SPE 99557
SSC Resistance of QT-900 and QT-1000 Coiled Tubing
T.H. McCoy and J. Thomas, Halliburton
Copyright 2006, Society of Petroleum Engineers
This paper was prepared for presentation at the 2006 SPE/ICoTA Coiled Tubing and Well
Intervention Conference and Exhibition held in The Woodlands, TX, U.S.A., 4–5 April 2006.
This paper was selected for presentation by an SPE Program Committee following review of
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Abstract
Laboratory sulfide stress cracking (SSC) tests were performed
on specimens taken from QT-900 and QT-1000 coiled tubing
(CT) test strings in an attempt to define zones of acceptable
sour service. Acceptable pH-PH2S zones of service for QT-900
CT were proposed in SPE 93786.1 This paper presents
additional QT-900 CT test data to further refine acceptable
zones of service, with and without use of a chemical inhibitor.
In addition, SSC testing was undertaken on QT-1000 CT. The
SSC tests on QT-1000 CT were performed in manner similar
to that conducted on QT-900 CT, using acidified aqueous
solutions with H2S partial pressures ranging from 0.00345 to
100 bars and pH from 3.5 to 6.5, with and without inhibitor.
Both as-milled and pressure-cycled tubing was tested. Test
specimens were taken from parent metal and bias weld
locations. The test data was used to construct acceptable zones
of service on a pH-PH2S diagram.
Introduction
High-pressure, high-temperature (HPHT) deep wells
containing hydrogen sulfide (H2S) increasingly challenge the
ability to service these wells by exclusively using lower
strength CT70 and CT80 grades of coiled tubing.2 In some
HPHT wells, only higher strength CT can be used.3 However,
preventing catastrophic CT failures is of utmost importance;
risk factors must be known and caution exercised to the fullest
extent possible. Several factors affect the hydrogenation of
steel, of which the most important are H2S concentration, pH,
and temperature.4 Therefore, control and understanding of the
environment to which the CT may be exposed is crucial. And
while other factors such as chemical composition, fatigue,
strength, hardness, mechanical damage, etc. are important,
they are not as critical as the environment.
It is believed that the use of chemical inhibition to mitigate
hydrogenation and the possibility of environmental cracking
can play an important role in preventing unexpected failures.
It has been shown in lab tests that the addition of inhibitor to
the aqueous solutions containing H2S can have significant
beneficial effects and is thought to be able to extend the use of
CT to more aggressive sour environments.1
Field Experience
Since the recommendations were made from the work
presented in SPE 93786,1 no failures have resulted to the
author’s knowledge by following the proposed SSC-No SSC
zones. Note that this paper basically confirms the QT-900 CT
SSC-No SSC zones but adds an area of uncertainty at the low
pH-low PH2S area (non-inhibited environments). However,
additional precautions are being taken, especially in western
Canada, to help prevent failures by routine use of chemical
inhibition. The tubing OD is coated with inhibitor CG using an
injector sub below the stripper as it is run in the well; in
addition, the inhibitor is mixed with nonacidic fluids pumped
through the coiled tubing. The proposed “No SSC” zone for
environments containing inhibitor CG was expanded up to 100
bars PH2S based on test results reported in this paper. For acid
systems, a different H2S inhibitor (not tested for this paper) is
being utilized.
Environmental Domains
SSC testing was undertaken with the ultimate goal of being
able to identify sour service severity domains where QT-900
and QT-1000 CT could be reliably used. Defining severity
domains is a common approach for carbon and low-alloy steel
components used in sour service production. This concept has
been adopted by EFC Publication Number 164 and NACE
MR0175/ISO 15156.5 It has also been recognized by a
consortium of major oil and gas and steel producers6 for use
with API 5L linepipe steels and their welds. Since CT grades
QT-900 and QT-1000 are high-strength, low-alloy (HSLA)
steels, similar in composition to the steels in the above
references, it is therefore expected that hydrogenation of these
steels is also similar. However, it is recognized that CT
operations place higher demands on the material than most
other applications (due to repeated plastic deformation), and
therefore, more restrictive conditions may be applicable.
The sour domains concept is based primarily on two
environmental conditions, pH and PH2S, along with a
consideration of the hardness or strength of the steel being
exposed to the environment (Fig. 1). Sour service severity is
divided into three domains: mild (domain 1), intermediate
(domain 2), and severe (domain 3) with an additional domain
0 typically considered an area where normally no precautions
are required for low- to medium-strength steels. Generally, it
could be considered that acceptable steels for domains 1, 2,
2 SPE 99557
and 3 would have maximum hardnesses of 248, 280, and 300
HV respectively.
Test Strings
Environmental testing was performed on specimens taken
from a 2.000-in. OD × 0.203-in. wall QT-900 test string and a
1.750-in. OD × 0.125-in. wall QT-1000 test string. All
sections of each individual string were made from the same
material heat and master coil. Both strings were manufactured
with multiple bias welds made according to standard mill
procedures. The full-body mill stress-relieving temperatures
for the QT-900 and QT-1000 strings were 1,225ºF and
