-
Accepted ManuscriptRoot Cause Analysis for 316L Stainless Steel
Tube LeakagesS. Kaewkumsai, S. Auampan, K. Wongpinkaew, E.
ViyanitPII: S1350-6307(13)00365-8DOI:
http://dx.doi.org/10.1016/j.engfailanal.2013.11.008Reference: EFA
2198To appear in: Engineering Failure AnalysisReceived Date: 2
August 2013Revised Date: 19 November 2013Accepted Date: 19 November
2013
Please cite this article as: Kaewkumsai, S., Auampan, S.,
Wongpinkaew, K., Viyanit, E., Root Cause Analysis for316L Stainless
Steel Tube Leakages, Engineering Failure Analysis (2013), doi:
http://dx.doi.org/10.1016/j.engfailanal.2013.11.008
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Root Cause Analysis for 316L Stainless Steel Tube Leakages S.
Kaewkumsai*, S. Auampan, K. Wongpinkaew, E. Viyanit
Failure Analysis and Materials Corrosion Laboratory (FAMC),
National Metal and Materials Technology Center (MTEC), National
Science and Technology Development Agency (NSTDA), 114 Thailand
Science Park, Paholyothin Rd., Klong 1, Klong Luang, Pathumthani
12120, Thailand
ABSTRACT
Perforation of ASTM A270 TP316L stainless steel tube, used for
transportation of ozonated high purity water in a pharmaceutical
plant, was discovered after 3 months in actual service. The current
investigation was conducted in order to explore the root causes of
failure. Various techniques including on-site investigation,
emission spectroscopy, ion chromatography, radioscopy, optical
microscopy, scanning electron microscopy, energy dispersive
spectroscopy, and intergranular corrosion testing were implemented
for failure analysis of the tube components. The results revealed
that the perforation of tube was initiated from the outer
wall and extended to the inner wall by pitting corrosion. The
stagnant state of chloride-containing water was the main reason for
inducing such corrosion attack. The weld metal was
the most susceptible to corrosion attack leading to perforation
of the wall thickness, although initiation sites of pitting
corrosion were also observed in the base metal. The dimensions of
each pit mouth are very small, but enlarged subsurface cavities
were observed. The selective dissolution of material due to
galvanic effects between delta-ferrite and the austenite matrix
occurred in the weld zone. It is suggested that failure prevention
could be achieved by
controlling the quality of the insulation system. In addition,
careful control of welding conditions must be implemented during
fabrication.
Keywords: Pitting corrosion; Welding defect; Tubing failure;
Stainless steel
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* Corresponding author. Tel.: +66 2564 6500x4736; fax: +66 2564
6332. E-mail address: [email protected] (S. Kaewkumsai).
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1. Background information A pharmaceutical plant has encountered
the leakage of an ozonated high purity water transfer tube. The
seamless tube was made of stainless steel grade ASTM A270 TP316L
[1]. Each section of tube was connected by manual circumferential
TIG welding with no filler metal. The tube has an outside diameter
of 50 mm and wall thickness of 2 mm. The welding process was
performed according to AWS D18.1 standard and each weld line was
inspected by visual inspection according to ASME BPVC - Section IX.
From the inspection, the qualities of welds were found to be within
the acceptable range. Leak testing of the tubing system was also
conducted at a pressure of 800 kPa for 6 hours using nitrogen gas.
The pressure testing showed no indication of leakages.
The tubing system was horizontally installed with thermal
insulation (EPDM non-halogenated synthetic elastomers) using
chlorine-free glue for joining the insulator material together. The
insulation was also externally wrapped by aluminum jacket with
using silicone for bonding and sealing jacket materials firmly
together. The insulation of tubing system was completely done ahead
of schedule by 4 months. When it was time for plant commissioning
test, plant personnel cleaned the inner wall of the tube system
with hot de-ionized water and were
passivated. After the passivation, the tubing system has been
running with the ozonated high purity water at a temperature of
297-299 K under the pressure of 500 kPa. However, after 3-month
utilization, the leakage was found in the tubes that were installed
outdoors on the plant roof. The perforation of the tube occurred in
a short period of service relative to plant shutdown and
replacement cost. Detailed investigation of the leakage of the
tubes is presented
in this paper.
