2009

Journal of ASTM International, Vol. 6, No.
3
Paper ID JAI101246
Available online at www.astm.org
Sankara Papavinasam,1 Michael Attard,1 and R. Winston Revie1
Electrochemical Impedance Spectroscopy Measurement

during Cathodic Disbondment Experiment of
Pipeline Coatings
ABSTRACT: Modified cathodic disbondment 共CD兲 experiments were carried out over a period of 14 months
using 13 coatings used to protect the external surfaces of oil and gas pipelines. During the experiments,
electrochemical impedance spectroscopy 共EIS兲 data were recorded, and after the experiments the cathodic
disbondment area was measured. From the EIS data, the increase in coating capacitance was determined.
Based on the comparison of coating capacitance values obtained from EIS data with the cathodic disbond-
ment data, the coatings were broadly divided into three types: 共1兲 high-performance coatings that did not
disbond despite increasing coating capacitance; 共2兲 poor-performance coatings that disbonded more than
predicted from the increase in coating capacitance; and 共3兲 average-performance coatings that disbonded
at a rate proportional to the increase in coating capacitance.
KEYWORDS: electrochemical impedance spectroscopy, pipeline coating, cathodic disbondment, fu-
sion bonded epoxy, oil and gas, pipelines, FBE
Introduction
Coatings are the first line of defense against corrosion of pipelines; if they fail, cathodic protection 共CP兲
should act as a back-up. Over the past 60 years, the pipeline industry has used several coatings including
asphalt, coal tar, epoxy, fusion-bonded epoxy 共FBE兲, polyethylene, and urethane coatings 关1兴. The type of
coating on a pipe has an effect on the formation of the environment that causes corrosion and stress-
corrosion cracking 共SCC兲.
As long as pipeline coatings are intact and completely insulate the pipeline from the surrounding
environment there should be no corrosion, but during service, coatings undergo changes that affect their
ability to insulate the pipeline from its environment. Any change in the chemical, physical, or electro-
chemical properties of external pipeline coatings can be considered as a failure. Some failures are cata-
strophic, whereas others have no or little effect on the coating performance. The eight most common
modes of failure of external polymeric pipeline coatings have been ranked in order of the impact of their
failure on the protection of the pipe 关2兴.
Many test procedures have been developed to evaluate protective coatings and standards have been
developed by various organizations for these tests. In previous papers, the historical perspectives of
coating evaluation have been reviewed; laboratory methodologies and their significance have been dis-
cussed; standards from various standards-making organizations for testing a particular property have been
compared; opportunities for harmonizing standards have been identified; and areas for developing new
methodologies to evaluate coatings have also been identified 关3–6兴. Among the various tests in use, the CD
test is the most frequently used. This test establishes the compatibility between the coatings and cathodic
protection. A number of standards have been developed to perform this.
The objectives of this paper are to modify the CD test to record EIS data, and to correlate the EIS data
obtained during the test to the cathodic disbondment area measured after the test.
EIS Measurement of Polymeric Coatings

