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 Anti-Corrosion Methods and Materials
Aspects of intergranular corrosion of AISI 321 stainless steel in high-carbon-containing environments
Jacek Ryl Anna Arutunow Mateusz T. Tobiszewski Joanna Wysocka
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To cite this document:
Jacek Ryl Anna Arutunow Mateusz T. Tobiszewski Joanna Wysocka , (2014),"Aspects of intergranular corrosion of AISI 321
stainless steel in high-carbon-containing environments", Anti-Corrosion Methods and Materials, Vol. 61 Iss 5 pp. 328 - 333
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 Aspects of intergranular corrosion of AISI 321
stainless steel in high-carbon-containing
environments
Jacek Ryl, Anna Arutunow, Mateusz T. Tobiszewski and Joanna Wysocka
Department of Electrochemistry, Corrosion and Materials Engineering, Gdansk University of Technology, Gdansk, Poland

Abstract
Purpose – The purpose of this paper is to present a case study of unexpected sensitization to intergranular corrosion of highly resistant AISI 321
steel in petrochemical conditions, where it was subjected to the simultaneous influence of elevated temperature of ⬃250°C and vapors from the
asphalt production process.
Design/methodology/approach – Corrosion coupons were exposed in an installation carrying asphalt vapors. To identify the susceptibility to
intergranular corrosion a standard Strauss test was performed. Scanning electron microscopy (SEM) micrographs show a degree of degradation as
a result of local corrosion. Influence of the carburization process occurred during exposure and depletion of chromium in the passive layer and was
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evaluated using X-ray photoelectron spectroscopy (XPS) and X-ray spectroscopy (EDX) techniques.
Findings – The paper provides information on origin of corrosion of AISI 321 steel in a high-carbon-containing environment. It was found out that
long-term exposure can lead to intergranular corrosion in temperatures that are much lower than those that have been considered to be required
for sensitization of austenitic steels. The high concentration of carbon introduced during the exposure is stated to be responsible for this effect.
Practical implications – The formation of chromium carbides, leading to intergranular corrosion of the Type 321 stainless steel, is a major concern.
The paper reports that in certain petrochemical environments, highly resistant stainless steels, such as AISI 321, can be susceptible to intergranular
carbide degradation.
Originality/value – The presence of titanium is not sufficient to increase resistance in multiple environments and sensitization can occur even at
relatively low temperatures of ⬃250°C.
Keywords Intergranular corrosion, Stainless steel, Petrochemicals, Failure investigation
Paper type Research paper

Introduction Cr23C6) or sigma phase (Fe–Cr–Mo) can occur. As a result,

The basic property of austenitic stainless steels (SS) is the
presence of the protective Cr2O3 oxide that forms a passive
layer, which, in many cases, protects the steel from the
influence of aggressive environments. The stable and
protective passive layer is generated when at least 13 per cent
of chromium is added to austenitic steel. Then, according to
accepted standards, austenitic steel can be defined as
corrosion-resistant steel.
Precipitation of intermetallic phases at grain boundaries
increases considerably the susceptibility of SS to intergranular
corrosion. This process is called sensitization. It should be
stressed here that intergranular corrosion is one of the most
dangerous forms of corrosion attack, as it occurs inside the
material without a reduction in cross-sectional area and may
be revealed only when some element of construction fails
catastrophically. If SS are exposed to heat treatment in the
range of 500 to 850°C, precipitation of carbides (such as
The current issue and full text archive of this journal is available at
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Anti-Corrosion Methods and Materials
61/5 (2014) 328 –333
© Emerald Group Publishing Limited [ISSN 0003-5599]
[DOI 10.1108/ACMM-04-2013-1260]
chromium depletion may take place and the ability of steel to
form a protective passive layer is decreased locally at grain
boundaries. Thus, a local active–passive cell is created, where
chromium is leached from grains and chromium carbides are
cathodes, and the anodes are localized in the
chromium-depleted region. When the cell works,
intergranular corrosion can take place (Lopez et al., 1997;
Michiuchi et al., 2006; Singh et al., 2003; Bhise and Kain,
2012; Martin et al., 2012; Sahlaoui et al., 2004; Aydogdu and
Aydinol, 2006; Kelly et al., 1993; Gaudett and Scully, 1993;
Bruemmer et al., 1992).
Chromium carbides are created during the chromium
depletion process, which is the result of changes in the
solubility of carbon in austenite as a function of
temperature. Above 1,050°C, the whole of the carbon
content present in steel is dissolved in the austenite and its
solubility decreases rapidly as the temperature decreases.
The addition of elements with higher chemical affinity to
carbon than chromium, such as Ti or Nb, stabilizes
austenitic steels and reduces its susceptibility to
intergranular corrosion or may even eliminate it entirely.
The content of the stabilizing element (Ti) is calculated in
relation to a percentage content of carbon present in steel to
bond the whole excess of the carbon. The percentage value
of titanium should be at least five times higher than the
percentage content of carbon (Cihal, 1984). AISI 321 is an
example of such a steel.

