PERGAMON Electrochimica Acta 44 (1998) 363±371

About coatings and cathodic protection: Properties of the

coatings in¯uencing delamination and cathodic protection
criteria
Isabel C. P. Margarit a, b, Oscar R. Mattos b, *
a
Federal University of Rio de Janeiro, EQ/DPI, Cidade, Universitaria-BLE, 21949-900, Rio de Janeiro, Brazil
b
Laboratorio de CorrosaÄo ``Prof. Manoel de Castro'', Federal University of Rio de Janeiro, EE/COPPE/PEMM, P.O. Box 68505,
21945-970, Rio de Janeiro, Brazil
Received 10 November 1997; received in revised form 12 December 1997

Abstract

Two aspects related to the deterioration process of organic coated structures under cathodic protection, detected
in a previous work, are analysed: (i) why the size of failures exposing the metallic substrate can in¯uence the level of
delamination and (ii) if there is a failure exposing the metallic substrate, why the appearance of blisters is fostered
even away far from the original failure. The results show that an improvement of laboratory procedures for coatings
selection can contribute to the development of coating/cathodic protection technology. Finally, the limitations of
usual cathodic protection criteria are discussed considering the impedance measurements of samples with electrodes
placed at the coating/metal interface. # 1998 Elsevier Science Ltd. All rights reserved.

Keywords: Organic coatings; Cathodic protection; Impedance; Delamination; Electrochemical monitoring

1. Introduction concerning the tendency to delaminate. The selection is

Cathodic protection and the use of coatings are
techniques for corrosion control that, although being
applied together for many decades, have still important
questions with respect to their utilization without a
precise answer [1±8]. The complicating factor is the
eventual presence of failures on the coatings, which
leads to delamination and the occurrence of true
crevices [1±3], making a uniform distribution of the
electric ®eld dicult and, in consequence, involving
great risk of corrosion [4±6]. Cathodic currents
enhance the delamination in areas of coating damage.
As delamination should be avoided, the selection of
a coating must take into account its characteristics
* Author to whom correspondence should be addressed.
Fax: +55 212906629; E-mail: omattos@metalmat.ufrj.br
usually made by procedures based on the introduction
of an intentional failure exposing the metallic substrate
to the action of a cathodic polarisation. There are
standards for the size of the failure, degree of polaris-
ation, electrolyte and time for observation [7].
Nevertheless, if more accurate cathodic protection de-
signs and methods for monitoring are desired, the age-
ing process of the coatings have to be characterised
and understood. In a previous paper [8] the adequacy
of several tests to promote the ageing of coatings in
laboratory was evaluated. During these tests two
observations were made which deserve deeper analysis:
(i) the size of arti®cial failures can in¯uence the
delamination process of some coatings and (ii) if there
is a failure with metal exposure, the appearance of
blisters is fostered far away from this area. The aim of
the present paper is twofold. First, to investigate the
in¯uence of the presence and the size of the failures on
coatings delamination. Second, to discuss the diculty

0013-4686/98/$19.00 # 1998 Elsevier Science Ltd. All rights reserved.

PII: S 0 0 1 3 - 4 6 8 6 ( 9 7 ) 1 0 1 9 3 - 1
364 I.C.P. Margarit, O.R. Mattos / Electrochimica Acta 44 (1998) 363±371

Table 1. Basic features of the samples

Coating Total Area

thickness (cm2)
(mm)

High built epoxy polyamide (A) 350 65

High built coal tar epoxy polyamine (B) 350 65

in establishing a criterion for cathodic protection in

the presence of a coating.

