of the pipe, in some of
the areas where the 3-layer coating failed.

LABORATORY ANALYSIS

Because of the many derived questions about why the coating failed, it was needed to
collect and evaluate samples of the metal substrate and of the disbonded coating, in order
to evaluate them in independent specialized labs by different techniques, such as:
Scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS), X-ray
diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) and differential scanning
calorimeter (DSC).

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SEM allows obtaining microscopic images from surface of different types of samples; in
addition, the use of EDS gives the microanalysis from points or selected areas to derive into
compositional patterns or elemental maps, which opens the possibility to evaluate corrosion
products, impurities or organic aggregates to help in the sample characterization. We used
a TESCAN SEM of the VEGA II Easy Probe series, and a Bruker EDS. We focused our
analysis on the metal substrate and samples of the coating collected from the sites. As it
can be observed in figure 4a the laminar structures are associated with iron aggregates,
which can be confirmed by the EDS spectra, which also denotes the presence of
manganese as expected for the type of steel of the pipelines.

a c

Figure 4. SEM micrographs of clusters with a) Mn and b) Cr, besides their corresponding
EDS spectra; and c) elemental mapping of a general view.

The use of elemental mapping allows identifying the iron matrix with small aggregates with
Si and Cr, besides inclusions on the alloy of Al and Mn. The general view of figure 4c with
the composition evaluation allows the determination of the presence of no contaminating
materials even at this microscopic scale.

Figure 5. a) SEM analysis of the polymeric matrix and b) a typical XRD pattern

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From the use of the SEM methods for the evaluation of the organic matrix (figure 5a), which
is obtained from the residues of the coating collected from the disbonded segments, it is
clear that the elements that compose the sample correspond to the expected elements,
which is reported in the specifications from the manufacturer.

The fundamental application of XRD is the identification of crystalline samples; because this
method is based on the optical interference between X-rays when they diffract in the
atomistic array of the samples. This particular behavior is studied under the fulfilling of
“Bragg law”, that allows identifying the conditions to diffract beams in a lattice. The use of
this technique was to identify the iron phases and the possible identification of major
contaminant materials. In figure 5b, a common X-ray pattern is shown, where the peaks are
associated to the expected iron crystals (alpha iron and hematite phases).

The Fourier transformed Infrared spectroscopy (FT-IR) technique is based on the infrared
light absorption capability of materials; the use of the vibrational analysis of molecules
allows identifying species that can determine the presence of a surface component on the
back of the FBE film, which could be the reason for the poor adhesion over the prepared
substrate (Fig. 6a).

Figure 6. Spectroscopy analysis of collected samples by a) FT-IR and b) DSC.

In the laboratory analysis, there were no evidences of any contaminating agent that could
be the cause of the identified failures. The differential scanning calorimetry (DSC) technique
is used to determine, between several other properties, the degree of cure of the FBE layer.
The results of the analysis indicate that the product reached its cure satisfactorily (Fig. 6b).

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 DISCUSSION AND CONCLUSIONS

The direct assessment made on the gas pipeline in the different excavations (illustrated in
figure 3a -3f) indicated the following:

