CORROSION SCIENCE SECTION
Intergranular Corrosion in a Martensitic
Stainless Steel Detected by Electrochemical Tests
N. Alonso-Falleiros, M. Magri, and I.G.S. Falleiros*
ABSTRACT
Quenched and tempered martensitic stainless steel UNS
S41000 was tested electrochemically for susceptibility to sen-
sitization in specimens quenched from 975°C (1,248 K) and
tempered for 2 h at different temperatures between 300°C
(573 K) and 700°C (973 K). Besides an oxalic acid etch test,
the following tests were performed using a potentiostat and
1 N sulfuric acid (H2SO4) solution: potentiokinetic polariza-
tion, potentiostatic etch, and electrochemical potentiokinetic
reactivation in the double-loop version (DL-EPR). Tested sur-
faces were observed metallographically. The maximum
susceptibility to intergranular corrosion was observed in the
condition tempered at 550°C (823 K), and a sensitized struc-
ture was detected. For lower tempering temperatures, steel
was less sensitized, or not at all, and for higher tempering
temperatures, steel was less sensitized. All tests except for
the oxalic acid etch were able to evaluate quantitatively dif-
ferent degrees of sensitization as a function of tempering
temperature. The DL-EPR method was the best to discrimi-
nate degrees of sensitization.
KEY WORDS: electrochemical tests, electrochemical
potentiokinetic reactivation, intergranular corrosion,
martensitic stainless steel, sensitization, sulfuric acid, UNS
S41000
Submitted for publication September 1998; in revised form, May
1999.
* Department of Metallurgical and Materials Engineering, Escola
Politécnica, University of São Paulo, Av. Prof. Mello Moraes, 2463,
05508-900, São Paulo (SP), Brazil.
0010-9312/99/000169/$5.00+$0.50/0
CORROSION–Vol. 55, No. 8 © 1999, NACE International
INTRODUCTION
In most cases, intergranular corrosion in stainless
steels is caused by sensitization, a condition of local
impoverishment in chromium, which is precipitated
in the form of carbides. This is an undesired result of
careless heat treatment or welding operations.
Most publications concerning intergranular
corrosion refer to austenitic steels. Study of inter-
granular corrosion in martensitic stainless steels
is not in current technical literature. Intergranular
corrosion is a potential problem in these materials
because martensitic steels always are used in
the tempered condition, in which carbides are
precipitated.
Common methods to check the susceptibility of
stainless steels to intergranular attack are described
in ASTM A2621 for austenitic steels and ASTM A7632
for ferritic steels. Practice A in ASTM A262 and Prac-
tice W in ASTM A763 have rules for etch tests in
oxalic acid. These are used for acceptance of materi-
als; rejection should be decided in connection with
evaluation by other practices, slow and destructive,
including mass loss or bending tests.
Electrochemical corrosion tests, which are quick
and may be nondestructive, are an attractive choice.
Polarization curves produced by the potentiokinetic
method have been used to indicate occurrence of
sensitization3-5 and to compare degrees of sensitiza-
tion.6 Potentials in anodic polarization curves that
cause the greatest intergranular attack are used as
guides for the potentiostatic etching method.7-8 Elec-
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CORROSION SCIENCE SECTION
Chemical Composition of UNS S41000 Steel (mass %)
C Mn Si
0.13 0.48 0.68
trochemical potentiokinetic reactivation (EPR) is
another method that has been used quantitatively
and nondestructively to evaluate intergranular corro-
sion susceptibility in austenitic steel pipe weldings.9
The objective of the present work was to study
sensitization in a UNS S41000(1) stainless steel in
different quenched and tempered conditions, using
an oxalic acid etch test and other electrochemical
methods to detect the presence and measure the
degree of sensitization.
MATERIALS AND METHODS
Steel
UNS S41000 steel had the (ladle) analysis shown
in Table 1. As-received samples were quenched and
tempered forged bars, from which cubic specimens
with edges of ~ 1 cm were taken. Each specimen was
austenitized at 975°C (1,248 K), which is recom-
mended for this steel,10 for 20 min and quenched in
oil. Some as-quenched specimens were reserved for
observations in this state, and others were tempered
for 2 h at fixed temperatures. Tempering tempera-
tures used were 300°C (573 K), 350°C (623 K), 400°C
(673 K), in 50 K steps, up to 700°C (973 K). Temper-
ing was interrupted by oil-cooling.
Specimens had all faces ground with silicon
carbide (SiC) papers to a 600-grit finish. A cold-
setting mounting resin was used to avoid microstruc-
tural changes in prepared specimens. Electrical
contact for electrochemical tests was made through
a threaded hole.
Electrochemical Tests
Tests used were oxalic acid etch, potentiokinetic
polarization, potentiostatic etch, and EPR in the
double-loop version (DL-EPR).
Specimens for oxalic acid test were polished with
1 g diamond and etched in 10% aqueous solution of
oxalic acid (H2C2O4·2H2O), under a current density of
1 A/cm2 for 90 s.
Other electrochemical tests were made with a
potentiostat, using naturally aerated 1 N sulfuric
acid (H2SO4) solution at a temperature between 21°C
(294 K) and 26°C (299 K). In each test, the specimen
was dipped in solution for 5 min without an applied
potential. The counter electrode was a platinum
(1)
UNS numbers are listed in Metals and Alloys in the Unified
Numbering System, published by the Society of Automotive
Engineer (SAE) and cosponsored by ASTM.
770
TABLE 1
P S Cr Ni Mo Fe
0.02 < 0.01 12.5 0.12 < 0.02 Bal.
sheet and the reference electrode was saturated
calomel electrode (SCE).
The potentiokinetic method was applied to speci-
mens polished with SiC paper to a 600-grit finish.
The potential was changed continuously from
–770 mVSCE to 1,300 mVSCE, at the rate of 1 mV/s.
Potentiostatic tests were made on specimens
polished down to 1 µm using a fixed potential, under
which chromium-impoverished regions should have
dissolved preferentially. Suitable potentials for etch-
ing stainless steels in H2SO4 solutions are those just
above the passivation potential.11
The same conditions of the surface, temperature,
and solution concentration used for the potentio-
kinetic tests were used for DL-EPR tests. The
potential was changed from –490 mVSCE, up to
500 mVSCE, and back to –490 mVSCE, with a scanning
rate of 1.67 mV/s. Tests produced values of maxi-
mum current densities in the activation stage (Ia) and
in the reactivation stage (Ir). The degree of sensitiza-
tion was measured by the ratio between the current
density maxima (Ir/Ia).
A test solution originally developed for austenitic
steels (0.5 M H2SO4 + 0.01 M potassium thiocyanate
[KSCN]) at 30°C (303 K) was too aggressive when
applied to the martensitic steel.12 No steady corrosion
potential was achieved and extensive corrosion
occurred.
Metallography
After electrochemical tests, the tested surface
of each specimen was observed by optical or
scanning electron microscopy (SEM). Metallographic
observations were matched to the electrochemical
test results. This was more necessary in quenched
and tempered martensitic steels than in austenitic
steels, because in the former, there was precipita-
tion of carbides in the original austenite grain
boundaries and inside the grains, mainly between
martensite laths.
RESULTS AND DISCUSSION
Oxalic Acid Etch Test
Figure 1 presents results of the oxalic acid etch
tests. In as-quenched and tempered specimens, up to
500°C (773 K), the etch revealed only the martensitic
structure (Figure 1[a], steel tempered at 400°C). Steel
tempered at 550°C (823 K) suffered preferential grain
boundary attack (Figure 1[b]). Tempering at higher
temperatures produced microstructures that suffered
CORROSION–AUGUST 1999

