Engineering Failure Analysis 11 (2004) 3–18

www.elsevier.com/locate/engfailanal

Analysis of service stress corrosion cracking in a natural gas

transmission pipeline, active or dormant?
J. Wang, A. Atrens*
Division of Materials Engineering, The University of Queensland (UQ), UQ, St Lucia, 4072, Qld, Australia

Received 1 July 2003; accepted 12 August 2003

Abstract
Stress corrosion cracks (SCC) had been found in a natural gas transmission pipeline during a dig-up and inspection
program. The question was raised as to whether the SCC was active or dormant. This paper describes the resultant
investigation to determine if a particular service crack was actively growing. The strategy adopted was to assess the
appearance of the fracture surface of the service crack and to compare with expectations from laboratory specimens
with active SCC. The conclusions from this study are as follows. To judge whether a crack in the service pipe is active
or dormant, it is reasonable to compare the very crack tip of the service crack and a fresh crack in a laboratory sample.
If the crack tip of the active laboratory sample is similar to that of the service pipe, it means the crack in the service
pipe is likely to be active. From the comparison of the crack tip between the service pipe and the laboratory samples, it
appears likely that the cracks in the samples extracted from service were most likely to have been active intergranular
stress corrosion cracks.
# 2003 Elsevier Ltd. All rights reserved.
Keywords: Stress corrosion cracking; Pipeline failiure; Fractography; Simulation tests; Crack growth

1. Introduction

Stress corrosion cracks (SCC) had been found in a natural gas transmission pipeline during a dig-up and
inspection program. The question was raised as to whether the SCC was active or dormant. This paper
describes the resultant investigation to determine if a particular service crack was actively growing. The
strategy adopted was to assess the appearance of the fracture surfaces of the service cracks and to compare
with expectations from laboratory specimens with active SCC.
This study was based on the following expectation regarding SCC. High pH SCC of pipeline steel is
expected to be intergranular, by a mechanism of active path dissolution, with the crack aspect maintained
by active crack-tip dissolution combined with passive crack sides. Immediate examination of a fresh SCC is
expected to reveal a fracture surface at the crack tip, which has a very thin surface layer consisting of a
passive film and other corrosion products. There would be a gradation of surface layer thickness, with

* Corresponding author. Tel.: +61-7-3365-3738; fax: +61-7-3365-3888.

E-mail address: a.atrens@minmet.uq.edu.au (A. Atrens).

1350-6307/$ - see front matter # 2003 Elsevier Ltd. All rights reserved.
doi:10.1016/j.engfailanal.2003.08.001
4 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18

increasing thickness with increasing distance away from the actively growing crack tip. The surface layer at
the crack tip may be so thin, 2–100 nm, that it is not apparent during examination using optical micro-
scopy and scanning electron microscopy so that the surface looks merely metallic in lustre.
The crack surface is expected to corrode with time, so that the surface layer thickness increases with time,
and the surface layer becomes more obvious. This phenomenom is routinely used in the examination of
fracture surfaces caused by fatigue. A thick obvious surface layer is to be expected for a dormant crack that
has been dormant for a significant period, and has been exposed to a corrosive environment during
that period of dormancy. However, a surface layer indistinguishable from that on an active crack could be
expected for a dormant crack that has been dormant for a significant period, but has not been exposed to a
corrosive environment during that period of dormancy. Conversely, a thick obvious surface layer is to be
expected for an active crack that has been exposed to a corrosive environment during that period between
active cracking and analysis in the laboratory.
Two pipe segments were received at UQ. These segments, designated A1 and A2, measured about
0.30.3 m. The samples were from the same excavation, with sample A1 about 10 m upstream. The pipe-
line had been in service for a considerable time. The SCC was found during a dig-up and inspection pro-
gram and documented in situ. The pipe was coated with luxepoxy and reburied until the pipe segments
were extracted for the present analysis. After cutting out the segments, the luxepoxy was removed by grit
blasting, and the samples sent to UQ.
At UQ, the surfaces of segments A1 and A2 were examined visually, magnetic particle inspection was
used to detect stress corrosion cracks in these two pipe segments and the detected cracks were photo-
graphed. The SCC were subjected to examination using: (1) detailed fractography involving scanning
electron microscopy (SEM) and (2) depth profiling using Auger Electron Spectroscopy (AES).
The examination had the following two aims.

