\
PERGAMON Corrosion Science 30 "0888# 558Ð573
The corrosion behavior of AISI 209 stainless
steel in thiosulfate ion containing saturated
ammonium chloride solution
Hong!Shi Kuoa\ Hsing Changb\ Wen!Ta Tsaia\
a
Department of Materials Science and Engineering\ National Cheng Kung University\ Taiwan\ 69090\
R[O[C[
b
Re_ning + Manufacturing Research Center\ Chinese Petroleum Corporation\ Taiwan\ R[O[C[
Received 15 February 0887^ accepted 10 September 0887
Abstract
The e}ect of thiosulfate ion on the corrosion behavior of 209 SS in saturated ammonium
chloride and 4 M sodium chloride solutions\ with or without the addition of 9[90 M sodium
thiosulfate\ was investigated[ Potentiodynamic polarization curves showed that a delayed
pitting corrosion was found in saturated ammonium chloride solution as compared with that
in 4 M sodium chloride solution[ The addition of 9[90 M sodium thiosulfate to the saturated
ammonium chloride solution caused a substantial e}ect on the electrochemical behavior[ At
the potential in the range of −9[24 to ¦9[04 V\ both the anodic polarization curves and the
microscopic observation indicated that S1 O 2 participated in the electrochemical reactions[
The anodic current density increase sharply and sul_de was formed on the specimen surface in
this potential range[ However\ once the potential was greater than 9[04 V\ the current density
decreased and a secondary passive behavior exhibited in the polarization curve[ The synergistic
e}ect of Cl− and S1 O
2 on pitting corrosion of 209 SS is also discussed[ Þ 0888 Elsevier Science
Ltd[ All rights reserved[
Keywords] Stainless steel^ Ammonium chloride^ Sodium thiosulfate^ Corrosion^ Sul_dation
0[ Introduction
Corrosion resistance of stainless steels"SSs# in sodium chloride solutions has been
an important subject of investigation in the past[ In oil re_nery systems\ ammonium
and sulfur may be present in the crude oil with high concentration of chloride ions
Corresponding author[ E!mail address] wttsaiÝmail[ncku[edu[tw "Wen!Ta Tsai#
9909!827X:88:, ! see front matter Þ 0888 Elsevier Science Ltd[ All rights reserved[
PII] S 9 9 0 9 ! 8 2 7 X " 8 7 # 9 9 0 2 6 ! 0
569 H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573
Table 0
Chemical composition of 209 SS used
Cr Ni Si Mn P S Cu Mo V C Fe
Wt) 14[7 08[22 9[54 0[68 9[910 9[995 9[06 9[32 9[02 9[907 bal[
ð0Ł[ The e}ect of thiosulfate ion on the corrosion behavior of stainless steels in chloride
containing solution has been extensively investigated recently ð1Ð6Ł[ However\ there
is limited information on the corrosion of stainless steel in ammonium chloride
solution without the presence of thiosulfate ion ð7Ł[ Hence\ the investigation on the
e}ect of thiosulfate ion on the corrosion behavior of stainless steel in ammonium
chloride solution is of particular interest[
It has been reported that 205 SS could be passivated in ammonium sulfate solution[
However\ the addition of chloride ion to the above environment could destroy its
passivity and cause pitting corrosion ð8Ł[ In a most recent study\ it was found that in
ammonium chloride solution 205 SS has a higher pitting potential and a lower
anodic passive current density than those in sodium chloride solution of the same
concentration ð09Ł[ In SO
3 :S1 O 2 solutions\ Newman et al[\ reported that pitting
corrosion would not occur on AISI 205L SS unless the chloride ion was present ð2Ł[
Furthermore\ in sodium chloride solution with the addition of sodium thiosulfate\
enhanced pitting corrosion as compared with that found in pure sodium chloride
solution was reported ð1\ 19\ 10Ł[ Although thiosulfate anions alone have not been
found aggressive enough to cause damage to stainless steel\ they have been shown to
act in synergy with other common ions\ such as chlorides or sulfate ð00\ 10Ł to cause
severe localized corrosion[ Whether the synergistic e}ect of Cl− :S1 O 2 still exists on
pitting corrosion of a more pitting resistant high Cr austenitic stainless steel such as
209 SS is of interest[ Furthermore\ the mechanism for the combined action of chloride
and thiosulfate are still not clear yet[ Hence\ in this study\ the e}ect of thiosulfate ion
on the corrosion behavior of 209 SS in saturated ammonium chloride solution is
explored[ The roles of ammonium and thiosulfate ions on pitting corrosion are of
particular interest[
1[ Experimental procedures
1[0[ Specimen and electrolyte preparations
Cold!rolled AISI 209 stainless steel plate in sheet form of 1 mm thickness was used[
The chemical composition is given in Table 0[ The specimens were cut from stainless
steel sheet to a dimension of 19×19×1 mm and the specimen was abraded on one