(a)
(b)
(c)
FIGURE 1. Optical micrographs of UNS S41000 steel specimens
after oxalic acid etch test: (a) tempered at 400 ° C (673 K),
(b) tempered at 550°C (823 K), and (c) tempered at 700°C (973 K).
general etching corrosion where grain boundaries
were hardly visible (Figure 1[c]).
Carbide precipitation at grain boundaries caused
sensitization only when an impoverished region
persisted in the matrix, a condition that might have
CORROSION–Vol. 55, No. 8
CORROSION SCIENCE SECTION
FIGURE 2. Polarization curves in 1 N H2SO4 for specimens as-
quenched and tempered at 550°C and 700°C, obtained from
potentiokinetic tests.
been relieved by eventual diffusion of chromium from
the bulk of the grain into a region initially impover-
ished (the process sometimes is called recovery or
healing). Literature suggests that the oxalic acid test
causes etching of carbides and not preferential disso-
lution of the surrounding chromium-impoverished
zones.13-14 This test alone was unable to reveal differ-
ences between a sensitized and recovered state.
Therefore, Figure 1(b) showed that when
tempered at 550°C (823 K), the material had grain
boundary precipitates. A chromium-impoverished
region, if present, should be identified by other
methods.
Potentiokinetic Polarization
Figure 2 presents polarization curves for differ-
ent heat treatment conditions. There was a change in
the shape of the curves for specimens tempered at
500°C (773 K) or higher, in comparison with the
specimens tempered at lower temperatures and with
as-quenched material.
The significant change in curves was the second
peak of anodic current, very clear in the specimen
tempered at 550°C (823 K). Current densities for
the specimen tempered at 500°C (773 K) and for
those tempered > 550°C (823 K) did not have a
peak, but showed a bump in the same region of po-
tential values.
In stainless steels tested in 1 N H2SO4, the known
causes of the second peak are oxidation of atomic
hydrogen absorbed by the metal,15 Fe2+ in the acid
solution,16 nickel enrichment in the surface of the
electrode,17 and chromium-impoverished regions.3-4
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TABLE 2
Data Produced in Potentiokinetic Polarization Experiments