1,200ºF, respectively. Mechanical properties and chemical
composition of each test string is shown in Tables 1 and 2,
respectively. It should be noted that the yield strength of the
QT-1000 string was at the upper limit (115.9 ksi vs. 100 ksi
minimum specified) for this grade of tubing.
Sections from each test string were then tested to
determine the pressure-bending fatigue life of the parent
metal. Fatigue cycling data is shown in Table 3. This baseline
was needed so that test samples could be fatigue cycled to
50% of the average CT fatigue life. In this manner, testing
would determine the effect of strain cycling on the SSC
susceptibility of each grade of tubing.
Test Specimens
After the test strings were processed, four-point bent beam
(FPBB) specimens were machined from extrados and intrados
locations on tubing that had been fatigue cycled to 50% NFT as
well as from as-milled tubing. For this paper, only parent
metal and bias weld locations were tested. The ERW seam
weld was not tested since previous work1,7 showed that the
seam weld consistently outperformed bias welds with respect
to hydrogen cracking resistance. In addition, no butt welds
were tested. Butt welds have consistently shown poor
performance in H2S cracking tests.1,7
Only FPBB specimens were tested. FPBB test specimens
were selected because they would provide crack orientation in
the same plane as occurs in field failures, i.e., cracking
transverse to the string length. All test specimens were
machined by an outside company skilled in making these test
specimens. All FPBB specimens were strained to 1.0% during
environmental cracking tests. Deflection required to obtain
1.0% strain was determined by using strain gauges on
representative samples. A total of 15 and 35 FPBB specimens
were tested from the QT-900 and QT-1000 test strings,
respectively. All environmental cracking tests were performed
by the same outside testing laboratory used for the FPBB
testing reported in SPE 93786.1
Hardness test measurements were made on representative
QT-900 and QT-1000 CT test specimens from each condition.
Multiple hardness readings were taken on at least 2 samples
from each condition after SSC testing. The average and single-
reading maximum hardness values obtained are given in
Tables 4 and 5. The average hardness of the parent material
from the QT-900 string met the NACE MR0175/ISO 15156-25
maximum hardness requirement of 22 HRC (248 HV) for all-
temperature sour service low-alloy steel. However, the
QT-900 CT bias weld hardness values exceeded this limit
somewhat. Of course, the QT-1000 CT samples showed
higher hardness values than QT-900 CT. The single-reading
maximum hardness measured at the bias weld of QT-900 and
QT-1000 CT was 259 HV and 314 HV, respectively for the
fatigue-conditioned samples.
Test Environments
The test environments are described in Table 6. The
environments were essentially NACE Standard TM0177-968
recommended environments with variable pH and PH2S. When
less than 100% H2S gas was used, the balance was made up
using CO2. Test environments were selected to represent a
wide range of sour environments in an effort to determine
acceptable zones of service on the pH-PH2S diagram (Fig 1).
Unless otherwise noted, all tests were conducted at room
temperature. SSC testing at a temperature of 75°F (i.e., room
temperature) is more severe for carbon and low-alloy steels
than testing at elevated temperatures.4
Inhibitor CG
Inhibitor CG, a relatively new inhibitor derivative, is an
organo sulfur anticracking agent used in conjunction with
corrosion inhibitors in a hydrocarbon solvent. SSC tests
performed in the environments shown in Table 6 utilized 0.2%
by volume inhibitor CG to treat the test fluid. Inhibitor CG
may also be applied neat to the tubing. Limited testing has
shown this application method may be even more effective;9
however, it was not applied neat in any of the tests reported by
this study.
Test Results
Test results are shown in Tables 7 and 8 and representative
test specimens are shown in Figs. 2 and 3. The only mode of
failure observed in the samples was SSC; other modes, such as
hydrogen-induced cracking (HIC) or stepwise cracking (SWC)
were not observed. Fig. 4 shows an SSC crack in a QT-1000
CT bias weld sample that propagated through approximately
75% of the sample. In addition, several of the samples
exhibited fissuring, which is a precursor to SSC. Fissuring can
be described as crack-like formations not severe enough to
completely separate the sample, as shown in Fig. 5. Fissuring
therefore is not as severe a failure, but certainly suggests that
caution be exercised.
As expected, QT-1000 CT was more sensitive to SSC than
QT-900 CT when chemical inhibition was not used. QT-1000
CT samples failed in equivalent or less severe pH-PH2S
conditions that did not produce a failure in QT-900 CT
samples. As a result, the “No SSC” zone for QT-1000 CT
without inhibitor must be more restrictive. Despite this
difference, the use of inhibitor CG provided the same level of
protection for both grades of QT-900 and QT-1000 CT, to the
extent of environmental conditions tested. Inhibitor CG
successfully prevented cracking in both QT-900 and QT-1000
CT, as none of the tests containing 0.2 vol% inhibitor CG
showed fissuring or cracking failures. Testing showed that
neither material failed when tested in environments as severe
as 100 bar PH2S and 3.5 pH with 0.2 vol% inhibitor CG. In fact
after testing in these environments with inhibitor CG, the
samples did not display any scale or corrosion attack (Fig. 5).
