Corrosion Science 48 (2006) 432–444

www.elsevier.com/locate/corsci

Study on hydrogen absorption of pipeline

steel under cathodic charging
Maocheng Yan, Yongji Weng *

Department of Material Engineering, University of Petroleum, Beijing 102200, China

Received 28 June 2004; accepted 8 January 2005

Available online 12 March 2005

Abstract

The hydrogen electrochemical oxidation method was used to determine the total amount of
hydrogen absorbed by pipeline steels under cathodic charging. The oxidation currents were
obtained for the hydrogen pre-charged specimen maintained at a certain positive potential
in dilute NaOH electrolyte. The area under the current curve demonstrated a relationship with
the hydrogen concentration. Hydrogen concentrations in pre-charged X70 and 16Mn steels
were estimated using this method. It is shown clearly that hydrogen concentration in speci-
mens increase as the applied current density increased, but the sensitivities of different mate-
rials to hydrogen are different. The effect of solution pH and pre-charging time on absorbed
hydrogen is also studied.

2005 Elsevier Ltd. All rights reserved.

Keywords: Pipeline steel; Cathodic charging; Hydrogen absorption; Oxidation; Near-neutral pH SCC

1. Introduction

The electrochemical evolution of atomic hydrogen is the most commonly cathode

reaction in cathodic protection, electroplating and other corrosion processes. In all
cases most of hydrogen atoms may encounter each other and quickly combine to

*
Corresponding author. Tel./fax: +8610 89733454.
E-mail addresses: yan_maoch@sina.com.cn (M. Yan), wengyj@bjpeu.edu.cn (Y. Weng).

0010-938X/$ - see front matter
2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.corsci.2005.01.011
 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444 433

H2 molecules and get off, but a portion of hydrogen atoms enter the metal surface
and remain as individual atoms in metal [1]. However hydrogen absorbed by steels
has a devastating effect on strength and ductility of metal resulting in high risk of
brittle failures, such as hydrogen induced cracking (HIC) and sulphide stress crack-
ing (SSC) [2]. In recent years, hydrogen is also suspected of playing an important role
in the development of near-neutral pH stress corrosion cracking (SCC) observed in
buried pipelines [2–7]. Hence entry of hydrogen in steel has been widely studied by a
variety of methods.
Although many modern technologies, like hot-extraction thermal conductivity
method [8,9], fusion extraction method, vacuum extraction technique [10], gas chro-
matography [11], Barnacle Electrode method [12], and secondary ion mass spectrom-
etry (SIMS) [13], etc. have been used to measure the amount of absorbed hydrogen
in steel, electrochemical methods [14,15], based on oxidizing reduced hydrogen ab-
sorbed in metal, are still powerful tools for their study. One of them, the most widely
used, is electrochemical hydrogen permeation method developed by Devanathan
et al. This method can give the amount of hydrogen passed through the steel using
a double-cell, one cell (the entry side) for hydrogen charging by a cathodic current
method and the other one (the exit side) for the oxidation current measurements.
Quantitative information, such as the diffusion coefficient (D), the steady-state per-
meation rate (i1) and trapping of hydrogen, etc. can be obtained based on the per-
meation curves which give the hydrogen flux versus time. And the charging sub-face
hydrogen concentration C0 was calculated [16] from
i1 L
C0 ¼ ð1Þ
FD
where F is the Faraday constant (=96,487 C mol
1), and L the thickness of the speci-
men (mm).
In the present paper, the hydrogen oxidation current (iH) and the corresponding
quantity of electricity (Q) were used to quantitatively determine the average hydro-
gen concentration in pre-charged pipeline steels.

2. Materials and experimental procedure

2.1. Materials and sample preparation

The materials used in this study were X70 pipeline steel and 16Mn pipeline steel.
The former is low carbon, micro-alloyed high-grade steel, a relatively newcomer as
pipeline material in China. And the latter is the typical material used in many aged
pipelines. Their compositions (in wt%) are presented in Table 1.
X70 specimens were intercepted from a domestic pipeline of spiral welding seam.
And 16Mn specimens were taken from a spiral welded pipe used more than twenty
years in south main line of Sichuan natural gas pipe networks.
The specimens were 1.2 mm thickness and coated with an insulating silicon rubber
on all surfaces except the side that was to operate as working surface, which was
434 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444

Table 1
Chemical composition of X70 and 16Mn steels (wt%)
Steels C Mn Si P S Cu Mo Cr Ti Nb V
X70 0.04 1.76 0.281 0.016 0.001 0.193 0.194 0.058 0.023 0.067 0.001
16Mn 0.16 1.40 0.40 0.02 0.05 – – – – – –

2.5 cm2. The working surface was polished under water with emery paper to 1000
grade and degreased with acetone. Specimens were heat treated at 200 C for 2 h
to outgas any hydrogen.

