ISSN 1831-9424 (PDF)

ISSN 1018-5593 (Printed)

Requirements for safe and reliable

CO2 transportation pipeline
(SARCO2)

Research and
Innovation EUR 28918 EN
EUROPEAN COMMISSION
Directorate-General for Research and Innovation
Directorate D — Industrial Technologies
Unit D.4 — Coal and Steel

E-mail: rtd-steel-coal@ec.europa.eu
RTD-PUBLICATIONS@ec.europa.eu

Contact: RFCS Publications

European Commission
B-1049 Brussels
 European Commission

Research Fund for Coal and Steel

Requirements for safe and reliable
CO2 transportation pipeline
(SARCO2)
Massimo Di Biagio
Centro Sviluppo Materiali S.p.A
Via di Castel Romano 100, Rome, Italy

M. Erdelen-Peppler, S. Jäger
Salzgitter Mannesmann Forschungsinstitut GmbH - Germany

C. Kalwa, C. Kassel
Europipe GmbH - Germany

H. Brauer
Salzgitter Mannesmann Line Pipe GmbH - Germany

W. Wessel
Vallourec Deutschland GmbH - Germany

N. Voudouris
Corinth Pipeworks S.A - Greece

C. M. Spinelli
eni S.p.A - Italy

S. Saysset
Engie (GDF Suez) - France

R. Cooper
National Grid plc - UK

Grant Agreement RFSR-CT-2011-00033

1 July 2011 to 30 June 2015

Final report

Directorate-General for Research and Innovation

2017 EUR 28918 EN

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Print ISBN 978-92-79-77024-1 ISSN 1018-5593 doi:10.2777/63802 KI-NA-28-918-EN-C

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 Table of Contents

Final summary ........................................................................................................................................................ 5

Scientific and technical description of the results ............................................................................................ 14
Objectives of the project ................................................................................................................................... 14
Description of activities and discussion ............................................................................................................ 15
WP1: Design and specification for full scale tests, Test pipes supply. Selection and analysis of CO 2 release
models .............................................................................................................................................................. 15
Task 1.1 Critical Analysis of existing know-how ............................................................................................ 15
Task 1.2 Design of experimental activities .................................................................................................... 26
Task 1.3 Pipes, crack arrestors and composite reinforced pipes supply. ...................................................... 26
Task 1.4 Base mechanical characterization and weldability of steel pipes selected for the full-scale leakage
and fracture propagation tests. ..................................................................................................................... 27
Task 1.5 State of the art and gap analysis of available modelling CO2 releases and subsequent dispersion.
Set-up of selected dispersion model ............................................................................................................. 40
WP2: Fracture initiation control ......................................................................................................................... 41
Task 2.1 Mechanical characterization of steel pipes selected for the full-scale tests .................................... 41
Task 2.2 Definition of dispersion instrumentation and its layout for Leak before Break tests ........................ 41
Task 2.3 Development of HSE requirements for full scale Leak before Break tests ..................................... 42
Task 2.4 Full-scale leakage tests .................................................................................................................. 43
First leakage test ....................................................................................................................................... 44
Second leakage test.................................................................................................................................. 49
Task 2.5 Collect data related to the release of large quantity of CO2 from a leak ......................................... 50
Task 2.6 Development and validation of Leak before Break fracture mechanical model for CO 2 pipeline. ... 51
Task 2.7 Analysis of dispersion results and comparison between experiments and modelling results. ........ 53
WP3: Fracture propagation control ................................................................................................................... 55
Task 3.1 Mechanical characterization of steel pipes selected for the fracture propagation full-scale tests ... 55
Task 3.2 Definition of dispersion instrumentation and its layout for the fracture propagation full-scale tests 55
Task 3.3 Development of Health, Safety and Environment requirements for the fracture propagation tests 56
Task 3.4 Full scale propagation tests ............................................................................................................ 58
First full scale propagation tests ................................................................................................................ 60
Second full scale propagation tests........................................................................................................... 64
Task 3.5 - Collection of data related to the release of very large quantity of CO2 from broken pipeline ........ 68
Task 3.6 Validation and final set-up of ductile fracture propagation models for CO2 pipeline ....................... 71
Task 3.7 Analysis of dispersion results and comparison between experiments and modelling results ......... 76
WP4: Corrosion and stress corrosion control.................................................................................................... 78
Task 4.1 Corrosion and stress corrosion behaviour of steel pipes and welded joints working in anthropogenic
CO2 environment: upgrade of actual state of the art .................................................................................... 78
Task 4.2 Corrosion and stress corrosion behaviour of steel pipes and welded joints working in anthropogenic
CO2 environment: development of needed new experimental data .............................................................. 82
WP5: Project Management, Procedure Deliverables and Result Dissemination .............................................. 99
Task 5.1 Project Management ...................................................................................................................... 99
Task 5.2 Definition of procedures ................................................................................................................. 99
Task 5.3 Dissemination and discussion of results ....................................................................................... 103
Conclusions .................................................................................................................................................... 105
Exploitation and impact of the research results .............................................................................................. 107
List of Figures ..................................................................................................................................................... 108
List of Tables ...................................................................................................................................................... 111
List of Acronyms and Abbreviations ................................................................................................................ 112
References ....................................................................................................................................................... 114

3
4
Final summary

The general aim of this RFCS proposal is to develop specific requirements and design criteria of steel
pipes for anthropogenic CO2 transportation pipeline systems, and to create the basis for proposing
European Guidelines for safe design and operation of anthropogenic CO2 pipeline networks.
This goal has been achieved through a series of advanced and extensive experimental activities, and
a critical analysis of the results and of the available standards.
As first step in Work package 1 a detailed critical analysis of existing know-how has been carried out
with a specific focus on the following issues:
 Identification of potential impurities for each capture technology. In particular, the three
main process of capture technologies have been considered (i.e. post-combustion, pre-
combustion and oxy-fuel) and the effect of impurities on corrosion and fracture propagation
have been studied together with the limits for the main impurities (e.g. NO x, SOx, H2O, O2….)
 Selection and evaluation of the physical models and computer codes to calculate the
thermodynamic properties of CO2 mixtures. The most acknowledge EOSs have been reviewed
and the main decompression codes have been compared (e.g. GASMISC, GASDECOM, SMIRK
….)
 Description of available models for the assessment of fracture initiation and propagation
events. In particular, the review of the models to predict leak vs. break evolution and of the
fracture control approaches to CO2 pipelines have been performed.
 State of Recommendations and Standardization for CO2 transportation via pipeline. The
recent Recommended Practice DNV-RP-J202, released in 2010, specifically devoted to CO2,
has been considered, together with other standards not developed specifically for the CO2
transportation, but worth to be considered as they are standard coming from oil and gas
industries that, in some cases, take into account the CO2 as possible transported medium
(e.g. ISO 13623, DNV-OS-F101, ASME B31.4…).
 Database of existing pipeline/project for CO2 transportation around the world.
The testing activities planned in the project were focussed on the following items:
 fracture initiation control (full scale activity);
 unstable fracture propagation control (full scale activity);
 corrosion and stress corrosion control (laboratory scale activity).
At the beginning of project all the required pipes for full scale activities have been produced and
delivered as reported in Table 1.
Pipe producer Use No. pipes Geometry Grade
Salzgitter Mannesmann Line Pipe Reservoirs 14 24”x18mm X70
Salzgitter Mannesmann Line Pipe Test line 4 24”x13.7mm X65
Salzgitter Mannesmann Line Pipe Test line 1 24”x13.7mm X65
Europipe Test line 4 24”x12.7mm X65
Corinth Pipeworks Test line 4 24”x12.5mm X65
Corinth Pipeworks Corrosion 1 24”x12.5mm X65
V&M Deutschland Leak tests 2 12”x17.5mm X65
Table 1: Pipe production for the project
Moreover some special components like Crack Arrestors, supplied by SMLP, have been planned to be
installed on both ends of the full scale propagation test line (see Figure 1).

Figure 1: Composite Crack Arrestor for the test line.

5
The materials have been characterized in terms of tensile and toughness properties. The welded
joints for the activity planned in WP4 have been produced according to the WPS developed. An in
depth activity has been carried out for the definition of the WPS and for the execution of the girth
weld joints required both for the corrosion and stress-corrosion activities, but also for the
identification of a good WPS (SMAW) required to the construction of the full scale propagation line
(220m). In fact, this is necessary condition to perform reliable propagation tests.
All the girth weld joints have been designed with SARCO2 partners’ experience, using information
gained by public literature review and with the support of international welding contractors that have
also realized the girth weld joints. All the weld joints realised (SMAW and GMAW) have been
characterized with the aim to verify the good quality. The good quality of the WPS has been also
validated with the two full scale propagation tests, where all the girth weld joints have exhibited a
good behaviour.
An analysis of dispersion models has been carried out, highlighting all PROS and CONS of different
solutions, and the most reliable models have been used for the prediction of the CO2 dispersion from
experimental tests. These models have been used also for the definition of the Health, Safety and
Environment procedures developed for all full scale activities foreseen in the project.
In Work Package 2 fracture initiation control issue has been addressed. Laboratory activities were
performed to obtain specific experiential data about the transition ductile/brittle fracture behaviour
of the selected pipes to be tested in this WP. In particular Crack Tip Opening Displacement (CTOD)
tests were conducted to determine the fracture toughness of the pipe material.
A modelling activity has been carried out to define Health and Safety and Environment (HSE)
Requirements & Loss Prevention Plan to be applied during preparation, execution and post-test full-
scale activities planned in WP2. This activity was focuses to obtain indications concerning the hazard
distances from the release point and the inaccessible time after the test. Moreover, such simulations
have permitted to identify the dispersion area and to design an environmental instrumentation
layout. In particular, a specific instrumentation to measure CO2 concentration and temperature
variations have been installed in the leak test area.
Two full-scale tests have been carried out to evaluate the structural and fluid dynamic phenomena
associated to the CO2 release from a pipe. The 12” test pipe, with a longitudinally oriented through-
wall defect manufactured on the pipe wall, was feed with supercritical CO2 at high pressure at room
temperature. The defect has been kept closed with a stopper device until the test pressure was
achieved and the testing conditions were good to start.
The testing conditions were as follows:
 Test #1: the through wall defect (12.5mm x 0.8mm) was designed so that it is not expected
to evolve into a pipe rupture and the gas will outflow through the leak in a steady state
condition. This was referred as “leak-test”;
 Test #2: the defect size (40.0mm x 0.8mm) was closer to the so called “leak-rupture”
boundary. In this way, the action of the gas outflow was near to border line between leak
and break (that means a potential crack growth).
The tests were correctly executed and in both cases the defect didn’t evolve in break. The acquisition
of temperatures around the defect has demonstrated that the temperature reduction is not so high
as expected from the literature information, in fact if the test is carried out in operating conditions
(simulating the whole length of line with an accumulator CO 2/N2 to maintain the mixture in dense
phase) the pipe wall temperature decreases in negligible way and doesn’t affect the actual toughness
of the pipe.

Figure 2: Leak test from side test#2. Figure 3: Temperature transducers results

A higher decrease of pipe wall temperature happens when the pressure inside the line decrease down
to the saturation pressure due to the fact the mixture inside the line is finishing. In this phase the

6
temperature is low, and as a consequence the pipe toughness could be lower, but also the internal
pressure decreased reducing the risk of change from leak to break.
This effect has been noted in both tests performed with low and higher flow rate due to the defects
dimensions.
During both leak tests, the dispersion of CO2 has been monitored by means CO2 and O2 sensors
located in front of the leak. For the two tests the dispersion data have been correctly acquired both
in terms of CO2 concentration and also in terms of temperature decrease in the area in front of CO 2
jet.
The results show that, in the first test with lower flow rate, the maximum CO 2 concentration was
achieved at 1m from the leak, showing a value of about 3%; and also in terms of temperature
reduction the effect of CO2 releasing was limited to 1-2°C.
In the second test with higher flow rate, the maximum CO2 concentration was achieved at 10m from
the leak, showing a maximum value of about 9% at 1 and 2m; and in terms of temperature reduction
the effect of CO2 releasing was limited to 2-3°C.
The releasing data have been compared with Ansys Fluent CFD code simulations.

Figure 4: Comparison between numerical calculation data and experimental data.

The comparison is very good, as shown in Figure 4; also considering the fact that in the full scale
test even if the wind was very low, it could affected slightly the jet direction with respect to centre
line where there was the line of sensors.
The activity foreseen in the WP3 is mainly related to two full scale fracture propagation tests on a
pipe section of 24in of outside diameter. The tests have been carried out using dense phase CO2
mixtures.
As propaedeutic decompression modelling activity has been carried out both for safety reason and
for the definition of the best location for the environmental sensors to monitor the CO2 dispersion.
This activity was aimed at the definition of specific instrumentation to measure CO 2 concentration
for the fracture propagation full-scale tests. A possible layout of the sensors location has been
defined, based also on the results provided by numerical simulations performed by Ansys Fluent,
ALOHA and Phast 6.7 modelling tools, for the fracture propagation tests.
The aim of the numerical simulations performed with the different codes was the identification of the
maximum dispersion distances from the test area where the CO2 cloud concentration was below 1%
during the propagation tests.
Concerning the Health, Safety and Environment (HSE) requirements, for the fracture propagation
tests, it has been used also the result of the previous calculations to perform a risk assessment
analysis as a support for the test planning and execution. Indications about the hazard distances
from the release point and about the inaccessible time of the test area are supplied with reference
to the possible CO2 levels that are foreseen in atmosphere. The safety limits included in the risk
assessment analysis, have been determined considering the CO2 thermo-fluid dynamics and the
consequences on human health deriving from exposition to different CO2 concentration levels.
The two full scale propagation tests have been carried out in the Military Shooting Range of Nettuno,
located 60km south of Rome where it was authorized the execution of full scale propagation test.
Main tests parameters are summarized in Table 2.
The test lines were instrumented with timing wires (TW) to measure the fracture speed, pressure
transducers (TP), to measure the test pressure and monitor the pressure decay during the fracture
propagation event and thermocouples (TG and T), to measure both the gas and the pipe wall
temperature respectively.