In addition, metallurgical mounts were made for several
samples. Of the samples examined, none that were run with
SPE 99557
inhibitor CG contained evidence of pitting, even at 100 bar
PH2S and pH 3.5, while several without did, as shown in Figs.
6 and 7. Usage of inhibitor CG has therefore been shown to
extend the useable regimes of both grades of CT and should be
considered for non-acidic treatments when expected downhole
environments fall into the SSC zone of the particular CT grade
being used.
Testing continued to show a difference in SSC between the
bias weld and the parent material. In tests conducted in the
same environment (environments 15, 17–19, and 22), the
parent metal samples always performed better than the bias
weld samples even though some of the parent samples
contained fissuring.
Although comparative test results are limited, no
difference in SSC resistance was noted between as-milled and
50% NFT pressure-cycled test specimens. Previous work1
indicated a slight increase in SSC susceptibility when QT-900
CT was pressure-cycled to 75% NFT.
It is well known that CT strength and hardness are
important factors with respect to environmental cracking
resistance. Other factors relative to the condition of the tubing
(e.g., OD surface mechanical damage) may also be critical to
avoidance of failures. Because these test samples were
machined specimens with no surface abnormalities, all tests
were run for 30 days. In addition, previous unreported work
conducted by the authors for a major oil company7 showed
that QT-1000 CT failed while exposed to an acidified aqueous
fluid containing H2S in the intermediate sour service domain,
but only after 3 days or more exposure time. Therefore, the
30-day test results reported herein add some conservatism to
the proposed “SSC–No SSC” zones.
SSC–No SSC Zones
Based on the test results, the SSC–No SSC zones in Figs. 8
and 9 are proposed for CT grades QT-900 and QT-1000
respectively. Basically, QT-900 CT without inhibitor should
only be used in mild to intermediate sour service
environments, while QT-1000 CT has been limited to very
mild sour service environments.
The SSC–No SSC zone for QT-900 CT without inhibitor
has been revised to show an area of uncertainty at the low
pH/low PH2S area as shown in Fig. 8. The area of uncertainty
contains the tested environments where fissuring occurred.
Since only pressure-cycled parent metal samples were tested
in these environments, it is uncertain whether failure may have
occurred if pressure-cycled bias weld samples had been tested.
With the addition of inhibitor CG, the No SSC zone
proposed for both grades widened significantly, up to 100 bar
PH2S, as shown in Fig. 10. Inhibitor CG is currently being used
in certain field operations and it is believed that its capabilities
can be fully realized outside the lab.
Of course, further work and field service experience may
modify these proposed boundaries. However, to the authors’
knowledge, when these recommendations have been followed,
no failures have occurred.
Conclusions
1. Environmental cracking tests in acidified aqueous
solutions containing H2S indicate that QT-900 CT
3
should only be used in mild to intermediate sour service
environments.
2. Environmental cracking tests in acidified aqueous
solutions containing H2S indicate that QT-1000 CT
should only be used in very restricted mild sour service
environments.
3. Use of inhibitor CG has been demonstrated to
significantly expand the No SSC zone for grades QT-
900 and QT-1000 CT. No failures of either grade CT
occurred in a very aggressive H2S aqueous environment
with 100 bar PH2S and 3.5 pH when 0.2 vol% inhibitor
CG was added to the aqueous environment.
4. The parent metal continued to show better resistance to
SSC in acidified aqueous solutions containing H2S than
the bias weld.
5. Although comparative test results are limited, no
difference in SSC resistance was noted between as-
milled and 50% NFT pressure-cycled test specimens.
6. In addition to increasing the SSC resistance of QT-900
and QT-1000 CT samples, containing inhibitor CG in
the H2S-containing aqueous solutions did not display
any scale or corrosion attack.
7. Field experience in western Canada suggests that
consistent use of inhibitor CG may increase the
reliability of QT-900 CT in sour fields.
Acknowledgements
The authors wish to thank the Halliburton personnel in
western Canada for providing their field experience and the
management of Halliburton for allowing publication of this
work.
Nomenclature
EFC European Federation of Corrosion
ERW Electric resistance weld
HAZ Heat-affected zone
HRB Hardness Rockwell “B” scale
HRC Hardness Rockwell “C” scale
HV Hardness Vickers
ISO International Organization for Standardization
NACE National Association of Corrosion Engineers
NFT Number of fatigue cycles to failure
PH2S Partial pressure of H2S gas; (%H2S)(Total Pressure,
psia) (where %H2S is in mol%)
References
1. McCoy, T.: “SSC Resistance of QT-900 Coiled Tubing,” paper
SPE 93786 presented at the 2005 SPE/ICoTA Coiled Tubing
Conference and Exhibition, The Woodlands, Texas, 12–13
April.
2. Patrick, K., el al.: “Extended Reach Simulation with Coiled
Tubing: A Case Study,” paper SPE 84162 presented at the
2003 SPE Annual Technical Conference and Exhibition,
Denver, Colorado, 5–8 October.
3. Turner, A. and Murdoch, B.: “High Pressure High Temperature
Coiled Tubing Intervention Operations in the North Sea Within
the Past Two Years,” paper SPE 93956 presented at the 2005
SPE/ICoTA Coiled Tubing Conference and Exhibition, The
Woodlands, Texas, 12–13 April.
4 SPE 99557