icrit i2max(A) ip,min(B) Q2max(C)

Condition Test (mA/cm2) (µA/cm2) (µA/cm2) (mC/cm2)

As-Quenched 1 22.2 92.5 13.2 41

2 23.0 99.0 15.2 45

Tempered at 300°C 1 20.6 68.4 11.6 32

2 16.0 43.2 8.86 21

Tempered at 350°C 1 16.6 53.1 8.34 24

2 17.2 57.9 9.00 27

Tempered at 400°C 1 20.9 85.4 11.3 38

2 19.8 60.4 9.08 30

Tempered at 450°C 1 17.9 131 10.61 56

2 18.9 114 19.55 54

Tempered at 500°C 1 16.6 380 25.1 123

2 19.4 450 28.4 145

Tempered at 550°C 1 21.6 5,180 142 1,290

2 23.0 5,875 161 1,463

Tempered at 600°C 1 26.2 501 12.5 165

2 30.6 543 10.7 178

Tempered at 650°C 1 31.9 511 15.9 182

2 32.2 487 10.5 170

Tempered at 700°C 1 32.6 320 15.0 126

2 33.1 351 10.5 139
(A)
Current density at potential –75mVSCE.
(B)
Minimum passive current density.
(C)
Area under the curve in the region of the second peak: between –221 mVSCE and the potential of ip,min.