2.2. Experimental procedure

Specimen was pre-charged with hydrogen in 0.5 M2SO4 solution by impression of

constant cathodic current density ic ranging from 0 to 70 mA cm
2 for 2 h. The pre-
tests showed that 2 h was a sufficient charging time for hydrogen saturation in steels.
On the completion of charging, the specimens were immediately rinsed with 0.2 M
NaOH solution and transferred to an electrochemical chamber contained 0.2 M
NaOH solution, in which the absorbed hydrogen oxidation current curve was mea-
sured. The electrochemical chamber, shown schematically in Fig. 1, consisted of a
glass container equipped with a saturated calomel electrode (SCE) through a salt-
bridge, a platinum foil counter electrode, and the steel specimen as the working elec-
trode. NaOH solution was de-aerated by bubbling nitrogen 1 h before testing and
throughout the test. The specimen potential was controlled at an anodic potential

POTENTIOSTAT

Fig. 1. Schematic diagram of the electrochemical monocell used to obtain hydrogen outgassing current.
 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444 435

+168 mV (SCE) and the resulting anodic current changes with time were monitored.
The background current curves for blank specimens with the same preparation but
without hydrogen pre-charging were also analysed. The hydrogen oxidation current
(iH) given by subtracting the background current from the anodic current for pre-
charged specimen was studied as a function of time.
To evaluate the influence of pH on absorbed hydrogen concentration, X70 spec-
imen were also pre-charged in a series of solutions with different pHs under the same
current density (ic = 35 mA cm
2). The solutions were 5 · 10
5 M H2SO4, tap water,
1 M Na2CO3 + 1 M NaHCO3, with pHs 4.0, 6.2 and 9.3 respectively.
All electrolytes used in the study were prepared with analytical grade reagents
and distilled water. All the experiments were performed at ambient temperature,
18 ± 1 C.

2.3. Hydrogen analysis

Hydrogen exists in the metal only as individual H-atoms and not H2 molecules. In
the act of positive electric field in dilute NaOH solution, the absorbed hydrogen
atoms diffuse out of the steel and are oxidated at the metallic surface, producing
the corresponding hydrogen oxidizing current (iH), according to the reaction
H ! Hþ þ e
The magnitude of oxidizing current is proportional to density of hydrogen atoms on
the metal surface. Based on iH and the corresponding quantity of electricity (Q), ab-
sorbed hydrogen concentration (C) in pipeline during cathodic charging steels was
determined, and the sensitivity of the material to hydrogen damage was evaluated.
Q in Coulomb was obtained by integrating iH with respect to time, namely by calcu-
lating the area under the iH curve. Therefore, according to FaradayÕs law, average
hydrogen concentration C (10
6 mol cm
3) is related to Q by the relation
Q
C¼ ð2Þ
zFv
where F is the Faraday constant (=96,487 C mol
1), v the effective volume of the
specimen (0.31 cm3 in this study), and z the number of electrons (z = 1).
On the other hand, hydrogen dissolved in metals at low concentrations exhibits a
linear relation between the concentration (C) and the half power of the equilibrium
partial pressure of the molecular gas (pH2) called the SievertsÕ law [17]:
1=2
C ¼ SpH2 ð3Þ

where S is the solubility of the hydrogen dependent on temperature. This also sup-
ports the view that hydrogen dissociates when it enters the metal. In some more
severe conditions, the hydrogen atoms may recombine to H2 molecules in microcavi-
ties the growth of which can produce linkage of the cavities and ultimately separa-
tion between grains. Hydrogen gas at a pressure in such separations or cracks is
also consistent with SievertsÕ law for the local hydrogen concentration.
436 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444