Electrochemical impedance spectroscopy has been used extensively as a laboratory-based research tool for
studying the performance of polymeric protective coatings 关7–89兴. EIS measurements have also been used
Manuscript received May 19, 2007; accepted for publication January 26, 2009; published online March 2009.
1
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2 JOURNAL OF ASTM INTERNATIONAL
to attempt to monitor coatings in various industrial environments 关28–35兴. It is claimed that EIS provides
information that is valuable in planning maintenance of coatings. A protective organic coating impedes
electrical transport between anodic and cathodic sites on the metal surface. Measuring the electrical
resistance of a protective organic coating provides a means of determining its ability to protect the
underlying metal from exposure to corrosive environments.
In earlier days, the electrical resistance of a coating was used to determine its corrosion protection
tendency. Later, coating capacitance, determined at a single audio frequency, was used to obtain informa-
tion on its corrosion protection tendency. The long-term performance of a coating was predicted from the
initial rate of increase in the coating’s capacitance. Since the 1970s, the electrical and electrochemical
responses of coatings were measured at various frequencies to evaluate their corrosion protection tenden-
cies 关7–9兴.
Typically during EIS measurements, the impedance 共Z兲 is measured at different frequencies by apply-
ing an ac potential and measuring the resultant current. The results are presented as Bode or Nyquist plots.
In Bode plots, Z, or the phase angle 共␪兲, is plotted as a function of log ␻, where ␻ is the frequency in rad/s.
Impedance consists of real and imaginary components. In a Nyquist plot, the real and the imaginary
components are plotted against one another. The EIS results are typically analyzed using an equivalent
circuit 共EC兲 model. Typical equivalent circuits, types of samples, amplitudes of ac potentials, frequency
range in which measurements are made, types of EIS plots, and nature of information obtained are
presented in Table 1.
An EC model that is widely used to analyze EIS data of a coated metal is shown in Fig. 1. Using this
EC, the coating capacitance 共Ccoat兲, double-layer capacitance 共Cdl兲, polarization resistance 共Rcorr兲共in-
versely proportional to corrosion rate兲, pore resistance 共Rcoat兲, and solution resistance 共Rs兲 are determined
关11–30兴. At the higher frequencies, Rs limits Z. Below a frequency of 106 rad/ s, Ccoat dominates the
measurement, and in this frequency range Z = 1 / ␻Ccoat. At frequencies between 103 to 105 rad/ s, Z ⬃ Rs
+ Rcoat. Below 103 rad/ s frequnency, Cdl dominates the measurement and in this frequency range Z
= 1 / ␻Cdl. Below 102 rad/ s frequency, Z ⬃ Rcorr + Rcoat + Rs.
EIS analysis of a coating on a metal surface can be performed by several methods. Some of them are
discussed in the following paragraphs.
Method 1
The impedance of a coating is measured at 0.1 Hz to evaluate its properties 关27兴.
• An excellent barrier coating has an impedance of 109 ohm/ cm2 or higher;
• A coating with capillaries has an impedance between 107 and 109 ohm/ cm2;
• A coating with pinholes has an impedance between 107 and 105 ohm/ cm2; and
• A coating with large holidays has an impedance less than 109 ohm/ cm2.
Method 2
The impedance of a coating with no defect has no real component. As the coating starts to develop defects,
the real component starts to contribute to the impedance by forming ionically conducting paths across the
coating between the electrolyte and the metal. Establishment of ionically conducting paths is represented
in the EIS plot by shorting of Ccoat by Rcoat 关14–17兴.
Method 3
When a coating absorbs water, its dielectric constant, ␧, increases. Because the dielectric constant of the
water phase is about 20 times that of the polymeric coating, the change in ␧ is pronounced. For low
volumes of water, ␯, assuming uniform distribution of water in the coating:
␧t Ccoat,t
= = 80␯ 共1兲
␧o Ccoat,o
where Ccoat,o is the initial coating capacitance, Ccoat,t is the coating capacitance at time t, ␧o is the initial
dielectric constant, and ␧t is the dielectric constant at time t 关50兴.
PAPAVINASAM ET AL. ON EIS MEASUREMENT TECHNIQUE 3
TABLE 1—EIS models for analyzing the degradation of polymeric coatings.
Equivalent Results Presented As