In UNS S41000 steel, atomic hydrogen and Fe2+
in solution did not cause a second peak.11 Nickel
enrichment in the surface and one peak were ob-
served after long time of immersion (~ 1 h or more) in
1 N H2SO4 solution. Although UNS S41000 had only
residual nickel content, the peak was present even in
material tempered at 350°C (623 K).11 Proceeding
with potentiokinetic polarization in a short time after
immersion, as in the present work (5 min), avoided
this effect.
This discussion discarded all known causes of
the second peak, except for chromium impoverish-
ment. The cause of the observed second peak in
potentiokinetic polarization curves was chromium
impoverishment in the neighborhood of carbides (i.e,
sensitization). The next step was the measurement of
the degree of sensitization.
Table 2 shows numerical data produced in the
potentiokinetic polarization experiments. The current
density in the second anodic peak is represented by
i2max. There was a clear local maximum only for the
specimen tempered at 550°C (823 K). For other speci-
mens, it was considered that i2max was the current
density measured at –75mVSCE. This was the average
potential of the second peak for curves of the mate-
rial tempered at 550°C (823 K).
The area under the curve, in the region of the
second peak, was proportional to the density of elec-
tric charge involved mainly in the corrosion of
chromium-impoverished regions (Q2max). Values were
calculated by potentiostat control software, integrat-
ing the curve between –221 mVSCE, the beginning
of the second peak for material tempered at 550°C
(823 K), and the minimum value of the current
density in the passive region (ip,min).
Table 2 also presents values of the critical
current density (icrit).
Values of i2max, ip,min, and Q2max for the specimen
tempered at 550°C (823 K) were larger than those for
other conditions. Taking into account oxalic acid test
results, these data were characteristic of a sensitiza-
tion process. Values of icrit had a small variation,
increasing with the tempering temperature, particu-
larly between 500°C (773 K) and 700°C (973 K). This
is consistent with a decrease in the amount of
chromium in solution in the bulk of material with
increasing tempering temperature, and suggests the
precipitation of this element in the form of carbides

772 CORROSION–AUGUST 1999

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and/or its diffusion from the bulk to regions impov-

erished by precipitation.
In the second peak, there was corrosion of chro-
mium-impoverished regions. The i2max or Q2max were
not the most suitable data for measurement of the
degree of sensitization. Both referred to the total area
of the specimen, and not exclusively to chromium-
impoverished areas, along precipitates in grain
boundaries or in martensite lath boundaries. Differ-
ent austenitic grain or martensite lath sizes would
have caused different current densities for the same
degree of sensitization. Even comparison between dif-
ferent analyses of the same steel might have been
troubled by small differences in chromium contents.
It was necessary to normalize results using a
parameter that represented the surface area of the
impoverished region and the average chromium con-
tent of the material. The suggested normalizing
parameter was icrit. Actually, this has been used in
such capacity in the DL-EPR method. FIGURE 3. Variation of i2max/icrit with tempering temperature obtained
Figure 3 shows the variation of i2max/icrit with from potentiokinetic polarization test.
tempering temperature, and Figure 4 shows the
variation of Q2max/icrit. These results were consistent
with metallographic observations of the oxalic acid
test, considering that there was impoverishment
associated to etched carbides.

Potentiostatic Etch
Potentiostatic etch test was made under a
potential that caused preferential etch of chromium-
impoverished areas. This suggested the use of the
potential corresponding to the second peak of anodic
current density of potentiokinetic tests. Nevertheless,
direct use of potentiokinetic results for potentiostatic
etching is not always valid. In the present case,
potentials between –150 mVSCE and 50 mVSCE,
under static conditions, were tested.11 The potential
corresponding to maximum current density was
–100 mVSCE, under which potentiostatic tests were
made.
Figure 5 shows current density as a function of
etching time and microstructures observed by SEM,
after a 10-min etch.
In the specimen tempered at 550°C (823 K),
FIGURE 4. Variation of Q2max/icrit with the tempering temperature
current densities were the highest and increased
obtained from potentiokinetic polarization.
strongly with test time (Figure 5[a]). Tests for other
heat treatment conditions did not show an increasing
current density. In the specimen tempered at 500°C (773 K),
In the as-quenched specimen (Figure 5[b]), there was local and deep etching along some marten-
etching was uniform, except for some inclusions or sitic plate interfaces (Figure 5[d]).
residual carbides that remained undissolved during Specimens tempered at 550°C (823 K) and above
austenitization. In specimens tempered up to 450°C were etched deeply along martensite plate interfaces
(723 K), etching showed small points scattered in the and austenite grain boundaries (Figure 5[e]).
microstructure (Figure 5[c]). Based on a study of In specimens treated at 650°C (923 K), there was
tempering stages in UNS S41000,18 etched points also localized corrosion (Figure 5[f]), but shallower
were possibly iron-rich, M3C-type carbides, where M than in material tempered at 550°C (823 K).
is mainly iron, causing no chromium-impoverished Figure 6(a) shows that there were precipitates
surroundings. left in ditches produced by the potentiostatic etch of