7
FULL SCALE FRACTURE PROPAGATION TESTs PARAMETERS
First test Second test
pipe nominal outside diameter 24in 24in
pipe nominal wall thickness 12.7mm Europipe 12.5mm Corinth Pipeworks
13.7mm SMLP 12.7mm Europipe
13.7mm SMLP
test section length 48m 48m
API 5L steel grade X65 X65
pressurizing medium CO2 mixture (3.8% N2 plus CO2) CO2 mixture (6% N2 plus CO2)
test pressure 129.5barg 127.0barg
test hoop stress 68% SMYS Europipe 68% SMYS Corinth Pipeworks
63% SMYS SMLP 68% SMYS Europipe
63% SMYS SMLP
Table 2: full scale fracture propagation tests general design parameters

Concerning the first propagation test, the fracture was successfully initiated by means of the
explosive charge and propagated on the upper pipe generatrix along both longitudinal directions
(referred as North side and South side according to the geographical position of the line). On site
measurements after the test revealed that fracture deviated from the straight trajectory after 0.8m
of propagation along the North side and after 0.4m along the South side.
Gas decompression behaviour was as expected according to its chemical composition and
thermodynamic condition.
Even if the fracture propagation was short, there exists evidence of a right initiation of fracture and
of two double arrests with typical spiral path. The analysis of the whole set of data and also the
comparison with the second test confirm the good execution of the test and the identification of the
test result as a valid arrest.

Figure 5: First propagation test execution.

Concerning the second propagation test, the fracture was successfully initiated by means of the
explosive charge and propagated on the upper pipe generatrix along both longitudinal directions
(referred as North side and South side according to the geographical position of the line).
In North side the fracture run in the top generatrix in fully ductile manner in the first pipe after
initiation pipe and also in the second pipe at constant speed (~110m/s) arresting in the composite
CA. The arrest in the CA was clear and quite rapid (10-15cm) without generating severance on the
line demonstrating the good design of the CA.
In South side the fracture run in the top generatrix in fully ductile manner in the first pipe after
initiation pipe at constant speed (~120m/s) and arrested in the second pipe after 4,3m. The arrest
in this pipe was clear and with a classical spiral path before arrest, also in this case without generating
severance on the line.
The ejection of line after the test due to the strong driving force and the pour resistance of trench
(sand soil) not affected the results of the test as demonstrated by the shape of the arrests and the
availability of TW data up to the arrest on both sides.
The higher driving force of second test respect to the first one has generated a longer propagation
on both sides as expected. The constancy of the crack speed is due to the fact the large plateau in
mixture decompression force the crack tip to maintain a minimum level of speed even if material
properties can change a little from pipe to pipe.
8
 Figure 6: Second propagation test, line after the test.
The results of the two tests have been used for the validation of the most recognized model for the
identification of minimum toughness requirements (Battelle Two Curve Method - BTC). For this
purpose, additional tests have been considered to the SARCO2 tests because in the same period of
present project, other three tests with CO2 have been carried out within the Cooltrans [1], [2] project
and the data have been published.
The analysis carried out showed that the application of BTC “as it is” is strongly un-conservative for
the application to CO2 transmission pipelines. In fact it is evident in Figure 7 that there are
propagations also for pipes that exhibit toughness values up two times the BTC prediction without
correction factor.

Plotting the arrest/propagation results for all the tests considered here, it is evident that it is not
possible to obtain a unique correction factor (that is the ratio between the toughness value of the
pipe which actually arrested the fracture in the test and the toughness value predicted for having an
arrest by BTCM); looking at Figure 7 a range can be, however identified, that is between 1.6 and
2.2. This range is bounded by an upper and lower line, the first one is the conservative limit on which
all the obtained propagations are avoided.

Figure 7: Evaluation of correction factor for BTC model in the CO2 mixture transportation

Although the correction factor range is not so wide, some tests (see test 4 in Figure 7) exhibited
unexpected results if compared with the others. In any case, due to the small number of tests
available, further investigations and tests are necessary before to considered as reliable the previous
correction factors, in particular because just some testing conditions have been taken into account
and also because these results exhibit a not negligible level of inherent scatter. As basis for
comparison for the natural gas transportation there exist more the 150 full scale propagation tests
available in public literature.
The SARCO2 tests and the other ones available permit now to have a more clear framework of the
limits of the application of BTC model to the CO2 transportation, moreover these tests permit to
state that a correction factor it is mandatory to be more confident to reach the arrest. A range of
correction factor has been identified even is the statistical relevance of this data is limited to five
tests.
The obtained results will be useful for the preliminary design of a new CO2 transporting pipeline in
particular for operating conditions close to those used for the validation of model. In any case due
9
to the fact the set of tests used for the identification of the correction factor is limited in particular in
terms of pipe geometry (medium diameters) it remains recommended, as suggested by the ISO
3183 in its specific annex for requirements to resist to ductile fracture propagation, the execution a
full scale burst test in particular in case of very severe conditions (approach 5, annex G, ISO 3183).
It is important to note that the mixture composition and the operating conditions (mainly operating
temperature) can affect strongly the saturation pressure of the CO 2 mixture generating toughness
requirements extremely high that are not achievable with present metallurgical technologies. This
means that in case of very high values of toughness requirement the use of external devices as crack
arrestors could be the unique solution to overcome the problem of running fracture.
The experimental activities carried out in this project confirm that the crack arrestors are able to
arrest the fracture also in CO2 transporting linepipes where the natural arrest (using just the
toughness of material) is not achievable. A carful design can assure both the arrest of fracture and
also the integrity of the line after the arrest (no severance). Moreover, as demonstrated in the
present project the dimension of the crack arrestor can be reduced with the aim to reduce the impact
on costs.
The consequences of the line rupture and the subsequent gas dispersion in the environment were
also evaluated. This was achieved by means of dedicated sets of transducers: CO2 sensors to directly
measure the CO2 concentration in atmosphere; Oxygen cells in order to estimate the CO 2 levels in
atmosphere from the variations of O2 concentration in air and a set of temperature sensors, to
measure the CO2 cloud temperature.
During both full scale tests the dispersion of the CO2 in the surrounding of the line has been measured
with the environmental conditions. All these data have been analysed and collected in two specific
databases. On the basis of those data, it is observed that:
 The absolute maximum CO2 concentration value is of 8% and it was detected by one
transducer that was located close to the fracture onset section.
 The remaining transducers detected maximum CO2 concentration vales not exceeding 5%;
 CO2 concentrations over 1%, which was considered a sort of safety level for humans in case
of long exposure time (up to 8 hr), are only observed within the first 200s after the pipe
rupture.
 The minimum temperature reached after the expansion of the CO2 in environment
corresponded to +2°C.
In Work Package 4 an upgrade of the actual state of the art has been performed regarding the
corrosion and stress corrosion behaviour of steel pipes working in anthropogenic CO2 environment
for the duration of SARCO2 project.
This literature review and gap analysis, on the likely internal corrosion phenomena relevant to CCS
fluids transportation pipelines, revealed that control of carbon steel CO 2 corrosion in pipelines has a
very significant industrial background in the Oil & Gas industry: mechanisms, modelling, factors
affecting and prevention of corrosion are covered extensively.
Corrosion management by means of corrosion inhibition has been essentially studied and applied, in
the present Oil and Gas industry domain, for equipment subjected to wall loss corrosion damage, i.e.
uniform and localised corrosion damages (including pitting corrosion, mesa corrosion and flow
induced localised corrosion i.e. erosion-corrosion).
In the Oil and Gas domain two main philosophies are adopted for pipelines’ internal corrosion
management and there is a substantial background regarding fundamental knowledge, corrosion
prediction and mitigation practices for their practical implementation. Both rely on the use of bare
steels:
 Wherever possible, the first one consists in operating the pipeline under “dry conditions”.
 The second one consists in operating under wet conditions, either without any inhibitor
treatment (usually where free water corrosivity is low) or with an inhibitor treatment,
together with the use of corrosion monitoring, pipe wall thickness over-sizing (corrosion
allowance) according to the fluid corrosivity, and periodic pipeline inspection, in order to
contain the integrity, throughout pipeline lifetime.
In the CCS context, these two philosophies, and most of the existing corrosion background, should
basically also be applicable. Nevertheless, with regards to the anthropogenic CO 2 transportation, the
range of operating factors covered by this Oil & Gas background is to some extent limited, particularly
as regards two factors, broadly speaking:
 CO2 partial pressure: The high CO2 pressure range involved in the dense or supercritical CO2,
typical of CCS context, which exceeds by far the 0-20 bar range typical of the Oil & Gas
domain, leads to lower water pH, in the range of 3.1 to 3.4.
 Nature and concentration of impurities depending on the captured CO2 fluid treatment.

10
The review has been concentrated on the following main topics:
a) Critical water content for significant corrosion. This is obviously a main topic when
considering the “dry conditions” operating philosophy in the CCS content. The review
revealed some significant recent works addressing this “critical water content level for
corrosion” topic. These results suggest the maximum water level (in the range of 500-600
ppm-vol. which, depending on the nominal pipeline operating conditions, corresponds to ca.
40-50 % of the water saturation level) adopted nowadays in the E.O.R. projects. The review
revealed also that there is a lack of data regarding the “safe” water level that has to be
specified in presence of these specific impurities, and how the level is affected by impurity
content.
b) Uniform and or localised corrosion. The review revealed a clear need to better substantiate
the impact of NOx, SOx, HNO3, O2, H2S impurities and their concentration levels on
uniform/localised corrosion rate of carbon steel exposed to high. The impact of these specific
impurities on the corrosivity of dense or supercritical CO2 mixtures is poorly known.
Moreover, the corrosion predictive models developed in the context of the Oil & Gas industrial
domain cannot be directly transferred to the CCS context. Only very few experimental works
have been dedicated to corrosion inhibition of high pressure dense liquid or supercritical wet
CO2 streams.
c) Concerning the stress corrosion cracking the review has been focussed on:
 Sulphide related cracking phenomena and mechanisms that are relatively well described
and there is no particular argument which could advocate that this background cannot
be applied to the CCS context. Hence, in any CCS project where significant amounts of
H2S impurity is currently expected in the transported CO2, careful consideration must be
paid to the actual water chemistry and pH, and systematic use of fit for purpose tests
accounting for the actual composition of the CO2 streams should be recommended, at
least, considering the present status of knowledge of the H 2S cracking damage scenario
under operational conditions relevant to the CCS pipelines.
 Requiring the simultaneous presence of CO, CO2 and free water, the stress corrosion
cracking damage, attributed to an inhibitive effect of CO linked with the characteristic of
its adsorption to the steel surface, is a well-recognised phenomenon that occurred in the
sixties, particularly in vessel steels and town gas pipelines
In Work Package 4 an extensive experimental activity addressing corrosion issue was performed.
The activity was aimed at investigating the effects of different environments of CO2-mixtures on girth
weld joints realized using two welding techniques: SMAW (Shielded Metal Arc Welding) and GMAW
(Gas Metal Arc Welding). In particular:
 GMAW-C: GMAW girth weld joint with Corinth Pipeworks pipes
 SMAW: SMAW girth weld joint with SMLP pipes
 GMAW-V: GMAW girth weld joint with Vallourec pipes
Three CO2-mixtures, derived from the corresponding CO2 capture techniques, have been selected
(Table 3).

H2O
Component CO O2 NO2 SO2 CH4 N2 Ar H2S H2 CO2
(ppm)

Post-Combustion Composition

600
ppmv 20 100 100 100 200 1690 - - - Bal.
6000
Oxyfuel Composition

Vol-% - 3 0.25 0.25 - 0.75 0.25 - - Bal. 6000

Pre-Combustion

Vol-% 0.4 - - - 0.08 0.6 0.2 3.4 1.8 Bal. 6000

Table 3: Environment Conditions

The corrosion and stress-corrosion resistance of girth weld joints was evaluated by:
 General and localised corrosion under stagnant conditions and rotating cage setup
 Stress Corrosion tests: Four Point Bent Beam spec. in duplicate loaded at 72% and 90% AYS
 Slow Stress Rate Tests
The results of general and localised corrosion under stagnant conditions are summarized in Table 4.

