Critical Evaluation of International Cathodic

Disbondment Test Methods

Benjamin T. A. Chang
(PolyLab LLC Houston, Texas)
Ole ystein Knudsen
(SINTEF Materials and Chemistry, Norway)
Dennis Wong, Jiri Holub
(ShawCor Toronto, Ontario, Canada)
Amal Al-Borno
(Charter Coating Service (2000) Ltd. Calgary, Canada)
J. Alan Kehr
(3M Austin Center Austin, TX)
Pipe laying is often not conducted under the most ideal of conditions
pipe-to-soil
Voltage meter
With attached
Reference cell
 Cathodic Disbondment (CD) resistance is always on the top of
the coating property list required by end users.

At least 22 International and national standard test methods

are available that evaluate the resistance to CD

There is no universal agreement on which standard to use

Test parameters vary over a wide range among the various

test standards
Review of Selected CDT Standard Methods

Voltage Temperature Solution Duration

Standard [V] [C] [aqueous] [days]
CSA Z-245 1.5 or 3.5 V Selection 3 % NaCl Selection
ASTM G8 1.5 RT Triple salt Selection
ASTM G42 1.5 Selection Triple salt 30
ASTM G80 1.5 RT Triple salt 60
ASTM G95 3.0 RT 3 % NaCl 90
ISO 15711 1.05 RT Sea water 182
AS 3862 3 mA Selection 3 % NaCl Selection
NF A 49-711 1.5 Selection 3 % NaCl Selection

Notes: 1. Selection means multiple choices.

2. Triple salt solution is 1%/1%/1% of NaCl/Na2CO3/Na2SO4.
 CD Results on Coating and Coating

Current Temp. Duration Disbondment [mm]

Standard [mA] [C] [days] Coating Coating
CSA Z-245 5-7 65 28 2-4 11 - 14
ASTM G8 20 - 25 RT 30 2 6
ASTM G42 40 - 55 65 30 4-5 8 - 14
ASTM G80 20 - 25 RT 60 2 6
ASTM G95 25 - 30 RT 90 5 15 - 25
ISO 15711 0.9 1.1 RT 182 7.5 13.5
AS 3862 3 mA 65 28 2-3 10 13.5
NF A 49-711 3-5 65 28 2.5 - 3 5-6
Notes:
1. The current draw corresponds to one sample being tested
2. The coatings were 800 to 900 m
3. CD tests were run with two 2-component liquid epoxy materials
 To develop a basis for a new international
standard for a cathodic disbondment test
method.

NACE has formed a Technical Exchange Group, TEG

#349x to investigate the effect of different test
parameters on test results and document the results to
assist the development of a new international standard.
This paper is a status report on the progress made by
the committee members of TEG #349X with the
objective states above .
1. Oxygen Concentration in the Electrolyte
2. Electrolyte Type and Concentration
3. Applied Potential
4. Dry Film Thickness
5. Test Duration
6. Pre-treatment of the Substrate and Surface Profile
7. Effect of hypochlorite
8. Effect of Temperature
9. Specimen Configuration Flat and Curved Steel
10. Holiday Size
11. Holiday Shape Cone or Straight Hole
12. Specimen Orientation
13. Selection of Reference Electrode and Its Calibration
 Oxygen concentration
1200
Note:
Dissolved oxygen 1000

Disbonded area [mm]

Oxygen
concentration in the
800
electrolyte affects the
disbonding rate 600
Specifically the disbonding
rate increases with 400
Air
dissolved oxygen content
200
Nitrogen atmosphere Nitrogen
resulted in much reduced 0
disbondment 0 25 50 75 100
Hours
 Electrolyte solutions used in the CD test:
synthetic seawater
mixed salt solution
NaCl solution
The 3% by weight NaCl solution is considered the
most suitable electrolyte solution.
The NaCl solution offers high conductivity and does
not form any calcareous deposit film on the metal
surface.
 Formation of Calcareous Deposits
400
350
Current density (mA/cm)

300
250
200
150
100
50
0
0 20 40 60 80
Days

Reduction in cathodic current density with time for steel samples exposed
in natural seawater polarized to -1050 mVSCE at 10C
 Effect of Cation

The rate of disbonding depends on the type of cation in the

electrolyte. Disbonding was proportional to the molar
conductivity of the cations.