2. Experimental

The coatings with the brief description shown on

Table 1 are the same as used before [8]. A and B are
coatings standardised by the Brazilian Petroleum
Company. A is commonly used in o€-shore structures.
B is characterised by high resistance to chemicals and
abrasion and is used on tide zones. The samples con-
sisted of coated steel with arti®cial failures, drilled
through the coatings, until the metal is exposed, with
di€erent areas: 0.36, 0.01 and 3  10 ÿ 4 cm2. The
0.36 cm2 hole was introduced in relation to the coating
thickness as recommended by ASTM G8 [7]. The two
other areas were introduced to determine the failure
dimension e€ect on the coating deterioration. Another
kind of sample consisted of free ®lms of A and B,
obtained by painting on acetate paper and manual Fig. 1. Special samples with silver electrodes at the metal/
coating interface.
detachment after curing. Special samples of coating A
were prepared with silver electrodes of 4 mm2 placed
at the metal/coating interface. The procedure consisted 2.3. Electrochemical monitoring
of embedding the silver electrodes with an epoxy resin
in the steel substrate, levelling the total surface and Impedance measurements were performed on the
applying the coating. Top and lateral sights of this samples shown in Fig. 1 with di€erent arrangements:
kind of sample are shown on Fig. 1. The working elec- (i) the impedance of the coated steel and of each
trolyte was 3.5% NaCl. coated silver electrode were measured under potentio-
static control, using a graphite auxiliary electrode and
2.1. Permeability a saturated calomel (sce) as reference; (ii) the impe-
dance of the coated steel was also measured having
The free ®lms had their permeability to OH ÿ some of the silver electrodes at the metal/coating inter-
measured in a cell with two compartments separated face as references. In order to complement this study,
by the ®lm. In one compartment there was distilled few impedance diagrams of a silver electrode (without
water and in the other there was an NaOH solution coating) were measured in 3.5% NaCl solutions with
with pH = 13. The pH increase on the water side was pH = 6 and pH = 14 adjusted with a NaOH solution.
monitored with a pH meter electrode and by conduc- The instruments consisted of Omnimetra PG09
tivity measurements. Potentiostats and a TFA Solartron 1250.

2.2. Polarisation curves

Polarisation curves were obtained for samples A and
B with the di€erent failures and for the samples shown
in Fig. 1. Steady-state curves were performed under
natural convection with an Omnimetra Mod. PG-05
Potentiostat/Galvanostat.
3. Results and discussion
3.1. Dimension of the failure
In the previous paper [8] the delamination of coat-
ings A and B was described taking into account the
 I.C.P. Margarit, O.R. Mattos / Electrochimica Acta 44 (1998) 363±371 365

Fig. 2. Variation of pH and conductivity in function of the OH ÿ ¯ow through A and B ®lms.

