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Comparison of the Rotating Cylinder and Pipe Flow Tests for Flow-
Sensitive Carbon Dioxide Corrosion

Article in CORROSION · October 1995

DOI: 10.5006/1.3293555

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 CORROSION SCIENCE

Comparison of the Rotating Cylinder

and Pipe Flow Tests
for Flow-Sensitive Carbon Dioxide Corrosion

˘ ´ G.T. Solvi,* and J. Enerhaug**

S. Nesic,

ABSTRACT KEY WORDS: carbon steel, carbon dioxide corrosion,

corrosion rate, impedance, mass transfer, pipe flow,
The effects of various hydrodynamic parameters on the cor- polarization resistance, potentiodynamic sweep, rotating
rosion rate of low-carbon steel in carbon dioxide (CO2) cylinder
environments were studied. Two different flow geometries,
rotating cylinder (RC) and pipe flow, were studied simulta- INTRODUCTION
neously in the same electrolyte within a glass loop.
Comparisons were made over a wide range of parameters: Corrosion can be affected by flow differently depend-
temperature (T) = 20°C to 80°C, pH = 4 to 6, CO2 partial ing on the mechanism governing the corrosion
pressure (PCO2) = 0 bar to 1 bar (0 kPa to 100 kPa), velocity
process. Two major cases can be distinguished: the
(v) = 0 m/s to 13 m/s. The hydrodynamic conditions studied
effect of flow on corrosion when no surface films are
covered the range from static to highly turbulent flow. The
corrosion process was monitored using polarization resis-
present and the effect of flow on corrosion in the
tance, potentiodynamic sweep, and electrochemical presence of surface films (precipitates, inhibitors,
impedance methods. The comparison of the two flow geom- etc.).
etries was carried out in terms of hydrodynamics, mass In the absence of films, the primary effect of flow
transfer, and CO2 corrosion. The measured mass transfer on corrosion is through mass transfer of the species
rates agreed well with published correlations for the RC and involved in the corrosion reaction at the metal sur-
straight pipe (SP) flow. In the case of CO2 corrosion, it was face. For mass transfer in turbulent liquid flow, due
possible to achieve good agreement between corrosion rates to very large Schmidt numbers, all the concentration
in the two flow geometries at low temperatures by having the changes occur in a very narrow layer adjacent to the
same water chemistry and mass-transfer conditions. This
metal surface, deep within the viscous sublayer in
conclusion was valid for cases where no protective corrosion
the so-called mass-transfer boundary layer. The
products, scale, or inhibitor films were present. However, at
higher temperatures, films with a certain degree of protec-
thickness of this layer is a function of the flow rate
tiveness were observed. In those cases, lower corrosion rates (Reynolds number) and flow geometry. Mass transfer
were obtained on the SP specimen because of more dense usually is associated with limiting currents (i.e., with
and protective films. situations where the electrochemical processes at the
metal surface proceed so fast that it is difficult to
transport enough reactants from the bulk). Con-
versely, sufficiently rapid removal of corrosion
Submitted for publication December 1994. Presented as paper no. products from the surface also can become limiting,
130 at CORROSION/95, March 1995, Orlando, FL.
* Institutt for energiteknikk, P.O. Box 40, N-2007, Kjeller, Norway. which can lead to accumulation, (super)saturation
** Statoil, Postuttak, 7004 Trondheim, Norway. and precipitation of surface films. However, if the
0010-9312/95/000179/$5.00+$0.50/0
CORROSION–Vol. 51, No. 10 © 1995, NACE International 773
CORROSION SCIENCE

corrosion process is under charge transfer (activa- cesses occurring. Therefore, the fruitless literature
tion) or chemical reaction rate control, changes in the search for a single scaling flow parameter (Reynolds
flow and associated mass transfer will have no effect number,3 shear stress,4-5 turbulence,2 etc.) that
on the corrosion rate. would capture the effect of flow on corrosion had
When surface films are present, they can reduce little chance of success.
the corrosion rate by hindering the transport of spe- Nevertheless, a way to predict what would hap-
cies involved in the electrochemical reactions at the pen in field conditions is needed. One way would be
metal surface. In the case of inhibitor films, parts of to use complicated, high-pressure, multiphase flow
the surface are “blocked” by the inhibitor, and the loops.
electrochemical double layer can be altered. The sur- With more knowledge of the processes, a small-
face films can be removed locally or globally by scale apparatus can be sufficient. This study was
chemical dissolution (in case of precipitates) or by concerned much with the transfer of data from one
mechanical forces, both of which lead to very high laboratory scale flow-corrosion system (rotating cylin-
corrosion rates. Both mechanisms of film removal are der [RC]) to another (pipe flow) and ultimately to the
related to flow and the transfer processes within. field.
Chemical dissolution of surface deposits is related to
mass transfer and to water chemistry. Mechanical EXPERIMENTAL
removal of films is related to momentum transfer and
often is encountered in single- and multiphase flows. Loop
In multiphase flow, film removal can be caused by The experimental glass flow loop used in the
the impact of solid particles present in the liquid, by present study is shown in Figure 1. The loop was
the impact of droplets present in the gas flow (ero- built to handle two-phase water and oil flow. How-
sion), or by pressure and shear stress fluctuations ever, only results from the single-phase water flow
due to slugging, etc. Even in single-phase flow, me- experiments are presented. Glass was selected as the
chanical film removal often is seen particularly at main loop material for two reasons: It enabled appli-
geometrical irregularities (e.g., weld beads, grooves, cation of aggressive cleaning procedures (in between
and areas of sudden diameter changes). It is not yet experiments with inhibitors), and because it was
clear which forces are responsible for mechanical optically transparent (important especially in two-
film removal. In the literature, the average wall phase flow).
“shear stress”1 and near-wall “turbulence fluctua- Two test sections were mounted in the loop —
tions”2 were connected with the onset of film removal. ␣ the straight pipe (SP) and the RC. The same
However, there has been no clear and detailed study electrolyte was circulated through both test sections
where this was investigated. to guarantee identical water chemistries for the cor-
The present study primarily was aimed at the rosion processes. The same idea was used previously
effect of flow on carbon dioxide (CO2) corrosion where by Efird, et al.6 The enlarged view of the SP test sec-
protective surface films are not present. This prob- tion made from polytetrafluoroethylene (PTFE) is
ably is the simpler of the two cases discussed above. shown in Figure 2. Three steel specimens were flush
However, in high-temperature experiments of this mounted in the pipe (diam [dp] = 15 mm [0.59 in.]
work, films with a certain degree of protectiveness inner diam [ID]). Up to three additional pipe test
did form and were affected by the flow. sections could be added to the existing one in series.
CO2 corrosion, as studied here, is related to The RC (diam [dc] = 10 mm [0.394 in.]) mounted in a
problems encountered in oil and gas production and cylindrical glass chamber with all the measuring
transportation. The intention was to create an experi- equipment is shown in Figure 3.
mental setup where real-life conditions would be Most of the components of the loop, including
simulated as accurately as possible. However, simu- the valves, were made form borosilicate glass and
lation of field conditions in the laboratory is PTFE. Some minor components (mostly fittings) were
extremely complicated and primarily is dependent made from polypropylene (PP), polyvinyl chloride
upon detailed knowledge of the processes occurring (PVC), polyvinylidene fluoride (PVDF), rubber, type
(both flow and corrosion). The processes occurring in 316 SS (UNS S31600)(1) and C-276 steel (UNS
the present system were so complicated that a simple N10276 ). The construction of the loop enabled reli-
scaling parameter most probably did not exist. This able control of the flow parameters, water chemistry
meant that successful transfer of data from one labo- and temperature, and stable and reliable automatic
ratory system to another and, further, to the field operation of the loop for extended periods of time (up
was possible only via a model describing the pro- to several weeks).