328
 Aspects of intergranular corrosion of AISI 321
Jacek Ryl et al.
Accurate simulation of the specific environments that are
present in petrochemical and chemical installations is
impossible in laboratory conditions using electrochemical
techniques. The influences can be very complex and often are
coupled with high temperatures. The presence of halide ions is
of great influence, destroying the passive layer of SS and
accelerating localized corrosion. For example, the corrosion
rate of SS is about 0.035 mm/year when exposed to 75 per
cent phosphoric acid in 550°C, and the concentration of Cl⫺
ions is 8 ppm. When the chloride concentration reaches 23
ppm, the corrosion rate is 13 mm/year, which is higher by
three orders of magnitude, making the steel unfit for use in this
environment (Kreysa and Schutze, 2004). Furthermore, the
high service temperature can have a very negative influence on
SS, accelerating the corrosion process and leading to changes
in the bulk of steel, such as high-temperature corrosion or
sensitization to intergranular attack. Austenitic steels with
carbon contents ⬍ 0.03 per cent C are considered to be
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resistant to intergranular corrosion, so they are not sensitized
during exposure to temperatures ranging from 500 to 850°C.
However, steels can be carburized, for example, during
acetylene welding or electrical welding, especially when
welded places are contaminated with oil or grease, and the
carburized areas can be sensitized to intergranular corrosion.
The complexity of such operating conditions means that the
most popular approach to material selection for installations
with aggressive high-temperature service environments is
long-term exposure of coupons in the installation. This work is
based on the analysis of coupon degradation after exposure to
gas off-take facilities carrying away asphalt vapors.
Materials and methods
In this work, AISI 321 steel was used due to its high resistance
to intergranular corrosion. The chemical composition of AISI
321 is almost the same as the composition of widely used AISI
304 steel. The only difference is that the Type 321 SS has up
to 0.7 per cent titanium added to provide resistance to
intergranular corrosion.
Two identical sets of samples were prepared; each sample
was 25 ⫻ 13 ⫻ 8 mm3 in size. One set was used as reference
samples and the second set were exposed in the plant prior to
examination. Part of the reference set was subjected to
microscopic inspection and the other samples were kept in the
furnace in 675°C for 24 hours to sensitize them. This
temperature is sufficient for chromium to diffuse to grain
boundaries and create carbides. A Strauss test was performed
in accordance with the ASTM Standard (ASTM A262-10,
2010) to assess the susceptibility of the test material to
intergranular corrosion. The examined set of coupons was
exposed to the carburizing environment for two years at a
temperature of 250°C. Before being placed in the
petrochemical installation, coupons were ground with abrasive
paper of an increasing gradation from 400 to 2,500 and
degreased with ethanol.
Samples exposed in the industrial installation were placed
for two years in a refinery in an off-take facility used to
transport asphalt vapors. The temperature in the installation
ranged from 180 to 250°C. Asphalt consists of carbon in ⬎ 80
per cent and is a composition of many kinds of hydrocarbons.
In general, the ingredients of asphalt contain parts of different
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Anti-Corrosion Methods and Materials
Volume 61 · Number 5 · 2014 · 328 –333
structures and individual molecules cannot be distinguished.
The main components are malthenes (oils and resins) and
asphaltenes (heavier fractions). At high temperatures of
asphalt processing, volatile compounds can evaporate. Thus,
in the vapor off-take installation, the most volatile and the
simplest hydrocarbons are present. To avoid electrical contact
of the samples with pipes, samples were screwed into Teflon
cylinder sleeves and placed inside the installation. The
locations of the test assemblies were right behind outlets of
tanks with asphalt, in pipes of 150-200 mm diameter.
After exposure was completed, the coupons were unscrewed
from the polytetrafluoroethylene (PTFE) cylinder sleeves and
washed out and cleaned with a solvent, tetrahydrofurane
(THF) in this case. The coupons then were conditioned in a
solution of corrosion inhibitors of Radiner Fs/Zn (Marcor
Company) to remove possible corrosion products. After being
dried in an oven (at a temperature of 50°C for 1 hour), the
samples were weighed on an analytical balance, with a 0.0001
g resolution, to measure the material loss. Prior to visual
inspection, all samples, the reference as well as examined set,
were etched in accordance with the ASTM Standard (Jiang
et al., 2012).
The surface topography was examined using a scanning
electron microscope (SEM), model VP-SEM S3400-N made
by Hitachi, using tungsten wire as a filament. The microscope
was equipped with an energy dispersive X-ray spectroscopy
(EDX) attachment (from Thermo Scientific) for elemental
analysis of the surface. This technique has a relatively high
depth at which response signal is registered, making it
desirable when examining samples with high roughness.
Detailed chemical analysis was supported by the X-ray
photoelectron spectroscopy (XPS) technique using an Escalab
250Xi spectroscope from Thermo Scientific equipped with a
monochromatic Al X-ray source. High-energy spectra were
realized for a pass energy of 20 eV in constant analyzer energy
(CAE) mode and an energy step-size of 0.1 eV. A
monochromatic radiation source with 250 ␮m spot diameter
was used, averaging the elemental composition to the spot
diameter. An ion gun operating in the 3,000V mode served to
remove a layer of contaminations and for depth profiling.
Results
For a sample exposed long-term in asphalt vapors at elevated
temperatures, an average mass loss of cross-section Vp, was
calculated according to equation (1). It is a common way of
assessing susceptibility of metals to general corrosion:
⌬m ⫻ 365 mm
关 兴
Vp ⫽ · (1)
1000 ⫻ S ⫻ t ⫻ ␳ year
where ⌬m is a mass loss during exposition time, S – sample
surface area, t – time of exposure in expressed in days and ␳ –
density of AISI 321 SS.
Each of the examined samples was examined using the
SEM. The surface of the reference sample is shown in Figure
1(a). The sample subjected to sensitization and Strauss test
looked similar [Figure 1(b)]. The elemental composition of
both; reference sample and sample that undergone Strauss test
are compared to the normalized composition of AISI 321 steel
in Table I. Chemical compositions of above samples were
 Aspects of intergranular corrosion of AISI 321 Anti-Corrosion Methods and Materials
Jacek Ryl et al. Volume 61 · Number 5 · 2014 · 328 –333