presence of arti®cial failures. It was checked that the curves are characterised by two regions: one
dimensions of the failure had no meaningful e€ect on corresponding to oxygen reduction (region I) and
the performance of coating A. On the contrary, on another corresponding to water reduction (region II).
coating B, which had higher impedances than A, the Comparing the curves concerning the 0.36 and
delamination process was in¯uenced by the dimensions 0.01 cm2 failures, it is possible to perceive that the cur-
of the failure. It was attested that delamination was rent densities at region II are lower in the case of
more important in the case of the hole with 0.01 cm2 0.01 cm2. In this region the current densities would be
rather than with the 0.36 cm2 one. This behaviour is charge transfer controlled and so identical, regardless
closely related to the cathodic polarisation, because the size of the failure. The explanation for this di€er-
samples tested without polarisation did not exhibit the ence may be that the geometry de®ned by the ratio
same di€erences. Obviously, the explanation for these between the diameter of the failure and thickness of
experimental results involves the coating properties the coatings promotes an electrolyte con®nement, mak-
because, the greater delamination occurs only in the ing the exchanges with the bulk medium dicult. This
case of the small hole and only for B. hypothesis is supported by the behaviour of the cur-
Indeed, it was seen that coating A is more permeable rent on region I, which assumes a very well de®ned
to water than B [8] and the same occurs for OH ÿ limit value for 0.01 cm2 and less pronounced for
ions, as shown on Fig. 2. In Fig. 2, the OH ÿ ¯ow 0.36 cm2. Thus, the increase on the pH to justify the
through the ®lms is monitored by pH measurements.
As the pH electrode is not very sensitive for low
changes of [H + ], the OH ÿ ¯ow was also monitored
with conductivity measurements. It can be observed
that the permeation laws for OH ÿ are distinct for the
two paints. In case B there is a tendency to establish a
plateau beyond 40 days, which would be associated
with a blockage to OH ÿ ¯ow. On the other hand,
coating A is inclined to promote the OH ÿ ¯ow.
The easier ¯ow of OH ÿ and the greater permeability
to water of coating A may imply in lower increases of
pH in the coating/metal interface, leading to a slower
propagation of delaminated area in comparison with
coating B. A question that remains is why the delami-
nation of B is enhanced when the failure size
decreases?
In Fig. 3 cathodic polarisation curves are shown for Fig. 3. Cathodic polarisation curves of samples A and B with
A and B samples with the various sizes of failure. All failures of various areas.
366 I.C.P. Margarit, O.R. Mattos / Electrochimica Acta 44 (1998) 363±371
important delamination of B in the case of the small
hole (0.01 cm2) cannot be explained by greater current
densities, but it is probably due to a merely geometric
reason associated with the permeability properties of
this coating. Higher current densities for small holes, if
present, could be explained by similarity with the
so-called microelectrode behaviour [9]. In this case, as
widely known, the mass transport is improved and
high current densities can be locally measured. Would
this aspect have any importance in the problem under
discussion? On Fig. 3 it can be understood that the
microelectrode-like behaviour de®nitely cannot be
observed for the 0.01 cm2 failure, but may occur for
smaller failures, as for example, 3  10 ÿ 4 cm2. Indeed
for this small hole the current density at region I is
higher and the oxygen plateau can be avoided because
the mass transport is enhanced. So, as a conclusion for
Fig. 3, it can be stated that the in¯uence of a failure
on a coating, depending on its size and paint thickness,
has two aspects to be considered: (i) the increase on
current densities and (ii) the electrolyte con®nement.
The ®rst one can be explained by microelectrode-like
behaviour and promotes an increase on the mass trans-
port at the coating/metal interface. The second one is
basically a function of the coating properties. In e€ect,
for the same kind of failure, identical current densities
for both coatings were measured in all applied poten-
tials. Nevertheless, only for coating B, and not for A,
the delamination process is intense, because it has
a very high impedance and lower permeability to
OH ÿ and water, making the exchanges between the
delamination area and the bulk solution dicult.
Delamination tests with failures of small dimensions
are not suggested by the usual standardised procedures
and can improve laboratory methodology for the selec-
tion of coatings to be used together with cathodic pro-
tection, as well as the consideration of permeability to
water and OH ÿ .
3.2. Appearance of blisters far from areas of
macroscopic defects
The other aspect to be considered, concerning the
presence of failures exposing the metal on coated
samples under cathodic polarisation, is the appearance
of blisters away from the area of metal exposure. The
®rst idea is that when there is metal exposure on coat-
ings of high impedance, as is the case of A and B, the
total current is concentrated on the area of exposed
metal. This aspect can be better analysed with the
samples on Fig. 1.
The aim of using this special kind of sample is to
exemplify/verify the electric ®eld distribution at the
coating/metal interface, measuring the current and the
impedance on small areas of the coating. For this pur-
pose, each silver electrode was connected as a working
electrode and the impedance diagrams could be taken
whenever a local potential was measured. Silver was
used instead of steel because these electrodes would
later be used as reference electrodes. Two samples of
coating A were used: one with a failure of 0.36 cm2
placed at the centre of the coupon and another with-
out failure. Aiming at the ageing of these samples,
ÿ1.43 Vsce was applied on the sample with failure and
ÿ10 Vsce on the one without failure. After 15 days the
polarisation was interrupted and after 12 h without
polarisation several measurements were performed as
described in the following. The open circuit potential
of each silver electrode was measured in relation to an
external sce. It was observed that in the sample with-
out failure, Fig. 4, only the electrodes 1, 2, 4 and 6, as
well as the steel one, exhibited steady-state values of
potential. This means that these areas had electroche-
mical contact with the bulk solution. At the areas of
electrodes 3, 5, 7 and 8 there was no contact and the
potentials could not be measured. In the case of the
sample with failure, only electrodes 1, 4, 5, 7 and 8
exhibited steady-state potentials, as shown in Fig. 5.
The impedance diagrams of each one of the silver elec-
trodes with steady potentials are also shown in Figs. 4
and 5. It can be seen that each local spot presents a
di€erent characteristic impedance which is a compro-
mise between the local coating impedance and the
behaviour of the respective silver electrode in each
electrolyte formed under the paint. This aspect is
exempli®ed in Fig. 6 where impedance diagrams
obtained for a silver electrode (without coating) in
di€erent electrolytes and potentials are presented. The
electrolytes consisted of chloride solutions with
pH = 6, Fig. 6(a), and an alkaline solution pH = 14,
Fig. 6(b), aiming at the simulation of the changes in
the electrolyte caused by the cathodic currents at the
silver/coating interface. Concerning the applied poten-
tials, Fig. 6(c), they were chosen based on the steady
values shown in Figs. 4 and 5.
In NaCl pH = 6, Fig. 6(a), it can be seen that the
diagram presents one loop centered at 0.1 Hz which
increases with immersion time. With respect to the
e€ect of pH, Fig. 6(b), it can be seen that two loops
are obtained just after the immersion and 24 h later
two loops are still present, but the one at high frequen-
cies (2.5 kHz) is very small. The presence of this loop
is better seen on an expanded scale in Fig. 6(b).
Concerning the silver behaviour in di€erent poten-
tials, Fig. 6(c), it is possible to see that the loop
detected in low frequencies, Fig. 6(b), tends to dimin-
ish and the loop in high frequencies disappears.
In conclusion to Fig. 6, it is possible to state that
the behaviour detected in Figs. 4 and 5 represents a
complex coupling between the silver electrodes in the
di€erent electrolytes present in the occluded cells
formed underneath the paint. From a qualitative point
 I.C.P. Margarit, O.R. Mattos / Electrochimica Acta 44 (1998) 363±371 367