2. Experimental On-site investigation was conducted to observe
the service conditions to investigate the
leakage site and to consider collection of samples including the
accumulated trap water on the insulator at the bottom of the tube
in the leaked site as well as the corroded specimens for laboratory
testing. After receiving the samples, bulk composition of one of
the failed tubes was determined using a spark emission spectrometer
for comparison with the standard specification. In order to
determine the corrosive species contained in the sample trapped
water, ion chromatography (IC) was used. To determine the nature of
metal loss through the tube thickness, radioscopy was conducted
before taking specimens for microstructure analysis. Surface
analyses were performed both on the outer and inner surface of the
corroded
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tube samples. The physical appearance of the tubes was captured
using a low magnification digital camera for damage analyses. High
magnification observation with a scanning electron microscope (SEM)
was conducted to study the surface morphology. Energy dispersive
spectrometry (EDS) was used for chemical composition analyses of
the substances or particles deposited at the surface. The samples
were then cross-sectioned and prepared for
microstructural analyses following these steps; cold mounting in
resin, grinding with silicon carbide paper, polishing with diamond
suspension, and etching in a glyceregia solution (one part of HNO3
and four parts of HCl with H2O2 as a catalyst). The microstructural
analyses were performed using a reflected light microscope.
Finally, the susceptibility of the weldment
to intergranular attack was conducted in accordance to ASTM A262
[2]. The samples were polished with silicon carbide papers and
subsequently etched in oxalic acid (10%) for 1.5 min after
polishing. The current density was controlled at 1 A/cm2. The
etched surfaces of each sample were studied by optical
microscopy.
3. Results 3.1 Visual examination During on-site investigation,
it was found that the tubing system had 5 parallel lines consisting
of two steam transfer tubes, one waste water transfer tube and two
ozonated water transfer tubes as shown in Fig. 1. The perforation
problem was only found on both ozonated water transfer tubes. Close
observation of the perforated tubing revealed that the aluminum
jacket was defective in that the silicone used for sealing joints
in the jacket was degraded (Fig. 2a), resulting in gaps between the
adjacent sections (Fig. 2b). After removing the jacket and
insulator from the tube, it was found that accumulated stagnant
water was trapped in the insulation as shown in Fig. 2c. It is
believed that the defects in the insulation system allowed the
entry of rain water and condensed moisture which accumulated in the
insulation at the bottom of the tube. The temperature outside the
tube monitored using an infrared thermometer
was 303.6 K (Fig. 2d). The trapped liquid was collected for
evaluation of anions by Ion Chromatography in the laboratory.
Observation on the outer surface of tube revealed the corrosion
attack in many locations. Strongly adhered of black insulator was
also observed on the outer surface. Then, two samples of stainless
steel tubes containing the corrosion pits were cut and removed for
metallurgical examination in the laboratory. They can be divided
into two groups as follows: 1) tube sample with corrosion in the
base metal (as labeled with SC-1) as illustrated in Fig. 3a and 2)
tube sample with corrosion in the weld (as labeled with WD-1) as
shown in Fig. 3b.
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3.2 Chemical analyses Bulk composition of the failed tube sample
using spark emission spectrometer is presented in Table 1. The
results were compared with the specification of ASTM A270 TP316L
according to ASTM standard practice for Seamless and Welded
Austenitic Stainless Steel Sanitary Tubing, A270-03. Based on the
analysis results, they are in agreement with the standard
specification.
Table 1 Chemical composition of the tube sample and standard
grade (wt.%). Element C Mn Si P S Cr Ni Mo Nb Cu N ASTM A270 TP
316L
0.035a 2.0a 0.75a 0.04a 0.03a 16-18 10-15 2-3 - - -
Failed tube 0.03 1.43 0.49 0.03 0.008 16.32 10.07 2.31 0.056
0.319 0.033 a Maximum.
In order to determine the corrosive ions contained in the
accumulated stagnant water, Ion
Chromatography was used to determine the anions in solution.
From this test, the concentration of chloride (Cl-) was 138.73 ppm,
sulfate (SO42-) 78.65 ppm and nitrate (NO3-) 61.96 ppm as presented
in Fig. 4. The presence of chloride ions can result in pitting
attack [3]. Furthermore, the simultaneous presence of sulfate in
the stagnant water could accelerate the
corrosion attack [4].