Figure 1 (a) SEM micrographs of reference sample and (b) sample after Strauss test ( ⫻ 3,000)

Table I Elemental composition of AISI 321 steel, according to the not take into consideration additional elements. Spectra
standard, reference sample and after Strauss test registered for both points are presented in Figure 4.
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Elemental composition (% weight) High-resolution XPS analysis was carried out to provide
Reference Sample after further analysis of the chemical states of chromium and
Element Normalized AISI 321 sample Strauss test carbon. The surface was etched with an ion-gun for 10 ks to
ensure maximum possible removal of the passive layer and
Fe Bal 70.17 70.08 corrosion products from the sample surface. Figure 5 presents
Cr 17.00-19.00 18.00 18.01 the XPS spectra obtained for the Cr2p3/2 and C1s peaks.
Ni 9.00-12.00 9.19 9.23
C maximum 0.08 ⬍ 0.1 ⬍ 0.1
Ti 5 ⫻ per cent C-0.70 0.33 0.38 Discussion
Mn maximum 2.00 1.53 1.54 The rate of diameter decrement for the AISI 321 steel samples
Si maximum 1.00 0.78 0.76 was 0.0005 mm/year, which indicates the high resistance of
the steel to general corrosion. As a general fact, consumption
of SS resulting from general corrosion typically is very low.
determined on the basis of EDX spectroscopy, and these did However, the mass loss corrosion rate determination method
not take into account the content of other alloying elements. is inadequate in the case of SS, as the primary forms of attack
Figure 2 presents micrographs of the sample which was are pitting, crevice or intergranular corrosion. These forms of
exposed in the environment of elevated temperatures and asphalt corrosion are characterized by an incommensurately greater
vapors for two years. Pictures made at two resolutions showed decrease in strength and of the physico-chemical parameters
completely different appearance of the sample surface, compared of the alloy than would be estimated on the basis of mass loss.
to the reference samples. In Figure 3, chemical maps of iron, SEM micrographs of the sample made before the exposure
carbon and chromium distribution were compiled, together with as well as of the sample on which the Strauss test was made
the SEM image. Table II compiles the elemental composition of without prior exposure to asphalt vapors [Figures 1(a and b))
AISI 321 steel at a grain boundary (⌬) and within the grains did not reveal any traces of the localized form of corrosion.
(224), as assessed using the EDX technique. The analysis does There was no visible corrosion at grain boundaries; only