The anions normally have little effect on the disbonding rate.

Disbonding rate is a Function of Applied Potentials

Linear relationship 4.5

between applied 4.0
potential and the

Disbonding rate (mm/h)

3.5
disbonding rate.
3.0

The charge transport 2.5

through continuous 2.0

coatings was found to 1.5

increase with increasing 1.0

R2 = 0.7242
cathodic potential. 0.5

0.0
-1500 -1300 -1100 -900 -700 -500
Potential mV SCE
 Dry Film Thickness
Disb. distance vs. coating thickness

6
Disb. distance [mm]

0
0 200 400 600 800 1000 1200 1400
Coating thickness []

For thin film coatings the disbonding rate was reported to decrease
almost linearly as the DFT increased up to 100 m
 Dry Film Thickness

Cathodic disbonding depends on transport of some

reactants through the coating film.

Thicker film slows the permeation of reactive

species and the cathodic disbondment rate.

The DFT of the test specimen should be clearly

recorded in the test report.
 Test Duration

Cathodic disbondment increases with test time.

Disbonded area is proportional to test time.

12 weeks vs. 28 days : Longer test duration is highly

recommended because cathodic blistering is more
likely to be observable with the longer test
Pre-treatment of the Substrate and Surface Profile
Surface profile and pre-treatment have significant impact on
cathodic disbondment.
The disbonding rate was found to decrease with increasing
surface roughness
Surface Pre-treatment: Phosphating the surface decreased the
disbonding significantly.

The steel surface profile shall be specified by the coating

manufacturer and in the range of 2.0 to 4.0 mil (50-100 m).

The surface profile and cleanliness shall be clearly recorded in

the report.
 Effect of hypochlorite

Anode Reaction:
2 Cl- Cl2 + 2 e-

Cathode Reactions:
2 H2O + 2 e- 2 OH- + H2
O2 + H2O + 2e 2 OH

Hypochlorite Formation:
Cl2 + 2 OH- H2O + Cl- + ClO-

Not normally seen in Field because of separation of anode from

cathode (holidays in the pipeline coating)
 Effect of hypochlorite
For Laboratory Testing:
Anode Isolation Effect of ClO- concentration on Rate of Delamination

affects hypochlorite 6

concentration 5

Refresh the
Rate of Delam. [m/day]
4

electrolyte solution
3
at least every 28 Coating
Coating

days 2

For smaller cell 1

sizes, weekly 0

changing of 0 1 2 3 4 5
Concentration [g/liter]
6 7 8

electrolyte solution
is necessary
 Effect of Temperature

Cathodic disbondment increases with temperature

For Laboratory Testing

Qualification Tests, maximum service temperature, RT and/or
65 C to be optional

Comparative coating performance, RT and/or 65 C

Testing >100 C, the electrolyte shall be cooled down to 95 C

 Specimen Configuration Flat and Curved Steel

The specimen Specimen Cathodic

Coating Diameter/Curvature Disbondment
curvature had Material
no significant mm inch mm
effect on CD Flat Flat 3.0
suggesting that Coating 114 4.5 3.0
flat or cylindrical (800-900 m) 60 2.2 3.1
samples can be 20 0.8 2.9
used for CD Flat Flat 11.0
testing. Coating 114 4.5 11.0
(800-900 m) 60 2.2 12.0
20 0.8 10.0
 Holiday Size
Two holiday sizes, 1/8 (3 Cathodic
Size Current, mA
mm) and (6 mm) are in Coating Disbondment
Material
common use for CD testing Inch (mm) Initial Final mm
The holiday size made no 1/8 (3.2)
significant difference to the 3.5 11.8 3.0
Coating 1/8 (3.2)
CD test results 3.6 8.2 2.0
(800- (6.4)
For thicker DFT specimens, 900m) 12.2 29.0 3.0
the hydrogen gas bubbles (6.4)
9.1 25.0 2.0
may be trapped at the 1/8 (3.2)
smaller size holiday 3.2 4.6 10.5
Coating 1/8 (3.2)
It is recommended to use (800-
3.0 7.2 13.5
(6.4)
only one holiday size of 6 900m)
12.3 27.4 12.0
mm for all coating (6.4)
11.7 23.1 12.0
specimens for the CD
CD test results (-1.5 V, 65C, 28 days)
 Holiday Shape Cone or Straight Hole