x Unusual values of the anchor profile on the pipeline surface (84 μm or 3.4 mils
average) were not found; these measured values meet those reported by the
applicator in its quality program; additionally, viewed under 30X magnification, the
surface profile seemed to be angular in shape. In all of the sites where disbondment
of the FBE was found, it could clearly be seen that the coating copied the angular
profile on the steel substrate (anchor profile values measured on the back of the
disbonded coating matched those taken on the pipe surface).
x Chloride was not found at any of the site evaluations the presence. Also, no bacterial
activity under the disbonded coating film was detected. The pH values found under
the coating film were between 6 and 7 (Figure 3d), which indicates that the cathodic
protection current did not contribute to the failure generation. Only in the surrounding
zones around a holiday could we obtain a pH value of 9, which indicates cathodic
activity around a discontinuity in the coating.
x In the segment of the pipeline where we found a delamination failure between the
adhesive layer and the FBE, the dry film thickness values (117.5 μm or 4.7 mils
average) coincide with those reported by the applicator in its quality program. In this
segment, the FBE first layer was found to have an exceptional adhesion to the steel,
which is characteristic of this type of coating. The inspection by UV light did not
detect grease, oil or any superficial agent that could have interfered with the
adhesion of the first layer of the coating system. In total, of the thirteen sections of
the gas pipeline evaluated, the disbondment failure of the three layers system was
identified in twelve of them, mainly in the substrate/FBE interface. Only one of the
pipelines showed a delamination failure at the FBE/adhesive interface.
x The evaluation of the cathodic protection system installed did not show indications of
overprotection, determining a mean potential “ON” value of -1.2 V and an average
“OFF” potential of -0.88 V. The DCVG inspection detected 67 defects in the coating
along the gas pipeline path; 2 in the range of 16 to 35 %IR drop and 65 between 0 to
15% IR drop. This indicates that the majority of the defects founds were very small,
which implies that even though the tendency to repair the areas with larger IR drops
because it’s the most commonly attacked, our findings show that there is the
possibility of corrosion under smaller identified IR drops; in this manner, although the
exposed metal section is considerably minor, under the circumstances that this
phenomenon is occurring, these areas require immediate attention and cannot be
postponed. The laboratory analysis using SEM-EDS, XRD and FT-IR did not detect
the presence of contaminants in the substrate or on the disbonded film. The DSC
analysis of the FBE film indicated that it was well cured.

There are several conclusions that can be derived from this case study:

1. Due to the fact that the massive adhesion failure occurred in most of the pipes
evaluated, but not in all of them, with the majority of the pipes presenting complete
disbonding of the FBE, at least one presenting a delamination failure in the
FBE/Adhesive interface, and at least one of the segments evaluated presented
excellent adhesion of the three-layer coating system, leads us to consider that the most
probable cause is the lack of control of the different parameters during the surface
preparation and application process.(1) However, under theoretical considerations and

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 recent reports, such as the fact that the FBE should thoroughly wet the surface,(3-5) our
own characterization results and field findings demonstrated this did not occur, and
because the known and documented performance of FBE, specially its adhesion to the
steel, we can also be conclusive about it.
2. The cathodic protection system did not have an observable effect in the failures
observed. The CIS evaluation showed no areas with an excess of cathodic protection
current that could be associated to the failures observed. This was also corroborated
during the field investigations.
3. Although the majority of the coating failures found by indirect inspection with the DCVG
were very small in size, the risk of underfilm corrosion and cathodic protection shielding
caused by the combination of poor adhesion of the FBE and high dielectric strength of
the HDPE is very high. More frequent in-line-inspections (ILI) are necessary to assess
the integrity of the gas pipeline and monitor the development of corrosion in areas not
evaluated directly.
4. More control of the project on behalf of the operator, through more strict project
specifications and the involvement of a third party coatings inspector during every step
of the process along the entire project, could have prevented or provided early
detection to the problem, helping the owner of the pipe take the necessary corrective
actions early on in the project, and minimizing the costly site rehabilitations and more
frequent in-line-inspections, and the possible loss of integrity of the gas pipeline.

REFERENCES

1. Colin Argent, David Norman, “Three Layer Polyolefin Coatings: Fulfilling Their
Potential?”

2. Alan J. Kehr, “Fusion Bonded Epoxy”, NACE International Publication, 2003.

3. Ali Ehsan Nazarbeygi, Ali Reza Moeini, “Three-Layer Polyethylene Coating Performance
in Iran”, MP November, 2009, page 32 – 34.

4. Benjamin T. A: Chang, Hung-Jue Sue, Han Jiang, Dennis Wong, Alan Kehr, Fabio
Aquirre, “Residual Stresses in 3LPO External Pipeline Coatings –Disbondment and
Craking”. BHR Europe Conference 2009.

5. Benjamin T. A. Chang, Han Jiang, Hung-Jue Sue, Shu Guo, Guylaine StJean, Ha Pham,
Dennis Wong, Al Kehr, Kim Him Lo, “Disbondment Mechanism of 3LPE Pipeline
Coatings”. BHR Europe Conference 2007.

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