Figure 2 SEM micrographs of sample exposed to asphalt vapor for two years (a) ⫻ 500 and (b) ⫻ 3,000

330
 Aspects of intergranular corrosion of AISI 321 Anti-Corrosion Methods and Materials
Jacek Ryl et al. Volume 61 · Number 5 · 2014 · 328 –333

Figure 3 SEM image (a) and chemical EDX maps for (b) iron,
(c) carbon and (d) chromium for sample exposed to asphalt vapor
for two years ( ⫻ 3,000)
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sample. In particular, areas between the grains were enriched
in carbon, proving the occurrence of a carburization process
on the steel, whereas the chromium content was
impoverished. Locally low chromium content is crucial, taking
into account its input to form a passive layer on SS. The
changes in iron distribution were less readily evident. The
presence of chromium carbides was not observed on the steel
surface. A possible explanation was that due to corrosion the
chromium carbides are loosened and detach from the grain
boundaries. This would be consistent with the depletion of
chromium at the grain boundaries, as observed on the sample.
Detailed analysis of the EDX spectrum (Table II)
confirmed that at the grain boundary, the amount of
chromium was depleted to a level that might not be sufficient
for the formation of a protective passive layer. At the same
time, the amount of carbon present strongly suggests that
carburization of the metal could take place. It is also worth
noting that the amount of titanium at the grain boundary was

much higher than in the interior of the grains, resulting from

its diffusion to form carbides. The chemical constitution
within the grains was very similar to the reference sample.
XPS analysis for chromium [Figure 5(a)] revealed the
presence of three main components of the Cr2p3/2 peak,
corresponding to different chemical states. The component (I),
scratches formed during mechanical polishing were visible. No
for energy 576.6 ⫾ 0.3 eV, is typical for chromium oxide, Cr2O3.
significant differences were noticed in the chemical compositions
Chromium oxide is a residue of the passive layer, which had not
of either of these two samples, based on EDX measurements.
been fully removed, as the high surface roughness made that
Both were recognized to fulfill the requirements for the
normalized AISI 321 steel (Table I). The carbon content was impossible. The peak was broadened and could also carry
below the spectroscope threshold level, which was ⬍0.1 per cent. information about other forms of Cr3⫹, such as Cr(OH)3 and
The analysis of SEM micrographs of the reference sample CrOOH which, according to the literature, exhibit peaks around
confirmed the resistance of AISI 321 SS to intergranular ⬃577.5 eV energy (Jiang et al., 2012; Stefanov et al., 2000;
corrosion, in accordance with the Standard. The Strauss test has Maury et al., 1990). Peak (III) corresponds to the elemental
proved the resistance of the Type AISI 321 samples to chromium, whereas the small peak (II) within the range of
intergranular corrosion. The sonic examination also suggested 574.7 ⫾ 0.2 eV is consistent with peaks for Cr–C bonds (Jiang
that both samples were free from intergranular corrosion. They et al., 2012; Maury et al., 1990; Cekada et al., 2002). The
both had a pure metallic sound, not damped as should be in the identification of residual carbide was confirmed in Figure 5(b) by
case of intergranular corrosion. a presence of the C1s peak for carbon–metal bonds at 283.8 ⫾
A completely different appearance is visible in Figure 2, 0.2 eV. Other carbon peaks, for 286.3 and 292.9 eV, correspond
presenting the sample after two years of exposure in the vapor to the C–C and C–O bonds, respectively. This is not surprising,
of asphalt at elevated temperatures. Advanced intergranular due to the presence of residual passive layer.
attack was evident, despite the negligibly low mass loss. As a result of the two-year-long exposure to the carburizing
Additionally, the surfaces of grains were covered with agent, the amount of carbon that had diffused into the surface
micropits of ⬍1 ␮m in diameter. These could be a result of region of the sample was very high. The aggressive medium
general corrosion of SS in an oxygen-depleted environment. attacked selectively the grain boundaries, where the passive layer
EDX chemical maps (Figure 3) proved the inhomogeneous was weaker, and intergranular corrosion could be noticed. At the
distribution iron, chromium and carbon on the surface of the same time, areas at grain boundaries were enriched with carbon,
which was attributed to a carburization process during the
exposure period. Its amount was 50 times higher than would be
Table II Elemental composition of AISI 321 steel after exposition in
asphalt vapor for two years typical of normalized AISI 321 steel, as was confirmed using both
the EDX and XPS techniques. Such high amounts of carbon
Elemental composition (% weight) could not be absorbed by the titanium, and thus the steel was no
Element At grain boundary (⌬) At grain interior (⌬) longer resistant to the intergranular corrosion. The EDX
Fe 71.8 70.2 spectrum revealed a higher Ti concentration at the grain
Cr 11.4 17.6 boundary, which suggests that titanium reacted with the carbon
Ni 9.4 9.2 and titanium carbides were created.
C 3.9 0.2 It can be assumed that carburization of AISI 321 steel
Ti 0.8 0.2 occurred as a result of long-term exposure to an
Mn 1.8 1.7 environment of simple hydrocarbons and at a temperature
Si 0.9 0.9 of around 250°C. According to the chromium depletion
theory, sensitization of the AISI 321 steel is not expected at