Amplitude Circuits Bode Bode
of ac 共Standard EC Plot Plot
Working Potential, Frequency Range, is Presented Nyquist 共␪ vs. 共log Z Information
Electrode mV Hz in Fig. 1兲 Plot log f兲 vs. log f兲 Obtained Reference
Not described 6.5⫻ 104 – 107 Rcoat and Ccoat ⫻ 关8兴
Standard and a
Not described 103 – 105 ⫻ Water-uptake 关13兴
complicated EC
Not described 107 – 5 ⫻ 108 Water-uptake 关34兴
Not described Standard ⫻ Delamination 关7兴
Not described 5 or 10 10−1 – 105 Standard ⫻ ⫻ 关43兴
Not described 100 10−1 – 105 关45兴
Coated specimen 106 – 107 Standard ⫻ Water-uptake 关42兴
Coated specimen 5 10−1 – 106 Standard+ Zw ⫻ Permeation 关41兴
Coated Diffusion and
10−1 – 106 Standard ⫻ ⫻ ⫻ 关50兴
specimen water-uptake
Coated specimen 10 or 20 107 – 6.5⫻ 107 Standard ⫻ Water-uptake 关51兴
Coated specimen 20 10−2 – 6 ⫻ 104 ⫻ ⫻ Corrosion resistance 关14兴
1, 2, 10,
Coated
60, and 10−3 – 104 Standard ⫻ ⫻ Disbondment 关12兴
specimen
500
Coated specimen 10 104 – 106 Standard ⫻ ⫻ Corrosion activities 关51兴
Coated specimen 50 10– 104 Standard+ Zw ⫻ Delamination 关52兴
Sensor attached to
10 5 ⫻ 106 – 108 ⫻ Coating degradation 关54兴
the coated specimen
Coated specimen 3 to 10 Standard+ RL ⫻ ⫻ Detemination 关53兴
Standard+ an
Coated specimen 10−3 – 105 additional ⫻ ⫻ ⫻ Moisture content 关55兴
resistance element
Coated specimen 10−3 – 105 Standard ⫻ ⫻ ⫻ Coating defects 关56兴
Coated specimen 10 105 – 106 Standard ⫻ ⫻ Long-term prediction 关61兴
Coated specimen 10−1 – 105 Standard+ Zw ⫻ ⫻ Coating resistance 关62兴
Merits and demerits
Coated specimen 20–50 104 – 107 Not described ⫻ 关63兴
of EIS
Coated specimen 20 5 ⫻ 10 – 10
−1 5
Standard ⫻ ⫻ Influencing factors 关64兴
Coated specimen 200 10−3 – 104 Standard ⫻ Coating degradation 关75兴
Standard and a
Coated specimen Not given 5 ⫻ 106 – 10⫻ 106 ⫻ Water penetration 关76兴
complicated EC
Coated specimen Not given 10−1 – 105 Standard ⫻ ⫻ Water-uptake 关77兴
Coated specimen 10 105 – 106 Standard+ Zw ⫻ ⫻ ⫻ Coating degradation 关78兴
Coated specimen 100 104 – 105 Complicated EC ⫻ Coating adhesion 关71兴
Coated specimen 25 to 100 6.5⫻ 103 – 107 Standard ⫻ ⫻ Long-term prediction 关82兴
Note: Zw = Warburg diffusion impedance, RL = coating resistance.
Method 4
The high-frequency break-point, f h, 共the frequency at which ␪ drops to 45°兲 is used to monitor the coating
关21兴. This break-point frequency occurs because ␻R f Ccoat = 1, when ␪ = 45°. Assuming R f 共film resistance兲
to be equal to Rcoat, f h is a measure of the area of coating disbonded.
Method 5
The Rmax is the sum of all resistances, i.e., Rcorr, Rcoat, and Rs.
• An excellent coating has an Rmax of 108 ohm/ cm2 or higher, and
• A poor coating has an Rmax of 106 ohm/ cm2 or lower 关19兴.
FIG. 1—Standard equivalent circuit.
Experimental
The standard procedures to conduct cathodic disbondment experiments are described in CSA Standard
Z245-20/Z245.21 关11兴. This procedure was modified as described in the following paragraphs to collect
EIS data during the test.
Experimental Chambers
Two chambers, each 2.4 m 共8 ft兲 in length and 1.2 m 共4 ft兲 in height were used. In Chamber A, the
temperature was varied between 5 and 65 ° C 共41 and 149 ° F兲; Chamber B was maintained at 65 ° C.
FIG. 2—Illustration of steel panel and probe orientation.