3.3 Radioscopic inspection From visual inspection of the failed
samples at the site, pitting corrosion was observed in all
samples. Therefore, radioscopy was used to determine the shape
of metal loss through the tube thickness. The results were useful
for considering the location for the samples for microstructural
analyses. Radioscopy of the failed tube sample in the pitted area
reveals large internal pores as shown in Fig. 5. It clearly shows
the evidence of pit centralizing is found to be a group together of
small pits as seen on the outer surface of the weldment.
3.4 Corrosion analyses 3.4.1 Corrosion at the base metal Visual
examination of the SC-1 sample revealed that corrosion pits were
only observed on the outer surface. Corrosion attack did not
penetrate through the wall thickness. Corrosion pits were found in
several areas but specify at the bottom half of the tube.
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Based on the corrosion analysis on the SC-1 sample, only
localized corrosion was found in a form of pitting corrosion which
is distributed around on the outer surface of the tube in the base
metal as shown in Fig. 6a. Strong adherence of black insulator was
also observed (Fig. 6a-b). The results from EDS showed that the
black insulator contained significant concentration of chlorine and
sulfur (Fig. 6c). After removing the black insulator, corrosion
attack was found on the surface of the tube (Fig. 6d). It is
believed that the adhered insulator acts as the preferential
adsorption of the corrosive species from the accumulated stagnant
water. High magnification observations with SEM on the pits show
corrosion characteristics as shown in Fig. 7a-b. The results from
EDS showed that the residue present within these pits
contained significant concentrations of chlorine and sulfur
(Fig. 7c). These elements were not found in the base metal area
(Fig. 7d). Cross-section through the pits (in Fig. 7a-b) indicated
that corrosion attack was initiated from the outer wall and
extended into the material (Fig. 8). The depths of the pitting
corrosion were measured to be approximately 200 and 260 micrometers
(along cross-section A-A and B-B), respectively.
From the corrosion analyses at the base metal, it can be
concluded that pitting had started from the outer surface and
penetrated into the wall thickness at several areas but did
penetrate
the wall. The corrosive species deposited in the pits mainly
contained chlorine and sulfur. The sources of chlorine and sulfur
should be attributed to the rain water or condensed moisture.
3.4.2 Corrosion at the weld Visual examination showed that the
tube sections of the WD-1 sample had been manually circumferential
welded. Rough surfaces of weldment were observed. Corrosion pits
were mostly found at the interface between the weld metal and heat
affected zone (HAZ). Examination the inner surface of the tube
revealed that severe discoloration was noticed in the HAZ region
(Fig. 9), indicating that the region might be sensitized during
welding.
Close examination of the WD-1 sample indicated corrosion attack
at the weld metal adjacent to the HAZ. The outer surface of the
perforation is shown in Fig. 10a. High magnification examination on
the outer surface with SEM found grain boundaries as shown in Fig.
10b probably caused by acid pickling during tube welding. The inner
surface of the perforation is shown in Fig. 10c, no intergranular
corrosion was detected. Comparing the corrosion damage between the
outer and inner surfaces of the tube around the perforation
location, there was more severe corrosion on the outer wall. High
magnification of area 2 in Fig. 10b show
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micro-galvanic corrosion at the interface between the -ferrite
and austenite (Fig. 10d). The small hole and black precipitates
deposited on surface of the weldment were further examined as shown
in Fig. 11a. High magnification of the small hole shows shrinkage
defect (Fig. 11b). High magnification observation with SEM of the
black precipitates deposited area indicated the presence of
skeletal dendritic structure [5] (Fig. 11c). From chemical
composition analysis of the black precipitates by EDS, contaminants
including sulfur and manganese were found (Fig. 11d). They could
segregate to shrinkage area in weld. Cross-section through the hole
indicated that the pitting corrosion occurred at the interface
between the weld metal and HAZ, and extended into the weld metal in
the transverse direction (through thickness), then extended further
into the base metal in the longitudinal direction with irregular
shape like tunnel (along tubing) as shown in Fig. 12a. The
microstructure of the fusion line as shown in Fig. 12a resembles
the cast structure consisting of -ferrite interdendritic structure
in an austenitic matrix. High magnification observation at the
fusion zone revealed general corrosion, which was caused by the
micro-galvanic effect between -ferrite and austenite (Fig. 12b).