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(a) (b)

(c) (d)

(e) (f)

FIGURE 5. Potentiostatic test at –100mVSCE: (a) current density dependence on etching time for different tempering
temperatures. SEM of specimen surfaces (after 10-min test): (b) as-quenched, (c) tempered at 450°C, (d) tempered at
500°C, (e) tempered at 550°C, and (f) tempered at 650°C.

774 CORROSION–AUGUST 1999

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(a)

FIGURE 7. Minimum current densities recorded in potentiostatic

tests at –100 mVSCE of specimens tempered at different temperatures.

the material tempered at 650°C (923 K). EDX analy-

(b)
(c)
FIGURE 6. (a) SEM image of the specimen tempered at 650°C, after
potentiostatic test at –100 mVSCE, showing precipitates in the
preferentially etched areas; (b) EDX analysis of the matrix; and
(c) EDX analysis of the precipitates.
sis for the matrix and for the precipitate detected
carbon in the precipitates (Figures 6[b] and [c]). Car-
bon analysis was made using a thin window detector.
Results sustained the possibility of a corrosion
mechanism caused by local chromium impoverish-
ment. The main tempering carbide at 550°C (823 K)
and above was iron chromium carbide of the type
M23C6, richer in chromium than M3C.18
If corrosion was caused by chromium impover-
ishment, the current density was proportional to the
surface area of impoverished regions, but was also a
function of the degree of impoverishment. In austen-
itic stainless steels, EPR tests have shown that
current density is related mostly to areas where chro-
mium is < 12.5 wt% ~ 13.5 wt%.19 There was no
similar information for martensitic steels. Conclu-
sions must stay at the general level: current density
that increases with the time of test is evidence of
sensitization.
The plot of the minimum current density (imin) for
different tempering temperatures is shown in Figure
7. The shape of the curve was similar to curves of
Figures 3 and 4, suggesting that this could have
been another base for the measurement of degree of
sensitization. Nevertheless, lack of a normalization
parameter for imin and the difficulty with more than
one cause for observed effects made this only a
tentative conclusion.
DL-EPR
Features of the surface tested, as revealed by
SEM and curves of current density vs potential, are
presented in Figure 8.

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(a) (b)

(c) (d)

(e) (f)
FIGURE 8. Scanning micrograph of specimens surfaces and current density vs potential curves obtained in DL-EPR test
for different heat treatment conditions: (a) and (b) as-quenched, (c) and (d) tempered at 550°C (823 K), and (e) and (f)
tempered at 700°C (973 K).

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The surface of specimens as-quenched and tem-