(1)
Water Chemistry
UNS numbers are listed in Metals and Alloys in the Unified
Numbering System, published by the Society of Automotive
Water chemistry is one of the most important
Engineers (SAE) and cosponsored by ASTM. factors affecting the corrosion rate, so significant

774 CORROSION–OCTOBER 1995

 CORROSION SCIENCE

FIGURE 1. Schematic of the glass flow loop.

attention was given to this matter. Water preparation Material

included: water purification by distillation or reverse In all experiments, the steel tested was a low-
osmosis and bubbling with CO2 typically for 1 day carbon API 5L Grade X-65 steel,(2) a typical pipeline
prior to the experiment. Continuous CO2 bubbling steel. Chemical composition of the steel is given in
was maintained throughout the experiment. The Table 1.
oxygen (O2) content was measured continuously and
kept < 40 ppb throughout the experiment. Hydro- Corrosion Measurements
chloric acid (HCl) and sodium bicarbonate (NaHCO3) The corrosion process was followed using the
were added to achieve the desired pH. It was possible electrochemical techniques of polarization resistance,
to control the concentration of iron cations (Fe2+) by alternating current (AC) impedance, and potentiody-
using an iron generator (to increase the Fe2+ concen- namic sweep. A three-electrode setup was used in all
tration), an ion exchanger (which could substitute electrochemical experiments, both in the SP and the
Fe2+ in the solution with hydrogen [H+] or sodium RC test sections. In the SP test section (Figure 2), the
[Na+] ions), and a high-temperature iron precipitator. working and the counter electrode were mounted
Typically once a day, samples of the loop water were flush with the pipe wall so that minimal flow distur-
taken for analysis to determine the amount of dis- bance was created. The working electrode made from
solved CO2 and the concentration of Fe2+. carbon steel and the counter electrode made from C-
The pH was measured with two independent 276 steel were identical in shape (area [AA] = 2.9 cm2
electrodes to register a possible drift. One electrode [0.45 in.2]) and were mounted diametrically opposite
was placed in a side stream taken from the main each other so that a symmetrical current distribution
circulation circuit, and the other was placed in the was obtained during polarization experiments. An
RC chamber. When the discrepancy in the readings external silver-silver chloride (Ag-AgCl) reference
on the two pH meters was > 0.1, the electrodes were electrode (filled with saturated potassium chloride
taken out, recalibrated, and eventually replaced. The [KCl]) was connected to the cell with an ion-conduct-
water temperature was kept constant within ± 0.5°C ing porous wooden plug.
in the range 20°C to 80°C. In the RC test section (Figure 3), a carbon steel
working electrode was mounted onto a rotator with a
(2)
American Petroleum Institute, 1220 L. St., N.W., Washington, DC,
speed control unit (0 rpm to 5,000 rpm). The speci-
20005. men was machined from the parent material into a

CORROSION–Vol. 51, No. 10 775

CORROSION SCIENCE

FIGURE 2. Schematic of the SP test section made from PTFE.

using a Luggin capillary with a porous wooden plug.

The rotating speed of the working electrode was
controlled occasionally using a stroboscope. Electro-
chemical measurements were made using a
potentiostat with an eight-channel multiplexer
connected to a 486/25 mHz personal computer.