Fig. 4. Impedances and potentials measured for the steel (total) and for the silver electrodes. External saturated calomel reference
electrode. Sample without intentional failure.

Fig. 5. Impedances and potentials measured for the steel (total) and for the silver electrodes. External saturated calomel reference
electrode. Sample with intentional failure.
368 I.C.P. Margarit, O.R. Mattos / Electrochimica Acta 44 (1998) 363±371
Fig. 6. Impedances of a silver electrode measured in a classi-
cal three electrodes cell in di€erent experimental conditions.
Scales in O. (a) 3.5% NaCl solution pH = 6 at open circuit
potentials: +, just after immersion (E OC = ÿ0.25 Vsce); w,
24 h later (E OC = ÿ85 mVsce); (b) 3.5% NaCl solution
pH = 14 at open circuit potentials: +, just after immersion
(E OC = ÿ1.14 Vsce); w, 24 h later (E OC = ÿ1.22 Vsce); (c)
3.5% NaCl solution pH = 14 at di€erent applied potentials:
+, E = ÿ0.23 Vsce; w, E = ÿ0.12 Vsce).
of view, it is even possible to identify some diagrams
in Figs. 4 and 5 with similar features to those given in
Fig. 6. However, the possibility of detecting the impe-
dance of the processes occurring at the silver electrode
surface underneath the coating will be determined by
the local impedance of the coating, as will be discussed
later in this paper.
In Fig. 7, the same sample analysed in Fig. 4 is rea-
nalysed by impedance taking the silver electrodes as
references. These results pin-point di€erent electroche-
mical activities of the steel in each place, which can be
explained by the di€erences on the electrolyte at the
coating/metal interface.
After the impedance measurements, a new polaris-
ation of the system began. The steel potential, in re-
lation to an external sce, was diminished in steps of
200 mV (cathodic polarisation), waiting for the stabilis-
ation of the global current. At this time, the new po-
tential of each electrode E i was read again. These
results are shown in Tables 2 and 3.
In the ®rst row of Tables 2 and 3, the open circuit
potentials (E OC) measured for each electrode (Figs. 4
and 5) are repeated in brackets. From Tables 2 and 3
and from Figs. 4 and 5 it is possible to conclude that
the value of the potential and the impedance are local
functions, varying from region to region. These results
con®rm the concept of ``D'' and ``I'' areas introduced
by Mayne [10] for a barrier paint.
From Tables 2 and 3 it can be observed that when-
ever the polarisation level (E ÿ E OC) of the steel is
changed, the polarisation level at spots i also changes,
but not homogeneously. The local properties of the
coatings, which will de®ne the level of the current pas-
sing through these points, determine the polarisation
level. Then, it is impossible to maintain the local polar-
isation level necessary for cathodic protection, es-
pecially considering that at these points the open
circuit potential will change in consequence of the
polarisation which will imply changes of the electro-
lyte. These changes were indirectly con®rmed by the
diagrams presented in Figs. 4±6 for the silver electro-
des and in Fig. 7 for steel.
As a way of validating the feasibility to measure the
impedance by an internal reference, the experiments
presented in Fig. 8 can be analysed. Fig. 8(a)±(e) were
obtained with the experimental arrangements schemati-
cally indicated on the same ®gure. Fig. 8(a)±(c) were
obtained from a ®lm of low resistance and Fig. 8(d)±
(e) from a more resistant one. Fig. 8(b) and (c) were
obtained with the ®lm separating the auxiliary elec-
trode from the working one (steel). In both cases, the
impedance of the steel was correctly measured.
Fig. 8(a) and (d) are the classical four electrode
measurements giving the ®lm impedance. For Fig. 8(c)
and (e) the auxiliary and reference electrodes were sep-
arated from the steel by the painting ®lm. As illus-
trated, when the coating has important defects [low
impedance, Fig. 8(a)], the measured impedance is able
to detect Faradaic processes occurring on the steel sur-
face, being a coupling of the coating and the steel.
Indeed, in Fig. 8(c) the Faradaic process occurring in
the Hertz range is well detected. However, for higher
impedance ®lms, only the coating is measured and the
Faradaic impedance is hindered by the paint, Fig. 8(e).
The results presented in Fig. 8 not only justify the
measurements made in Fig. 7, where the silver electro-
des were used as references underneath the paint, but
also show the diculties of detecting Faradaic impe-
dances under high resistant coatings. This last aspect
was better emphasised in two recent papers [11, 12]
and also explains the diculty of having the same dia-
grams when one compares Figs. 4 and 5 with Fig. 6.
Further analysis concerning Figs. 4 and 5 can still
be done. Comparing the impedances of the electrode,
E1, of the sample with failure (Fig. 5) with E6 of the
sample without failure (Fig. 4), it can be observed that
these two regions have identical impedances.
Nevertheless, for the sample with failure, compared to
the sample without failure for a given polarisation
level, the total current that ¯ows is higher because of
the metal exposure (Tables 2 and 3). Then, polaris-
ation at E1 is more important than at E6. Indeed for
 I.C.P. Margarit, O.R. Mattos / Electrochimica Acta 44 (1998) 363±371 369

