Failure Analysis of Stainless Steel Heat

Exchanger Tubes in a Petrochemical Plant

D. N. Adnyana

Journal of Failure Analysis and

Prevention

ISSN 1547-7029
Volume 18
Number 2

J Fail. Anal. and Preven. (2018)

18:413-422
DOI 10.1007/s11668-018-0422-8

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 Author's personal copy
J Fail. Anal. and Preven. (2018) 18:413–422
https://doi.org/10.1007/s11668-018-0422-8
TECHNICAL ARTICLE—PEER-REVIEWED
Failure Analysis of Stainless Steel Heat Exchanger Tubes
in a Petrochemical Plant
D. N. Adnyana
Submitted: 9 November 2017 / in revised form: 21 December 2017 / Published online: 15 February 2018
 ASM International 2018
Abstract A shell and tube heat exchanger had failed its
four tubes after just over a year in service. One of these
tubes was analyzed in this examination. This heat
exchanger is used to transfer heat from steam on the shell
side to slurry on the tube side. The tube material was made
of SA 249 TP 304L, a standard specification for welded
austenitic stainless steel tubes. A failure investigation was
carried out on the leaked tubes by performing a number of
examinations including visual and macroscopic examina-
tion, chemical analysis, metallographic examination,
hardness testing and scanning electron microscopy equip-
ped with energy-dispersive spectroscopy analysis. Results
of the failure analysis showed that the leaked tubes of the
heat exchanger had primarily experienced stress-corrosion
cracking (SCC) in the longitudinal direction caused by the
combined effects of tensile stress and corrosion. Most of
the stress-corrosion cracks initiated at multiple sites of the
external surface of the tubes where corrosion pits and other
surface defects were present. Formation of surface defects
was most likely associated with some excessive contact
and/or collision between tube and adjacent tubes or with
baffles or other support in the heat exchanger. In the early
stage, most of the cracks were not branched, but later
continued by cracks branching in transgranular manner.
Some of the trace elements found on the fracture surface
deposit may have been responsible for the formation of
corrosion pits and SCC on the tubes, acting either alone or
in combination. In addition, at location close to the mul-
tiple parallel cracks in the longitudinal direction, the tube
D. N. Adnyana (&)
Department of Mechanical Engineering, Faculty of Industrial
Technology, National Institute of Science and Technology
(ISTN), Jakarta, Indonesia
e-mail: adnyanadn@yahoo.com
also experienced other multiple parallel cracks, but in its
circumferential direction. None of these cracks had reached
the internal wall of the tube.
Keywords Heat exchanger