331
 Aspects of intergranular corrosion of AISI 321 Anti-Corrosion Methods and Materials
Jacek Ryl et al. Volume 61 · Number 5 · 2014 · 328 –333

Figure 4 Spectra registered with EDX technique, with peaks marked for the main elements of AISI 321 steel
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this temperature. However, the significantly higher carbon
content, i.e. about 2 per cent, was measured, increasing the
influence of the sensitization conditions. The amount of Ti
was constant and was approximately 0.4 per cent. It can be
assumed that carburization resulted in a decrease in the
relative sensitizing temperature of AISI 321 steel to 250°C.
This temperature, in combination with the pressure vapor
of the asphalt, could lead to anaerobic decomposition of
hydrocarbons to carbon, which subsequently diffused into
the steel and formed chromium carbides. The presence of
the sensitization process was confirmed by the XPS peaks
for energies corresponding to Cr–C bonds.
Elemental analysis proved chromium depletion at grain
boundaries to a value at which a stable and barrier passive
layer could not be formed. As a consequence, the metal was
locally unprotected and corrosion cells evolved between the

Figure 5 High-resolution spectra for (a) Cr2p3/2 and (b) C1s after 10,000 seconds of etching with ion gun; 3,000 V (high), CAE 20 eV and
step size 0.1 eV

332
 Aspects of intergranular corrosion of AISI 321
Jacek Ryl et al.
chromium carbide cathodic region and the anodic region at
the grain boundary. Chromium carbides may eventually
detach as the region surrounding them is dissolved,
additionally explaining the smaller concentration of chromium
at grain boundaries and the broad corroded areas in between
the grains. No changes in concentrations of inert elements,
such as Ni, Mn or Si, were observed.
Intergranular corrosion occurs even for materials that are
considered to possess resistance to this type of attack, if certain
conditions are met. In particular, the presence of elevated
temperatures and long-term exposure to carburizing agents
such as simple hydrocarbons may lead to failures and
premature breakdown of industrial installations.
Summary
● As shown for Type AISI 321 steel, exposed for two years in
vapor of asphalt at temperatures of 180-250°C, long-term
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exposure to carburizing conditions can increase the
susceptibility of this SS to intergranular corrosion,
reducing its sensitization temperature.
● EDX analyses revealed the high carbon content,
confirming the presence of carburizing conditions.
● XPS revealed that the examined steel had a locally depleted
passive layer and chromium was present in the form of
chromium carbides. The chromium carbides form cathodic
regions, leading to dissolution at the grain boundaries.
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Corresponding author
Jacek Ryl can be contacted at: jacek.ryl@pg.gda.pl