11
 Corrosion Rates (mm/y)
Water
Test Gas Content Inhibitor GMAW-C SMAW GMAW-V
(ppmv)
Weld BM Weld BM Weld BM
Post Combustion 600 No 0.001 0.006 0.004 0.003 0.003 0.004
Post Combustion 6000 No <0.001 <0.001 <0.001 <0.001 <0.001 <0.001
Oxyfuel 6000 No 0.314 0.215 0.348 0.271 0.293 0.292
Post Combustion 6000 Yes <0.001 <0.001 <0.001 <0.001 <0.001 <0.001
Table 4: Results in under Stagnant conditions (BM = Base Material)
The Oxyfuel condition was the worst and all the specimens (base and welded material) suffered of
general and localised corrosion. The inhibitor (HTABr) was not influenced the corrosion rate for the
Post Combustion condition. The results of general and localised corrosion under simulated flow in
rotating cage setup are resumed in Table 5 below.

Corrosion Rates (mm/y)

Water
Test Gas Content Inhibitor GMAW-C SMAW GMAW-V
(ppmv)
Weld BM Weld BM Weld BM
Post Combustion 600 No 0.08 0.04 0.21 0.04 0.15 0.04
Post Combustion 6000 No 0.28 0.26 0.35 0.24 0.30 0.23
Oxyfuel 6000 No 0.12 0.08 0.43 0.09 0.32 0.08
Post Combustion 6000 Yes 0.31 0.21 0.34 0.18 0.22 0.14
Table 5: Results of rotating cage tests
With respect to general corrosion, no substantial differences are found among the three tested
circumferential welded joints in the rotating cage tests. With a water content of 600 ppmv corrosion
rates remain below or in the vicinity of 0.1 mm/a. Water contents of 6,000 ppmv lead to corrosion
rates above this critical value, independent of the applied CO 2-mixture. For all investigated test
conditions corrosion rates are generally independent of the welding procedure. The effect of the
tested inhibitor model substance was exiguous, not leading to significant decrease of the corrosion
rates compared to the benchmark test. At large there is also no significant difference between base
material and weld concerning the corrosion rates. Determination of corrosion rates on specimens
with retained original inner pipe wall is hindered by residua on the test specimens. During pickling
and possibly testing part of these residua might be removed simulating higher corrosion rates. On
the other hand, these residua might evoke higher corrosion rates by facilitating formation of crevice
corrosion conditions beneath the original scales.
Localised corrosion was not observed on machined surfaces of the GMAW-C and SMAW welded joints.
Testing in the Oxy-fuel CO2-mixture led to a heterogeneous attack without formation of pits. In the
Post-combustion CO2-mixture, certain localised attack in form of shallow pits was observed in the
range of the hot pass area of the GMAW-V weld. The roots pass, i.e. the surface exposed to CO 2 in
a pipeline, is not affected.
The results of stress corrosion tests performed on weld material (Table 6) highlighted no evidence
of cracks was observed by stereo microscope, incipient cracks were observed on the cross sections
of GMAW-V and SMAW samples in each test. At 25°C the GMAW samples show a blistering and pitting
attack on the surface.

Temp. Exposure
Test N° Envir. Material AYS% SCC Note
(°C) time (h)
90 No
GMAW Blistering Pitting attack in the Side A
72 No
Pre- 90 No
1 25 720 SMAW MLP Incipient cracks
Combustion 72 No
90 No
GMAW V&M Incipient cracks
72 No
90 No -
GMAW
72 No -
Pre- 90 No
2 Combustion 70 720 SMAW MLP Incipient cracks
72 No
90 No
GMAW V&M Incipient cracks
72 No
Pressure 100 bar – 6000 ppm H2O

Table 6: Results of the SCC corrosion tests

12
The results of the Slow Stress Rate Test are summarised in Table 7.
Sample Test Temperature Fracture Necking Necking Elongation Fracture Fracture Classification
Atmosphere (°C) location % Ratio % elongation elongation acc.to TM0198
% % ratio %
inert WM,HAZ 84.39 7.5 24.19
CO2 Mix 5 BM 80.33 95.19 7.0 22.58 93.33 1
GMAW-C

CO2 Mix WM,HAZ 82.64 97.93 6.8 21.94 90.67 2

inert WM,HAZ 78.5 6.3 20.32
CO2 Mix 70 BM 73.96 94.22 6.3 20.32 100 1
CO2 Mix WM,HAZ 66.72 84.99 5.1 16.45 80.95 2
inert WM 81.92 7.3 23.55
CO2 Mix 5 WM 36.33 44.35 5.1 16.45 69.86 4
SMAW

CO2 Mix WM 37.38 45.63 4.9 15.81 67.12 4

inert WM 83.34 6.8 21.94
CO2 Mix 70 WM 49.38 59.25 4.5 14.52 66.18 4
CO2 Mix WM 35.87 43.04 5.0 16.13 73.53 3
inert WM 85.16 7.3 23.55
CO2 Mix 5 WM 28.58 33.56 4.5 14.52 61.64 4
GMAW-V

CO2 Mix WM,HAZ 47.36 55.61 5.8 18.71 79.45 4

inert WM,HAZ 88.03 6.5 20.97
CO2 Mix 70 WM,HAZ 50.02 56.82 5.3 17.10 81.54 4
CO2 Mix WM 54.82 62.27 5.7 18.39 87.69 4
Table 7: Results of the Slow Stress Rate Tests

Two of the specimen fractures on sample GMAW-C occurred outside the actual weld area. All other
fractures on specimens from this sample occurred on the weld, but on the border area to the base
material (HAZ). In case of the GMAW-V sample also three fractures in the border area (HAZ) were
observed, while on sample SMAW all fractures occurred in the weld metal area.
Dissemination of the SARCO2 project results has been regularly carried out during the whole project
execution, thanks to the large participation of European Companies to the project. Just to remember
EPRG was involved since the beginning and the majority of EPRG members (namely Eni, Shell,
Corinth, SZMF, SMLP, Europipe, etc.) actively participated to meetings where SARCO2 results were
presented and discussed. Also DNV was deeply involved (>15 meetings) before and after major
testing activities and in the results discussion as well with the specific aim to drive the outcomes of
the SARCO2 project inside the new release of Standard (DNV-RP J202).
In addition to that a specific workshop on fracture propagation and CO2 main topics has been
organized in May, 2015, in coincidence with the EPRG-PRCI-APGA Joint Technical Meeting on Pipeline
Research held in Paris. In that occasion SARCO2 results were presented, discussed and compared
with R&D results on similar topics coming from other world institutes. Participants were in fact not
only from Europe but also from USA (PRCI1 members) and Australia (APGA2 and Energy Pipelines
CRC3 members) in addition to worldwide recognised experts (e.g. Andrew Cosham from Atkins)
representing both operator, pipe maker and standardization body points of view.
Concluding, SARCO2 project, through the extensive experimental activity performed including full
scale tests, allowed to collect a comprehensive set of information related to anthropogenic CO2 large
diameter pipeline critical issues, and to give a contribution to the update of the existing standards
and to the ones under development. The outcomes of the SARCO2 project have been collected in
indications and comments to supply support for future releases of actual standard requirements.

1 Pipeline Research Council International, http://prci.org/index.php/about/

2 Australian Pipelines and Gas Association Ltd, www.apga.org.au/about/
3 Energy Pipelines CRC, http://epcrc.com.au/about
13
Scientific and technical description of the results

Objectives of the project

The general aim of this RFCS proposal is to develop specific requirements and design criteria of steel
pipes for anthropogenic CO2 transportation pipeline systems (including also crack arrestors and
composite reinforced pipes), and to create the basis for proposing European Guidelines for safe
design and operation of anthropogenic CO2 pipeline networks. The Guidelines encompass short and
long distance pipelines made using high grade steels and incorporate the crack arrest design criteria
to improve the equivalent toughness of large diameter pipes and composite reinforced pipes.
The specific programme objectives of this proposal are the following:
 to achieve a relevant improvement of know-how and experimental data about toughness
requirements for steel pipes to control initiation and prevent unstable ductile fracture
propagation event;
 to generate new data and collect the available information from public domain on dispersion
of anthropogenic CO2 released from a suddenly fractured pipeline;
 to improve existing safety and reliability predictive tools available on the public domain for
natural gas onshore pipelines and use those for the relevant hazards typical of CO2 pipeline
transportation systems, with particular emphasis on the unstable fracture propagation event.
Moreover, in regard to the fracture event, specific goals of this project were the following:
 development of crack arrest design tools for anthropogenic CO2, in order to guarantee safe
larger diameter pipeline for anthropogenic CO2 transportation, including also composite
reinforced pipes;
 collection, improvement and analysis of existing and available data and knowledge about the
corrosion and/or stress corrosion resistance of both pipe body and welded zone working in
the anthropogenic CO2 environment.

14
Description of activities and discussion

WP1: Design and specification for full scale tests, Test pipes supply. Selection and
analysis of CO2 release models

Task 1.1 Critical Analysis of existing know-how

In work package 1 a detailed critical analysis of existing know-how has been carried out with a
specific focus on the following issues:
 Evaluation of potential impurities for each capture technology.
 Selection and evaluation of the physical models and computer codes to calculate the
thermodynamic properties of CO2 mixtures.
 Description of available models for the assessment of fracture initiation and propagation
events
 State of Recommendations and Standardization for CO2 transportation via pipeline.
 Database of existing pipeline/project for CO2 transportation around the world.
Identification of the potential impurities for each capture technology
First step was the identification of the potential impurities for each capture technology. In fact,
Carbon dioxide may be captured from a wide range of industrial processes. As a consequence, the
resulting CO2 stream may contain several impurities whose concentrations depend on different
aspects, such as the fuel type, the energy conversion and the capture process.
The main processes for the capture of carbon dioxide emitted at fossil power plant are:
 Post-combustion - Where the CO2 is separated from the flue gases produced after combustion
in air environment of a primary fuel.
 Pre-combustion – Where the CO2 is removed from the fossil fuel before combustion, through
gasification (coal) or reforming (gas) and produces a synthesis gas.
 Oxy-fuel – Where fuel oxidation is driven by almost pure oxygen (95-99%) and the resulting
post-combustion flue gas consists of mainly carbon dioxide and water vapour, with little
amount of nitrogen.
Typical composition for each separation processes is reported in Table 8.
Component Post-combustion Pre-Combustion Oxy-fuel
N2 Yes Yes Yes
O2 Yes Yes Yes
Ar Yes Yes Yes
H2O Yes Yes Yes
NOx Yes - Yes
SOx Yes - Yes
NH3 Yes - -
Hg, and other trace metals - Yes Yes
H2 - Yes -
H2S - Yes -
HCN - Yes -
CH4 - Yes -
CO Yes Yes Yes
COS - Yes -
Residues from washing Yes Yes -
Table 8: Expected impurities in CCTS stream from different capture technologies.
The amount of impurities in the stream transported by pipelines for CCTS purpose should be limited
in order to guarantee good levels of safety for transportation and storage. The limit values for the
concentration of the different species should be established taking into account both technical and
health and safety topics.
As an example, in order to control corrosion effects in CO2 pipelines, it is possible to employ one or
more of the following strategies:
 to dry the CO2 to sufficient low levels;
 to make use of corrosion inhibitors;
 to use corrosion resistant material like stainless steel;
 to make use of protective coating and cathodic protection.
A second issue on which the control of amount of impurities is important is related to the fracture
control where the presence of high level of impurities can produces effect on the decompression
path, with an increase in saturation pressures at higher impurities concentrations that results in very
high driving force.
15
Physical models and computer codes to calculate the thermodynamic properties of the CO2
mixtures
A review about the physical models and computer codes to calculate the thermodynamic properties
of the CO2 mixtures has been performed. In order to predict fracture propagation and arrest it is
therefore necessary to compare gas decompression behaviour, i.e. crack driving force, with material
resistance, known as resistance force. This approach has been pursued by Maxey in the early 1970s
[3] and it has led to the formulation of the Battelle two-curve model (BTCM). The evolution of
pipelines operating conditions, i.e. higher pressure and temperature, has been the pushing factor for
developing a detailed gas model for the decompression phase. In particular, the tool to be used for
the driving force description is required to handle real gas mixtures decompression, from operating
pressure through potential phase changes. In this respect it has to be underlined the importance of
correctly predicting the plateau of the decompression curve (corresponding to saturation pressure),
since small error on its evaluation can lead to significant changes in the required minimum arrest
toughness level. Recourse is made to the equations of state (EOS), the relations between pressure,
compressibility factor, temperature and volume which define the thermodynamic state of the fluid in
equilibrium. A review of the EOS has been performed. EOS can be classified on the basis of several
criteria [4] and, referring to the type of equation, the following three main groups may be identified:
 Virial EOS: the compressibility factor is expressed as a power series in the density;
 van der Waals type (vdW) equations of state, which is based on the contributions of attractive
and repulsive intermolecular forces;
 Equations of state based on molecular considerations.
EOSs implemented in most diffused decompression codes belong to virial or vdW type. In particular,
Peng-Robinson (PR) and Soave-Redlich-Kwong (SRK) are typical vdW, while Benedict-Webb-Rubin-
Starling (BWRS) and GERG (2004 and 2008) are virial. Table 9 reports type of EOS implemented in
some decompression codes adopted in the oil&gas field.
Decompression model EOS
GASMISC PR, SRK
GASDECOM BWRS
Shell SMIRK, LKP
University of Calgary (isentropic approach) SRK
University of Calgary (non-isentropic approach) PR
DECAY PR
University of Tokyo BWRS
Exxon BWRS
University of Bochum GERG 2008
University of Edinburgh SRK
Table 9: EOS implemented in most diffused decompression codes.
The previous EOSs are generally implemented in numerical codes with the aim to describe the
decompression behaviours of a real CO2 mixture by plotting the relative decompression curve. The
decompression curve is expressed in terms of the velocity of expansion waves, related to the different
pressure levels reached during the fracture propagation.
The fundamental requirements of a decompression model can be summarized as follows:
 solve the decompression for pure species or for a mixture of different chemical compounds;
 provide complete database for the chemical species, able to reproduce typical mixture
compositions as transported by pipelines (mainly CH4 and CO2 based mixtures);
 ensure a good accuracy for all pressure and temperature values related to pipelines operating
conditions.
At the base of this calculation there are some hypotheses:
 the flow is assumed as one-dimensional;
 decompression is considered isentropic and in homogeneous equilibrium;
 no chemical reaction occurs between species; only molecular interactions are considered;
 negligible effect of fluid velocity prior to the rupture is considered;
 effects of friction and heath transfer are not considered.
In this project the comparison among three codes have been carried out:
 GASMISC, developed by Centro Sviluppo Materiali (CSM) is based on SRK and PR EOS in
conjunction with the MHV1 model.
 SMIRK, developed by Shell is based on Shell Cubic Plus Association equation of state (CPA).
 GERG-2008, as implemented in REFPROP code developed by NIST