Austenitic stainless steel tube

Stress-corrosion cracking (SCC)
Corrosion pits

Transgranular cracks
Multiple parallel cracks
Introduction
Failures in heat exchangers are commonly associated with
methods of manufacturing of tubing, handling methods
during fabrication, testing methods in the shop and in the
field and the total environment to which the unit is exposed
after fabrication, including conditions during shipment,
storage, start-up, normal operation and shutdown [1–3]. In
addition, process fluids and cleaning methods applied to the
heat exchanger may also influence the level of carryover
contaminants that contribute to the corrosion [4].
As in other equipment, stress-corrosion cracking (SCC)
can also occur in the heat exchanger as a result of corrosion
and stress at the tip of a growing crack. The stress level
necessary for SCC is below that needed for fracture with-
out corrosion, and the type of stress may be applied or
residual [4, 5]. Austenitic stainless steel heat exchanger
equipment can also fail by SCC in acidic chlorides and
fluorides or by polythionic acids if the microstructure is
sensitized [5, 6]. In the presence of chlorides austenitic
stainless steel, particularly the AISI type 304 stainless
steel, is generally susceptible to pitting corrosion [6]. In
addition to chlorides, the SCC in austenitic stainless steel is
also influenced by the presence of any caustic environment
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414
containing corrosion agents such as sodium (Na) and/or
potassium (K), especially at high temperatures [7].
This paper presents a failure analysis performed on
leaked tubes of a heat exchanger used in a petrochemical
plant. This heat exchanger had four tubes which fail in just
over 1 year in service. This heat exchanger was a typical
shell and tube heat exchanger with a cross/counter flow
arrangement used to transfer heat from steam on the shell
side to slurry on the tube side. The heat exchanger tubes
laid out in a triangular 60 pattern and mounted together as
a bundle with tube sheets, baffles and tie rods, inside the
cylindrical shell. The operating parameters of the heat
exchanger were as follows: operating pressure in the shell
side was 49.0 kg/cm2g, while in the tube side was
112.2 kg/cm2g; operating temperature in the shell side was
261.5 C (inlet) and 261.2 C (outlet), while the operating
temperature in the tube side was 221.2 C (inlet) and
249.0 C (outlet). The tube dimension was 19.05 mm in
diameter and wall thickness of 2.11 mm, and its material
was SA 249 TP 304L, a standard specification for welded
austenitic stainless steel tubes.
The purpose of this failure analysis was to verify the
material properties and to determine whether the material
used for the heat exchanger tubes met the specification or
suitable for its operating condition. Furthermore, this fail-
ure analysis was also aimed to establish the type, cause and
mode of failure of the leaked tubes of the heat exchanger,
and based on the determination, some corrective or reme-
dial action may be initiated that will prevent similar
failures in future.
Examination Details
In this failure analysis, one leaked tube was pulled out of
the heat exchanger and cut away into two tube pieces, A
and B each of about 750–800 mm in length for laboratory
examination. The tube piece A exhibited multiple parallel
cracks on its surface either in the longitudinal direction
along the tube or in the circumferential direction around
the tube. Tube piece B, which was cut about 2–3 m away
from tube piece A, did not show any visual surface
cracking. Both tube pieces A and B were initially tested
using dye penetrant to identify any crack(s) and subse-
quently cut into several specimens at different locations for
laboratory examination. Macroscopic examination on the
fracture surfaces of the leaked tube samples was performed
using a stereomicroscope. Chemical analysis on the pre-
pared samples was carried out using an optical spark
emission spectrometer. The purpose of this chemical
analysis was to determine whether the material used for the
leaked tube met the specification.
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In addition, metallographic examinations were per-
formed on the prepared samples using an optical
microscope at various magnifications. The metallographic
samples were mounted using epoxy and prepared by
grinding, polishing and etching. The etchant applied was
aqua regia solution. A hardness survey was also carried out
on the same metallographic samples using the Vickers
hardness method at a load of 5 kg (HV5). Moreover,
examination of some fracture surfaces of the leaked tube
samples was performed using scanning electron micro-
scopy (SEM) to determine the fracture surface topography
and nature of the failure. This SEM was also equipped with
EDS (energy-dispersive spectroscopy) analysis to detect
the presence of any corrosion by-product.
Results and Discussion
Visual and Macroscopic Examination
Tube piece A after being tested using dye penetrant clearly
showed two adjacent sets of cracks (see Fig. 1a). Elongated
parallel cracks were observed in the longitudinal direction,
and shorter cracks were also observed in the circumferen-
tial direction. Among the longitudinal parallel cracks
observed, one large longitudinal crack appeared as the
primary crack since through this crack the tube leaking
most likely occurred. In addition to the two sets of cracks,
most of the external surface of tube piece A was severely
damaged by bruises, scratches, wear, cuts, dents, etc. (see
Fig. 1b). Formation of these surface defects may have been
associated with collision, rubbing movement and/or other
fretting contacts that may have occurred between the tube
and adjacent tubes during the heat exchanger operation.
For tube piece B, a similar crack pattern was also
observed after being tested using dye penetrant (see
Fig. 2a). All the cracks in tube piece B were continuations
of the cracks in tube piece A. Similarly, the cracks in tube
B also consisted of elongated cracks in the longitudinal
direction of the tube and shorter cracks in the circumfer-
ential direction. In addition, from the dye penetrant test on
the tube piece B it was found that at a location approxi-
mately 1800 from the primary sets of cracks, some
intermittent parallel cracks formed in the longitudinal
direction of the tube, see Fig. 2b. On this side of tube piece
B, there were no circumferential cracks observed. Multiple
circumferential cracks only formed along the weld seam of
the tube.
Macroscopic examination performed on the external
surface around the tube circumference of tube piece A is
shown in Fig. 2c, showing the longitudinal tube weld seam
and the primary longitudinal crack, together with other
adjacent longitudinal cracks. The weld seam was located
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Fig. 1 Dye penetrant test (a) and surface damage appearance of the tube piece A (b)

Fig. 2 Dye penetrant test on the tube piece B (a) and (b) and macroscopic examination on the external surface of the tube piece A (c)