Procedure
The glass loop was filled with ≈ 56 L (14.8 gal) of
electrolyte: distilled water + 1 mass% sodium chlo-
ride (NaCl). Then, the CO2 was bubbled continuously
through the electrolyte (usually for 24 h prior to the
experiment) to deoxygenate and saturate the solu-
tion. Monitoring of pH and O2 concentration was
used to judge when the solution was in equilibrium.
Then, the pH was adjusted by adding HCl or
NaHCO3. Prior to immersion, the carbon steel speci-
men surfaces were polished using 500- and 1,000-
grit silicon carbide (SiC) paper, degreased with
acetone, and washed with alcohol.
The polarization resistance measurements were
conducted by polarizing the working electrode
± 5 mV from the free corrosion potential and scan-
FIGURE 3. Schematic of the RC test section made from glass. ning at 0.1 mV/s. The solution resistance was mea-
sured independently using AC impedance and
subtracted from the polarization resistance. The AC
cylinder 10 mm (0.394 in.) in diameter and 10 mm impedance measurements were made by applying an
(0.394 in.) long. The exposed area of the specimen oscillating potential to the working electrode ± 5 mV
was 3.14 cm2 (0.49 in.2) concentric platinum wire around the free corrosion potential using the
ring served as a counter electrode. An external frequency range 1 mHz to 100 kHz. At the end of
Ag-AgCl reference electrode was connected to the cell each experiment, the potentiodynamic sweeps were

776 CORROSION–OCTOBER 1995

 CORROSION SCIENCE

TABLE 1
Chemical Composition of the X-65 Pipeline Steel Used for the Working Electrode (mass%)
C Mn Si P S Cr Cu Ni Mo Al V Sn Ti Nb

0.064 1.54 0.25 0.013 0.001 0.05 0.04 0.04 0.07 0.041 0.035 0.002 0.002 0.041

TABLE 2
Experimental Parameters

Test solution 1 mass% NaCl

Temperature 20°C to 80°C
Pressure 1 bar CO2
pH 4 to 6
Dissolved oxygen < 40 ppb
Velocity in pipe Static – 13 m/s
Rotating speed Static – 5,000 rpm
Test duration 1 to 7 days
Sweep rate 0.1 mV/s
Potentiodynamic sweep limits –600 mV to 150 mV vs Eoc
AC impedance ±5 mV vs Eoc from 1 mHz to 100 kHz
Polarization resistance sweep limits –5 mV to 5 mV vs Eoc

conducted, starting 600 mV below and finishing tions used in the present experiments satisfied both
150 mV over the free corrosion potential. The typical requirements. By testing the two flow geometries
scanning rate used was 0.1 mV/s. Experimental using the same electrolyte, it could be assumed that
conditions are summarized in Table 2. After removing water chemistry was identical, and the work could
the specimens from the loop, they were prepared for be focused on the differences in the CO2 corrosion
inspection by scanning electron microscopy (SEM) process that arose from hydrodynamic and mass-
and energy dispersive x-ray analysis (EDXA). transfer considerations.
The choice of the SP test section for a principal
Difficulties test geometry required no special justification: The
Numerous difficulties followed the experimental practical importance and resemblance of this geom-
program. Even very small quantities of contamina- etry to real systems is obvious. In addition,
tion leaking from loop components were found to be hydrodynamics and mass transfer in turbulent pipe
detrimental and capable of leading to erroneous mea- flow have been investigated thoroughly, both experi-
surements. Lead contamination was encountered, mentally and theoretically.7
with lead dissolving from a minute seal in a rotame- A rotating disc first was considered instead of
ter used to monitor the flow rate through a bypass the RC because of its well-defined hydrodynamics
stream. It was found that tin was dissolving from a and mass transfer.8 However, as a rotating disc is
graphite pump bearing. In both cases, the contami- primarily suitable for laminar flow studies, the RC
nating metals were deposited on the surface of the geometry was selected. It enabled studies of turbu-
present specimen. The most serious contamination lent flow and provided very uniform current
was discovered to come from a short nitrile rubber distribution. In addition, detailed hydrodynamic and
hose used to connect the pumps with the loop. The mass-transfer studies of the RC flow geometry could
mysterious contaminant was a very effective corro- be found in the literature.9-10
sion inhibitor. All previous sources of contamination Before proceeding with comparisons of the two
had to be removed before meaningful measurements flow geometries in terms of hydrodynamics, mass
could be made. transfer, and corrosion, it might be useful to summa-
rize what is known about the mechanisms of the CO2
RESULTS AND DISCUSSION corrosion process. Figure 4, generated with an elec-
trochemical model of CO2 corrosion, illustrates this
Selection of an adequate laboratory scale appa- explanation.11 When CO2 is added to an aqueous
ratus for testing flow effects in CO2 corrosion is a solution, it is hydrated and forms a weak carbonic
difficult task. The selected experimental setup must acid (H2CO3). Typically, only a very small proportion
have well-defined hydrodynamic and mass-transfer (0.25%) of dissolved CO2 is hydrated into H2CO3. In
characteristics. In addition, good control of water addition, this is a slow process. H2CO3, as any other
chemistry must be possible. The SP and RC test sec- weak acid, provides a source of H+ ions at a given pH.