This general attack could initiate the preferred sites for growth
of pits [5-6]. This observation indicated that corrosion was
initiated from the outside and propagated to the inner wall. As the
corrosion progresses, the wall thickness will decrease, and
finally, leading to
perforation.
Base on the corrosion analyses at the welds, it can be concluded
that the perforated hole had started from the outer surface and
propagated to the inner surface at the interface between the
weld metal and HAZ. Although the openings of the corrosion pits
are very small, the large subsurface cavities are formed. Grain
boundary corrosion on the outer surface at the HAZ and the black
precipitates containing the elemental sulfur and manganese were
also observed. The microstructure of the base metal was normal
austenitic structure, while the dendritic structure
of -ferrite and austenite was present in the weld. No evidence
of chromium carbide precipitate at the grain boundaries was
observed.
3.4.3 Intergranular corrosion test Due to the presence of grain
boundary corrosion observed in the HAZ of the WD-1 sample,
specimens of this sample were prepared for intergranular corrosion
tests. They were cut from
the base metal and near the weldment areas. The susceptibility
to intergranular attack was conducted in accordance to ASTM A262,
Practice A. It is used to assess the intergranular corrosion
resistance of stainless steel through the three basic morphologies:
step, dual and
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ditch [6]. Based on the test results (Fig. 13), the HAZ and base
material showed no degree of sensitization and were classified as
step. The presence of steps between grains is an acceptable
structure after oxalic acid etching for stainless steel components
[7]. It also confirmed that the stainless steel samples were not
likely to be susceptible to intergranular corrosion attack.
Evidently, chromium carbides were not precipitated at the grain
boundary.
4. Discussion From the experimental results, it is evident that
the tube failed from pitting corrosion mechanism. It is well known
that the susceptibility of austenitic stainless steel to
pitting
corrosion depends on environmental factors [8, 9], their
chemical compositions and metallurgical features. For the
environmental factor, localized corrosion of austenitic stainless
steel; the severity of which chloride can induce depends on the
temperature and pH [10]. Furthermore, the simultaneous presence of
chloride and sulfate in the stagnant water could accelerate the
corrosion attack [4]. Therefore, the presence of sulfates in the
trapped liquid that accumulated in the insulation at the bottom of
the tube as shown in Fig. 4 increase the susceptibility of
stainless steels to pitting corrosion.
In stagnant waters with the presence of corrosive species, the
corrosion resistance of stainless steels could be decreased due to
lower protective film stability, which leads to pit initiation. In
the present study, the stagnant trapped water (Fig. 2c) could
result from the defective insulation system as observed during
onsite investigation (see Fig. 2a-b). It is believed that the
initial source of accumulated water could come from the diffusion
and/or the penetration of condensed moisture/rain water through the
defective joints in the insulation. Most likely, leaked water from
the tube interior could increase the volume of accumulated water.
Furthermore, chemical analysis indicates that the trapped water
contains Cl- (138.73 ppm), SO42- (78.65 ppm) and NO3- (61.96 ppm).
These results are consistent with the EDS analyses of the deposit
present within the corroded area, which contains significant
concentrations of chlorine and sulfur (see Fig 7c). The adhered
insulator could facilitate the adsorption of corrosive species as
suggested by EDS results (Fig. 6c) since the thermal insulation was
made of non-halogenated synthetic elastomers and the glue for
joining the insulating material together was chlorine-free, the
source of chloride and sulfate must have come mainly from the rain
water or condensed moisture.
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Pitting morphology was clearly observed on both the base metal
and the weld metal. The most severe attack, complete penetration
through wall thickness, was found at the weld metal whereas the
base metal suffered only from pitting not complete perforation. In
many cases, welding decreases corrosion resistance of metal
[11-12]. In this case, the austenitic base metal, which has higher
corrosion resistance, was changed to dual austenite-ferrite
microstructure in the weld area. When the welded tube is exposed
in the electrolyte, the weld metal therefore acts as an anode
whereas base metal acts as a cathode leading to preferential attack
at the weld. The rate of localized attack is very fast in a system
with a large cathode (base metal) and a small anode (weldment) [13]
as in this case. Welding can also alter the stability of the
passive layer and its corrosion behavior [12, 14]. When the
affected area is exposed to the corrosive environment, the defect
sites on passive film could promote the localized corrosion such as
pitting corrosion [11, 15]. The residual stresses introduced in
weld metals could enhance the contribution factor of corrosion
attack in the weld [2]. However, correct weld anneal along with the
carefully surface cleaning after welding could prevent this problem
[16]. In the case of stainless steel, welds and HAZ are most
susceptible to pitting corrosion [17]. Base metal attack is less
common, although it has been observed as presented in this
case.