FIG. 3—Cross section of EIS probe during sample preparation.
Experimental Cell
Figure 2 is a schematic illustration of the design of the coated steel panels and electrode housings. Each
coated sample had four ports—two for EIS measurements, one for an electrochemical quartz crystal
microbalance 共EQCM兲 probe, and one for a pH probe.
For each cell, three types of EIS data were collected—using either the coated steel panel, electro-
chemical probe #1, or electrochemical probe #2 as the working electrode. The counter electrode was a
TABLE 2—Outline of coating application process.
Thickness Required
共Nominal兲 Surface Profile Surface Cleaning Coating Process
Coating 共mm兲共mils兲 Standard Temp. 共°C兲 Coating Standard
Fusion bonded epoxy 共FBE兲 0.4 1.5–4.0 SSPC-SP10/NACE No.2 250 NACE RP0394
2-Layer 3 1.5–4.0 SSPC-SP10/NACE No.3 50—60 CSA Z245.21
3-Layer 4.5 1.5–4.0 SSPC-SP10/NACE No.2 250 CSA Z245.21
Composite 0.8 1.5–4.0 SSPC-SP10/NACE No.2 250 CSA Z245.21
Urethane 共brush兲 0.8 ⬎2.0 SSPC-SP10/NACE No.2 10–100 CSA Z245.20
Urethane 共spray兲 0.6 ⬎2.0 SSPC-SP10/NACE No.2 10–100 CSA Z245.20
Epoxy 共brush兲 0.7 ⬎2.0 SSPC-SP10/NACE No.2 10–100 CSA Z245.20
Epoxy 共spray兲 0.6 ⬎2.0 SSPC-SP10/NACE No.2 10–100 CSA Z245.20
Coal tar 5 2.0–3.0 SSPC-SP10/NACE No.3 246–274 AWWA C203
Tape 0.8 2.0–3.0 No specific requirements 25 No standard
Asphalt 8.5 Coating obtained from an operating pipeline
TABLE 3—Chemical composition of solution used in CD tests.
Chemical Compound Quantity 共mg/L兲

KCl 122
NaHCO3 483
CaCl2 · 2H2O 181
MgSO4 · 7H2O 131
0.51 mm 共0.02 in.兲 diameter, 99.95 % platinum wire. The reference electrode was a gel-filled, epoxy
bodied saturated calomel electrode 共SCE兲. The reference electrode tip was placed directly above the
holiday in the coating.
Specimen and Solution Preparation

Both specimen and probes were made of carbon steel. The specimen was placed test side 共the side on
which coating would be applied兲 down, on a clean, hard, flat surface. High-temperature epoxy was applied
to cover the inside walls of the EIS ports. A ceramic sleeve was then inserted into each port so that the
sleeve protruded through the test side of the specimen. The epoxy was cured in an oven at 150 ° C 共302°F兲
for 20– 30 min.
Figure 3 illustrates a cross section of an EIS probe during sample preparation. From the test side, the
ceramic sleeve end was covered with “Searset” quick-dry cement. The cement was allowed to set for
approximately five minutes, and the specimen was returned to the hard, flat surface, once again with the
test side down. A duct tape was temporarily placed to secure the parts until the cement dried. Using a
syringe, the epoxy was injected into the ceramic sleeves until they were half-full; then a metal electrode
was placed in the sleeve until it touched the quick-dry cement at the opposite end. The epoxy was cured
in an oven at 150 ° C 共302 ° F兲 for 20– 30 min. Finally the ceramic sleeves/metal electrodes were ground
until they were flush with the test surface. The panels were then sent to different coating companies for
application of coatings.
The specific procedures followed in the application of 13 coatings are presented in Table 2. The
composition of the solution used in the CD test is presented in Table 3. A 60-channel Yokogawa DA-100
FIG. 4—Variation of temperature in Chamber A (fluctuating temperature).