16
The accuracy of GASMISC, Shell and GERG-2008 in the evaluation of saturation pressure for CO 2
under decompression has been analysed. Average and maximum errors (Eq. 1) respect to
experimental data (from NOVA shock tube test campaign [5]) are reported in Table 10.

pexp  p pred
emax %   100 Eq. 1
pexp
CO2+N CO2+O CO2+CH CO2+H CO2+C CO2+A Antr+H Antr+A
CO2
2 2 4 2 O r 2 r
GASMIS 19.
22.2 22.4 22.7 14.1 5.7 30.8 9.0 25.7
C 7
emax
27.
(%) GERG 23.8 42.4 28.4 8.9 9.7 31.6 3.7 37.4
6
29.
Shell 18.8 14.1 27.7 11.2 1.0 17.8 6.9 14.0
3
GASMIS
emea 8.5 9.3 15.3 13.3 9.8 5.7 17.0 6.7 10.1
C
n
GERG 6.2 8.8 28.9 14.8 4.9 9.7 20.5 2.4 16.3
(%)
Shell 7.0 8.0 10.3 14.0 6.6 1.0 11.2 4.4 6.6
Table 10: difference in measured and predicted saturation pressure.

Models to predict leak vs. break evolution

One of the most relevant threats for the structural integrity of a pipeline is the presence of a part-
wall defect (that is a non-perforating defect) due to external interference with third parties or
corrosion. Due to the continuous action of the internal pressure the external part-wall defect may
evolve into a through-wall defect and lead to a consequent fluid out-flowing.
Once at this stage, a defect may leak steadily or it may evolve into a rupture thus giving rise to a
fracture propagation along the pipeline (see Figure 8). Both these options are highly undesirable, but
the latter implies consequences of larger extent both in terms of economic consequences (service
interruption, pipes replacement, line reopening, etc.), environmental damages, injuries and fatalities.
Therefore, an important question arises about how to predict whether a through-wall defect will leak
steadily or will evolve into a rupture.
Under this light the longitudinally oriented defects are more critical than the circumferential oriented
defects, since they are subjected to hoop stress which is more intense than the axial action.

Figure 8: leak-rupture development.

A number of methods have been proposed for evaluating the evolution of a through wall defects.
Here in the following two different approaches are proposed which may be adopted when CO 2
pipelines are considered:
 the leak-rupture Battelle NG18 formula;
 the Failure Assessment Diagram.
For the scope of the present project, the first approach has been considered in the WP2 where the
design of the defect dimensions for the full scale test has been done.

Fracture control approach to CO2 pipelines

Fracture control is a key point in the design phase of a new pipeline, in particular when the
transported medium is gaseous fluid. A fracture control plan has to take into account two different
stages (Figure 9):
 Initiation control
 Propagation control

17
Initiation control is related to the capability of pipe material to withstand a certain dimension of
defect produced for example by means an external excavator or a local corrosion problem. Criteria
for assessing the resistance of steel pipelines to initiation of fracture from axial defects are well
established, although based on semi-empirical approaches. All these models state critical defect size,
a defect with greater dimensions became a break/rupture. In this case the pipe loses the capability
to maintain stable the defect dimensions and a fracture starts to propagate in the pipeline.

Figure 9: Fracture control scheme

The aim of this paragraph is focussed on the second part of this sequence, the fracture propagation
control.
Longitudinal propagation of brittle and ductile fracture in gas pipelines represents a critical event
which can seriously affect a long extension of the line, thus causing a long and costly gas delivery
service breakdown.
For natural gas pipelines, there exists a wide literature on fracture propagation control for
conventional and high strength steels operated with lean and rich gases; hundreds full scale burst
tests have been carried out in the last 40 years with the aim calibrate empirical and semi-empirical
models for the prediction for toughness value for arrest the fracture. Otherwise for CO2 transportation
pipelines there is a very pour literature on this topic and, at the beginning of present project, just
the results of two full scale burst tests were available. Moreover these tests were focussed to evaluate
the capability of crack stoppers to arrest the fracture propagation and so not useful for the scope of
present project [6]. This is the reason why the approach to the fracture propagation control for CO2
pipelines is based on the experience gained for the natural gas projects.
As first instance, fracture propagation phenomenon differs depending on the nature of fracture. In
particular, it has been observed that different features appear according to whether the pipe
temperature is above or below a certain transition value, named Fracture Propagation Transition
Temperature (FPTT, [7]). If temperature is above the FPTT, a fracture will propagate in a ductile
mode; on the contrary, the propagation will occur in a brittle manner dependently on how below
FPTT the temperature is.
A good assessment of FPTT in the pipe can be achieved in correspondence of an 85% shear fracture
area in DWTT specimens (ISO 3183:2007 Annex G, [8]).
Ductile fracture is typically characterized by wide crack flanks opening, relevant bulging at the crack
tip and large amount of plastic deformation on the flaps. On the contrary, brittle fracture propagation
is mainly driven by the elastic energy amount stored in the pipe wall thickness, while a small amount
of plastic deformation occurs near the crack tip. Brittle fracture is characterized by a low level of
energy required to propagate, which makes it very difficult to be controlled once that initiated. Very
high crack speeds are experienced and instable phenomena such as fracture “branching” may occur,
thus making brittle conditions highly undesirable.
For these reasons, the brittle fracture is prevented in design phase specifying a value of FPTT lower
that in-field operating conditions for the pipes production. Otherwise the ductile fracture propagation
is controlled requiring a minimum value of toughness of base material. This value is calculated
starting from semi-empirical models developed in the last 30 years.
The majority of models to prevent the ductile fracture propagation events developed for natural gas
applications cannot be applied to the CO2 transportation (EPRG Recommendations, AISI equation,
Battelle short formula, ect.) due to the fact these models are based on interpolation of experimental
data of full scale burst tests carried out with natural gas. The application to the transportation of
supercritical CO2 cannot take into account the different decompression behaviour of gas that exhibits
an important phase transition. The only approach that is able to take into account the CO 2 specific
decompression behaviour is the Battelle Two Curve Approach (BTC).

18
Battelle Two Curve approach
Battelle Two Curve Method is generally considered as the most reliable among the empirical
correlations proposed in the past. The Battelle Two Curve Method was firstly proposed by Maxey [3]
and the key point of this model is that the decompression behaviour of gas is taken into account
using the decompression curve of the used gas. This is the reason why its application can be extended
to the CO2 pipeline transport.
In particular, this model is based on the comparison between the force driving the ductile fracture
propagation and that resisting it. On one hand the crack driving force is given by the gas
decompression curve which is directly connected to the pressure acting on flaps behind the crack tip
and depends on initial operative conditions and chemical composition; on the other hand the fracture
resistance curve which depends on the line pipe geometry, the material toughness and strength.
In practice, this approach considers the gas decompression and the dynamic crack propagation as
uncoupled processes but both related to the crack propagation speed.
Driving Curve
The pressure trend at crack tip is regulated by the decompression process which takes place because
the gas flows through the breach. Each pressure level and its propagation velocity are strictly
correlated and depend uniquely on the thermodynamic properties of the fluid. It means that the
curve pressure-velocity can be simply determined by knowing the gas composition and its boundary
conditions. For large diameter pipelines the decompression process is treated as one-dimensional,
adiabatic and isentropic. But also using these assumptions the decompression behaviour cannot be
foreseen using the well-known equation of state for ideal gases. In fact, the natural gas at high
pressure does not behave as ideal gases, in particular if heavy components are considered (rich
gases) and more so if CO2 in dense/supercritical condition is considered.
So the decompression curve is the result of an output of different gas decompression models based
on several real gases equations of state (Soave Redlich–Kwong; Peng-Robinson, Benedict-Webb-
Rubin-Starling,…). The outputs of these models are decompression curves as those shown in the
Figure 10 on which is evident the large differences in the decompression behaviours between natural
gas (lean and rich) and CO2.

Figure 10: Decompression curves for Pure Methane, Natural Rich Gas and Pure CO2
The presence of a plateau in the decompression curve represents a transition of phase of gas mixture.
In terms of fracture propagation this means that, in these conditions, a decrease of fracture speed
does not produce a decrease of pressure at the crack tip. So these types of gases are more severe
for the fracture propagation phenomenon.
Resistance Curve
According to Battelle model, the variation of the crack speed with pressure is determined through
the analysis of the available full-scale tests under the assumption that the crack speed depends on
flow stress and fracture resistance. It is expressed in the following form:
1
 P  6
Eq. 2
VC  C   1
R  Pa 
where:
Vc : fracture velocity,
C : constant accounting for backfill constraint equals to:
S.I. American Units
Soil Backfill 2.75 0.47
Sea Backfill 2.34 0.40
No Backfill 3.791 0.648

19
 R : material resistance to fracture,
 : flow stress (  = yield stress + 69 MPa)
Pa : arrest pressure.
P : gas pressure.
The C values for the No Backfill and Soil Backfill conditions were proposed by Maxey [3], on the base
of the results of two sets of full scale burst tests, one for pipe having approximately 30 inches (1
meter) of soil and sand cover (neither clay nor rock were used) and the second for a pipe lying in an
open ditch with no soil around it. The C value for Sea Backfill [9] was obtained from three full scale
tests carried out in shallow water (12 m deep), and substantially confirmed by two full scale tests in
open sea (water depth about 30 m) performed by CSM from 1981 to 1987 [10].

The arrest hoop stress a , corresponding to the pressure arrest level Pa is given by:

 
2  E 
a  cos exp 
1
 Eq. 3
3.33  Dt 
 24
2

 2 
where:

E : modulus of elasticity,
D, t : pipe outer diameter and wall thickness

Maxey also demonstrated that R, originally identified with the strain energy release rate G, could be
represented by the upper shelf energy of the Charpy-V specimen per unit area. Relation between
parameter G, equal to K 2IC E and the Charpy-V energy per unit area was found to be:

CVN  E
K 2IC  12 Eq. 4
AC
where:

CVN : Charpy-V Upper Shelf energy, 2/3 Charpy-V notched specimen,

E : modulus of elasticity,
AC : Fracture surface area of the 2/3 Charpy-V notched specimen.

Eq. 3 provides the intercept on the pressure axis of the fracture speed curve. In practice the
procedure consists in the determination of fracture velocity variation with pressure, for pressure
levels higher than the arrest pressure Pa . Then the driving and the resistance force curves are
compared as in Figure 11. The relative position of the two curves determines the potential for
sustained fracture propagation or its arrest. According to the example of Figure 11, if the two curves
do not intercept (curve 3) the decompression velocity is higher than the fracture one for all pressure
levels so that an arrest occurs; if interception is present (curve 1) crack propagation continue
indefinitely since at the interception point the driving and resistance forces have the same value 4;
finally, the arrest/propagation boundary is represented by tangency between the two curves (as in
curve 2) and is associated to the minimum arrest toughness value.
This model is one of the five approaches mentioned in the ISO 3183:2007 Annex G, [8] for preventing
the ductile fracture propagation event, the others, with the exception of the last one that foreseen
the execution of a full scale burst test on real conditions, cannot be applied to the evaluation of
toughness requirements for ductile fracture propagation events because do not take into account the
decompression behaviour of dense/supercritical CO2.