CORROSION–Vol. 51, No. 10 777

CORROSION SCIENCE

encountered. For 2,000 < Rep < 3,000, transition

to turbulent flow occurs. Translated to the present
experimental conditions (dp = 15 mm ID, T = 20°C)
turbulent flow was achieved for all velocities
> 0.2 m/s. At higher temperatures, the transition
occurred at even lower velocities. For a RC geometry,
laminar flow typically is encountered for Reynolds
numbers Rec = vcdc/␯ < 200 (where vc = ␻dc/2 is the
peripheral velocity of the RC, the rotational [angular]
speed in rad/s, and dc is the cylinder diameter in m).
This means that in the present conditions (dc =
10 mm, T = 20°C), already for rotation speeds
> ␻ = 40 rpm, turbulent flow was encountered in the
FIGURE 4. Most important electrochemical reactions in CO2 corrosion vicinity of the cylinder. This corresponded to a RC
at pH 4, 20°C, 1 m/s, 1 bar CO2. peripheral velocity of vc = 0.02 m/s.
Turbulent flow in the two geometries has many
similarities. Fully developed turbulence is encoun-
In an acidic solution, the reduction of H+ is usually tered in the bulk liquid. As solid walls are ap-
the most important cathodic reaction. It has been proached, the turbulent fluctuations are damped so
shown previously that the rate limiting step in the H+ there exists a layer near the metal surface where
reduction reaction can be the diffusion rate of H+ ions viscous forces dominate and any turbulence is dissi-
from the bulk of the fluid to the surface.12 At higher pated rapidly. Between this so-called viscous
pH values, the availability of H+ ions decreases, and sublayer and the turbulent core, there is a transition
other competing cathodic reactions become impor- layer, often called the buffer sublayer, where the
tant. viscous and turbulent forces are of the same order of
In CO2 systems at low pH (pH < 4), there are so magnitude. For aqueous systems which typically
many H+ ions that the H+ reduction is still the domi- have large Schmidt numbers (Sc ≈ 103), the mass-
nant cathodic reaction. At intermediate pH (4 < pH transfer boundary layer is very thin and is imbedded
< 6, the range of the primary present interest) in deeply into the viscous sublayer.
addition to the H+ reduction a new cathodic reaction The shear stress exerted at the wall in pipe flow
becomes important: the direct reduction of H2CO3. can be determined from the pressure gradient along
This additional cathodic reaction often is seen as the a pipe by:
cause for CO2 solutions to be more corrosive than pH
alone would suggest. The reduction of H2CO3 can be ∆p dp
τw = (1)
under activation (charge-transfer) control13 or under ∆L 4
chemical reaction control14-15 when the slow hydra-
tion step limits the rate of the overall reaction. At where τw is the wall shear stress in Pa and ∆p/∆L is
currents higher than the limiting for H+ or H2CO3 the pressure drop along the pipe. However, the pres-
reduction, the dominant cathodic reaction changes to sure drop was not measured in the experiments so
direct reduction of water.16 The governing mechanism the shear stress had to be determined from existing
depends on where the anodic and cathodic lines in- correlations. For turbulent pipe flow, such a relation-
tersect. ship can be found only empirically in terms of laws of
In water-CO2 corroding systems, it most often friction. One of the simplest such correlations is the
has been assumed that the sequence of anodic Blasius equation:7
dissolution of iron is the same as it is in other
acids13,17 (i.e., the pH-dependent mechanism pro- ƒp = 0.079 Re–0.25 for Rep > 3,000 (2)
p
posed by Bockris, et al.18). However, some recent
findings11,19 do not support this assumption. It seems
where ƒ = 2τw/␳v2 is the Fanning friction factor and ␳
that the iron dissolution reaction in CO2-containing
solutions proceeds without the influence of pH (for is the density in kg/m3. However, for high Reynolds
numbers (Rep > 105) this formula is in error. It is then
4 < pH < 6).
most appropriate to use the Coolebrook equation:20
Fluid Flow
From a practical point of view, turbulent flow 1 ε 1.256
regimes are of the primary interest. For pipe flow at = –4 log + for Rep > 3,000 (3)
ƒp 3.7dp Rep ƒp
Reynolds numbers below Rep = vpdp/␯ = 2,000 (where
vp is velocity in m/s, dp is pipe diameter in m/s, and
␯ is the kinematic viscosity in m2/s), laminar flow is which for smooth pipes (ε/dp = 0) reduces to Prandtl’s

778 CORROSION–OCTOBER 1995

 CORROSION SCIENCE

universal law of friction:7

1
= 4 log Rep ƒp – 0.4 for Rep > 3,000 (4)
ƒp

and for very rough pipes to von Karman’s equation:7

1 dp dp/ε
= 4 log + 2.28 for < 0.01 (5)
ƒp ε Rep ƒ

For the RC in the case of a turbulent flow regime

(smooth surfaces), the friction factor is:10
FIGURE 5. Calculated shear stress as a function of v at T = 20°C, dc
= 0.01 m, dp = 15 mm (0.59 in.).
ƒc = 0.158 Re–c 0.3 for Rec > 300 (6)

For very rough surfaces, similar as for pipe flow, the

drag on a RC is independent of the Reynolds number
and is a function of relative roughness:10

1 dc
= 5.76 log + 1.25 (7)
ƒc ε

In Figure 5, the calculated shear stress is com-

pared for SP and RC flow in the loop at 20°C. The
velocity plotted on the x axis is the average cross-
section velocity (vp = Qp/Ap where Qp is the volumetric
flow rate in m3/s and Ap is the pipe cross section in
m2) for SP flow and the RC peripheral velocity (vc =
␻dc/2) for the RC. The smooth surface correlations
were used to calculate the shear stress. This was
justifiable because the surface roughness varied from
ε/dp ≈ 1 x 10–4 for the freshly polished specimens to
ε/dp ≈ 4 x 10–4 for heavily corroded surfaces (as deter-
mined by looking at the surface cross section using
SEM). Calculated from the previous correlations,
even for the highest velocities, the effect of maximum
roughness on shear stress was < 10%.
FIGURE 6. Potentiodynamic sweep; effect of v on mass-transfer
From Figure 5, it could be concluded that, with
limiting currents; water, 1% NaCl solution, pH 3, T = 20°C, PN2 = 1 bar,
the RC, shear stresses up to 25 Pa could be achieved
ptotal = 1 bar.
at maximum rotation speed (5,000 rpm, which corre-
sponded to vc = 2.61 m/s). In the SP, as much as
300 Pa was achieved at vp = 12 m/s. For the “equal”
velocity (vp = vc), similar shear stress was obtained for domain of the present work, mass-transfer character-
the two flow geometries. This will hold true only ization of the two flow geometries in the loop was
when the RC and SP diameters are of the same order done.
of magnitude, as in the present case. Most of the This was achieved by conducting experiments
present experiments were conducted at 2 m/s, where at pH 3 in a 1% NaCl water solution purged with
the calculated shear stress was 16 Pa and 12 Pa for nitrogen gas (N2). Under these conditions, the domi-
the RC and the SP, respectively. nant cathodic reaction for modest overpotentials
(␩ < –0.5 V, where ␩ is the overpotential in V) was the
Mass Transfer reduction of H+ ions. For overpotentials between
According to general understanding of the CO2 –0.2 < ␩ < –0.5 V, it was possible to obtain clear
corrosion mechanisms, mass transfer is important mass-transfer limiting currents (Figure 6). Potentio-
primarily at pH < 5, when it affects the limiting cur- dynamic sweeps were conducted beginning from the
rents for H+ reduction. Since this pH range is in the corrosion potential and finishing 0.8 V below. This