1. From the two coupons cut from the pipeline containing the service SCC, determine whether the SCC
was active or dormant.
2. Evaluate the possibility of taking small cuts from the surface of the pipeline in-situ that would be
suitable for carrying out the above assessment rather than cutting out a coupon.

2. Experimental

2.1. Fractography

The surface was examined and documented for the two pipe segments A1 and A2 in the as received state
to document the location and appearance of the SCC. Typical fracture surfaces were prepared for exami-
nation as follows. The pipe segments were sectioned into smaller segments, these segments were broken
open, and the fracture surfaces were examined using optical and SEM. This also allowed the SCC to be
examined on polished sections. SEM examination was also carried out of the comparison fracture surfaces
from laboratory specimens soon after active SCC in the laboratory.

2.2. Depth profiling

Depth profiling made use of the extreme surface sensitivity of AES. That is, the AES technique provides
information from a very thin surface layer  1 nm in thickness. The AES apparatus included a sputter gun
that allowed sputtering the surface over a controlled area. That is, the material on the surface within a
circle  0.5 mm in diameter was progressively removed, atom layer by atom layer at a controlled rate.
 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18 5

Interrupted sputtering combined with periodic analysis allowed depth profiling in terms of a measurement
of oxygen concentration [O] and iron content [Fe] as a function of sputter time or depth. The sputter time
was converted to an equivalent depth using calibration experiments to measure the sputter rate through
Ta2O5 [1]. The depth profiles were interpreted to give a thickness for the surface oxide layer.

2.3. Laboratory SCC samples

Fresh stress corrosion cracks were produced in the laboratory using the LIST apparatus [2]. The LIST
samples JQ1 and JQ2 were machined from X65 pipeline steel. One side had an ‘‘original’’ surface and the
other side was electropolished. The applied potential was 600 mV selected according to the fast and slow
potentiodynamic scans as shown in Fig. 1. Two kinds of LIST test were performed as shown in Fig. 2. For
sample JQ1, the constant loading rate was 1.9110 3 MPa/s, until the stress exceeded the initiation stress
as determined in reference [3]. Thereafter the loading rate was 1.9110 4 MPa/s until the sample necked.
After the sample necked, the stress was maintained for 3 additional days before the sample was pulled to
fracture. Sample JQ2 was loaded at a constant loading rate of 1.9110 3 MPa/s until the stress
exceeded the initiation stress as determined in our prior work [3]. Thereafter the loading rate was
1.9110 4 MPa/s for about 10 h during the day and then kept constant overnight; then 1.9110 4
MPa/s for about 10 h and then kept constant overnight. This process was repeated four times until
the sample necked during an overnight dwelling, the stress was increased to fracture, the fracture surface
was washed using ethanol and distilled water, and then dried using a hair drier. The fracture surface was
observed using SEM.

3. Service crack in segment A1

3.1. Section

Fig. 3 shows a section through a SCC in segment A1.The thickness of the pipe was 8 mm, and the ver-
tical depth of the crack was about 4 mm, about half of the pipe thickness. The crack path zigzaged at the
beginning. The crack propagated along an angle about 45 to the surface as shown by the arrow at A.
There was a vertical crack propagation after the first sloping crack (arrow B). The crack propagated along

Fig. 1. Slow and fast potentiodynamic scans for X65 in 1 N Na2CO3+1 N NaHCO3 solution at 70  C.
6 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18

Fig. 2. Loading procedures for JQ1 and JQ2 LIST tests, (a) JQ1; (b) JQ2.

Fig. 3. Cross section of segment ‘‘C’’.

 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18 7

the three-dimension strain field ahead of the crack tip. When the crack changed direction, there was a fine
branch (e.g. at arrows C, D, E) along the original direction of cracking. The fine branches did not keep
growing. When the crack was sufficiently deep, there was crack branching (arrow F) and two cracks pro-
pagated. The long crack was about 5.5 mm in length, and the short one was about 4.6 mm in length. Before
the arrow at F, the crack was more open.