Examination of the weld metal at the leaked site revealed the
grain boundaries corrosion surface as shown in Fig. 10b. Such
evidence indicated that the protective film was imperfect and
inhomogeneous. Onsite welds are usually welded from the exterior of
the tube using
shielding gas inside. Normally, it is difficult or even
impossible to clean the root of the weld after welding properly. If
the shielding gas contains even a relatively small amount of
oxygen, heat tint layers (discoloration) will be formed close to
the weld as seen on the inner surface of the tube in Fig. 9. The
outer surface probably experienced the same degree of
discoloration, but it has been removed by abrasive treatment or
acid pickling. These heat tint layers could
promote the initiation and growth of corrosion pits even in
seemingly harmless environments. Furthermore, improper cleaning of
the heat tint could generate intergranular corrosion as seen in
Fig. 10b although the results from evaluation of the corrosion
behavior of the weldment show that there was no susceptibility to
intergranular corrosion (Fig. 13). However, the presences of
inhomogeneous surface at the weld metal are susceptible areas for
chloride induced pitting corrosion [2, 18].
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Cross-sectional analyses through pits at the welds indicated
that the initiation of pitting started from the outer surface of
the tube and propagated toward the inner surface. Surface analyses
of the failed area revealed that the openings of the corrosion pits
are very small but cross-section of the pit showed networks of
interconnecting tunnels through the tube wall (see Fig. 12a).
Corrosion propagation tends to be migrating downward and slightly
to the sides rather than straight down through wall thickness. Such
evidence could further confirm by the results from radioscopy as
shown in Fig. 5. It differs from the general pitting morphology,
which is normally spherical in nature, but, in this finding, pits
are of irregular shape. From the results, it is suggested that the
pitting corrosion at the weld is very dangerous for engineering
structure because sometimes there were no clear evidence of
corrosion attack on the outer surface, but inside the material was
very severe attack.
Autogenous welding, without adding filler metal, of the
austenitic stainless steel produced a fusion zone with a dendritic
structure of chromium-rich delta ferrite in a Ni-rich austenite
matrix [16]. Such structure is generated from the high cooling rate
of fusion line after welding. From chemical composition of the
failed tube as shown in Table 1, the chromium and nickel
equivalents can be calculated to predict the ferrite content in
fusion zone according
to the WRC-1992 [15] as follows;
Creq = Cr + Mo + 0.7Nb = 16.32 + 2.31 + 0.7(0.056) = 18.67 Nieq
= Ni + 35C + 0.25Cu + 20N = 10.07 + 35(0.03) + 0.25 (0.32) +
20(0.033) = 11.86
From this calculation the amount of delta ferrite in fusion zone
is about 7%. The presence of 3-8% delta ferrite is optimal to
reduce hot cracking [19]. However, this amount of Cr-rich delta
ferrite could contribute to general corrosion and pitting corrosion
susceptibility of the weld [17]. Microstructural analysis through
the weld metal indicated the general corrosion of the fusion zone,
as seen in Fig. 12b, results from micro-galvanic effects between
delta ferrite and austenite matrix. The high content of chromium in
delta ferrite, in turn causes Cr depletion in the adjacent
austenite matrix, making the material very sensitive to localized
corrosion. Therefore, corrosion at the fusion zone is localized and
acts as the initiation mechanism for pitting.
From the discussion above, it is clear that the defective
insulation and the presence of stagnant chloride containing
solution caused to the perforation of the ASTM A270 TP316L
stainless
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steel tube by pitting corrosion. The presence of dual delta
ferrite/austenite phases and welding defects in the weld metal
could lead to the fast rate of tube leakage. Thus, the leakage of
tube in this case occurred in a short service life.
Therefore, to prevent such failure from occurring in the future,
it is necessary to keep the
thermal insulation free from gaps at the joints to prevent the
surrounding corrosive media from reacting with the tube surface.