CORROSION–Vol. 51, No. 10 779

CORROSION SCIENCE

For the RC flow the correlation of Eisenberg,

et al., was appropriate:22

kmdc
Shc = = 0.0791 × Re0.7
c × Sc
0.356
(10)
D

The measured and calculated mass-transfer coeffi-

cients as a function of velocity are shown in Figure 7.
The value D(H+) = 9.31 x 10–9 m2/s was been used to
obtain km from the Sherwood number.23 In Figure 7,
it was again arbitrarily selected to compare km for the
matched velocity (vp = vc). However, the most impor-
tant conclusion was that, for the RC and for the SP
FIGURE 7. Measured and predicted mass transfer coefficient as a flow, the agreement between the measured mass-
function of ␯ for the two flow geometries; T = 20°C, dc = 0.01 m, dp = transfer coefficient in the present loop and the one
15 mm (0.59 in.). predicted using the previous correlations was good.
This meant that good control of the mass-transfer
conditions was achieved in the loop for both flow
geometries. A somewhat larger discrepancy between
predicted and measured km was obtained for the SP
flow. The working electrodes in the SP test section
(Figure 2) were only 20 mm (0.787 in.) long (1.33 x
dp), and it could be assumed they were too short to
eliminate the effect of developing mass-transfer
boundary layers completely.
The mass-transfer measurements enabled selec-
tion of the velocity in the SP and the corresponding
rotating speed for the RC, which gave identical mass-
transfer rates for the two geometries.24-25 By selecting
vp = vc = 2 m/s, practically identical mass-transfer
FIGURE 8. Corrosion rate vs time followed from beginning of the coefficients (km)p = (km)c ≈ 4 x 10–4 m/s were measured
experiment at T = 20°C and equivalent mass-transfer conditions: ␯p at 20°C. This was approximately in the middle of the
= 2 m/s, ␯c = 2 m/s (3,820 rpm); water, 1% NaCl, pH 5, PCO2 = 1 bar,
region where the two curves overlapped (Figure 7).
Ptotal = 1 bar; 䡬, 䡺, ∆ – pipe flow; 䢇 – RC.
The majority of the conducted CO2 corrosion experi-
ments presented below were done at vp = vc = 2 m/s
(3,820 rpm), where the mass-transfer conditions
was repeated for different SP velocities and RC were approximately equal.
speeds. The measured limiting currents were con-
verted to the mass-transfer coefficient by using: CO2 Corrosion
Corrosion experiments were carried out over a
idlim (H+) wide range of parameters: T = 20°C to 80°C, pH = 4
km = (8) to 6, PCO2 = 1 bar (100 kPa), and v = 0 m/s to 13 m/s.
F × 10–pH Experiments were started by measuring the polariza-
tion resistance (corrosion rate) every 30 min at
where km is the mass transfer coefficient in m/s, idlim vp = vc = 2 m/s (matching mass-transfer conditions).
is the diffusion limiting current density in A/m2, and In most of the experiments, a stable corrosion rate
F is the Faraday constant (96,490 coul/equiv). was observed (Figure 8). In this experiment, good
Mass-transfer coefficients for turbulent flow are agreement was obtained between the corrosion rates
well established in the literature for the two flow for the RC and SP specimens.
geometries under investigation. In the case of SP Typically 24 h after the beginning of the experi-
flow, the correlation of Berger and Hau could be ments, measurements of the polarization resistance
used:21 (corrosion rate) and the corrosion potential as a func-
tion of velocity were performed. The velocity was
kmdp varied from 0 m/s to 13 m/s and back in the SP
Shp = = 0.0165 × Re0.86
p × Sc0.33 (9)
D section and from 0 rpm to 5,000 rpm and back in the
RC chamber.
where Sh is the Sherwood number, D is the diffusion Subsequently, velocity was adjusted back to vp =
coefficient in m2/s, and Sc is the Schmidt number. vc = 2 m/s. After a waiting period of 12 h (to obtain