surface to a 799 grit _nish\ then ultrasonically cleaned in distilled water\ and dried with
air jet[ The working surface was partially masked with anti!acid tape\ leaving a 0 cm1
area exposed[ A copper wire was connected to each specimen for electric conduction[
H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573 560
All solutions were prepared from reagent grade chemicals and distilled water[
Saturated ammonium chloride solution "½5 M# was prepared 37 hr before test[ The
pH was measured to be in the range of 4 to 5[ Sodium thiosulfate with a concentration
of 9[90 M was added to saturated ammonium chloride solution just prior to each test[
The solution temperature was controlled at 1121>C[
1[1[ Electrochemical tests
Before electrochemical measurements\ the specimens were immersed in dilute
sodium hydroxide solution and under an applied potential of −1[9 V:04 min for
cathodic cleaning[ The potentiodynamic tests were conducted at a scan rate of
9[4 mV:s from −0[9 V toward the noble potential in deaerated solution[ The instru!
ments used were an EG+G Model 251 electrochemical system coupled with a Yok!
ogawa LR3009 recorder to monitor the potential and current during the experiment[
A saturated calomel electrode"SCE# was used as the reference electrode[ In all tests\
the solution in the cells were deaerated by purging argon for 1 h before and during
the measurements[
1[2[ Surface analysis
For further understanding the corrosion reaction of 209 SS in the testing solution
at a _xed potential\ potentiostatic test was also employed[ After potentiostatic tests\
the specimens| surfaces were examined using scanning electron microscopy "SEM#
and analyzed the chemical state of corrosion product using X!ray photoelectron
spectroscopy"XPS#[
The XPS analyses were performed with a VG ESCA 109 instrument\ with excitation
by Mg!Ka radiation "hy 0142[5 eV#[ The binding energies were calibrated against
the binding energy of C "0s# "hy 173[5 eV#[
2[ Results
2[0[ Electrochemical tests
Figure 0 shows the potentiodynamic polarization curve of 209 SS in saturated
ammonium chloride solution with and without 9[90 M sodium thiosulfate addition[
The results show that 209 SS exhibits a wide passive potential range with an extreme
low anodic current density "½1×09−5 A:cm1# in saturated ammonium chloride solu!
tion[ Pitting corrosion potential was found to be 9[5 V[ In the same environment\ the
pitting corrosion potential of 205 SS was found to be 9[0 V ð09Ł[ These results indicated
that 209 SS was more resistant to pitting corrosion than 205 SS in saturated
ammonium chloride solution[
A dramatic change in the polarization behavior occurred\ as shown in Fig[ 0\ when
9[90 M sodium thiosulfate was added to the saturated ammonium chloride solution[
The polarization curve shows that 209 SS could still be passivated in this environment[
561 H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573
Fig[ 0[ Potentiodynamic polarization curves of 209 SS in ammonium chloride solution with or without
sodium thiosulfate addition[
But a sharp increase in the current density took place at −9[24 V[ The anodic current
density increased rapidly up to −9[04 V\ and then became less rapidly till 9[04 V[
Immediately beyond this potential\ a sharp decrease in the anodic current density of
approximately two order of magnitude was observed[ The second passive region
extended to 0[0 V until the transpassive reaction occurred[
For comparison purpose\ the potentiodynamic polarization curves of 209 SS in 4 M
NaCl solution were also determined "Figure 1#[ As can be seen in this _gure\ the
corrosion potential of 209 SS in concentrated NaCl solution was −9[65 V\ which was
9[11 V more negative than that in saturated ammonium chloride solution "−9[43 V#[
Furthermore\ the passive potential range of the former case was not so wide as that
found in the latter case[ The _lm breakdown potential for pitting corrosion was −9[0 V
in NaCl solution[ The changes in corrosion potential\ pitting corrosion and the passive
potential range were obviously associated with the cations presented in the chloride
containing solution[ In saturated ammonium chloride solution\ the higher corrosion
potential determined as compared with that in 4 M NaCl solution was due to the lower
solution pH of the former case[ On the other hand\ the adsorption of ammonium ion
on the stainless steel surface may reduce the surface concentration of chloride ion and
eventually causes a delay in pitting corrosion[ The wide and extended passive potential
range found for 209 SS in saturated ammonium chloride solution may thus be explained[
The e}ect of 9[90 M sodium thiosulfate addition on the potentiodynamic pol!