4. Guidelines on Materials Requirements for Carbon and Low
Alloy Steels for H2S, second edition, EFC Publication Number
16.
5. “Petroleum and Natural Gas Industries—Materials for Use in
H2S-containing Environments in Oil and Gas Production,”
NACE International Standard MR0175, ISO 15156-2, first
edition.
6. Kermani, M.B., et al.: “Limits of Linepipe Weld Hardness for
Domains of Sour Service in Oil and Gas Production,” NACE
Paper No. 00157 presented at Corrosion 2000 Conference.
7. Internal Halliburton Report MER 1307, dated October 28,
2005.
8. “Laboratory Testing of Metals for Resistance to Sulfide Stress
Cracking and Stress Corrosion Cracking in H2S
Environments,” NACE International Standards TM0177-96.
9. Internal Halliburton Report MER 1277, dated March 14, 2005.

Table 1—Mechanical Properties of Test Strings

Property QT-900 QT-1000
1
Hardness 98 HRB 26 HRC1
Yield strength, ksi
93.2 115.9
(0.2% offset)
Ultimate tensile
102.2 122.0
strength, ksi
Elongation, % 29 24.5
1
Base metal and weld metal as reported by the material
certificate.

Table 2—Chemical Composition of the Test Strings (wt%)

C Mn S P Si Cr Ni Mo Cu V Nb
QT-900 0.150 0.87 0.0017 0.011 0.42 0.57 0.09 0.23 0.24 — —
QT-1000 0.120 1.50 0.0007 0.020 0.42 0.60 0.09 — 0.25 0.070 0.05

Table 3—Pressure-Bending Fatigue Parameters

Parameters QT-900 QT-1000
Pressure, psia 5,000 3,000
Mandrel bend radius, in. 72 72
1
Average cycles to failure 544 403
1
At parent metal location only. Bias weld locations
assumed to have same fatigue life as parent metal.

Table 4—Hardness (HV1.0kgf) of

QT-900 and QT-1000 CT Parent Metal
% NFT QT-900 QT-1000
221 average 247 average
0 1
234 maximum 250 maximum1
216 average 258 average
50 1
219 maximum 260 maximum1
1
Maximum recorded single value reading.
SPE 99557 5

Table 5—Hardness (HV1.0kgf)

of QT-900 and QT-1000 CT Bias Weld
% NFT QT-900 QT-1000
250 average 282 average
0
267 maximum1 293 maximum1
250 average 289 average
50
259 maximum1 314 maximum1
1
Maximum recorded single value reading.