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approximately 2 mm from the primary crack. This indi- or other surface defects that formed on the outer surface of
cated that formation of the multiple longitudinal cracks of the tube. It is also seen in Figs. 4 and 5 that after the stress-
the tube was not associated with the welding of the tube. corrosion cracks had reached a certain length, the crack
Adjacent to the primary crack, several parallel cracks subsequently continued in a transgranular manner with
formed over the weld seam in the circumferential direction some branching [4–7]. In the sample obtained from tube
(see Fig. 2c). piece B (see Fig. 5), the microstructures obtained were
The typical appearance of the fracture surfaces of the very much similar with those obtained from samples A.
primary crack of tube piece A is shown in Fig. 3. Most of Although somewhat less extensive, all of these parallel
the fracture surface had a brittle appearance and exhibited cracks were typical of SCC. All of these parallel cracks
crack topography consistent with crack propagation originated from some corrosion pits or surface defects on
through the tube wall from the external surface to the the tube external surface until the crack paths had reached
internal surface of the tube. In addition, oxides and cor- some certain length and subsequently continued by crack
rosion products were observed on most of the fracture branching in a transgranular manner.
surface shown in Fig. 3. In addition to the longitudinal parallel cracks formed
adjacent to the weld seam of the tube, the tube pieces A and
Chemical Analysis B had also experienced other cracks located approximately
180 or at the opposite side from the primary cracks, see
The results of chemical analysis obtained from the material Fig. 6. The topography of these cracks was very much
used for the tube pieces A and B in comparison with the similar to the primary cracks in which the crack(s) were
standard material are given in Table 1. It can be seen that originally formed from corrosion pits at the external
all of the elemental contents of the tube pieces A and B are
within or very close to the material specification of SA 249 Table 1 Results of chemical analysis of the tube material of the heat
TP 304L, a standard specification for welded austenitic exchanger in comparison with the standard material
stainless steel tubes [8, 9]. Composition (wt.%)
Measured value
Metallographic Examination and Analysis
Tube Tube Standard material (SA
A number of specimens were prepared from tube piece A at Element piece A piece B Average 249 TP 304L)
different locations. All the macrostructures and Iron 68.8 69.1 68.95 Balance
microstructures obtained were similar from one sample to Carbon 0.0351 0.0244 0.0298 0.03 (max)
another. The macrostructures shown in Fig. 4a and b Manganese 1.53 1.53 1.53 2.00 (max)
clearly exhibit weld seam structure and one large through Silicon 0.289 0.256 0.273 1.00 (max)
wall crack that had caused leakage in the tube. This large Chromium 19.7 19.6 19.65 18.0–20.0
crack appeared to be the primary crack located at Nickel 8.40 8.35 8.375 8.0–12.0
approximately 2 mm from the weld seam. According to the Phosphorus 0.0289 0.0399 0.0344 0.045 (max)
microstructures shown in Fig. 4a and b, this primary crack Sulfur 0.0058 0.0072 0.0065 0.03 (max)
topography was typical of stress-corrosion cracking (SCC) Molybdenum 0.153 0.155 0.154 …
[1–5]. The appearance of this SCC was brittle, and most of Cobalt 0.175 0.168 0.172 …
the cracks were transgranular. The other parallel longitu-
Copper 0.283 0.287 0.285 …
dinal cracks adjacent to the primary crack also showed
Niobium 0.332 0.323 0.328 …
similar topography typical of SCC. As seen in Figs. 4 and
Vanadium 0.139 0.143 0.141 …
5, most of these parallel cracks initiated from corrosion pits