Two popular ways Cathodic

Coating Size Current, mA
Disbondment
to drill the holiday Material
Shape

using either flat mm Initial Final mm

head end mill or Flat 3.2 6.7 10.2 2.0
cone shape drill bit Cone 3.2 7.0 10.7 3.5
Coating
Flat 6.4 20.6 26.0 4.0

There was no Cone 6.4 11.9 20.4 4.0

Flat 3.2 4.0 5.7 17.0
significant
Cone 3.2 6.4 11.0 15.0
difference between Coating
Flat 6.4 15.3 29.1 17.0
the straight and
Cone 6.4 15.1 22.6 13.0
cone shape holiday
CD test results (-1.5 V, 65C, 28 days)
 Specimen Orientation

There are generally two orientations that can be used

in the CD test; horizontal or vertical:

There is no significant difference for the specimen

orientation as long as the hydrogen gas bubbles
escape freely and are not trapped at the holiday
Selection of Reference Electrode and Its Calibration

Cu/CuSO4: up to 57 C
Calomel: 60 C
Ag/AgCl: up to 90 C

Note that the accuracy of the electric potential measured by the

reference electrode shall be checked.
 CONCLUSIONS
The disbonding rate increases with dissolved oxygen content.
The rate of disbonding depends on the type of cation in the
electrolyte.
The anions normally have little effect on the disbonding rate.
CD increases with decreased (more negative) potential.
Thicker film slows the permeation of reactive species and the
CD rate.
Disbonded area is proportional to test time.
Surface profile and chemical treatment affects cathodic
disbonding rate.
Hypochlorite formation in test attacks the coating.
 CONCLUSIONS
Cathodic disbondment increases with temperature.
The specimen geometry has no impact on the cathodic
disbondment.
The holiday size variation of 3 6 mm has no impact on
CD.
Cone or straight shaped holiday has no influence on
cathodic disbondment.
There is no significant difference for the specimen
orientation (flat or vertical)
Ag/AgCl reference electrode is recommended
.
RECOMMENDATIONS
# Test Parameter
1 Dissolved Oxygen
Concentration in the
Electrolyte
2 Electrolyte Type and
Concentration
3 Applied Potential
4 Coating Dry Film Thickness
5 Test Time
6 Surface Pre-treatment and
Surface Profile of Substrate
Test Condition
Equilibrium solubility of oxygen in the
electrolyte solution at the test temperature
3% by weight NaCl in DI water solution
-1.5 VDC for buried pipeline coating and -1.0
VDC for offshore / marine structures,
measured by Ag/AgCl reference electrode
DFT shall be specified by the coating
manufacturers for the specific field
application.
12 weeks at maximum service temperature
and 28 days (4 weeks) at room temperature
(optional)
The surface cleanliness and surface profile is
very important and must be recoded.
 RECOMMENDATIONS
# Test Parameter
7 Effect of hypochlorite
8 Test Temperature
9 Specimen Geometry
10 Holiday Size
11 Holiday Shape Cone or Cone shaped drill bit to prepare holiday
Straight Hole
12 Specimen Orientation
13 Reference Electrode and
Calibration
Test Condition
Anode Isolation
Changing the electrolyte solution
Maximum service temperature and room
temperature and/or 65 C (optional).
Above 100 C, the electrolyte temperature
shall be cooled to 95 C.
Specimen can be either flat, curved panel or
tube.
6 mm
Specimen can lay flat horizontally with the
attached cell or hang vertically in the bath.
Cu/CuSO4, Calomel, or Ag/AgCl (latter
recommended) can all be used in their
allowable temperature range.
 Acknowledgements

Thanks to members of NACE Technical Exchange

Group TEG#349X for their valuable discussions
on the evaluation of test parameters used in
cathodic disbondment test methods.