3.2. Fracture surface

The SCC was broken open and the fracture surface was examined. There were some crack branches close
to the pipe outer surface because there were some small facets at the fracture surface. Most of the SCC
surface was covered with a visible back film. Parts of the fracture surface were brown in colour, these were
closer to the original pipe surface. This is interpreted as being due to easier access of the external envir-
onment along the more open crack before the position F in Fig. 3.
There were several crack initiation sites at this fracture surface. The small facets close to the pipe surface
showed that the cracks initiated and propagated individually first. The cracks coalesced when they grew
deeper. The structure of the oxide film at the different positions on the fracture surface was characterised
and a typical topography is shown in Fig. 4. The oxide film at the edge formed for a longer time than that
close to the crack tip. Most of the crack surface was covered by oxide film. Fig. 5 showed the structure
around the crack tip. There was a narrow region of the crack tip that was not covered by an obvious oxide
film. It showed intergranular stress corrosion cracking. The crack tip front was next to a tearing surface
produced by the ductile overload as the sample was broken open to reveal the SCC surface for
observation.

3.3. Depth profiles

Depth profiles of the surface film on the SCC fracture surface A1 were analysed by Auger electron
spectroscopy (AES), at the edge, middle and tip positions as shown in Fig. 6. The relationship between the
thickness of the oxide film and the crack length is shown in Fig. 6(d). The edge had the thickest film
because of the longest time for corrosion, and the tip had the thinnest film because of the shortest time
exposure to the environment. Due to the resolution of the AES, it is impossible to analyse the thickness of
the oxide film right at the crack tip.

Fig. 4. Oxide film on crack surface.

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Fig. 5. Fracture surface at crack tip from service pipe A1-upper crack (a) and (b) B2 side; (c) B1 side.
 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18 9

Fig. 6. (a) B2 side of fracture surface from crack at B piece, (b) and (c) oxygen and Fe Auger signals at different positions on B2
fracture surface, and (d) oxide thickness evaluations: ‘‘cross’’ corresponding to O and Fe peak to peak line cross, and ‘‘half’’ corres-
ponding to halfway of O peak to peak.

4. Service crack in segment A2

4.1. Section

A segment of the pipe, known to contain SCC, was sectioned. The segment of steel pipe was about 30
mm in length. There were about 23 cracks in this cross section. The longest crack was about 0.8 mm, and
the shortest was about 0.1 mm, so all the cracks were shallow. The cracks were intergranular and bran-
ched. Most of the cracks propagated almost vertically, and some cracks branched when they grew longer.
The cracks were not very open.

4.2. Fracture surface

Because the cracks were shallow, it was hard to break the section to open the cracks for SEM exami-
nation. A sliver 3 mm in depth was cut parallel to the pipe surface, and bent. Although there were many
cracks in this piece, only two cracks opened allowing examination.
Most of the crack surface was covered by an oxide film as for the crack surface of the SCC in segment
A1. The exception was the crack tip region. The details of this crack tip region of the longer crack is shown
in Fig. 7, and of the smaller crack is shown in Fig. 8. There was a narrow region of the crack tip front that
10 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18

Fig. 7. Crack tip of crack I observed by SEM in SE and BSE modes.

was not covered by an obvious oxide film. It showed intergranular stress corrosion cracking. The crack tip
front was next to a tearing surface as for the crack in segment A1.

5. JQ1 sample

5.1. IGSCC on electropolished surface

After the LIST test, the electropolished surface was covered by an oxide film. Because the surface was
electropolished, there were no deep scratches on the surface. The surface oxide was removed by a gentle
polish using 1200 grit silicon paper and a fine polish using diamond paste. The sample was etched using 2%
nital and observed using SEM. IGSCC was obvious as shown in Fig. 9. Stress corrosion cracks had initi-
ated at ferrite grain boundaries and had grown to a size of several grains. Not all grain boundaries were
attacked, as would be expected if there was just intergranular corrosion. Thus it is concluded that there was
intergranular stress corrosion cracking rather than just intergranular corrosion.

5.2. IGSCC observations on cross-section

After surface observation, the sample was cross-sectioned using a slow speed saw. The cross section
surface was polished using 220–1200 grit silicon paper and fine polished using diamond paste, and etched
 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18 11

using 2% nital. A typical section is shown in Fig. 10. The surface was covered by an oxide film. Breaks in
the oxide film corresponded to intergranular cracks. The cracks initiated at ferrite grain boundaries, and
grew to a depth of below 10 mm. A layer of oxide film could be seen at the sample surface, but not at the
surface of the cracks.

Fig. 8. Small crack (crack II) at surface and its tip at different positions.
12 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18

6. JQ2 sample

6.1. IGSCC observations on cross -section

The loading procedure for JQ2 was aimed at producing longer cracks. As shown in Fig. 11, the cracks at
the cross section were longer than that in JQ1. Fig. 11 shows that the crack can branch along different
grain boundaries at an early stage. Fig. 11(c) and (d) shows wider cracks; these are interpreted as having
been opened due to overload at the end of the SCC test.