arization curve of 209 SS in 4 M NaCl solution was similar to that found in saturated
ammonium chloride solution[ They have almost the same feature as can be seen in
Fig[ 0 and Fig[ 1[ At the potential where a rapid increase in current density occurred\
H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573 562
Fig[ 1[ Potentiodynamic polarization curves of 209 SS in 4 M sodium chloride solution with or without
sodium thiosulfate addition[
a black corrosion product was found to precipitate on the specimen surface[ However\
as the potential was higher than 9[04 V\ the corrosion product disappeared[
Figure 2 shows the current density vs[ time curve of 209 SS polarized at −9[1 V in
saturated ammonium chloride solution[ The result showed that the current density
decreased drastically at the early stage when the potential was polarized at −9[1 V[
The decrease in current density was associated with the formation of passive _lm[
The current density then reached a steady state of approximately 9[4 mA:cm1[ Several
current density peaks were found in the steady state region[ These peaks were believed
to be associated with the formation of metastable or unstable pits formed on the
surface\ which repassived rapidly[ Once 9[90 M thiosulfate was added to the saturated
ammonium solution\ the anodic current density was upturned and more peaks
appeared with high frequency than that without thiosulfate addition "Fig[ 2#[ About
799 s after the addition of 9[90 M thiosulfate ion\ the current density started to raise
sharply as can be seen in Fig[ 2[ The surge of current density was due to the formation
of a large number of pits on the specimen surface[ This observation indicated that
thiosulfate ion could assist the initiation of pit[
2[1[ SEM micro`raph
To further elucidate the electrochemical reaction occurred and the corrosion prod!
uct formed in the potential range of −9[24½9[04 V\ potentiostatic test was conducted
in thiosulfate containing ammonium chloride solution at −9[1 V[ Figure 3"a# shows
the SEM micrograph of the specimen held in the above environment at −9[1 V for
563 H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573
Fig[ 2[ The current density vs[ time of 209 SS prepolarized at −9[1 V in plain ammonium chloride solution
and then added sodium thiosulfate to bulk solution[
29 s[ This micrograph shows that some pits had already been formed for a time as
short as 29 s[ Discrete spots in black color were also found on the specimen surface[
These black spots were the positions where sul_des were formed[ As the holding time
increased to 4 min\ the specimen surface was covered with a layer of sul_de[ After
cleaning the specimen in 19) nitric acid to remove the surface corrosion product\ a
signi_cant number of pits were found on the specimen surface ðFig[ 3"b#Ł[ But most
of the pits were of the same size with only a few number of large pits[ It was noted
that these large pits had a low aspect ratio[ The high rising of the anodic current
density observed in the potentiodynamic polarization curves in thiosulfate!containing
chloride solutions could also be associated with the formation of pits[ As the holding
time was further increased to 04 min\ thick and loose corrosion products were found
on the specimen surface ðFig[ 3"c#Ł[ The specimen was then immersed in 19) nitric
acid to remove the sul_de on the surface[ The surface was again examined under SEM
with the micrograph shown in Fig[ 3"d#[ Crystallographic etching was manifested in
this micrograph showing the grain and twin boundaries as well as some etch pits[
Interestingly\ as compared with that shown in Fig[ 3"b#\ the large pits did not grow
in size and the small pits disappeared indicating the nature of uniform corrosion[
2[2[ XPS analysis
The XPS spectra of pure Ni2S1 "88[6)\ Aldrich Chemicals# and NiS"88[8)\ Strem
Chemicals# powder are shown in Fig[ 4[ The standard binding energies of Ni2S1\ NiS
analyzed in this study and those obtained in the literature ð05\ 06Ł were summarized
H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573 564
Fig[ 3[ SEM micrograph showing the surface morphology of 209 SS after being held in saturated