pered up to 450°C (723 K) did not show etching or
corrosion evidence. Even polishing scratches were
unchanged (Figures 8[a] and [b]).
Specimens tempered at 500°C (773 K) and 550°C
(823 K) were etched along grain boundaries and
martensite lath interfaces. Scratches of SiC paper
polishing were lightly visible (Figures 8[c] and [d]).
The etching effect showed that the DL-EPR test
could detect chromium-impoverished regions in
UNS S41000, like potentiostatic and potentiokinetic
polarization tests.
In specimens tempered at higher temperatures,
the DL-EPR also produced etching along original
austenite grain boundaries and martensite lath inter-
faces, but shallower than that produced in material
tempered at 550°C (823 K). The specimen tempered
at 700°C (973 K) did not show localized corrosion
and was etched evenly (Figures 8[e] and [f]). Uniform
corrosion was indication of a general impoverishment FIGURE 9. Values of Ir/Ia for different tempering temperatures
of chromium in solution. The observation suggested obtained in DL-EPR test.
diffusion of chromium from the bulk of the grain into
carbides and/or initially impoverished areas in these
high-tempering temperatures. The material was not
prone to localized corrosion, but was less resistant to
general corrosion.
Three DL-EPR tests for each condition were per-
formed, producing similar curves. Important points
in the curves were the two current density maxima:
Ia and Ir. Analysis was made with the ratio Ir/Ia.
In the reversion stage, reactivation of the surface
happened mainly in chromium-impoverished regions.
If the material was not sensitized, passive film
remained and the reactivation peak was small or
absent. The reversion peak always should be lower
than the activation peak, because in the later, the
whole surface is active. In material tempered at
550°C (823 K), the reactivation peak was higher than
the activation peak. This could be explained by the
asperity of the etched surface increasing the effective
surface area.
Figure 9 gives values of Ir/Ia for different temper-
ing temperatures. The graph was similar to those
FIGURE 10. Comparison among electrochemical tests to discriminate
produced by other tests, suggesting that the DL-EPR
degrees of sensitization for different tempering temperatures.
test measures also degrees of sensitization.
Characteristic values are Ir/Ia for the DL-EPR, imin for the potentiostatic
test, and i2max/icrit and Q2max/icrit for the potentiokinetic polarization. To
Degrees of Sensitization make different tests comparable, the ratio was plotted between the
Evaluated by Different Tests characteristic value for the material tempered at different temperatures
Figure 10 presents results of different types of and the same for the material tempered at 300°C.
tests made. In the vertical axis are ratios between
values that characterize degrees of sensitization and
values for the state tempered at 300°C (573 K). This Results of the potentiostatic etch showed also a
state was chosen as reference because it was not good discrimination between different states. Never-
sensitized. In the horizontal axis are the tempering theless, lack of normalization of imin should be borne
temperatures. in mind.
Differences between maxima and minima in the Potentiokinetic polarization results also showed
ratios showed that the DL-EPR test had the best dis- discrimination between degrees of sensitization,
crimination for different degrees of sensitization. although the peak was lower than the one of DL-EPR.

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All the tests were enough for detection of differ-
ences in the corrosion behavior of UNS S41000 in
different quenched and tempered conditions. Each
test also measured degrees of sensitization in differ-
ent tempering temperatures.
In all instances, observations could be inter-
preted in terms of chromium impoverishment,
suggesting that the study may be a model for the
detection and evaluation of sensitization in other
martensitic stainless steels.
CONCLUSIONS
❖ Martensitic stainless steel UNS S41000 tempered
for 2 h at temperatures 500°C (773 K) or higher was
sensitized. Maximum degree of sensitization mea-
sured by electrochemical tests occurred in specimens
tempered at 550°C (823 K).
❖ Results of corrosion tests, for materials tempered
between 500°C (773 K) and 700°C (973 K), could be
explained by the chromium-impoverishment mecha-
nism and recovery.
❖ Electrochemical tests (potentiokinetic, potentio-
static, and DL-EPR) and SEM observations identified
chromium-impoverished regions along grain bound-
aries and martensite lath interfaces.
❖ All the electrochemical tests could be used to
evaluate quantitatively different degrees of sensitiza-
tion as a function of tempering temperature. The
DL-EPR method was the best to discriminate degrees
of sensitization.
ACKNOWLEDGMENTS
The authors acknowledge CNPq (Council for
Scientific and Technological Development/Brazil) for
financial support under Project #300020/93-7.
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CORROSION–AUGUST 1999