4
Note that only one of the two interception points corresponds to a stable propagation.

20
 Figure 11: Interaction between gas decompression and fracture velocity curves.
The applicability of BTC method is limited to welded pipe, for operating pressures up to 12,0 MPa,
grade up to X80 and diameter over wall thickness ratio in the range 40-115. It is important to note
that if the CVN absorbed energy value derived by this approach exceeds 100 J, based upon full-size
test pieces, the ISO3183 states that the arrest toughness value requires correction and that specialist
advice should be obtained to determine such corrections.
It is important to note as reported in the Recommended Practice DNV-RP-J202 “Design and Operation
of CO2 Pipelines" [11] that:
“The Battelle Two Curve Model is an empirically derived parametric model validated for
Natural Gas and liquids by large scale tests. Even though a number of tests has been
performed for liquids resembling liquid state CO2, at the time of publication of this RP it has
not yet been sufficiently validated with CO2 as test medium”
One of the aims of this project is also to verify the capability of such model to predict the required
toughness level for ensuring the arrest of fracture propagation.
With respect to the application to natural gas pipelines, there are some issues that require a mention.
In particular the first one is related to the shape of decompression curve of dense/super-critical CO2
mixtures. Considering a rupture in a CO2 pipeline, the CO2 initially decompresses rapidly as a liquid
(line A-B Figure 12). The decompression path then crosses the phase boundary on point “B”, and
enters in the two phases zone on which the decompression is much more slow (line B-C Figure 12).
The last part of curve is related to the gas phase decompression (line C-D). The discontinuity in the
decompression curve occurs when the decompression path crosses the phase boundary; the pressure
at which it crosses the phase boundary is the saturation pressure Ps.

Figure 12: CO2 decompression curve Figure 13: Saturation pressure Ps and arrest
pressure Pa
The shape of the decompression curve, and the presence of this large plateau, permits to simplify
the application of Battelle Two Curve model, because it can be assumed that tangent point between
resistance curve and driving curve occur on plateau.
For this reason the model can be simplified imposing that arrest pressure P a has to be equal to
saturation pressure Ps of gas.

 
4 t  RE 
Ps  Pa  cos 1 exp   Eq. 5
3.33 D  Dt 
 24
2

2 
 
21
Related to this point is it important to highlight another difference respect to the fracture propagation
experience gained from natural gas application. The common idea, that increasing the pressure of
gas transported, the requirement of material toughness has to increase decays in case of CO2
transportation. This is due to the above mentioned point that the key value of decompression curve
is the saturation pressure. In fact in some conditions (that are those common used for the transport
of CO2) starting from the same initial temperature, the decompression from higher pressure produce
a stronger cooling of CO2 mixture respect to the decompression from lower value of pressure. This
means that pipelines operating at higher pressure exhibit more lower saturation pressure values
respect to the pipelines operating at lower pressure as showed in Figure 14.

Figure 14: Isentropic decompression path [12]

Another important issue related to the definition of toughness requirement for avoid the fracture
propagation phenomenon in a CO2 pipeline, is presence of impurities on the CO2 mixture. In fact the
presence of impurities such as Methane, Nitrogen and Hydrogen increase a lot the saturation pressure
of mixture and, as a consequence, the toughness required to arrest ductile fracture.

Main issues related to the design of CO2 pipelines

In the design of a CO2 transportation system for the CCTS process, particular attention has to be
paid to some aspects that, due to the nature of the transported fluid, can be critical.
The CO2 is typically transported in a dense phase (supercritical or liquid phase) for economic reasons
(less energy for compression and smaller pipeline diameter) and for transportation purposes
(avoidance of two phases flow).
At the initial design stages of a pipeline, several essential issues need to be considered:
 materials selection
 maximum operating pressure (MOP)
 minimum operating pressure (MinOP)
 depressurization along the pipeline
 effects of impurities
 operating temperatures
The answer to all these issues starts from the know-how related to the natural gas, but in many
cases has to take into account big difference in terms of gas behaviour when applied to CO 2 mixture
transportation.

Materials selection
Different aspects have to be taken into account during the choice of the pipeline materials and the
pipeline components in the CO2 transport:
 When liquid water is present, CO2 partially dissolve and form carbonic acid that give corrosion
problem in carbon steel pipelines;
 In transient simulations involving rapid depressurization the material can be exposed to
temperature below the critical point (<-60 °C);
 Supercritical CO2 is used as an industrial solvent: this solving ability must be taken into
account;
The existing CO2 pipelines are usually constructed of Carbon-Manganese steel (API X60-X80 grade
material, [13]). To reduce the possibility of corrosion occurrence, pipelines typically have an external
22
coating of fusion-bounded epoxy or polyurethane with full cathodic protection. Internal pipeline
coatings are also available and can be applied where appropriate [14].
CO2 is corrosive in the presence of free water but not corrosive if it is dehydrated, even if CO 2 contains
contaminants. Therefore, CO2 has to be properly dehydrated before transportation to avoid corrosion
inside the pipeline. The water inside the pipeline has to be removed completely after hydro testing
using ad-hoc procedures. Total dehydration (100% free water) is possible in theory only a level of
water under the solubility level can be accepted usually <500ppm, but this value is function of
transporting conditions.
CO2 pipelines are considered more susceptible to fast propagating fractures compared to gas
pipelines. During the material selection and dimensioning, the occurrence of a fracture has to be
minimized specifying both a proper value of Fracture Propagation Transition Temperature (FPTT) to
avoid the brittle fracture occurrence and also specifying a minimum level of base material toughness
to ensure the arrest of ductile fracture propagation. The evaluation of minimum level of toughness
required for the arrest of toughness can be done as described in previous paragraph. In some cases,
high temperature and high impurities concentration, it could be very difficult to find a value of
toughness of base material that can permit a natural arrest of fracture. In this case the use of
external devices like crack arrestors can be used.
The construction of a CO2 pipeline requires the use of a lot of components in addition to the steel
pipes: fittings, flanges, pig traps, etc. Some of these components contain also elastomers. The
transport of CO2 requires some specific investigations on that issue because CO 2 diffuses into
elastomers under pressure. When the system pressure is rapidly decreased and the gases that have
permeated or dissolved into elastomers expand, explosive decompression and blistering can occur.
Also in this case there exist some types of elastomers that exhibit better properties for CO2 transport
application as for example the Ethylene-Propylene co-polymers or the Ethylene Propylene Diene
Monomer.
Maximum and Minimum Operating Pressure
The definition of the Maximum Operating Pressure (MOP) is affected by design standards, the
environment, regulations of the government and economic considerations whereas the Minimum
Operating Pressure (MinOP) has to be determined to avoid multi-phase flows and to provide a
sufficient outlet pressure at the end of the pipeline. Besides pressure drops along the pipeline are an
important issue while the intensity of the pressure drops is dependent on the length, the roughness
of the pipeline and the properties of the fluid. The length is given normally by the route between the
existing CO2 capture site and the CO2 storage site. At the points where the pressure falls under the
MinOP, booster stations have to be built to raise the pressure and to avoid phase changes. Phase
changes have a significant and unfavourable impact on the transportation capacities and therefore
on the profitability of the project.
Depressurization along the pipeline
This issue, as above mentioned, is strongly related to avoid the achievement of Minimum Operating
Pressure that can produce the multi-phase flow. As well know the friction loss is function of fluid
properties (viscosity and density), pipe diameter, internal roughness and speed of fluid. One
important issue is that the transport of CO2 in supercritical or dense phase is similar to liquid
transportation in terms of values of viscosity and density. Moreover, it is necessary to take into
account the differences in altitude that produce local pressure variations.
Influence of impurities in CO2 mixture
The different capturing methods produce difference concentrations of impurities in the CO2 mixture,
and here in the following it will be shown the influences of these components on several
transportation issues, in particular the amount of impurities of CO2 have an impact on:
 the critical point at which the present phases changes either from liquid to supercritical or
from supercritical to liquid. A higher amount of impurities results in a movement to a higher
pressure level and a lower temperature of this point.
 frequency and distance of compressor stations. Due to the fact that pressure drops can be
led back to the viscosity of the transported fluid and the friction of the fluid with the pipe.
 pipeline capacity. In fact, the flow rate is dependent on critical properties such as pressures,
temperatures, compressibility, density, elevation and friction factor, most of which depend
on the composition of the transported fluid.
Operating temperature
The transportation temperature has a significant effect on the phase of CO2 for this reason further
consideration on this matter is necessary. Changes in temperature can result in changes of phase
and have to be avoided because they affect the properties of the CO 2 significantly. The internal
friction among the molecules is dependent on the viscosity and cannot be avoided. But viscosity is

23
dependent on temperature and pressure - therefore the detrimental impact can be reduced by
adjusting these parameters. The increase of temperature due to compression can be reduced by a
cooling system after the compression if required.
CO2 standard reference
Despite of a 30 year of CO2 transportation in pipelines for industrial purposes in particular in North
America mainly from natural deposits and gas processing plants for enhanced oil recovery (EOR),
currently only few standards consider carbon dioxide for the design of a pipeline.
In particular, with the exception of recent Recommended Practice DNV-RP-J202, released in 2010,
and the ISO 27913, released in 2016, the other standards are not developed specifically for the CO2
transportation, but are standard coming from oil and gas industries that, in some cases, take into
account the CO2 as possible transported medium. This group of standard contains;

 ISO 13623 “Petroleum and Natural Gas Industries – Pipeline Transportation System” of
International Organization for Standardization (ISO)
 DNV-OS-F101 “Submarine Pipeline Systems” of Det Norske Veritas (DNV)
 ASME B31.4 “Pipeline Transportation Systems for Liquid Hydrocarbons and other liquids”
of American Society of Mechanical Engineers (ASME)
 ASME B31.8 “Gas Transmission and Distribution Piping System” of American Society of
Mechanical Engineers (ASME)
 DEP 31.40.00.10-Gen. “Manual Pipeline Engineering” Design and Engineering Practice by
Royal Dutch / Shell Group
Concerning the DNV-RP-J202 [11] Recommended Practise, that will be soon updated also taking into
account the results of present project, its objective is to provide guidance on safe and reliable design,
construction and operation of pipelines intended for large scale transportation of CO 2 to meet the
requirements given in the referenced pipeline standards.
CO2 specific topics that require special focus on the Standard are:
 Proximity distance: for establishing minimum distances of pipelines from occupied buildings
as function of type of the fluid, the pipeline diameter and its maximum operating pressure.
 Human impact to inhaled CO2: to evaluate the effects on humans exposure of CO2 in terms
of values concentration and duration of exposure.
 Design factor: as function of fluid category and location class
 Specific material selection: in particular, against the corrosion topics in presence of water
Existing CO2 pipeline network
Table 11 lists existing long-distance CO2 pipelines around the world. It is clear, from this table, that
the larger amount of CO2 pipelines is located in North America more than 90% of total, also if in the
last years several projects have been launched regarding the CCTS in particular in Europe.
The most important CO2 pipelines are:
 Canyon Reef. This CO2 transportation pipeline was the first large CO2 pipeline in the USA,
built in 1970 by the SACROC Unit in Scurry County, Texas. Its 289 km moved 12,000 tonnes
of anthropogenically produced CO2 daily (4.6 Mt yr-1) from Shell Oil Company gas processing
plants in the Texas Val Verde basin.
 Bravo Dome Pipeline. Oxy Permian constructed this 508 mm (20-inch) line connecting the
Bravo Dome CO2 field with other major pipelines. It is capable of carrying 7.3 MtCO2 yr-1 and
is operated by Kinder Morgan.
 Cortez Pipeline. Built in 1982 to supply CO2 from the McElmo Dome in S.E. Colorado, the 762
mm (30-inch), 803 km pipeline carries approximately 20 Mt CO2 yr -1 to the CO2 hub at
Denver City, Texas. The line starts near Cortez, Colorado, and crosses the Rocky Mountains,
where it interconnects with other CO2 lines.