780 CORROSION–OCTOBER 1995

 CORROSION SCIENCE

stable corrosion rates), AC impedance measurements

were conducted. Finally, potentiodynamic sweeps
were done, and the specimens were taken out from
the loop and prepared for SEM analysis.
Experiments at 20°C — The potentiodynamic
sweeps measured at vp = vc = 2 m/s (equivalent
mass-transfer conditions) and different pH are shown
in Figure 9. The measured curves are overlaid with
theoretical curves predicted with the model of Nesic,
˘ ´
et al., for easier interpretation of the corrosion
mechanisms.11 The data obtained for the RC elec-
trode were in good agreement with data from the SP
section over the whole potential range for all three
pH. At pH 4, a large contribution of the H+ reduction
reaction could be seen. This contribution diminished
at pH 5 and completely disappeared at pH 6. At pH 5
and 6, the dominant cathodic reaction at the corro-
sion potential was direct H2CO3 reduction, and for
higher negative overpotentials, the dominant ca-
thodic reaction was H2O reduction. Good agreement
between the RC and SP measurements was clear for
all three cathodic reactions, as well as for the anodic
reactions. This led to a conclusion that the mecha-
nism of the CO2 corrosion in the two flow geometries
(RC and SP) was the same at 20°C. It then was not
difficult to understand that the measured corrosion
rates shown in Figure 8 were very similar for the two
geometries.
The potentiodynamic sweeps shown in Figure 9
were corrected for the solution resistance found by
FIGURE 9. Potentiodynamic sweeps for different pH values conducted
the AC impedance technique. In Figure 10, results of at T = 20°C and equivalent mass-transfer conditions: vp = vc =
the AC impedance measurements (Nyquist plot) at 2 m/s (3,820 rpm); water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; 䡬, 䡺,
20°C, pH = 6, and vp = vc = 2 m/s are shown. A good ∆ – pipe flow; 䢇, 䡵, ▲ – RC.
agreement between the measured polarization resis-
tance values for the RC and SP geometry was
evident. Taking into account the difference in area for
the two sample geometries (10% larger for the RC),
the measured polarization resistances in Ω-m2 for the
two geometries were even closer. The similar shape of
the measured curves confirmed that an identical
mechanism of CO2 corrosion was present in both flow
geometries.
The obtained corrosion rates as a function of
velocity at 20°C are shown in Figure 11 for the differ-
ent pH.(3) The corrosion current is shown on the left
and the corresponding corrosion rate on the right
side (for iron dissolution, the relation 1 mm/y =
1.155 A/m2 was used). The corrosion rates at static FIGURE 10. AC impedance measurement at T = 20°C, pH 6 and
conditions were approximately the same for all three equivalent mass-transfer conditions: vp = vc = 2 m/s (3,820 rpm);
pH values, as were the corrosion potentials (Figure water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; ∆ – pipe flow; ▲ – RC.
12). The only difference in the corrosion rates for the

(3)
In this and in all subsequent figures where the effect of velocity three different pH values came from the H+ reduction
has been shown, the results were corrected for the effect of the reaction. However, in static conditions, the mass-
presence of oxygen by subtracting the contribution of the oxygen
reduction current. Measured oxygen concentrations varied from transfer limiting current for H+ reduction was very
10 ppb to 40 ppb in different experiments. Previously shown small in all three cases, so the chemical reaction-
mass-transfer correlations and the diffusion coefficient (DO2 =
2.09 x 10–9 m2/s at 20°C) were used to calculate the limiting
controlled reduction of H2CO3 was the dominant
currents for oxygen reduction. cathodic reaction.

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FIGURE 11. Effect of v on the corrosion rate at different pH values FIGURE 12. Effect of v on the corrosion potential at different pH
and T = 20°C; water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; 䡬, 䡺, ∆ – values and T = 20°C; water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; 䡬,
pipe flow; 䢇, 䡵, ▲ – RC. 䡺, ∆ – pipe flow; 䢇, 䡵, ▲ – RC.

As velocity was increased, the limiting current to 12 m/s, another flow-dependent reaction had to
for H+ reduction increased, leading to an increased be identified. It was proposed that the higher ca-
overall cathodic reaction and higher corrosion rate. thodic current observed at higher velocities (pH 6)
The increase of the corrosion rate with velocity was came from an accelerated H2CO3 reduction reaction.
most pronounced at pH 4, where the concentration In other words, it was proposed that there was a
of H+ was highest. At pH 4, already at 1 m/s, the diffusion-controlled component of the H2CO3 limiting
contributions of H+ reduction and H2CO3 reduction current in addition to the chemical reaction-
were equal (Figure 4). For higher velocities, the flow- controlled component, as already proposed by
dependent H+ reduction dominated. At pH 5 and Schmitt and Rothman.14 The concept of pure chemi-
1 m/s, the H+ reduction was only 10% of the overall cal reaction-controlled limiting current is strictly
cathodic reaction, while at 10 m/s,the H+ and H2CO3 valid only when the thickness of the mass-transfer
reduction were of the same order of magnitude. boundary layer is much larger than the thickness of
Thus, the increase in corrosion rate as a function the “reaction” layer.26 As a first approximation, it
of velocity at pH 5 still could be explained by the could be said that this is correct at higher tempera-
increasing contribution of mass transfer-controlled tures and low velocities. In the present case (pH 6,
H+ reduction. However, this was not the case for high velocity, and low temperature), in addition to
pH 6. the H2CO3 being formed by the slow hydration step
At pH 6, there were so few H+ ions that, even near the metal surface, significant amounts of H2CO3
at the highest velocity tested, they give a small con- were transported by diffusion from the bulk. This
tribution to the overall cathodic current (10% at meant that the limiting current for H2CO3 generally
10 m/s). To explain the observed doubling in the had two components: a flow-independent (chemical
corrosion rate when the velocity changed from 1 m/s reaction-controlled) part and a flow-dependent (mass

782 CORROSION–OCTOBER 1995

 CORROSION SCIENCE

(a) (b)
FIGURE 13. SEM images of the cross section of the corroded surfaces exposed for 63 h at T = 20°C, pH 5 and equivalent
mass-transfer conditions: vp = vc = 2 m/s (3,820 rpm); water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; (a) RC specimen and (b)
SP specimen.