FIG. 5—Variation of temperature in Chamber B (constant temperature).
data-acquisition unit applied the potential and recorded the resulting current from the test specimens. It
also recorded the temperature of the chambers.
EIS Measurements
The CP to the specimen to be tested was switched off before recording the EIS data. EIS measurements
were conducted using a Solartron SI 1287 Electrochemical Interface and a Schlumberger SI 1250 Fre-
quency Response Analyzer. They were recorded sequentially in a set of eight cells using a Scribner
FIG. 6—Typical EIS plot (Bode plot—log Z versus frequency).

FIG. 7—Typical EIS plot (Bode plot—phase angle versus frequency).
Associates Inc. Model 314 8-Channel Multiplexer. Before each of the EIS measurements, corrosion po-
tentials were recorded for two hours. EIS measurements were performed at frequencies between 0.01 and
106 Hz.
Post-Mortem Analysis
At the end of 14 months, the temperature in Chamber A was 5 ° C 共41 ° F兲; it was increased to 65 ° C
共149 ° F兲 and held constant for two days to stabilize. This protocol ensured that all the coatings in both
FIG. 8—Variation of cathodic current demand with time of a blistered coating.

TABLE 4—Failure modes of external polymeric pipeline coatings in Chamber A (fluctuating chamber).
% Disbondment As
Predicted from EIS Data Current Current
%
Applied Prior to After Disbondment
Coating Potential Failure Mode Probe Probe Blistering Blistering 共After CD
Type 共V兲 Holiday 共Days兲 Panel 1 2 共mA兲共mA兲 Test兲
Asphalt −0.78 Yes Disbondmenta 100 0.03 0.1 100
−0.78 Yes Disbondmenta … 1.16 0.7 26
−0.93 Yes Disbondmenta 0 0.2 0.1 37
−0.93 Yes Disbondmenta 0.1 0.01 37
Coal tar A −0.78 Yes Blistering 共193兲 0 0.1 0.8 92
−0.78 Yes Disbondmenta … … 36 100
Coal tar B −0.78 Yes Disbondmenta … 0.1 0.1 0
−0.78 Yes Blistering 共304兲 0 0.1 0.4 0.051 0.104 75
−0.93 Yes Disbondmenta … ⬍0.1 ⬍0.1 0
−0.93 Yes Disbondmenta 0 … 0.1 78
Tape −0.78 Yes Wrinklinga 100 0.6 0.9 100
−0.78 Yes Wrinklinga 100 0.1 0.1 100