6.2. Fracture surface of JQ2

An overview of the fracture surface is shown in Fig. 12. Location ‘‘A’’ is the original surface. Locations
B, C, D are the fracture surface. Location E is the electropolished surface. Location F is a crack at the edge
of the specimen. The high-magnification observation at different locations indicated as follows. Location

Fig. 9. IGSCC at surface grew along ferrite grain boundaries.

Fig. 10. Cross-section showing IGSCC.

 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18 13

Fig. 11. Cross section showing IGSCC, (a) small cracks and crack branch at early stage; (b) and (c) bigger cracks; and (d) crack
opened after necking.

Fig. 12. Overview of the fracture surface for JQ2.

‘‘A’’ showed an oxide-covered surface. Most of locations B, C & D showed dimple rupture indicative of a
ductile fracture process.
Then the sample was tilted for detailed observation of the stress corrosion cracks on the electropolished
side. As shown in Fig. 13, there were three kinds of structure at the edge at locations D and E. These
indicate that intergranular stress corrosion cracks formed on this surface during the LIST test. During the
overload, the fracture propagated first in a tearing mode, then by microvoid coalescence to produce the
14 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18

Fig. 13. Observation at locations D and E after 25 tilt.

 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18 15

dimple areas that made up most of the fracture surface. The detailed observations of the opened IG cracks,
as shown in Fig. 13, indicate that the electropolished surface was covered by an oxide film. This oxide film
grew to a thickness of several microns during the LIST test, and is clearly visible in sections of LIST
samples (e.g. Figs. 10 and 11). At the opened cracks, there was a narrow region of intergranular stress
corrosion cracking. Following this IGSCC, there was a tearing structure (which was also present in JQ1,
the service crack in segment A1, and also in a LIST sample fractured in air). The tearing structure was
followed by dimple fracture.
Further observation was carried out particularly in an attempt to determine the presence or absence of
surface oxide on the intergranular stress corrosion cracks. The results are shown in Fig. 14. There were
many small open cracks on the electropolished surface. The detailed observation of the opened cracks is
shown in Fig. 14. These observations were consistent with the prior observations. Fig. 14 shows a crack at
the oxide film, and that crack was associated with an intergranular crack in the metal underneath, ie the
crack in the oxide propagated along the metal grain boundary. This region of IGSCC was not covered by
an oxide film, which was visible by SEM. The grains at the crack tip were detached from the tearing region,
ie there was often a crack between the IGSCC region and the tearing region. The IGSCC region extended
about two or three grains, which means the stress corrosion cracks did not grow to be very long.

7. Discussion

7.1. Oxide film and analysis methods

For a long term service pipe, the oxide film on the crack surface has been built up for many years. The
service crack in the cross-section, as shown in Fig. 3, was open at the beginning, and became narrower
gradually to the crack tip. The analysis methods used in this work were AES and SEM. The AES analysis
showed that the thickness of the oxide film decreased from the crack beginning to the crack tip. But with
the limitation of AES resolution (sputter spot size about 0.5 mm), it is impossible to analyse the thickness
of oxide film right at the crack tip. SEM can give us the second electron (SE) image and backscatter elec-
tron (BSE) image. BSE image can give the composition information because the heavy elements scatter
back more electrons to generate a much brighter image than the light elements. Due to its oxygen content,
the oxide film is darker than the steel matrix. But a thin layer of oxide film may produce an identical con-
trast compared to the steel matrix. This circumstance may happen at the fresh crack tip.

Fig. 14. Detailed observation of fresh crack surface.