transfer-controlled) part. A detailed theoretical

treatment of this concept will be published in the
future.
Figure 11 shows good agreement obtained for the
corrosion rates of the RC and SP specimens. The
same was true for the measured corrosion potentials
(Figure 12). This suggested that, in the absence of
surface films, identical corrosion rates could be ob-
tained by setting equivalent water chemistry and
mass-transfer conditions at the two flow geometries.
It also confirmed that, in this case, the present un-
FIGURE 14. Effect of v on the corrosion rate at T = 50°C, pH 4 and
derstanding of CO2 corrosion mechanisms permitted
equivalent mass-transfer conditions water; 1% NaCl, PCO2 = 1 bar,
the transfer the data from one flow system to an-
Ptotal = 1 bar; 䡬 – pipe flow; 䢇 – RC.
other.
In Figure 13, SEM images of the cross sections of
a specimen exposed for 63 h at 20°C and pH 5 are
shown. An evenly attacked surface virtually free of ments conducted at pH 5 and pH 6 at the same tem-
any films was evident. perature.
Experiments at 50°C — Potentiodynamic sweeps It initially was difficult to explain why the good
measured at 50°C, pH 4, and vp = vc = 2 m/s (equiva- agreement between the two flow systems found at
lent mass-transfer conditions) are shown in Figure 20°C was not obtained again at 50°C until SEM im-
14. A higher rate of the overall cathodic reaction was ages of the corroded surfaces cross section were
observed over the whole range of negative overpoten- analyzed. In both cases (SP and RC specimens), there
tials for the RC electrode compared to the SP. The were films on the surfaces (Figure 17). The film found
difference between the anodic reactions seemed to be on the RC specimen (Figure 17[a]) was more porous,
smaller. However, it was difficult to judge this be- consisting primarily of iron carbide (uncorroded part
cause of the low slope of the anodic lines. of the steel) and probably presented a very weak dif-
It was no surprise then that the velocity test fusion barrier for the corroding species. The film
done in the same experiment failed to show good found on the surface of the SP specimen (Figure
agreement between the RC and SP curves (Figure 17[b]) was more dense, consisting of an iron carbide
14). The shape of the measured curves (Figure 15) matrix filled partially with iron carbonate. This film
was similar for the two geometries, suggesting a looked laminated and fractured (which probably
similar corrosion mechanism. The same conclusion occurred during drying). However, it could be as-
could be reached by looking at the AC impedance sumed that it acted as a stronger diffusion barrier.
measurements conducted in the same experiment The previous observations helped explain the dis-
(Figure 16). Similar results were obtained in experi- crepancy in the electrochemical measurements

CORROSION–Vol. 51, No. 10 783

CORROSION SCIENCE

FIGURE 15. Potentiodynamic sweep conducted at T = 50°C, pH 4 FIGURE 16. AC impedance measurement at T = 50°C, pH 4 and
and equivalent mass-transfer conditions: vp = vc = 2 m/s (3,820 rpm); equivalent mass-transfer conditions: vp = vc = 2 m/s (3,820 rpm);
water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; 䡬 – pipe flow; 䢇 – RC. water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; 䡬 – pipe flow; 䢇 – RC.

(a) (b)
FIGURE 17. SEM images of the cross section of the corroded surfaces exposed for 175 h at T = 50°C, pH 4 and equivalent
mass-transfer conditions: vp = vc = 2 m/s (3,820 rpm); water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; (a) RC specimen and (b)
SP specimen.

shown in Figures 14 and 15. It could be concluded difference between the two flow systems was a small
that more dense (protective(4)) films formed on the SP pressure gradient that existed at the RC electrode
specimen compared to the RC specimen at 50°C. and came from the centrifugal force acting in the
The question to be answered was how the protec- direction perpendicular to the steel surface. It was
tive films formed in the first place. It is known that, estimated roughly that the difference between pres-
at pH 4, the solubility of iron carbonate is quite high sure at the surface of the RC and the bulk pressure
(much higher than measured values in the present was of the order of 1 Pa in these experiments. In
experiments) and that the likelihood of forming pro- addition, the calculated shear stress at the RC elec-
tective films is low.27 However, since iron carbide trode was a few Pa higher than the one in the SP for
films were formed, they could have created more the same mass-transfer conditions (vp = vc = 2 m/s)
favorable conditions at the steel surface for iron car- in the present loop (Figure 5). Finally, a small cen-
bonate precipitation. This was aided by the higher trifugal force acting on the forming solid film which
temperatures (50°C) that accelerated the precipita- was present at the RC did not exist in the SP flow. It
tion of iron carbonate.27 only could be speculated that these very mild forces
The next question was why more dense and pro- were responsible for noticeably different film struc-
tective films formed on the SP steel electrode. The tures at the two flow geometries.
(4)
Experiments at 80°C — At 80°C, similar results
Surface films that enable corrosion rates of several mm/y could
hardly be called protective in a practical sense. However, they do were obtained as for 50°C. The difference between
act as a diffusion barrier and reduce corrosion. the RC and SP specimens was even more pronounced