Fig. 7. Impedances of the steel coated with A obtained with the silver electrodes as local references. Sample without failure.

200 mV of polarisation level on the steel, E6 is
polarised by 33 mV while E1 by 125 mV. From this
result it is understandable why in the presence of a
failure with metal exposure, beyond the delamination
around the failure, blisters tend to appear far from it.
Instead of what would be expected, the electric ®eld is
not totally concentrated in the area of the metal ex-
posure. There is a parcel which still in¯uences other
weak areas of the coating. So, if there is a failure with
metal exposure, higher currents ¯ow in the system,
which cause higher polarisation at weak areas of the
coatings, which then cause speci®c changes of electro-
lyte at the coating/metal interface and the appearance
of blisters. The above results also raise a discussion
about the diculty in establishing cathodic protection
criteria for metals in the presence of an organic
coating.
3.3. Cathodic protection criteria
In a previous work [8] the validity of the potential
ÿ0.78 Vsce [13] to assure cathodic protection on coated
steel was questioned. In that work, the variation of the
open circuit potential of samples with or without inten-
tional failures was monitored during and after pro-
longed cathodic polarisation. It was shown that the
open circuit potential of the system changed to more
cathodic values after the polarisation e€ects and it was
dependent on the size of the failure and on the nature
of the coating. Based on these results and on the

Table 2. Cathodic polarisation of steel with respective polarisation levels (Eÿ E OC)i at spots i measured in relation to an external
saturated calomel reference electrode. Sample without failure

(Eÿ E OC)steel (mV), (E ÿ E OC)1 (mV), (Eÿ E OC)2 (mV), (Eÿ E OC)4 (mV), (E ÿ E OC)6 (mV),
E OC = ÿ1.01 Vsce E OC = ÿ 0.14 Vsce E OC = ÿ0.18 Vsce E OC = 0.00 Vsce E OC = ÿ0.002 Vsce

200 107 129 163 33

400 212 280 312 68
600 369 440 463 104
800 533 609 621 150
1000 678 776 769 178
370 I.C.P. Margarit, O.R. Mattos / Electrochimica Acta 44 (1998) 363±371