16 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18

7.2. Crack tip

Since the oxide film at the crack tip can not be characterised by AES and SEM, the structure of the crack
tip became the important factor.
As shown in Fig. 15, there are three types of crack:

Type I: Actively growing crack with the crack sides covered by an oxide film
Type II: Old dormant crack with a newly initiated crack tip
Type III: Dormant crack with the crack sides and crack tip both covered by an oxide film

The first two kinds of cracks have an active crack tip which is not large in size, so the crack tip should be
a narrow area. Because the crack tips are freshly produced without too much corrosion they should reveal
IGSCC features. There may be a thin layer of oxide film on the crack tip surface, but this film can not be
identified using SEM. For the third kind of crack, the oxide film should cover all the crack surface
including the crack tip, and there should be no region between oxide film covered crack and the tearing
structure produced by the overload.
For a type I crack, the crack propagates gradually and the oxide film is built up on the crack surface
gradually, so the thickness of the oxide film on the crack surface should gradually decrease from the crack
beginning to the crack tip front. For a type II crack, the oxide film should cover the whole old dormant
crack surface except for the newly initiated crack tip. The newly initiated crack tips for types I and II can
be identified from the structure observed by SEM. For a type III crack, the oxide film should cover all the
crack surface including the crack tip.

7.3. How to judge whether the crack is dormant or active?

For a long term service pipe, the oxide film on the crack path has been built up for perhaps many years.
The crack tip may be produced newly and should indicate whether the crack is active or dormant rather
than the crack sides. That is, it is more important to examine the details of the region at the very crack tip
than the bulk of the crack surface.

Fig. 15. Three types of crack tip.

 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18 17

Consequently, if we want to judge whether the crack in the service pipe is active or dormant, it is rea-
sonable to compare the crack tip of the service pipe crack and the fresh crack produced in the laboratory
LIST sample. If the crack tip of the LIST sample is similar to that of the service pipe, it means the crack in
the service pipe is probably active.

7.4. Laboratory samples JQ1 & JQ2

The loading procedure for JQ2 provided a longer time for a crack to propagate, so JQ2 did have longer
cracks than JQ1. The crack size was less than 10 mm for JQ1, and about 50 mm for JQ2.
As shown in Fig. 11(a), the small cracks were open. If the two sides of the crack sides are closed again,
they meet together very well. It means there was no serious dissolution at these crack sides.
The big cracks for JQ2 were more open, which is attributed to the overload. If the two crack sides of
each crack are closed again, they meet very well when the crack size is small as shown in Fig. 11(a), and
also meet nearly exactly as shown in Fig. 11(b) and (c). It means the crack surface was not subjected to
significant corrosion. A crack close to the overload fracture surface is shown in Fig. 11(d). The crack tip
front was broad. The outer layer of the sample was weakened by cracks. When the sample was overloaded,
the stress concentrated at the crack tips and the crack tip front was torn to be broad. Although there was
corrosion and a significant oxide on the specimen surface caused by the 10 days of the SCC test, there was
clear IGSCC at the sides of the newly created cracks and furthermore, there were few corrosion products
on the sides of these newly created cracks.

7.5. Service SCC in segments A1 and A2

The crack tips of service SCC in segments A1 and A2 were shown in Figs. 5, 7 and 8. Most of the crack
surface was covered by an obvious oxide film except for the crack tip. Between the oxide film and the
tearing structure, there was a narrow region that showed a feature similar to the narrow IGSCC area in the
JQ2 sample. It indicates that the crack tip in the service pipe is not very old at all. If the crack is
dormant as type III, there would not be any region between the crack surface covered by an oxide
film and the tearing structure. From the above observation and comparison of the crack tip between
service pipe and the laboratory samples, it can be concluded that the cracks in segments A1 and A2 are
most likely active.

7.6. Small cut—v- coupons

This study indicated that examination of the very crack tip was indeed the critical aspect needed for a
decision on whether or not the service SCC was likely to be active. It is thus a logical deduction that any
sampling technique is adequate as long as the sampling technique can guarantee extraction of the very crack
tip. Cutting a sample from the service pipe is indeed one way to guarantee extraction of the very crack tip.
It is also possible to imagine a trepanning procedure whereby the crack is extracted from the service pipe.

8. Conclusions

 To judge whether the crack in the service pipe is active or dormant, it is reasonable to compare the
very crack tip of the service pipe crack and the fresh crack in the laboratory sample. If the crack tip
of the active laboratory sample is similar to that of the service pipe, it means that it is wise to deduce
that the crack in the service pipe is active.
18 J. Wang, A. Atrens / Engineering Failure Analysis 11 (2004) 3–18

 From the comparison of the crack tips between the service pipe and the laboratory sample, it
appears likely that the cracks in the samples extracted from service were most likely to have been
active intergranular stress corrosion cracks.

Acknowledgements

This study was supported by an ARC SPIRT Grant supported by Agility Team Build, One Steel Oil and
Gas Pipe and Woodside Energy Ltd.

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