784 CORROSION–OCTOBER 1995

 CORROSION SCIENCE

at 80°C (Figure 18). The potentiodynamic sweep done

at 80°C, pH 4, and vp = vc = 2 m/s (equivalent mass-
transfer conditions) showed once again that it was
easier to notice the difference in the corrosion pro-
cess for the two flow geometries on the cathodic
reactions. The AC impedance measurements (Figure
19) suggested a similar corrosion mechanism for the
two geometries and the presence of a diffusion-con-
trolled process in both cases. This further reinforced
our hypothesis that protective films were responsible
for the observed differences in CO2 corrosion at the
RC and SP specimens. By looking at the SEM images
FIGURE 18. Potentiodynamic sweep conducted at T = 80°C, pH 4
of the cross section of specimens from the same ex-
and equivalent mass-transfer conditions: vp = vc = 2 m/s (3,820 rpm);
periment exposed for 70 h (Figure 20), films could be water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; 䡬 – pipe flow; 䢇 – RC.
noticed with an iron carbide porous structure and
dense iron carbonate precipitates in between. Again,
the films formed on the RC specimen looked more
porous and less protective than the films formed on
the SP specimen.
Despite the presence of surface films, a signifi-
cant increase was evident in the rate of the overall
cathodic reactions at higher temperatures (50°C and
80°C) as shown in Figures 15 and 18. Surprisingly,
the anodic reactions were not accelerated signifi-
cantly at higher temperatures. This apparent
anomaly will be the subject of more detailed investi-
gation.
In general, the corrosion rate was higher at
higher temperatures. It could be noticed further that
the flow dependence of the corrosion rate was less FIGURE 19. AC impedance measurement at T = 80°C, pH 4 and
pronounced at higher temperature (Figures 11, 14, equivalent mass-transfer conditions: vp = vc = 2 m/s (3,820 rpm);
water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; 䡬 – pipe flow; 䢇 – RC.
and 21). This was contrary to what Eriksrud and
Søndvedt reported previously.15 The present findings
could be explained by remembering that flow depen-
dence comes from the mass-transfer limiting ❖ Flow-dependent CO2 corrosion rates at pH 4 and 5
currents. At higher temperatures, the chemical reac- and 20°C were obtained that could be explained by
tion-controlled limiting current for H2CO3 reduction the flow-dependent mass-transfer limiting current for
dominated as it was accelerated more rapidly than H+ ions. The observed flow dependence at pH 6 and
the diffusion limiting currents for H+ and H2CO3 re- 20°C could not be explained with the mass-transfer
duction. The overall corrosion process, which was limitation of H+ ions. It was proposed that there was
under partial mass-transfer control at lower tempera- a diffusion-controlled component of H2CO3 limiting
tures (20°C), changed to a mixed charge transfer/ current, in addition to the chemical reaction-
chemical reaction control at higher temperatures controlled component, as previously proposed by
(50°C and 80°C). The surface films which formed and Schmitt and Rothman.14
acted as a mass-transfer barrier also could have been ❖ A significant increase in the corrosion rate at
partially responsible for the observed lack of flow higher temperatures (50°C and 80°C) was obtained
dependence at higher temperatures. as a consequence of the increased rate of the overall
cathodic reactions. It was observed that the anodic
CONCLUSIONS reactions were not accelerated significantly at higher
temperatures.
❖ Good agreement was obtained between the mea- ❖ The flow dependence of the corrosion rate was less
sured mass-transfer coefficients and the ones pronounced with increasing temperature because of
predicted using the correlation of Berger and Hau21 the change in the corrosion mechanism from mixed
for SP flow and the correlation of Eisenberg, et al.,22 charge/mass-transfer control at low temperature
for the RC flow geometry. This enabled selection of a (20°C) to mixed charge transfer/chemical reaction
velocity in the pipe and the corresponding rotating control at higher temperatures (50°C and 80°C).
speed for the RC, which gave approximately equal At higher temperatures, the chemical reaction-
mass-transfer conditions for the two geometries. controlled limiting current for H2CO3 reduction was

CORROSION–Vol. 51, No. 10 785

CORROSION SCIENCE

(a) (b)
FIGURE 20. SEM images of the cross section of the corroded surfaces exposed for 170 h at T = 80°C, pH 4 and equivalent
mass transfer-conditions: vp = vc = 2 m/s (3,820 rpm); water, 1% NaCl, PCO2 = 1 bar, Ptotal = 1 bar; (a) RC specimen and (b)
SP specimen.

understanding of CO2 corrosion mechanisms in the

absence of surface films permitted the transfer of
data from one flow system to another and ultimately
to the field.

ACKNOWLEDGMENTS
This work was supported financially by Statoil.

LIST OF SYMBOLS
A area (m2)
FIGURE 21. Effect of v on the corrosion rate at T = 80°C, pH 4 and d p, d c pipe and cylinder diam) (m)
equivalent mass-transfer conditions; water, 1% NaCl, PCO2 = 1 bar, D diffusion coefficient (m2/s)
Ptotal = 1 bar; 䡬 – pipe flow; 䢇 – RC.
ƒ = 2␶w/␳␯2 Fanning friction factor
F Faraday constant (96,490
coul/equiv.)
accelerated more rapidly than the diffusion limiting i current density (A/m2)
currents for H+ and H2CO3 reduction. idlim diffusion limiting current
❖ At higher temperatures (50°C and 80°C), films density (A/m2)
formed on the metal surface and acted as a mass- km mass-transfer coefficient (m/s)
transfer barrier that somewhat reduced the corrosion l characteristic length (m)
rate. In general, more dense and protective films L pipe length (m)
formed on the SP specimen compared to the RC p pressure (bar)
specimen. It was speculated that the somewhat PCO2 partial pressure of CO2 (bar)
higher shear stress and a small radial pressure gra- Q volumetric flow rate (m3/s)
dient at the RC electrode were responsible for R universal gas constant (8.3143
noticeably different film structures at the two flow J/[mol K])
geometries. The surface films also could have been Re = ␳␯l/µ Reynolds number
partially responsible for the observed lack of flow Sc = µ /␳D Schmidt number
dependence at higher temperatures. Sh = kml/D Sherwood number
❖ In the absence of surface films, it was possible to T temperature (°C)
achieve the same mechanism and obtain approxi- v velocity (m/s)
mately the same rate of the CO2 corrosion process at
a RC as at a SP electrode by setting identical water Greek Symbols
chemistry and mass-transfer conditions at the two ε pipe roughness (m)
flow geometries. This confirmed that the present ␯ viscosity (kg/m-s)

786 CORROSION–OCTOBER 1995

 CORROSION SCIENCE

␳ density (kg/m3) 13. C. deWaard, D.E. Milliams, Corrosion 31 (1975): p. 131.

14. G. Schmitt, B. Rothman, Werkst. Korros. 28 (1977): p. 816.
␶w wall shear stress (Pa) 15. E. Eriksrud, T. Søntvedt, “Effect of Flow on CO2 Corrosion
␻ rotation (angular) speed (rad/s) Rates in Real and Synthetic Formation Waters,” in Advances in
CO2 Corrosion, vol. 1, Proc. CORROSION/83 Symp. CO2 Corro-
sion in the Oil and Gas Industry, eds. R.H. Hausler, H.P.
Subscripts Goddard (Houston, TX: NACE, 1984), p. 20.
p pipe 16. P. Delahay, J. Amer. Chem. Soc. 74 (1952): p. 3,497.
17. L.G.S. Gray, B.G. Anderson, M.J. Danysh, P.G. Tremaine,
c cylinder “Mechanism of Carbon Steel Corrosion in Brines Containing
Dissolved Carbon Dioxide at pH 4,” CORROSION/89, paper no.
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