High quality welding to ensure the delta ferrite content as well as
prevention of trapped liquid is also highly advisable. Post-weld
annealing will increase the intergranular corrosion resistance as
well as decrease the susceptibility to general
corrosion at the fusion zone [11, 16]. To ensure that the tube
and weld are free from defects i.e. porosity, cavity, and etc., the
non-destructive testing technique such as radiography, etc., is
recommended before implementing the components in service.
5. Conclusions The ASTM A270 TP316L stainless steel tube was
leaked due to pitting corrosion. Leakage of the tube was initiated
from the outside and propagated toward the inside. The rapid rate
of wall penetration resulted from defects and discontinuities in
the weld metal. It is recommend
that the thermal insulation be kept free from gaps at the joint
and the quality of welding be closely monitored to prevent this
failure from occurring in the future.
Acknowledgment
The authors are grateful to Dr. John T. Harry Pearce and Dr.
Amnuaysak Chainpairot for valuable comments and Failure Analysis
and Materials Corrosion Laboratory, MTEC for support the testing
instruments.
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(ASTM A262, ASTM Standards, 1998. [3] Wu W, Cheng G, Zhu W, Xu
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Captions for Illustrations Fig. 1. The tubing systems have 5
parallel lines consisting of two steam transfer tubes, one waste
water transfer tube and two ozonated water transfer tubes.
Fig. 2. (a) The degradation of silicone used for joining and
sealing sections of insulation jacket (b) the gap between the
overlapped insulation jackets and (c) the stagnant trapped water
under the insulator and (d) surface temperature of the tube. Fig.
3. Stainless steel tube samples for analysis: (a) samples with
corrosion in the base metal and (b) samples with corrosion in the
welds. Fig. 4. Chromatograph showing the anions of the trapped
water. Fig. 5. Radioscopic image of the pitting area of the failed
tube sample showing a large internal defect (white spots). Fig. 6.
Corrosion of the SC-1 sample: (a) pitting corrosion in the base
metal on the outer surface of the tube (b) SEM photograph showing
pitting corrosion on the strongly adhered insulation (c) EDS
spectrum of the black insulator and (d) corrosion attack under the
insulation. Fig. 7. Microanalyses of the SC-1 sample: (a-b) SEM
photographs showing pitting on the outer surface and small
particles depositing in the holes (c) EDS spectrum of the residue
within the pit showing significant concentrations of chlorine,
sulfur, silicon and aluminum and (d) EDS spectrum of the normal
area.
Fig. 8. Cross-section through the pits of the SC-1 sample
showing morphologies of the pits initiated from the outer surface:
(a) along cross-section A-A in Fig. 7a and (b) along cross-section
B-B in Fig. 7b.
Fig. 9. Severe discoloration on the inner surface of the HAZ of
WD-1 sample. Fig. 10. Corrosion characteristic of WD-1 sample: (a)
The perforation was initiated on the outer surface at the interface
between the weld metal and HAZ (b) grain boundary corrosion was
found near the perforation (c) the characteristics of the inner
surfaces around the perforation and (d) high magnification image of
area 2 in Fig. 10b showing micro-galvanic corrosion at the
interface between the -ferrite and austenite structures.
Fig. 11. (a) the small hole and black precipitates deposited on
surface of the weldment (b) High magnification image of the small
hole show a shrinkage (c) high magnification image of the black
precipitates deposited area indicated the presence of skeletal
dendritic structure and (d) chemical analysis of the black
precipitates showing contaminants including sulfur and
manganese.
Fig. 12. Cross-section through the pit of WD-1 sample: (a) the
network of interconnecting tunnels within the tube wall and (b) the
general corrosion caused by the micro-galvanic effect between
-ferrite and austenite structures.
Fig. 13. The HAZ and base material showed zero degree of
sensitization and were classified as step structure according to
ASTM A262.
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Fig. 1.
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Fig. 2.
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Fig. 3.
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Fig. 4.
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Fig. 5.
Fig. 6.
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Fig. 7.
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Fig. 8.
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Fig. 9.
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Fig. 10.
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Fig. 11.
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Fig. 12.
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Fig. 13.
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13/12
The highlight in this article are consists of;
1. The initiation of pitting was propagated anti-gravity and
only found at the bottom half of the tubes.
2. The rapid rate of wall penetration resulted from defects and
discontinuities in the weld metal.
3. The perforation of the tube occurred in a short service time
relative to downtime and replacement cost.