24
 Nat / ONshore Year of Steel Grade Design Stress Usage
Country Operator Pipeline Diameter Wall Thickness Length Amount CO2 MAOP
Antrhop OFFshore construction SMYS Temp Level factor
[in] [mm] [MPa] [km] [Mton/Y] [MPa] [°C] [MPa]
N ON USA Exxon Mobil McElmo Creek Pipeline 8 25 60MMCFD
N ON USA Chevron SACROC 16 12,7 450 356 6,8 16,5 264 0,59
N (note1) ON 1984 USA Kinder Morgan Cortez 30 17,5 450 808 19,3 17,9 43 390 0,87
N (note2) ON USA BP Sheep Mountain 1 20 11,1 485 296 6,4 16,6 380 0,78
N ON USA BP Sheep Mountain 2 24 360 9,2
N ON 1984 USA BP Bravo 20 351 7,4 12,3
A (note3) ON 2000 USA/CDN Dakota Gasification Company Weyburn 12 9,5 485 330 4,6 20,2 323 0,67
(note4) 14 9,5 485 18,4 343 0,71
N ON 1986 USA Denbury NEJD (North East Jackson Dome) 20 295 11,6
N ON 1996 USA Transpetco Transpetco Bravo Pipeline 12,75 193 3,3
N (note5) ON USA Kinder Morgan Central Basin Pipeline 26 14,4 485 119 15,0 65 ÷-30°C 343 0,71
N(note6) ON USA Kinder Morgan Central Basin Pipeline 16 10,1 485 37 11,5 17,0 65 ÷-30°C 343 0,71
N ON USA Kinder Morgan Central Basin Pipeline 20 11,1 485 7 15,0 65 ÷-30°C 343 0,71
N ON USA Kinder Morgan Central Basin Pipeline 24 13,9 485 30 15,7 65 ÷-30°C 343 0,71
N ON USA Kinder Morgan Central Basin Pipeline 20 12,4 485 32 16,7 65 ÷-30°C 342 0,71
N ON USA Exxon Mobil Este Pipeline 12 191 4,8
14
N ON USA Trinity West Texas Pipeline 8 79 1,9
12 6
N (note7) ON 1970 USA Kinder Morgan Canyon Reef Carriers 12,75 8,7 450 64 4,6 14,0 259 0,58
1972 USA Kinder Morgan Canyon Reef Carriers 16 9,5 415 225 14,0 299 0,72
ON 1983 Turkey Turkish Petroleum Bati Raman 90 1,1
OFF 2005 Norway Statoil Hydro Snohvit 8 153 0,7
A (note8) ON 1998 USA Petrosource Valverde 10 130 2,5
ON 2005 USA Denbury Free State 20 138 6,7
ON 2008 USA Denbury Delta 49 7,7
ON 2008 USA Denbury Cranfield 82 2,88
ON USA Kinder Morgan Slaughter Pipeline 12 64 160 MMCFD
ON USA Canion Reef Comanche Creek Pipeline
ON USA Exxon Exxon Pipeline
ON USA Trinity Pipeline LLANO System 8 33 100MMCFD
12
ON USA Chevron; Amoco; UNOCAL; Marathon; Raven Ridge Pipeline
Equity; Cameron Family Trust
ON USA Exxon Seminote to Meand Pipeline
ON USA The Wiser Oil Company; Apache; Diverse; Wasson to Wellman Unit
Shore Oil Company Pipeline
ON 2007 USA The Blue Lake Pipeline 26 0,35
ON USA Denbury Choctaw 20 115
OFF 1996 Norway Statoil Sleipner 13 1
N OFF Brasil Petrobras Miranga 6 50
ON 2004 Algeria Sonatrach BP Statoil Hydro In Salah
ON 2010 USA Denbury The Green Pipeline 24 534 "800mcf/d)
ON 2003 USA La Barge 458,00 2,5
ON 2012 Canada Alberta Carbon Trunk Line Enhance Energy 240 14,6
(note9) ON 20XX USA Petrosource Baroil to Dakota CO2 12 7,92 450 249 12,42 239 0,53
ON Baroil to Dakota CO2 8 6,35 450 11 12,42 199 0,44
ON 2011 USA Encore Acquisition Company Greencore CO2 370 1
ON 20XX USA Bell Creek 8 331 100 MMSCF/Day Capacity
Table 11: Database of existing CO2 pipelines

25
 Note CO2 N2 CH4 C2+ H20 H2S O2 CO
% % % % ppm ppm ppm
Note 1 95 <4 mole % 1-5 <5 mole % 257 <0,002 mole
Note 2 96,8 0,9 1,7 0,6 120
Note 3 95,30 0,01 2,00 2,30 20,00 0,30 0,03 0,10
Note 4 96,80 0,30 1,00 1,1%
Note 5 98,50 1,30 0,20 240,00 <20 <10
Note 6 > 95 <20
Note 7 85-98 <0,5 2-15 50 <200
Note 8 99,7 0,3
Note 9 96 3% < 1%
Table 12: Information concerning the chemical compositions

Task 1.2 Design of experimental activities

The aim of this task is to plan and to design the experimental activities, in particular the full scale
tests foreseen in WP2 for fracture initiation control and in WP3 for unstable fracture propagation
control, and also the plan of laboratory scale tests regarding the corrosion and stress-corrosion issue.
In particular requirements and number of pipes to be supplied for the experimental work have been
defined, as well as test parameter conditions for both fracture initiation and fracture propagation
tests.
These activities have been regularly carried out, but for clarity of exposition this part has been
included in this report as incipit of related activity. In particular:
 the leak test rig layout, the definition of defect dimensions and the evaluation of expected
flow rate are reported in WP2 paragraph,
 the test layout for ductile fracture propagation tests, line preparation and the definition of
testing condition in terms of mixture composition, initial pressure and temperature are
reported in WP3 paragraph
 the number of girth weld joints, the number of samples and the testing conditions for the
corrosion and stress corrosion tests are reported in WP paragraph.

Task 1.3 Pipes, crack arrestors and composite reinforced pipes supply.
All pipes for the full scale testing activity have been produced. In particular pipe producers have
produced pipes for:
a) Full scale propagation tests
b) Full scale leak tests
c) For girth welded joints for corrosion small scale laboratory activity
The selected pipes and crack arrestors were made available by the steel-making and pipe-making
industrial partners of the project; these are Europipe GmbH (EP), Salzgitter Mannesmann Line Pipe
GmbH (SMLP), V&M Deutschland GmbH (V&M) and Corinth Pipeworks S.A (CPW). The EP tubes,
which were manufactures pipes using the UOE-formed (UOE) method, and the SMLP and CPW tubes,
which were done using the High-Frequency-Induction (HFI) process, are foreseen for the full scale
propagation test. The seamless pipes from V&M are used for the full scale leakage tests. In total,
about 30 pipes were supplied (some of them have been used for the full scale tests program and the
remaining ones has been used to build the two reservoirs needed for the full scale propagation burst
tests planned in WP3). Also two crack arrestors with were manufactured on HFI pipe sections. Before
the pipes were shipped to the testing area, a section which has been used for the mechanical
characterization was separated from each pipe.
In Table 13 it has reported the list of pipes produced for this project with their relevant information
concerning grade, geometry and employment.

Pipe producer Use No. pipes Geometry Grade

Salzgitter Mannesmann Line Pipe Reservoirs 14 24”x18mm X70
Salzgitter Mannesmann Line Pipe Test line 4 24”x13.7mm X65
Salzgitter Mannesmann Line Pipe Test line 1 24”x13.7mm X65
Europipe Test line 4 24”x12.7mm X65
Corinth Pipeworks Test line 4 24”x12.5mm X65
Corinth Pipeworks Corrosion 1 24”x12.5mm X65
V&M Deutschland Leak tests 2 12”x17.5mm X65
Table 13: Pipe production for the project
Pipes for the construction of the test line and reservoirs are available in CSM full scale burst (Figure
15).

26
Concerning the crack arrestors (CA), for the first test, is foreseen one CA on both ends of the test
section line. These CAs have been supplied by SMLP.

Figure 15: Pipes for full scale activity. Figure 16: Composite Crack Arrestor.
The selected CA typology is the glass fibres composite crack arrestor. This CA has been applied
directly on the two pipes at the end of line as reported in Figure 16. The solution for the second full
scale burst test was the same for the first test due to the fact the proposed CA were not involved in
the fracture.
Concerning the composite CA design, the most sensitive parameter is the reinforcement thickness.
The crack arrestors are designed according to the recommendations reported within RFCS Linespec
[15]. Within the Linespec project a procedure has been developed which permits to derive the
minimum thickness to achieve an arrest of a fracture in a particular range of conditions. According
to the Practical Guideline, which is presented in the Linespec-report, the CAs is fabricated as follows:

Figure 17: Minimum requested composite reinforcement thickness to assure a fracture arrest

HFI Pipe Geometry: D 609,7 x t 12,7 mm, D/t=48

Design Guideline Linespec

tCA=1,15∙t 14,61 mm
LCA=0,8∙D 487,7 mm
Decision

tCA 15 mm
LCA 500 mm
Wrapping O+B = 70 % O, 30% B Flat ending CA-Ends
Figure 18: Winding patterns with 70 %
Table 14: Crack Arrestor Design O (circumferential) and 30 % B (±20 °
inclined)

Task 1.4 Base mechanical characterization and weldability of steel pipes selected for the
full-scale leakage and fracture propagation tests.
In this task laboratory activities have been performed to obtain information about both the base
mechanical properties of selected pipes and their weldability in relation to the construction of samples
for full scale tests.
The complete base mechanical characterization has been carried out on all the pipes used for the
tests (Vallourec, Europipe, SMLP and Corinth Pipeworks pipes). For these pipes the following tests
have been performed:
 Strength mechanical properties – longitudinal and transverse direction at room temperature
and -20 °C (only for seamless pipes)
27
  Toughness testing:
o Charpy V-notch (CVN) – ductile-to-brittle transition curve
o Battelle Drop Weight Tear Test (BDWTT) – at room temperature and -10 °C
Seamless Pipes Results (V&M)
The seamless pipes are foreseen for the full scale leakage tests foreseen in WP2. Both pipes were
produced in one heat and consequently show very similar mechanical properties. The results of the
tensile tests show pronounced yield point and Lüders-elongation, independent of the sampling
direction. In longitudinal direction, the full wall specimens show slightly higher values than the
comparable round bar tensile specimen.
Pipe 1 Pipe2
ReL (RT), MPa 499 - 503 480 – 483
ReL (-20 °C), MPa 496 - 517 463 – 468
Rp0,2 (RT), MPa 484 - 506 459 – 488
Rp0,2 (-20 °C), Mpa 466 - 521 469 – 475
Rm (RT), Mpa 589 - 592 571 – 580
Rm (-20 °C), Mpa 610 - 623 594 – 599
A (RT), % 31,5 – 33,5 29 – 33
A (-20 °C), % 30 – 32,5 30 – 32,5
Ag (RT), % 13,6 – 14,8 13 – 14,6
Ag (-20 °C), % 11,7 – 12,3 12 – 13,6
Table 15: Seamless pipes tensile properties.
Concerning the toughness properties, the Charpy-V notch energy values range from 344 J at -10 °C
to 23 J at -90 °C. The transition temperature defined by a shear area of 50% is in the range of -70
to -80 °C.
Temperature Charpy-V energy SA Temperature Charpy-V SA
°C (J) (%) °C energy (J) (%)
-10 339 100% -10 344 100%
-20 311 100%
-30 301 100% -30 308 100%
-40 317 100% -40 308 100%
-50 294 100% -50 288 98%
-60 249 82% -60 285 97%
-70 249 90% -70 213 75%
-80 60 10% -80 222 78%
-90 76 22% -90 23 5%
Table 16: pipe “1” – Charpy-V energy results. Table 17: pipe “2”–Charpy-V energy results.
The BDWTT specimen had to be fully flattened because the gull winged specimen exhibited a strong
buckling effect in testing. The specimens were tested at three temperatures. Tests at -20 °C and -
30 °C showed a fully ductile behaviour. The specimens tested at -40 °C were invalid according API
RP 5L3 [02], because these specimens showed an inverse fracture with ductile crack initiation
followed by brittle fracture. The determination of shear area portions on the fracture surface produced
values in the range of 30%.
Pipe Specimen Temp SA Total en. Initiation Propagation remarks
[°C] [%] [J/cm2] en. [J/cm2] en. [J/cm2]
1 KM2_003 -20 Invalid-buckling occurs
(dovetail)
1 KM2_004 -20 Invalid-buckling occurs
(dovetail)
1 KM2_005 -30 99 1865 504 1361 flatted
1 KM2_006 -30 99 1725 549 1176 flatted
1 KM2_001 -40 25 682 524 158 Invalid-inverse fracture (flatted)
1 KM2_002 -40 40 1093 477 617 Invalid-inverse fracture (flatted)
2 KM2_007 -20 100 1500 463 1038 flatted
2 KM2_008 -20 100 No measurement (flatted)
2 KM2_011 -30 100 2142 459 1683 flatted
2 KM2_012 -30 99 2157 572 1585 flatted
2 KM2_009 -40 34 1022 562 460 Invalid-inverse fracture (flatted)
2 KM2_010 -40 24 698 431 266 Invalid-inverse fracture (flatted)
Table 18: Battelle drop weight tear test results