In cathodic charging, pH2 is proportional to the steady-state pre-charging current

density (ic) [18]:
pH2 / ic : ð4Þ

In fact, in the study, the concentration of absorbed hydrogen C is uniquely

C / i1=2
c ð5Þ

At this rate, the C–ic curve should be a straight line in log–log scale. Hence, some
figures in this paper were plotted in the log–log grid.
Cathodic charging has been widely used as a highly efficient method for introduc-
ing hydrogen into metals. The hydrogen retention ratio is interesting because it can
give some idea on the relationship between the rate of hydrogen diffusion into the
steel and that of hydrogen recombination on the surface. However, few studies
[19] dealing with this method directly discuss the ratio. In this work, the hydrogen
retention ratio (R) of the pre-charging process is figured out in term of the charge
of absorbed hydrogen (Q) compared with the total charge in the pre-charging pro-
cess (ict0), i.e.
Q
R¼ ð6Þ
ic t0
where t0 is the pre-charging time (2 h in this study). Hence, based on Eqs. (2), (5) and
(6), the hydrogen retention ratio is
R / ic
1=2 ð7Þ
The R–ic curve should also be a straight line with ic in log–log scale.

3. Results and discussion

3.1. Hydrogen oxidation current curves

The anodic current (i) measured in pre-charged specimen comprised the hydrogen
oxidation current (iH) produced by oxidization of the desorbing hydrogen and the
background current (i0), as shown in Fig. 2. The current i0 was determined in the
experiment with the uncharged specimen. Thus the current iH could be resolved eas-
ily. For that it is necessary to form, on steel, an oxide layer which was stable and
not modified by the absorbed hydrogen. The stability of this oxide layer could be
checked by the stability of the passive current. Fig. 3 shows three i curves measured
with the same specimen in the different conditions: curve a was with uncharged spec-
imen, for which a steady current state about 0.34 lA was reached with the formation
of the passive film. Then, the specimen was slightly polished with 600 grade emery
paper and pre-charged 2 h at current density ic = 18 mA cm
2, and curve b was ob-
tained. And after that the specimen was heat treated at 200 C for 2 h to outgas any
hydrogen and curve c was obtained, under exactly the same conditions as curve a.
 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444 437

10

i (µA cm-2)

1
Uncharged, i0
Charged with 18 mA/cm2, i
iH= i-i0

1 10
time (min)

Fig. 2. Evaluation of the hydrogen oxidizing current for X70 specimen.

10

a, Uncharged
8 b, Precharged with 18 mA/cm2
c, After outgased
i (µA cm-2)

0
5 10 15 20 25 30 35 40
time / min

Fig. 3. Reproducibility of steel oxidizing current (i0) for X70 specimen.

Curve c and b largely overlap each other, which indicates that the background
current (i0) of the steel was reproducible and not modified by hydrogen.
Additionally, absorbed hydrogen may affect the anodic current through other
ways, such as accelerating the anodic dissolution [5], decreasing the stability of the
passive film or retarding the passive film formation [20]. But these factors can be
ignored in this study.
438 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444

3.2. Influence of the pre-charging current density on iH, hydrogen concentration

and the hydrogen retention ratio

Some iH curves for X70 and 16Mn steels pre-charged under a series of current
densities are presented in Fig. 4. In all cases, iH for pre-charged specimen decreases
smoothly with time to a minimum constant value which is approximate to the back-
ground current at the corresponding time. The curves also show reproducibility of
the results. It is obvious that the more pre-charging current, the higher iH, the more
quickly oxidation current decays and the longer time to attain steady-state current.
The oxidation current density taken after 10 min of the test, referred to as iH,10, can
be as an index of the current density. As expected, iH,10 increases with increasing
pre-charging current density as shown in Fig. 5. The higher iH,10 is indicative of
the higher hydrogen concentration in 16Mn steel compared to X70 steel under the
same pre-charging conditions.
Hydrogen concentration C obtained using Eq. (2) approximately increases line-
arly with pre-charging current densities in log–log scale, as shown in Fig. 6. The
slope coefficients of the fitting straight lines are 0.491 (for X70) and 0.442 (for
16Mn), both approximately close to the theoretical values 1/2, which shows that
the pre-charging current dependence of CH accords with the SievertsÕ law, i.e. Eq. (5).
The absorbed hydrogen concentration of X70 steel is distinctly higher than that of
16Mn steel at a given, especially a relatively lower than 20 mA cm
2, pre-charging
current density. Under the condition of ic = 2 mA cm
2, the total hydrogen concen-
tration was found to be 0.43 · 10
6 mol cm
3 in X70 steel, and 0.91 · 10
6 mol cm
3
in 16Mn steel, and when ic = 70 mA cm
2, the total hydrogen concentrations are
3.57 · 10
6 mol cm
3 and 4.22 · 10
6 mol cm
3, respectively. The difference can
be attributed to the compositional and structural variations in these two steels pro-
viding a variation in hydrogen trapping and hydrogen repelling effects. The plots of