Table 6—Test Environments1

Environment PH2S (bar) Initial pH Vol% CG
2
14 0.00345 (0.05psi) 4.5 None
2
15 0.01 3.5 None
15a 0.012 3.5 0.2
2
16 0.01 4.0 None
17 0.012 4.5 None
2
17a 0.01 4.5 0.2
2
18 0.01 5.0 None
19 0.12 4.5 None
2
19a 0.1 4.5 0.2
20 0.12 5.0 None
21 0.12 5.5 None
21a 0.12 5.5 0.2
2
22 0.1 6.0 None
23 1.0 5.5 None
23a 1.0 5.5 0.2
24 1.0 6.5 None
24a 1.0 6.5 0.2
25 10 5.5 None
26 10 6.0 None
27 10 3.5 0.2
3
28 100 3.5 0.2
1
All environments NACE Standard TM0177-96 Method B test solutions
modified as described in the table.
2
Balance CO2.
3
Test performed at 100°F. All other tests performed at room temperature.
6 SPE 99557

Table 7—Test Results, No Inhibitor1

Environment QT-900 QT-1000
Bias Weld (0%) NF
14 — —
Parent (0%) NF
Parent (50%) Fissuring Bias Weld (50%) F
15
Parent (50%) Fissuring Parent (50%) Fissuring
Parent (50%) Fissuring
16 — —
Parent (50%) Fissuring
Bias Weld (50%) F
17 — —
Parent (50%) Fissuring
Bias Weld (50%) F
18 — —
Parent (0%) NF
Bias Weld (50%) F
19 — —
Parent (50%) Fissuring
Parent (50%) NF
20 — —
Parent (50%) NF
Parent (50%) NF Bias Weld (0%) F
21
Parent (50%) NF Bias Weld (50%) F
Bias Weld (50%) F
22 — —
Parent (0%) NF
Parent (50%) NF Bias Weld (0%) F
23
Parent (50%) NF Bias Weld (50%) F
Parent (0%) NF
24 — —
Parent (50%) NF
Bias Weld (50%) F
25 — —
Bias Weld (50%) F
26 Parent (50%) NF Bias Weld (0%) F
1
NF= No Failure; F= Failure
SPE 99557 7

Table 8—Test Results with 0.2% CG Inhibitor1

Environment QT-900 QT-1000
Bias Weld (50%) NF
15a — —
Parent (50%) NF
Bias Weld (50%) NF
17a — —
Parent (50%) NF
Bias Weld (50%) NF
19a — —
Parent (50%) NF
Bias Weld (0%) NF
21a — —
Bias Weld (50%) NF
Bias Weld (0%) NF
23a — —
Bias Weld (50%) NF
Parent (0%) NF
24a — —
Parent (50%) NF
Bias Weld (50%) NF
27 — —
Bias Weld (50%) NF
Bias Weld (50%) NF Bias Weld (50%) NF
28
Bias Weld (50%) NF Bias Weld (50%) NF
1
NF= No Failure; F= Failure

Fig. 1—Sour service domains (regions) adopted by NACE MR0175/ISO 15156.

8 SPE 99557

Environment 21
Bias weld, 0%
Bias weld, 50%

Environment 23
Bias weld, 0%
Bias weld, 50%

Environment 24
Parent, 0%
Parent, 50%

Fig. 2—QT-1000 CT FPBB samples after 30 days testing in various

environments without inhibitor CG.

Environment 21a
Bias weld, 0%
Bias weld, 50%

Environment 23a
Bias weld, 0%
Bias weld, 50%

Environment 24a
Parent, 0%
Parent, 50%

Fig. 3—QT-1000 CT FPBB samples after 30 days testing in various

environments with inhibitor CG

Fig. 4—Micrograph of a QT-1000 CT bias weld FPBB sample in

Environment 23 with an SSC crack (unetched, 50x original
magnification).
SPE 99557 9

Fig. 5—Close-up photograph of a QT-900 CT FPBB sample exposed

to Environment 15 showing fissuring.

Fig. 6—Micrograph of a QT-1000 CT bias weld FPBB sample in

Environment 28 with inhibitor CG showing no pitting (3% nital etch,
50x original magnification).

Fig. 7—Micrograph of a QT-1000 CT bias weld FPBB sample in

Environment 23 without inhibitor CG showing pitting (3% nital etch,
50x original magnification).
10 SPE 99557

Fig. 8—SSC–No SSC zones for QT900 CT, no inhibitor.

Fig. 9—SSC–No SSC zones for QT1000 CT, no inhibitor.

SPE 99557 11

Fig. 10—SSC–No SSC zones for QT900 and QT1000 CT with 0.2 Vol% inhibitor CG.