−0.93 Yes Wrinklinga 100 1 0.1 100
−0.93 Yes Wrinklinga 100 0.1 0.5 100
FBE A −0.78 Yes Blistering 共304兲 … … 0.1 97
−0.78 Yes Blistering 共122兲 … 0.1 0.1 0.000 0.056 51
−0.93 Yes Blistering 共92兲 … ⬍0.1 2.0 35
FBE B −0.78 Yes Blistering 共91兲 … 0.1 … 0.001 0.118 91
−0.93 Yes Blistering 共396兲 0.000 4.497 42
−0.93 Yes Blistering 共334兲 100 0.1 0.1 58
−0.78 No Blistering 共91兲 100 0.1 0.1 68
Liquid −0.78 Yes Discolorationa 100 0.6 0.8 0
epoxy −0.78 Yes Discolorationa 0 0.8 0.1 0
共brush兲 −0.93 Yes Discolorationa 100 0.7 0.1 0
−0.93 Yes Discolorationa 100 0.1 0.1 0
−0.78 No Discolorationa 0 0.1 0.1 0
Liquid −0.78 Yes Blistering 共212兲 … 0.1 0.1 0.001 0.080 0
epoxy −0.78 Yes Discolorationa … 0.1 0.1 0
共spray兲 −0.93 Yes Discolorationa … 0.1 0.1 0
−0.78 No Discolorationa … 0.1 0.1 0
Liquid −0.78 Yes No changea … 0.1 0.1 0
urethane −0.78 Yes No changea … 0.1 0.1 0
共brush兲 −0.93 Yes No changea 100 0.1 0.1 0
−0.93 Yes No changea … 0.1 0.1 0
−0.78 No No changea … 0.1 0.1 0
Liquid −0.78 Yes Discolorationa 100 0.1 0.1 0
urethane −0.78 Yes Discolorationa 100 0.1 0.1 0
共spray兲 −0.93 Yes Discolorationa 100 0.1 0.1 0
−0.78 No No changea 100 0.1 0.1 0
2-Layer −0.78 Yes Disbondmenta … 0.8 0.1 6
−0.78 Yes Coating slippage 共199兲 … 0.1 0.1 100
TABLE 4— (Continued.)
% Disbondment As
%
Coating Potential Failure Mode Probe Probe Blistering Blistering 共After CD
Type 共V兲 Holiday 共Days兲 Panel 1 2 共mA兲共mA兲 Test兲
3-Layer −0.78 Yes No changea … ⬍0.1 ⬍0.1 0
−0.78 Yes No changea … ⬍0.1 ⬍0.1 0
−0.93 Yes No changea … ⬍0.1 ⬍0.1 0
−0.93 Yes Discolorationa … ⬍0.1 ⬍0.1 0
−0.78 No No changea … ⬍0.1 ⬍0.1 0
Composite −0.78 Yes Discolorationa 100 0.1 0.4 0
−0.78 Yes Discolorationa … 0.6 90 0
−0.93 Yes No changea 100 1.8 0.1 0
−0.78 No No changea … 6.6 0.1 0
a
After the experiment during the measurement of disbonded area.
Chambers A and B were at the same temperature when the experiments were concluded. The disbondment
test was conducted according to CSA Z245.20, Sections 12.8.3.6 through 12.8.3.9 关11兴.
Results and Discussion