28
UOE Pipes Results (Europipe)
Europipe supplied three UOE pipes for the first full-scale propagation test. These pipes have been
selected with increasing toughness values with the aim to have lower toughness pipe in the initiation
section of the line and tougher pipes on the ends of the line (telescopic toughness). For this reason,
EP was asked to supply pipes with Charpy V notch energy of 100J to 150 J. It must be stressed that
this toughness level is exceptionally low for modern steel and is difficult to achieve in praxis. Special
measures had to be taken to come as close as possible to these desired values.
Strength properties required for grade X65 are outnumbered both in yield and ultimate strength. The
values range between 456 and 571 MPa for YS and between 567 and 660 MPa for UTS, respectively.
As to be expected for a cold formed pipe there is a degree of anisotropy between longitudinal and
circumferential properties where the latter yields higher values. The test results obtained at -20 °C
show a slight increase in strength as compared to ambient temperature.
Pipe 125734 Pipe 125728 Pipe 125740
type trans. long. trans. long. trans. long.
Rt0,5 (RT), MPa flat 498 - 506 - 502 - 507 - 464 - 482
Rt0,5 (RT), MPa round 547 - 552 504 - 520 542 - 545 492 - 494 500 - 501 456 - 460
Rt0,5 (-20 °C), MPa round 569 - 571 523 - 525 561 - 566 514 - 520 526 - 529 476 - 490
Rp0,2 (RT), MPa flat - 489 - 500 - 494 - 500 - 451 - 472
Rp0,2 (RT), MPa round 454 - 553 495 - 514 541 - 545 479 - 483 498 - 499 445 - 448
Rp0,2 (-20 °C), MPa round 566 - 568 513 - 514 558 - 564 504 - 512 523 - 525 461 - 476
Rm (RT), MPa flat - 588 - 579 - 584 - 567 - 596
Rm (RT), MPa round 626- 631 607 - 609 622 - 625 597 596 - 597 572 - 577
Rm (-20 °C), MPa round 663 636 - 637 657 - 660 631 631 - 632 610 - 611
A (RT), % flat - 21,5 - 25,5 - 22,5 - 24 - 24,5 - 26
A (RT), % round 21,5 – 22,5 20,5 – 22,5 20,5 – 21,5 23,5 - 25 26,5 – 27 28 – 28,5
A (-20 °C), % round 24 - 26 23 - 24,5 21,5 - 22,5 26 - 27 29,5 - 33 30
Table 19: UOE pipes tensile properties.
In terms of Charpy impact toughness there is a large difference between the highest and lowest
results obtained in the different pipes, as asked for within this project. At ambient temperature, the
values range between 135 J and 260J. The pipe exhibiting the lowest toughness has been served as
crack initiation pipe; the other pipes have been placed in ascending order with respect to their
toughness values. Results of toughness test are summarized in following tables.
Charpy-V energy DWTT energy
Pipe Temperature energy SA Total en. Initiat. En. Prop. En. SA
(ID) (°C) (J) (%) (J/cm2) (J/cm2) (J/cm2) (%)
125734 20 °C 135 100 % 622 179 443 98
125734 -10 °C 120 100 % 506 137 369 98
125734 -50 °C 89 100 % - - - -
125734 -90 °C 55 95 % - - - -
125734 -110 °C 41 85 % - - - -
125728 20 °C 173 100 % 681 231 450 97
125728 -10 °C 153 100 % 562 192 370 95
125728 -50 °C 100 100 % - - - -
125728 -90 °C 66 95 % - - - -
125728 -110 °C 42 80 % - - - -
125740 20 °C 258 100 % 942 295 647 96
125740 -10 °C 228 100 % 742 265 478 97
125740 -30 °C 201 100 % - - - -
125740 -50 °C 155 100 % - - - -
125740 -90 °C 78 80 % - - - -
Table 20: Europipe Pipes toughness properties.
HFI Pipes Results (SMLP)
Two HFI pipes were supplied by SMLP to serve as test pipes in the first full scale propagation test.
Both pipes comply with strength requirements for grade X65. There is no marked difference between
results in longitudinal and transverse direction (see Table 21).
In contrast to the UOE pipes, these SMLP HFI pipes do not exhibit a large difference in Charpy impact
toughness as they simply taken from running production and thereby reflect typical values for
modern pipes. Both pipes exceed 300 J at ambient temperature easily.

29
 Pipe LYO 970/7 Pipe LYO 973/1
type transverse longitudinal transverse longitudinal
Rt0,5 (RT), MPa flat - 504 - 508 - 492
Rt0,5 (RT), MPa round 495 - 497 501 - 506 460 – 464 480 - 485
Rt0,5 (-20 °C), MPa round 505 - 514 528 - 529 505 - 506 505 - 512
Rp0,2 (RT), MPa flat - 499 - 504 - 484 - 486
Rp0,2 (RT), MPa round 484 - 488 502 - 506 459 - 464 483 - 488
Rp0,2 (-20 °C), MPa round 496 - 501 527 - 528 500 507 - 511
Rm (RT), MPa flat - 572 - 579 - 563 - 563
Rm (RT), MPa round 592 589 - 591 578 - 580 571 - 572
Rm (-20 °C), MPa round 617 - 622 617 - 622 614 - 615 600 - 607
A (RT), % flat - 27,5 - 27 – 28,5
A (RT), % round 31,5 - 32 29 - 33 29,5 – 31,5 29 - 33
A (-20 °C), % round 30 – 31,5 38 30 – 33 33
Table 21: SMLP pipes tensile properties.
Thereby, they have the highest toughness level of all 4 pipes to be tested within the first full scale
propagation test.
Charpy-V energy DWTT energy
Pipe Temperature energy SA Total en. Initiat. En. Prop. En. SA
ID (°C) (J) (%) (J/cm2) (J/cm2) (J/cm2) (%)
LYO 970/7 20 °C 320 100 % 1390 419 971 99
LYO 970/7 -10 °C 283 100 % 798 265 533 97
LYO 970/7 -50 °C 246 98 % - - - -
LYO 970/7 -70 °C 216 98 % - - - -
LYO 970/7 -90 °C 23 10 % - - - -
LYO 973/1 20 °C 321 100 % 1381 405 977 99
LYO 973/1 -10 °C 315 100 % 1315 381 934 98
LYO 973/1 -50 °C 265 100 % - - - -
LYO 973/1 -70 °C 242 95 % - - - -
LYO 973/1 -90 °C 23 10 % - - - -
Table 22: SMLP pipes toughness properties.
HFI Pipes Results (Corinth Pipeworks)
Four HFI pipes were supplied by Corinth Pipeworks to serve as test pipes in the second full scale
propagation test. The tensile properties of these pipes is reported in Table 23.
Pipe 7950 17/4 Pipe 7953 17/7 Pipe 7960 18/4 Pipe 7962 18/6
trans. long. trans. long. trans. long. trans. long.
Rt0,5 (RT), MPa 483-447 497-504 467-468 518-521 437-445 489-494 422-437 485-492
Rp0,2 (RT), MPa 470-424 495-502 449-448 517-518 422-426 481-486 399-418 482-486
Rm (RT), MPa 597-586 574-574 608-602 584-586 576-580 565-562 581-573 562-565
A (RT), % 25-25 28-27 26-26 27-27 26-26 30-30 27-27 31-28
Table 23: Corinth Pipeworks pipes tensile properties.
Concerning toughness properties all the pipes have been tested at different temperatures both using
Charpy-V and DWTT samples. All these results are reported in Table 24.
Charpy-V energy DWTT energy
Pipe Temperature energy SA Total en. Initiat. En. Prop. En. SA
(ID) (°C) (J) (%) (J/cm2) (J/cm2) (J/cm2) (%)
7950 17/4 20 °C 260 100 % 810 309 501 100
7950 17/4 -10 °C 256 100 % 746 327 419 100
7950 17/4 -50 °C 219 100 % - - - -
7953 17/7 20 °C 296 100 % 702 287 415 100
7953 17/7 -10 °C 276 100 % 657 281 376 100
7953 17/7 -50 °C 266 100 % - - - -
7960 18/4 20 °C 271 100 % 729 262 467 100
7960 18/4 -10 °C 252 100 % 742 242 500 100
7960 18/4 -50 °C 206 100 % - - - -
7962 18/6 20 °C 274 100 % 795 293 502 100
7962 18/6 -10 °C 243 100 % 786 293 493 100
7962 18/6 -50 °C 218 100 % - - - -
Table 24: Corinth pipes toughness properties.

30
Welding procedure specifications (WPS)
The requirements for CO2 pipeline are more stringent in terms of minimum service temperature (that
is lower temperature) for both base material and welded joints in than in natural gas pipeline, that
is from -5°C ÷ -10°C (typical values of onshore natural gas European pipelines grid) down to -25°C
÷ -30°C (values used in the CO2 “Cortez” pipeline made in USA).
Such lower design service temperature reflects in more demanding requirements for welding
consumables also and the need of specific developed Welding Procedure Specification (WPS) which
should guarantee girth welded joints with good toughness also at such low service temperature.
Welding procedure specifications (WPS) have been developed, in collaboration with a selected
contractor in order to produce the girth welded joints of test samples.
In particular concerning WPS/girth welded joints and the type of welding process as reported in Table
25
Welding Pipe producer Pipe WT Diameter
process
GMAW Salzgitter Mannesmann Line Pipe HFW 13.7 24”
SMAW Corinth Pipeworks HFW 12.5 24”
GMAW V&M Deutschland SMLS 17.5 10 ¾ ”
Table 25: Girth welded joints produced for the project
Three different WPSs have been developed for different techniques (GMAW and SMAW) and for
different pipe geometries. A summary of WPS parameters are reported in Table 26
pWPS id. OD/WT Pipe Welding Preheat / Filler metal Shielding
producer process interpass gas
470 323.9 mm / V&M 5G GMAW 80°C / (AWS ER70S-6) Root: C1
17.5 mm Max 250°C Union K56, M21 (C18)
Ø1.0÷1.2 mm
Sarco2/X65 24’’ / Corinth 5GGMAW 15°C / (AWS 5.28:ER80S-Ni1) Root: C1
GMAW 12.5 mm Max 250°C FILCORD Ni, Ø1.0 mm M31
Sarco2/X65 24’’ / MLP 5GSMAW 50°C / (AWS A5.5-96: E8016-GH4 R) -
SMAW Basic 13.7 mm Max 200°C FOX EV60 PIPE, Ø3.2÷5.0mm
Table 26: Summary of WPS parameters
The girth welded joints have been executed and the qualification is in progress according to European
standards such as EN12732, EN ISO 15614 Part 1. In particular toughness and tensile tests have
been performed both at room and low temperature (as -10°C or lower).
The welding activities were carried out by Pipeline Welding Contractors with international experiences
in gas pipeline construction, such as Ghizzoni S.p.A. (headquarters Parma, Italy) and F.lli Aguzzi
s.r.l. (headquarters Rieti, Italy).
GMAW process (OD 323.9 mm, WT 17.5 mm)
The girth welds were carried out in 5G position (downhill) by GMAW (Figure 20). The welding
procedure specification (WPS, Figure 19) was prepared and approved by the project partners. Root,
hot, filler and cap passes were welded using a consumable of AWS ER70S 6 (Union K565). The pipes
were fixed by tack welds (without a gap) to avoid offset of the edges. The preheating and interpass
temperatures were kept between 80°C and 250°C. In total 4 girth welds were carried out (labels QH,
QI, QJ and QK). One girth weld (QK) was subjected to mechanical tests. Following tests were
conducted:
 Non-destructive testing:
- Visual inspection;
- Radiographic examination;
- Ultrasonic inspection;
 Destructive testing:
- Macro;
- Hardness (HV10 root + cap);
- CVN in notch positions in WM and HAZ
- transverse weld tensile tests;
- side bend tests.

5
The test certificate of the consumable is given in http://www.mip-
co.com/Download.ashx?f=/Uploads/Photos/Bohler-Welding-Germany119.pdf

31
Figure 19: WPS for GMAW girth welding of X65M 323.9 mm pipe

32
 Figure 20: Orbital welding system. Figure 21: Sketch of the sampling points, girth weld QK.
The sampling points of the different test coupons are sketched in Figure 21.
The welded sample was subjected to surface and volumetric NDT. Regarding the girth welds QH, QI
and QJ only some welder related defects such as gas pores were found during x-ray testing, but led
to the assessment acceptable. In case of girth weld QK a small part of the weld failed the radiographic
examination. In agreement with the partners this part was excluded from mechanical testing.
The macrograph is presented in Figure 22. No weld imperfections were found within the prepared
cross section.

Figure 22: Macrograph of girth weld QK, Figure 23: Hardness ranges of the root and cap area as a
X65, 3 o´clock position function of the position.
Hardness HV10 measurements were carried out in the BM, HAZ and WM of the cap and root layer in
2 mm distance to the corresponding surface. The main results are illustrated in Figure 23. The HAZ
hardness ranges from 191 to 224 HV10 in the root and the cap area. However, in the WM hardness
values in the range of 230 to 237 HV10 were measured. The BM hardness is in the range of 181 to
207 HV10.
The cross weld tensile test was carried without reinforcement. The results are summarized in Table
27. The tensile strength of both test specimens exceeded the SMTS of 535 MPa (X65) acc. ISO 3183.
Both specimens broke in the BM. The corresponding tensile strength ranges from 566 to 571 MPa.
Type N° Tensile strength (MPa) Failure position
QK2 571 Parent wall
QK3 566 Parent wall
Table 27: Transverse weld joint tensile test results (cap removed) of girth weld QK, X65.
Transverse side bend tests were carried out according to the standard ISO 5173. All specimens
passed a 180° lateral bending on a 50 mm diameter mandrel. Both specimens passed the
examination without any indications.
Charpy tests were conducted in notch positions WM, FL (HAZ 50/50) and FL+2 at -20°C. The results
are given in Table 28. Summarizing the results good impact toughness can be stated in all notch
positions at -20°C test temperature. 86 J / 182 J (minimum / averaged) impact energy was achieved
in notch position FL (27 J are required according ISO 3183 and 38 J / 45 J are required acc. DNV OS
F101). In notch position WM impact energies in the range of 140 to 154 J were measured. The
highest impact test results were observed in notch position FL+2. Here values in the range of 368 to
420 J were gained.

Sampling Temperature Adsorbed energy Average

(°C) (J) (J)
WM -20 140 150 154 146
FL 420 406 368 398
FL+2 86 200 182 156
Table 28: Impact test results at -20°C, girth weld QK, X65.