Fig. 3 Appearance of the fracture surfaces of the leaked tube piece A

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(a)
(b)
Fig. 4 (a) Macrostructure and microstructures obtained from some
specimen of tube piece A at location (a), showing one large crack and
other cracks propagated in transgranular manner through the
austenitic grains of the tube material. Most of the cracks originated
from the tube external surface where some corrosion pits were
present. The microstructures also containing several twins and some
dispersed oxides or inclusions and/or other second-phase particles. In
addition, no grain boundary thickening due to formation of chromium
carbides or sensitization was observed. Etched with aqua regia
solution. (b) Macrostructure and microstructures obtained from some
specimen of tube piece A at different location from that obtained in
Fig. 4a, showing similar microstructures with that shown in Fig. 4a.
Etched with aqua regia solution
417
surface of the tube and then propagated by branched SCC
in a transgranular manner through the austenitic grains of
the tube material.
The tube also experienced multiple parallel cracks in its
circumferential direction (see Figs. 1 and 2). In order to
reveal these circumferential cracks in more clearly, some
samples as shown in Fig. 7 were prepared. Most of the
circumferential cracks observed (see Fig. 7a) were trans-
granular and formed over the weld seam of the tube. All the
cracks initiated from the tube external surface either from
corrosion pits or from other stress concentration. Some of
these stress concentrations likely influenced by formation
of bruises, cuts or scratches on the tube surface. In order to
determine the crack length or crack depth of those cir-
cumferential cracks, another sample shown in Fig. 7b was
also prepared and the resulting microstructures are seen in
Fig. 7b. It is seen that the cracks that formed in the cir-
cumferential direction were also probably typical of stress-
corrosion cracking. However, the crack paths tended to be
bulbous with a number of lobes, and the crack tips them-
selves appeared somewhat blunted and filled with oxides
and/or corrosion product [10]. None of these cracks had
reached the inner wall of the tube. Moreover, none of these
type cracks were observed elsewhere on the other tube
surface, including the opposite side of the tube.
Hardness Test and Analysis
Hardness testing on all specimens at different test locations
obtained from tube pieces A and B was performed using
Vickers hardness method at a load of 5 kg (HV5). From the
results obtained, the average hardness values of the weld
metal and the base metal for each sample are summarized
in Table 2.
All the test results shown in Table 2 clearly exhibit that
the average hardness values obtained from all specimens
were ranging from 206 to 233 HV. This hardness level is
approximately higher than the hardness value of the tube
material according to the standard material of SA 249 TP
304L which is at 90 HRB (max) [8, 9]. This relatively high
hardness value obtained most likely influenced by cold
working introduced during fabrication and/or operation of
the heat exchanger. In addition, the relatively high hardness
values obtained may have been associated with the pres-
ence of some dispersed oxides or inclusions and/or other
second-phase particles within the austenitic matrix phase
introduced during the tube manufacturing process [9]. In
general, the tube material having high hardness values may
have reduced its ductility and could promote the material
susceptible to cracking. Although most of the cracks that
had caused the tube failure were due to SCC, the presence
of such imperfections in the tube material may have also
contributed to the acceleration of tube failure in service.
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418
Fig. 5 Microstructures obtained from some specimen of tube piece
B, showing several cracks initiated from multiple sites where
corrosion pits were present. Most of the cracks propagated in
transgranular manner through the austenitic grains of the tube
material. The microstructures also containing several twins and some
SEM Fractography and EDS Analysis
Samples for SEM fractography and EDS analysis were cut
from tube piece A at two different locations. The first
sample was used to examine the fracture surface of the
primary longitudinal crack of the leaked tube from the
outside diameter to the inside diameter. The second sample
was obtained by opening the primary longitudinal crack to
examine its crack surface similar to the first sample. This
second sample was located a few centimeters away from
the first sample.
A SEM microfractograph of the through wall fracture
surface of the first sample is presented in Fig. 8. Most of
the fracture surface topography exhibited a flat and cleav-
age appearance, typical of brittle fracture appearance. This
SEM microfractograph further confirms that the leaked
tube experienced SCC during its operation. The deposits
present on the fracture surface were analyzed using the
EDS technique, and the results obtained are presented in
Fig. 8. The deposits generally contained a number of ele-
ments from which the tube was made such as Fe, Cr, Ni,
Mn, Si and some Al. The deposits also contained oxygen
and carbon as elements that may be coming from some
oxides and/or other surface contamination. From the results
of EDS analysis in Fig. 8, most of the trace elements found
in the deposit included Na, Ca, Cl, Mg, K and S. Similar
test results were also obtained from the SEM/EDS analysis
of the second sample (see Fig. 9) showing the crack
topography initiated from the corrosion pits at the outside
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dispersed oxides or inclusions and/or other second-phase particles. In
addition, no grain boundary thickening due to formation of chromium
carbides or sensitization was observed. Etched with aqua regia
solution
surface of the tube. Most of the fracture surfaces covered or
filled by oxides and/or corrosion product. From the results
of EDS analysis obtained from the second sample (Fig. 9),
most of the trace elements found in the deposits formed
around the outside and inside diameter of fracture surface
included Ca, Na, Mg, S and K.
Some of the trace elements found in both samples of
Figs. 8 and 9 may have been responsible for the occurrence
of SCC on the tubes, acting either alone or in combination.
These trace elements may have entered into the shell side
steam of the heat exchanger due to accidental carryover of
dissolved solids or trapped in the heat exchanger after the
tubing was periodically cleaned by chemical solution
containing such trace elements. Another possible source of
the trace elements may have been the use of contaminated
water during hydrostatic testing.
Conclusions
From the results of the analysis, a number of conclusions
can be drawn as follows:
1. The material used for tubing of the heat exchanger is
very much close to the material specification of SA
249 TP 304L, a standard specification for welded
austenitic stainless steel tubes. The microstructures
obtained showed austenitic grains containing several
twins. In addition, no any grain boundary thickening
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Fig. 6 Microstructures obtained from some specimens of tube pieces A (a) and B (b) at the opposite side from location where the primary crack
formed. Similar microstructures also obtained from that shown in Figs. 4 and 5. Etched with aqua regia solution
due to formation of chromium carbides or sensitization
was observed.
2. The leaked tubes of the heat exchanger had primarily
experienced stress-corrosion cracking (SCC) caused by
the combined effects of tensile stress and corrosion.
All the stress-corrosion cracks obviously initiated from
the external surface of the tube where corrosion pits
and other surface damage were present. The stress-
corrosion cracks had propagated toward the tube
internal wall in a transgranular manner with branching
through the austenitic grains of the tube material. In
addition to SCC, the leaked tubes of the heat exchanger
had also experienced some fretting wear on most of its
external surfaces. Formation of this surface damage
was most likely caused by excessive contact and/or
collision between the tube and adjacent tubes or with
baffles or other supports in the heat exchanger and may
have acted as initiation sites that could promote the
acceleration of SCC failure in the tubing.
3. The trace elements that were found on the fracture
surface deposit of the leakage tube include sodium (Na),
419
calcium (Ca), chloride (Cl), magnesium (Mg), sulfur (S)
and potassium (K). Some of these trace elements may
have been responsible for the occurrence of SCC in the
tube, acting either alone or in combination. The corrosive
trace element(s) may have entered into the heat
exchanger in the shell side steam due to accidental
carryover of dissolved solids or trapped in the heat
exchanger after the tubing was periodically cleaned by
chemical solution containing such element(s). Another
possible source for the presence of any corrosive agents
in the heat exchanger may have been from the application
of contaminated water during the hydrostatic testing.
4. The primary crack that had caused the tube leaks
clearly revealed large and longitudinal cracks extended
along the length of the tube. At locations adjacent to
the primary longitudinal crack, other parallel cracks
also formed in the longitudinal direction of the tube.
All of these longitudinal cracks were apparently
located outside of the weld seam of the tube, the
nearest being the primary fracture which was approx-
imately 2 mm apart from the weld seam.
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Fig. 7 Microstructures obtained from some specimens of tube piece A that revealed multiple parallel cracks in the circumferential direction: (a)
at the external surface and (b) at the transverse section of the tube