The temperatures of the chambers over the 14-month period are presented in Figs. 4 and 5. Because most
standard tests are carried out at 65 °C 共149 ° F兲, and because the temperature of most pipelines varies over
time and distance, two sets of experiments were carried out—one at 65 ° C 共149 ° F兲 and another at
temperatures selected on the basis of the annual temperature profile of a transmission pipeline in Canada.
Because 117 samples were to be analyzed using one EIS instrument, only about 7–10 measurements were
made in each cell. The results were analyzed using the equivalent circuit illustrated in Fig. 1, and Ccoat
values were determined and analyzed as described in Method 3.
Because of the nonconductive nature of the organic coatings, the coated metal samples exhibited high
impedances. In fact, the impedance of the system appeared to be far higher than the operating capability
of the instrument used in this investigation; therefore satisfactory EIS measurements could not be obtained
for many of the samples during the first few months. Another reason for this inability to obtain reliable
readings early in the experiments may be the smaller potential amplitude 共10 mV兲 used. In some coatings
共especially thicker coatings兲, larger signals are suggested, but care must be taken to ensure that the system
is linear over the ac potential range and that the potential does not alter the coating-steel interface. It
should also be noted that the coatings investigated in this study were relatively thick 共Table 2兲. Most of the
studies on the application of EIS were conducted on thinner 共up to 0.1 mm thick兲 coatings. In any event,
EIS data were collected only after stable corrosion potentials were recorded. In many of the coatings, the
corrosion potentials hovered around −0.5 to − 0.7 V versus SCE.
Ccoat,o was taken as the maximum value obtained during the first six months of the experiment. This
value was compared with Ccoat,t to determine the percent increase in capacitance values. Ccoat,t was taken
as the maximum value obtained during the final eight months of the experiment. Figures 6 and 7 show
typical EIS plots obtained.
The percent increase in capacitance determined using steel as the working electrode 共panel兲 was far
higher than when either Probe #1 or Probe #2 was used as the working electrode 共Tables 4 and 5兲. When
steel was used as the working electrode, the holiday provides an easy location for water uptake. On the
other hand, when probes placed far away from the holiday were used as the working electrodes water took
longer to reach the probe surface. Another reason for this may be that the surface area of the steel panel
was different than that of the probes. The percent increase determined from the EIS capacitance measure-
ments was compared with the percent disbondment obtained from post-mortem analysis. As can be seen
from Tables 4 and 5 a linear relationship could not be established between cathodic disbondment and EIS
parameters for any of the 13 coatings. Quantitative correlation between coating capacitance and disbond-
TABLE 5—Failure modes of external polymeric pipeline coatings in chamber B (constant temperature).
% Disbondment As
%
Coating Potential Failure Mode Probe Blistering Blistering 共After CD
Type 共V兲 Holiday 共Days兲 Panel Probe 1 2 共mA兲共mA兲 Test兲
Asphalt −0.78 Yes Disbondmenta … 0.1 0.1 100
−0.78 No Disbondmenta … 0.1 0.1 100
Coal tar A −0.78 Yes Disbondmenta … 0.1 0.1 100
Coal tar B −0.78 Yes Disbondmenta 100 0.1 0.1 100
−0.93 Yes Disbondmenta … … … 100
Tape −0.78 Yes Wrinklinga … 0.1 ⬍0.1 100
−0.78 Yes Wrinklinga … 0.1 ⬍0.1 100
−0.93 Yes Wrinklinga 100 0.1 ⬍0.1 100
−0.93 Yes Wrinklinga … 0.1 ⬍0.1 100
−0.78 No Wrinklinga … 0.1 ⬍0.1 100
FBE A −0.78 Yes Blistering 共131兲 100 0.1 0.1 0.003 0.305 91
−0.78 No Blistering 共122兲 100 0.1 0.1 68
FBE B −0.78 Yes Disbondmenta … 0.1 0.1 97
epoxy −0.78 Yes Blistering 共74兲 … 0.1 0.1 0.021 0.080 7
共brush兲 −0.93 Yes Blistering 共197兲 … 0.1 0.1 0.004 0.164 27
epoxy −0.78 Yes Blistering 共304兲 … 0.1 0.1 0.069 0.135 88
共spray兲 −0.93 Yes Blistering 共212兲 … 0.1 0.1 0.031 0.118 100
urethane −0.78 Yes Blistering 共334兲 … 0.1 0.1 0.006 0.423 1
共brush兲 −0.93 Yes No changea … 0.1 0.1 0
urethane −0.78 Yes Blistering 共273兲 … 0.1 0.1 0.073 0.210 61
共spray兲 −0.93 Yes Blistering 共304兲 100 0.1 0.1 0.006 0.226 62
2-Layer −0.78 Yes Coating slippage 共42兲 … 0.1 0.1 100
−0.78 Yes Disbondment … 0.1 0.1 100
−0.78 No No changea … 0.1 0.1 5
TABLE 5— (Continued.)
% Disbondment As
%
Coating Potential Failure Mode Probe Blistering Blistering 共After CD
Type 共V兲 Holiday 共Days兲 Panel Probe 1 2 共mA兲共mA兲 Test兲
3-Layer −0.78 Yes No changea 100 0.1 0.1 0