Table 3. Cathodic polarisation of steel with respective polarisation levels (Eÿ E OC)i at spots i measured in relation to an external
saturated calomel reference electrode. Sample with failure

(Eÿ E OC)steel (mV), (Eÿ E OC)1 (mV), (E ÿ E OC)4 (mV), (E ÿ E OC)5 (mV), (Eÿ E OC)7 (mV), (E ÿ E OC)8 (mV),
E OC = ÿ0.71 Vsce E OC = ÿ0.12 Vsce E OC = ÿ0.14 Vsce E OC = ÿ 0.12 Vsce E OC = ÿ0.05 Vsce E OC = ÿ0.23 Vsce

200 125 42 58 55 174

400 247 85 101 108 351
600 375 126 172 210 526
720 434 223 218 284 641

measurements analysed in Section 3.2, a more wide
discussion concerning criteria for cathodic protection
on coated structures can be developed.
Actually every coated structure has defects, with or
without metal exposure. Although assured in every
point of the structure by a well distributed electric
®eld, certi®ed by the solution of the Laplace equation
for the potential distribution, the criterion of a ®xed
potential value cannot guarantee the cathodic protec-
tion along time, as previously shown [8]. Another cri-
terion proposed in the literature, which seems
interesting, is to decrease the potential to maintain a
minimum local polarisation at the areas of failure.
Nevertheless, this criterion is not feasible and under
some aspects it is dangerous. The polarisation will be
minimum only in the areas where the potential had
changed signi®cantly, in other areas it would favour
the hydrogen reaction increasing the failure. As a con-
sequence, with the increase on the delaminated areas,
the assurance of a local minimum polarisation level
would have to take into account the changes on the
open circuit potential and, at the same time, the fea-
tures of the coating, which are responsible for the elec-
tric ®eld distribution in these areas.
Summarising the study, it was shown that the cri-
teria usually applied to assure cathodic protection on
bare steel have limitations when applied to coated
steel. The use of the special samples with electrodes at
the coating/metal interface not only con®rmed the
existence of weak areas on the coatings, but also
showed that the coating/metal interface is hardly equi-
potential. Similar samples have been used before [14]
and with them new perspectives for the research and
characterisation of coatings have been opened. As

Fig. 8. Impedances measured with di€erent arrangements of the electrodes in a cell with two compartments separated by ®lms of
coating A. Scales in O.
 I.C.P. Margarit, O.R. Mattos / Electrochimica Acta 44 (1998) 363±371
there is no criteria to guarantee the cathodic protection
in delaminated areas of a coating, these areas must be
detected for repair. Direct inspection is mostly unfeasi-
ble. An alternative is an indirect non-destructive
method like impedance. The possibility of using elec-
trochemical impedance as a monitoring technique for
coatings and cathodic protection performance has been
discussed elsewhere [11].
4. Conclusions
It was shown that an improvement of laboratory
procedures for coating selection can contribute to the
development of coating/cathodic protection technol-
ogy. Each coating presents particularities that must be
known. Among coatings characterised by very high
impedances, which are normally used coupled with
cathodic protection, the coating with the highest impe-
dance is not always the most suitable. Indeed a mini-
mum of permeability is required to minimise the e€ects
of the OH ÿ generated by the cathodic reaction. From
the tests used it can be outlined which ones performed
with a distinct dimension of failures as complementary
to the conventional measurements as proposed by
ASTM and also the placement of electrodes on the
metal/coating interface, that will undoubtedly improve
the knowledge of physico-chemical processes in the
coatings. The experimental results allowed us to state
that the metal/coating interface is not equipotential
and the usual criteria applied to assure cathodic pro-
tection on bare steel are not valid in the presence of a
coating. It was shown that the existence of failures,
with or without metal exposure, will lead to a situation
where the traditional criteria fail, regardless of the
quality of the cathodic protection design.
371
Acknowledgements
The authors are grateful to Joaquim Pereira
Quintela from Petrobras for his technical support and
to CNPq, CAPES and FINEP for their ®nancial assist-
ance. The authors also thank Dr H. Takenouti for
fruitful discussions and the referee whose remarks
allowed us to improve the text.
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