20 40

35
Precharging current densities
Precharging current densities
15 2.0 mA/cm2 30 2.0 mA/cm2
10 mA/cm2 6.0 mA/cm2
iH (µA cm-2)

iH (µA cm-2)

18 mA/cm2 25 30 mA/cm2
30 mA/cm2 40 mA/cm2
10 20
50 mA/cm2 70 mA/cm2
15

5 10

0 0
5 10 15 20 25 30 35 40 5 10 15 20 25 30 35 40
(a) time (min) (b) time (min)

Fig. 4. The oxidation current curves for X70 (a) and 16Mn (b) steels cathodic pre-charged under a series
of current densities for 2 h.
 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444 439

10 X70
16Mn

iH,10 (µA cm-2)

1
1 10 100
iC (mA cm-2)

Fig. 5. Effect of cathodic charging current on iH,10.

10

X70
16Mn
C (10-6 mol cm-3)

0.1
0 1 10 100
iC (mA cm-2)

Fig. 6. The total hydrogen concentration vs cathodic pre-charging current densities.

iH,10–ic in Fig. 5 and the plots of C–ic in Fig. 6 are quite identical which means that
the steel sensitiveness to hydrogen can be evaluated by iH,10.
The order of magnitude of hydrogen concentration determined by this method is
in good agreement with the literature data obtained by other methods [10], which
gives confidence that the proposed method provides reliable data for absorbed
hydrogen concentration in pipeline steels.
The absorbed hydrogen refers to the total hydrogen concentration in the material
comprise hydrogen in solution and hydrogen at trapping sites. And it has been
440 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444

reported for annealed iron that the hydrogen located in traps composed most (about
97.7%) of the total absorbed hydrogen using the classical permeation method [21].
In the cathodic charging process, only a few fractions of hydrogen atoms enter
steel and the rest combine to form H2 and bubble away, and the hydrogen retention
ratio of the process was obtained using Eq. (6). As seen in Fig. 7, for both of the two
steels, R decreases linearly with respect to ic in log–log scale. Under the condition of
this study, the values of R are relatively low, about in the magnitude range of 0.01–
0.1%. For both X70 and 16Mn steels, it can be expected that owing to the small
diffusion coefficient of hydrogen within the steel (about 7 · 10
7 cm2/s), surface satu-
ration will be attained rather quickly, resulting an increased share of the hydrogen
recombination process, thereby decreasing the hydrogen retention ratio. The hydro-
gen retention ratio is also largely dependent on the pre-charging time, see Fig. 10.
The hydrogen oxidation currents show an approximately exponential fall with
time. At 40 min the current is not more than 30% of the original current, hence,
approximately, less than 9% of the total amount of hydrogen is neglected and the
precision is sufficient for the study.
Most experiments studying hydrogen permeation use the double-cell method with
a membrane covered on the exit side by a palladium layer. But with the monocell in
this work, the specimen cannot be palladium plated, because if so both hydrogen
absorption and detection would be influenced by the Pd layer itself, and, maybe,
not relate to the steel investigated. However, the electrochemical detection of hydro-
gen is more complicated on the anodically oxidised metal than on the palladium
coated one. Without a Pd coating, the applied potential causes also the dissolution
of the steel, the formation of a surface film and recombination of a part the H-atoms
to give molecular hydrogen (H + H ! H2) [22] which cannot be oxidised and cannot
be measured in the hydrogen oxidation current.
On the other hand, the reliable hydrogen permeation measurements without a
palladium coating have been reported for iron and some mild steels [23–25]. In

1E-3
R

X70
16Mn
1E-4

0.1 1 10 100
iC (mA cm-2)

Fig. 7. The hydrogen retention rate (R) as a function of the pre-charging current density (ic).
 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444 441

the experiments of this work, by applying such a potential (+168 mV(vs SCE)) much
higher than the hydrogen equilibrium potential, the atomic hydrogen combination
reaction on the specimen surface can be restrained effectively. Moreover, no gas bub-
bles were observed on the specimen during the hydrogen outgassing test.