−0.78 Yes No changea … 0.1 0.1 0
−0.93 Yes No changea 100 0.1 0.1 0
−0.93 Yes No changea 100 0.1 0.1 0
Composite −0.78 Yes No changea 100 0.1 0.1 0
−0.78 Yes No changea … 0.1 0.1 0
−0.93 Yes No changea 100 0.1 0.1 0
a
After the experiment during the measurement of disbanded area.
ment data could not be established for several reasons including: the output parameters from different
probes were different; the probes were located at different points; and EIS probes monitored only one
property, e.g., capacitance change, whereas disbondment data included all effects, including chemical,
electrochemical, and physical 共cutting and pulling the coating兲. The comparison, however, revealed that
good coatings performed well despite water uptake, whereas water uptake facilitated the deterioration of
poor coatings. Based on the results, the coatings could be broadly divided into three types: high-
performance coatings 共three-layer and composite qualified by CSA Z245.21.B1 and CSA Z245.21.B2,
respectively兲 that did not disbond despite an increase in coating capacitance; poor-performance coatings
共asphalt, coal tar, and tape兲 that disbonded more than predicted by an increase in coating capacitance; and
average-performance coatings 共epoxies, urethanes, and FBE兲 that disbonded at rate proportional to the
increase in coating capacitance.
Attempts were also made to correlate other EIS parameters with coating performance. For instance, the
Rmax was determined, as described in Method 5, from the values of Rs, Rcorr, and Rcoat. Rmax was compared
with the cathodic disbondment rate, but no correlation was found for any of the 13 coatings.
Characteristic CP current spikes were observed whenever a coating blistered 共Tables 4 and 5兲. For
example, the CP current of a panel increased on Day 131 共Fig. 8兲 from 0.003 mA to 0.475 mA, remained
high for about ten days, and then decreased to 0.007 mA. Physical observation of that panel on Day 132
showed the formation of blisters 关90兴, but none of the EIS data signaled this behavior. It should be noted
that the frequency at which the EIS measurements were recorded was far less than the rate at which the CP
currents were recorded. Therefore it is reasonable to assume that EIS measurements would have picked up
the information had it been conducted at the time of blister formation.
Summary
• The coating capacitance values obtained from the EIS measurements were correlated with the
cathodic disbondment rates measured after the experiments. Based on the results, it was found that
coating performance can only be qualitatively predicted from an increase in coating capacitance.
• Pipeline coatings can be broadly divided into three types:
• High-performance coatings that do not disbond despite an increase in coating capacitance;
• Poor-performance coatings that disbond more than predicted by the increase in coating capaci-
tance; and
• Average-performance coatings that disbond at a rate proportional to the increase in coating
capacitance.
Acknowledgments
The authors would like to acknowledge the helpful discussions and financial support from the Canadian
Federal Government’s Program of Energy R&D 共PERD兲 and members 共3M Canada, Enbridge Pipelines,
AEC Pipelines, Korea Gas 共KOGAS兲, Reilly Industries, Shaw Pipe Protection, Speciality Polymeric Coat-
ings 共SPC兲, and Trans Canada Pipelines兲 of the CANMET/NRC/Industry Consortium on External Pipeline
Coatings for Prevention of Corrosion and Stress-Corrosion Cracking.
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Journal of ASTM International, Vol. 6, No.

Sankara Papavinasam,1 Michael Attard,1 and R. Winston Revie1

Electrochemical Impedance Spectroscopy Measurement

EIS Measurement of Polymeric Coatings

TABLE 1—EIS models for analyzing the degradation of polymeric coatings.

Equivalent Results Presented As

FIG. 1—Standard equivalent circuit.

FIG. 2—Illustration of steel panel and probe orientation.

FIG. 3—Cross section of EIS probe during sample preparation.

TABLE 2—Outline of coating application process.

TABLE 3—Chemical composition of solution used in CD tests.

Chemical Compound Quantity 共mg/L兲

Specimen and Solution Preparation

FIG. 4—Variation of temperature in Chamber A (fluctuating temperature).

FIG. 5—Variation of temperature in Chamber B (constant temperature).

FIG. 6—Typical EIS plot (Bode plot—log Z versus frequency).

FIG. 7—Typical EIS plot (Bode plot—phase angle versus frequency).

FIG. 8—Variation of cathodic current demand with time of a blistered coating.

Results and Discussion

Appl. Electrochem., Vol. 25, 1995, p. 1143.

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