NH3Cl¦9[90 M Na1S1O2 solution at −9[1 V "a# for 29 s\ "b# for 4 min and immersed in 19) nitric acid to
remove the surface corrosion product\ "c# for 04 min\ and "d# for 04 min and immersed in 19) nitric acid
to remove the surface corrosion product[
in Table 1[ The XPS spectra recorded after the electrochemical treatment at −9[3 V
are shown in Fig[ 5[ For nickel species\ the binding energy of 741[7 eV represented
the existence of metallic state of nickel[ No combined forms of nickel were identi_ed
in the XPS analysis at −9[3 V[ For sulfur species\ the peaks at 057[5 eV and 051[4 eV
represented the adsorption of S1 O 21− ion on the specimen surface after being polarized
in the above solution at −9[3 V for 04 min[ There was no sul_de detected\ indicating
the absence of sul_dation of the 209 SS[ As revealed in Fig[ 0\ the specimen would be
in passivated state at −9[3 V\ and the passivation was mainly attributed to the
formation of oxide _lm[
Figure 6 shows the XPS results for the specimen held at −9[1 V for 04 min[ As
mentioned early\ a black layer of corrosion product precipitated on the surface of 209
SS[ The binding energies of Ni"1p2:1# and Ni"1p0:1# were 745[7 eV and 751[3 eV\
565 H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573
Fig[ 4[ "a# XPS spectra of pure Ni2S1 powder[ "b# XPS spectra of pure NiS powder[
H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573 566
Fig[ 4[*continued[
567 H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573
Table 1
Binding energy of nickel and sulphur in various compounds
Region Compound Binding energy Ref[
Ni Ni9 741[7 ð05Ł
Ni"OH#1 745[3 ð05Ł
Ni2S1 Ni"1p2:1# 745[2 our work
Ni"1p0:1# 750[7
NiS Ni"1p2:1# 745[7 our work
Ni"1p0:1# 751[3
S S1 O 21− peripheral 051[4 ð06Ł
central 057[4
Ni2S1 051[4 our work
NiS 052[1 our work
respectively\ corresponding to Ni in the form of NiS[ The binding energy of S"1p#
was 052[1 eV\ consistent with that of NiS[ These results are summarized in Table 1[
The XPS spectra for the specimen potentiostatically polarized at ¦9[3 V are shown
in Fig[ 7[ The results showed that only Ni "met[#\ Ni"OH#1\ and S1 O
2 were identi_ed
while sul_de was not observed[ As shown in Fig[ 0\ 209 SS was in the secondary
passive state in saturated NH3Cl¦9[90 M Na1S1O2 solution with the potential higher
than ¦9[04 V[ Under this condition\ NiS was no longer stable and oxidized to form
Ni"OH#1[
3[ Discussion
It has been reported that austenitic stainless steels\ such as 293 SS\ 205 SS and 210
SS\ etc[\ could be passivated in plain thiosulfate solution without the occurrence of
pitting corrosion ð1Ł[ But with the presence of NaCl\ enhanced pitting corrosion was
found[ In this investigation\ similar behavior was observed for the high Cr and Ni
209 SS[ But it is interested to note that the cations may also a}ect the corrosion
behavior of austenitic stainless steel by comparing the polarization curves in Fig[ 0
and Fig[ 1[ At almost the same concentration of Cl−\ the presence of ammonium ion
rather than Na¦ could assist the passivation by expanding the passive region more
than 499 mV[ The enhanced passivation was mainly due to the preferential adsorption
of ammonium ion on the specimen surface ð07\ 08Ł[
The addition of 9[90 M sodium thiosulfate to the saturated ammonium chloride
solution caused a substantial e}ect on the electrochemical behavior as revealed in
Fig[ 0[ In the _rst passive region "below −9[24 V#\ the XPS analysis showed that no
sulfur!containing metallic compounds were found\ indicating no involvement of
S1 O
2 on the electrochemical reactions[ But with the potential in the range of −9[24
to ¦9[04 V\ both the anodic polarization curves and the microscopic observations
H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573 568
Fig[ 5[ XPS analysis of 209 SS after held in saturated NH3Cl ¦9[90 M Na1S1O2 solution at −9[3 V "SCE#
for 04 min[
579 H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573
Fig[ 6[ XPS analysis of 209 SS after held in saturated NH3Cl ¦9[90 M Na1S1O2 solution at −9[1 V "SCE#
for 04 min[
H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573 570