Table 2 Results of hardness test obtained from tube pieces A and B approximately around 180 or at the opposite side
using Vickers hardness method from the primary fracture.
Test location Tube piece A (HV) Tube piece B (HV) 6. In addition to the multiple parallel cracks that extended
in the longitudinal direction along the length of the tube,
Base metal (BM) 206–210 214–218 there were also other multiple parallel cracks observed
Weld metal (WM) 221 225–233 in the circumferential direction at a location close to the
primary crack. These cracks formed around the weld
seam of the tube. However, none of these cracks had
5. In addition to the primary fracture and multiple parallel reached the internal wall of the tube. No such cracks
cracks in the longitudinal direction of the tube, there
were observed elsewhere on the other tube surfaces,
were also other longitudinal cracks, but less extensive,
including on the opposite side of the tube.
observed on the tube external surface located

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Element Mass Percentage %

C 18.66
O 23.25
Na 3.49
Mg 0.17
Al 0.44
Si 0.68
S 0.28
Cl 1.53
K 0.29
Ca 0.56
Cr 24.58
Mn 0.98
Fe 22.09
Ni 3.00

Fig. 8 SEM microfractograph of the through wall fracture surface of first sample obtained from the tube piece A and the corresponding EDS
spectrum of elements

Element Mass Percentage %

C 6.62
O 26.52
Na 0.36
Mg 0.29
Al 1.18
Si 2.40
S 0.07
Cl 0.02
K 0.12
Ca 3.29
Cr 34.40
Mn 1.28
Fe 20.86
Ni 2.60

Fig. 9 SEM microfractograph of the through wall fracture surface of second sample obtained from the tube piece A and the corresponding EDS
spectrum of elements

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422
7. All the tube materials that had been tested exhibited
relatively higher hardness values compared to the
allowable maximum hardness value according to the
tube material specification of SA 249 TP 304L. This
relatively high hardness of the tube material was most
likely influenced by cold working introduced during
fabrication and/or operation of the heat exchanger and
could promote the material susceptible to cracking.
Acknowledgments The author wishes to express his gratitude to the
Head and Members of Department of Mechanical Engineering, Fac-
ulty of Industrial Technology of the National Institute of Science and
Technology (ISTN), for their support and encouragement in pub-
lishing this work.
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