3.3. Influence of pH on iH and hydrogen concentration

The iH curves for X70 specimens pre-charged in a series of solutions with different
pHs at the same current density (ic = 35 mA cm
2) are shown in Fig. 8(a) and the
corresponding iH,10 and C in Fig. 8(b). It is clear that both iH,10 and C decrease with
increasing pH. For specimens pre-charged in solutions with the lower pH than 6, a
decreasing straight line is obtained for the curve of iH,10 (or C)–ic, which shows
that iH,10 varied from 10.54 lA cm
2 at pH 0 to 2.68 lA cm
2 at pH 6.2, and the
corresponding hydrogen concentration from 0.61 · 10
6 mol cm
3 to 0.18 · 10
6
mol cm
3. While in the neutral and alkaline solutions, a change in pH from 6.2 to
9.3 only resulted in a little decrease in iH,10 and C. The difference may be resulted
from the different hydrogen generation mechanism in the acid solution and in the
alkaline solution. Additionally, in an alkaline solution, the electrode is easily covered
by a layer of Fe(OH)2 which may hinder hydrogen absorption on the metal and pen-
etration into it.
As expected, the results indicate that the solution pH, as well as pre-charging cur-
rent, plays an important role in steel absorbing hydrogen. And a higher hydrogen
retention rate can be obtained for a more acidic solution.

3.4. Influence of pre-charging time on iH and hydrogen concentration

The hydrogen oxidation currents for X70 specimens pre-charged for a series of
times are presented in Fig. 9(a), and the corresponding iH,10 and C in Fig. 9(b). It

20 12
0.5
10
pH=2.0
15
iH,10 (µA cm-2)

pH=4.0 iH,10
iH (µA cm-2)

C (10-6 mol cm-3)

pH=6.2 0.4
8 C
pH=9.3
10
6 0.3

5 4
0.2

2
0 0.1
10 20 30 40 0 2 4 6 8 10
(a) time (min) (b) pH

Fig. 8. Influence of pH on the oxidation currents (a), and the corresponding iH,10 and C (b) for X70 steel
(ic = 35 mA cm
2).
442 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444

30 10 3.0

25 5min 2.5
10min 8

C (x10-6 mol/cm3)
iH,10
20min
20
iH (µA cm-2)

C 2.0

iH (µA cm-2)
40min
60min 6
15 120min 1.5

10 4 1.0

5 0.5
2
0
0.0
5 10 15 20 25 30 10 100
(a) time (min) (b) time (min)

Fig. 9. Pre-charging time dependence of oxidation currents (a), iH,10 and C (b) for X70 steel.

0.00030

0.00025

0.00020
R

0.00015

0.00010

0.00005
0 20 40 60 80 100 120
tC / min

Fig. 10. Pre-charging time dependence of the hydrogen retention rate for X70 steel (ic = 35 mA cm
2).

has been shown that the longer pre-charged time, the higher iH,10 and C obtained,
and saturation is approximately approached after pre-charging 120 min. Especially,
both iH,10 and C increase linearly with the logarithm of pre-charging time.
Fig. 10 shows the pre-charging time dependence of hydrogen retention ratio for
X70 over a time range of 5 to 120 min. A peak value of R is observed at about
10 min, and then R decreases the pre-charging time.

4. Conclusions

A hydrogen oxidation current method has been proposed to investigate the

absorbed hydrogen concentration in hydrogen pre-charged pipeline steels. In con-
 M. Yan, Y. Weng / Corrosion Science 48 (2006) 432–444 443

trast to the classical hydrogen permeation method, the method described here does
not require the diffusion coefficient and the steady-state permeation rate. It is easy to
use with monocell, especially in field, as a sensitive and convenient tool for analyzing
the hydrogen absorbed into metals.
Results from this method show that hydrogen concentrations increase with
increasing pre-charging current density, which is approximately consistent with the
SievertsÕ law. The hydrogen oxidation current and hydrogen concentration in
16Mn steel pre-charged steel are marginally higher than those in X70 steel which
means that the former is more susceptible to hydrogen absorption than the latter.
More acid solution (lower pH) is conducive to hydrogen entrance into the steel.
And, approximately, hydrogen Concentration increases linearly with the logarithm
of pre-charging time.

Acknowledgement

The research was financially supported by PetroChina Company Limited, and the
help rendered by Prof. Li Xiangyi is gratefully acknowledged.

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