Fig[ 7[ XPS analysis of 209 SS after held in saturated NH3Cl ¦9[90 M Na1S1O2 solution at ¦9[3 V "SCE#
for 04 min[
571 H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573
indicated that S1 O
2 participated in the electrochemical reactions[ It is believed that
thiosulfate ion reduced to S"ads# and H1S"aq# on the surface and subsequently reacted
with the dissociated Ni¦¦ to precipitate NiS which was identi_ed by XPS analysis[
The sequence of reactions is explained as following[ At _rst\ S1 O 2 was oxidized to
form S by the following reaction ð01Ł
S1 O ¦
2 ¦5H ¦3ec1S¦2H1 O "0a#
which contributed to the signi_cant increase in the anodic current density as shown
in Fig[ 0[ S1 O
2 might also undergo disproportional reaction ð01\ 02Ł
S1 O ¦ −
2 ¦H cS¦HSO 2 "0b#
¦
to form S and HSO − 2 [ S was further oxidized and incorporated with H according
to the following reaction ð01Ł
S¦1H ¦ ¦1ecH1 S "1#
to form H1S\ which eventually reacted with the dissolved Ni¦¦ to precipitate NiS
according to the following reaction ð03Ł[
Ni1¦¦H1 ScNiS"ads# ¦1H ¦ "2#
It was also possible that the pre!existing metal oxide reacted with H1S to form sul_de
in accordance with the following reaction
MO¦H1 ScMS¦H1 O "3#
The sul_des formed in the potential range of −9[24 V to 9[04 V were thick but with
loose structure as shown in Fig[ 3"c#[ Marcus pointed out that a retardation of
repassivation of stainless steel might happen once sul_de was formed in sulfur!
containing environments ð04Ł[ The loss of passivity might also promote the occurrence
of pitting corrosion on the surface as manifested in Fig[ 3"b and d#[ The increase in
current density in saturated ammonium chloride with 9[90 M sodium thiosulfate
solution in the range of −9[24 to 9[04 V as shown in Fig[ 0 was partially attributed
to the formation of corrosion pits[
At potentials greater than 9[04 V\ the transformation of NiS to form Ni"OH#1
occurred as demonstrated by the XPS analysis[ The results were compatible with that
reported in the potential vs[ pH diagram of Ni!S!H1O system ð04Ł[ It is known that
thiosulfate ion itself would not cause pitting corrosion of stainless steels in aqueous
environments ð1Ł[ However\ with the presence of pitting agent such as Cl−\ an accel!
eration of pitting corrosion would occur[ The synergistic e}ect of Cl− and S1 O 2 on
pitting corrosion of 209 SS is demonstrated in Fig[ 2[ In plain saturated ammonium
chloride solution and at −9[1 V\ 209 SS was in the passivated condition as revealed
in the polarization curve in Fig[ 0[ The initiation of corrosion pits as manifested by
the appearance of peaks in the current density vs[ time curve was observed[ But these
pits were unstable and could not be developed into active pits[ But with the presence
of S1 O
2 \ the embryos of pits could not be repassivated[ As a result\ the pits became
H[!S[ Kuo et al[ : Corrosion Science 30 "0888# 558Ð573 572
stable and continued to grow\ which leaded to an sharp increase in the current density
as shown in Fig[ 2[
4[ Conclusions
0[ The pitting corrosion potential of 209 SS in saturated ammonium chloride "½5 M#
solution was higher than that in 4 M sodium chloride solution[ Enhanced pitting
corrosion was observed\ as indicated by the decrease in pitting corrosion potential\
by the addition of 9[90 M sodium thiosulfate in both chloride solutions[
1[ At less noble potential "³−9[24 V#\ chromium oxide was stable in thiosulfate!
containing chloride solution[ But as the potential was increased to −9[24 V\ the
oxidation of nickel to form sul_de became feasible[ As a result\ an increase in
current density was observed[ At even higher potential "×9[04 V in saturated
ammonium chloride solution\ for instance#\ sul_de dissolved to form a more
protective metal hydroxide\ and consequently caused a reduction in current density
as can be seen in the polarization curves[
Acknowledgements
The authors are very grateful for the support of this research by the Re_ning +
Manufacturing Research Center of Chinese Petroleum Corporation under Contract
No[ 74!06!8039!9091
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