33
GMAW process (OD 24’’, WT 13.0 mm)
As a part of the project the weld joints were carried out on pipes of the grade ISO 3183 X65 (OD 24’’
mm x WT 13.0 mm) using fully mechanized GMAW in welding position 5G (downhill).
Welding was performed by 2 orbital bug-and-band type machines, each connected to a computer-
controlled GMAW inverter (Figure 24). The welding conditions were pre-programmed and stored
inside the equipment electronic memory for consistent quality along the various pipe sectors.

Figure 24: Orbital welding system Figure 25: GMAW girth welding of X65M 24’’ pipe
The WPS was prepared by CSM and approved by the project partners. Welding consumable chosen
as follows:
 Root was welded using a consumable of AWS ER70S-6 (LINCOLN - SupraMIG Ultra6);
 Hot, filler and cap passes were welded using a consumable of AWS ER80S-G (OERLIKON -
Carbopipe 80 Ni7).
The preheating and interpass temperatures were kept between 80°C and 250°C. In Figure 27 is
shown the WPS.
In total three girth welds were carried out (Figure 25). One girth weld was subjected to mechanical
tests. Mechanical characterization of girth weld joint was the same of previous paragraph.
The welded sample was subjected to surface and volumetric NDT. No significant imperfections were
pointed out, with consistent evidence of:
 Regular ripples and correct edges fusion;
 WM merging smoothly with the parent plate;
 No spattering revealed on the cap surface.
The macrograph is presented in Figure 26. No weld imperfections were found within the prepared
cross section. Examples of the microstructure observed in the weld and HAZ (cap and root) are
shown in Figure 28 and Figure 29, respectively.

Figure 26: Macrograph of girth weld.

6 The test certificate of the consumable is given in http://www.lincolnelectric.com/assets/global/Products/

ConsumableEU_MIGWires-SUPRAMIG-SUPRAMIGUltra/Supramig-Ultra-it.pdf
7 The test certificate of the consumable is given in http://www.oerlikon-welding.it/file/otherelement/pj/ee/5f/bf/44/ catalogo
consumabili oerlikon 7195806365469887355.pdf
34
Figure 27: pWPS for GMAW girth welding of X65M 24’’ pipe.

35
 Figure 28: Microstructure near the weld cap: WM (left) and HAZ (right).

Figure 29: Microstructure near the weld root: WM (left) and HAZ (right).
Hardness survey was carried out using the Vickers method with a test force of 98.07 N (HV10) on
transversal sections taken across the joint. Hardness was recorded in rows across the WM, the HAZ
and the BM.
The results are shown in Figure 30. The HAZ hardness ranges from 187 to 226 HV10 in the root and
the cap area. The WM hardness values in the range of 208 to 223 HV10 were measured. The BM
hardness is in the range of 190 to 214 HV10.

Figure 30: Hardness profiles on transversal section.

The transverse weld tensile test was carried without reinforcement. The results are summarized in
Table 29. The tensile strength values of both test specimens are just below the SMTS of 535 MPa
(X65) according ISO 3183, but both specimens broke in the BM.
Type N° Tensile strength (MPa) Failure position
24_RT1_TT1 525 Parent wall
24_RT1_TT2 533 Parent wall
Table 29: Tensile test results.
Transverse side bend tests were carried out according to the standard ISO 5173. All specimens
passed a 180° lateral bending on a 50 mm diameter mandrel.
Charpy tests were conducted in notch positions WM and FL at room temperature and -40°C. The
results are given in Table 30. Summarizing the results good impact toughness can be stated in at
test temperature (27 J are required according ISO 3183 and 38 J / 45 J are required acc. DNV OS
F101).

Sampling Temperature Adsorbed energy Average

(°C) (J) (J)
WM 132 120 157 136
RT
HAZ 228 272 237 246
WM 52 41 65 53
-40
HAZ 213 78 218 170
Table 30: Impact test results at room temperature and -40°C.

36
SMAW process (OD 24’’, WT 13.0 mm)
As a part of the project the activity on SMAW girth weld joints was carried out on pipes of the grade
ISO 3183 X65 (OD 24’’ mm x WT 13.7 mm) using SMAW (Figure 31) in welding position 5G (uphill).

Figure 31: SMAW girth welding of X65M 24’’ pipe Figure 32: SMAW girth welding of X65M 24’’ pipe
The welding procedure specification (WPS) was prepared by CSM and approved by the project
partners. Welding consumable chosen as follows: root, hot, filler and cap passes were welded using
a consumable of AWS A5.5-96: E8016-G (Böhler - FOX EV60 PIPE8). The preheating and interpass
temperatures were kept between 50°C and 200°C. In Figure 35 is shown the pWPS.
In total three girth welds were carried out (Figure 32). One girth weld was subjected to mechanical
tests.
The welded sample was subjected to surface and volumetric NDT. It was difficult to retain a regular
inner WM profile over the whole circumference (Figure 33). Anyway, SMA weldments were found to
have acceptable volumetric imperfections level (isolated pores) and some WM root concavity.

Figure 33: Irregular inner WM profile Figure 34: Macrograph of girth weld.
The macrograph is presented in Figure 34. No weld imperfections were found within the prepared
cross section. Examples of the microstructure observed in the weld and HAZ (cap and root) are
shown in Figure 36 and Figure 37, respectively.

8 The test certificate of the consumable is given in http://www.mestriner.it/easyUp/file/1562_fox_ev60_elettrodo.pdf

37
Figure 35: pWPS for SMAW girth welding of X65M 24’’ pipe.

38
 Figure 36: Microstructure near the weld cap: WM (left) and HAZ (right).

Figure 37: Microstructure near the weld root: WM (left) and HAZ (right).
Hardness survey was carried out using the Vickers method with a test force of 98.07 N (HV10) on
transversal sections taken across the joint. Hardness was recorded in rows across the WM, the HAZ
and the BM. The results are shown in Figure 38. The HAZ hardness ranges from 194 to 209 HV10 in
the root and the cap area. The WM hardness values in the range of 176 to 217 HV10 were measured.
The BM hardness is in the range of 191 to 241 HV10.

Figure 38: Hardness profiles on transversal section.

The transverse weld tensile test was carried without reinforcement. The results are summarized in
Table 31. The tensile strength of both test specimens exceeded the SMTS of 535 MPa (X65) according
ISO 3183. Both specimens broke in the BM.

Type N° Tensile strength (MPa) Failure position

24-SM-TT1 566 Parent wall
24-SM-TT2 567 Parent wall
Table 31: Tensile test results.
Transverse side bend tests were carried out according to the standard ISO 5173. All specimens
passed a 180° lateral bending on a 50 mm diameter mandrel.
Charpy tests were conducted in notch positions WM and FL at room temperature and -40°C. The
results are given in Table 32. Summarizing the results good impact toughness can be stated in at
test temperature (27 J are required according ISO 3183 and 38 J / 45 J are required acc. DNV OS
F101).

Sampling Temperature Adsorbed energy Average

(oC) (J) (J)
WM 236 218 192 215
RT
HAZ 263 298 240 267
WM 42 74 44 53
-40
HAZ 148 70 62 93
Table 32: Impact test results at room temperature and -40°C.

39
Task 1.5 State of the art and gap analysis of available modelling CO2 releases and
subsequent dispersion. Set-up of selected dispersion model
The available modelling approaches for the analysis of atmospheric dispersion of CO2 released from
a fractured pipeline have been reviewed. Basically, three main types of gas dispersion models exist
(for continuous releases), listed from low-to-high complexity:
 Gaussian models,
 Integral models,
 Computational Fluid Dynamics (CFD) models.
These different types of models are adapted for specific dispersion scenarios.
In the present study, Gaussian, integral and CFD models have been analysed and their advantages
and drawbacks are following summarized:

Gaussian models
 based on simplified fluid dynamic relations;
 flow emission from the release source is modelled in quasi-one dimensional way;
 the dispersion phase is mainly driven by transporting and diffusion conditions;
 generally easy to implement;
 give a quick overview of the spatial and time dependent evolution of CO2 concentration in
the atmosphere;
 many simplifications are considered, especially related to the emitting source modelling and
to the atmospheric conditions;
 give usually highly conservative results.
Integral models
 based on the solution of Gaussian-like transport and diffusive functions;
 more advanced than Gaussian models, since adopting less simplifying hypotheses;
 interactions with buildings is usually not allowed;
 give fast response without any specific skill required for its adoption.

CFD models
 able to solve the fundamental Navier-Stokes equations of fluid dynamics;
 applicable from basic to complex fluid dispersion problems;
 solve the contaminant evolution in time and space;
 account for the real atmospheric conditions in terms of spatial and time dependent wind
velocity and temperature profiles;
 high computer capabilities and strong user competences are required;
 time consuming technique.
To conclude, CFD and simple models as Gaussian or Integral ones can be complementary. The
advantage of the CFD is to limit the simplification of the governing equations, and allows to take into
account different influencing flow features, such as turbulence, Joule-Thomson effect, that play an
important role in the vicinity of the release source, particularly if velocities are high. When passive
dispersion area is reached, simple models can be used, provided the wind profile is correctly declared.
Therefore, for a release with high velocities generating strong turbulence, especially in presence of
obstacles, it is advised to use CFD model. The implementation of the test case for a CFD simulation
requires a strong user experience, devoted mainly to choose the domain size that does not influence
the results and to create a grid able to correctly solve the boundary layer. However, a trade-off must
be searched to reduce the cell number and calculation time.
For more passive release with no obstacles, simple models may be appropriate, particularly for fast
in-field analyses.
For each of the model considered it has been selected one commercial code able to solve CO2 release
and dispersion from a pipeline as a consequence of leak or rupture:
 ALOHA 5.4.3 for Gaussian model;
 Phast as integral model;
 Ansys Fluent 13.0 for CFD modelling.

40
WP2: Fracture initiation control

Task 2.1 Mechanical characterization of steel pipes selected for the full-scale tests
Additional to the mechanical characterization on base material in task 1.3, laboratory activities were
performed to obtain specific experiential data about the transition ductile/brittle fracture behaviour
of the selected pipes to be tested in this WP2. In particular Crack Tip Opening Displacement (CTOD)
tests were performed to complete this mechanical characterization of the full scale leakage test
tubes.
CTOD tests were conducted to determine the fracture toughness of the pipe material. With view to
a leak scenario in a pipe when the crack tips may cool down locally due to the Joule-Thomson effect,
temperatures well below service temperature have to be anticipated. There are indications in the
literature that the crack tips may cool down to at least -40°C. Therefore, CTOD tests were conducted
at ambient and -40°C on both pipes. In order to reflect the constraint condition inherent in a pipe,
shallow notch specimens were tested in addition to standard deep notch specimens. The tests were
conducted on SENB specimens.
All results were clearly on the upper shelf, regardless of both test temperature and constraint in the
specimen. There is no difference in CTOD values between ambient and -40°C, merely the lower
constraint in the shallow notch specimens led to higher values in these tests which were again
uninfluenced by the temperature. The deep notched specimens led to CTOD values of 0,6mm to
0,8mm whereas the shallow notch specimens ranged between 0,8mm and 1,5mm.

Specimen no. Pipe no. T a/W Crack length KI CTOD

[°C] [mm] [N/mm3/2] [mm]
KM2_53 1 20 0,3 3,6 2394,3 0,96
KM2_55 1 20 0,3 4,1 2301,2 0,84
KM2_56 1 -40 0,3 3,43 2519,7 1,19
KM2_58 1 -40 0,3 2,68 2655,8 1,55
KM2_226 1 -40 0,3 2,94 2504,3 1,36
KM2_62 1 20 0,5 5,28 2045,7 0,67
KM2_63 1 20 0,5 5,26 2055,7 0,67
KM2_64 1 20 0,5 5,47 2055,5 0,61
KM2_65 1 -40 0,5 5,73 2178,2 0,62
KM2_66 1 -40 0,5 5,34 2304,5 0,69
KM2_67 1 -40 0,5 5,28 2287,5 0,81
KM2_71 2 20 0,3 2,9 2520 1,32
KM2_72 2 20 0,3 3,1 2417 1,11
KM2_73 2 20 0,3 2,84 2446 1,53
KM2_74 2 -40 0,3 3,12 2578 1,33
KM2_75 2 -40 0,3 3,17 2596 1,13
KM2_76 2 -40 0,3 3,31 2513 1,1
KM2_80 2 20 0,5 5,28 2037,1 0,79
KM2_81 2 20 0,5 5,23 2030,1 0,75
KM2_82 2 20 0,5 5,24 2008,5 0,7
KM2_83 2 -40 0,5 5,32 2290,6 0,72
KM2_84 2 -40 0,5 5,2 2276 0,78
KM2_85 2 -40 0,5 5,14 2253,9 0,67
Table 33: CTOD result on V&M pipes

Task 2.2 Definition of dispersion instrumentation and its layout for Leak before Break tests
This task is aimed at the definition of specific instrumentation to measure CO 2 concentration for the
full-scale leak tests. A layout of the sensors location has been defined, based also on the results
provided by numerical simulations performed by Phast 6.7 modelling tool, for the leak before break
tests. The CO2 dispersion in the atmosphere has been evaluated for possible scenarios of WP2 full-
scale tests, characterized by:
 12” outer diameter pipe;
 liquid CO2 pipeline connected to a supercritical storage reservoir in order to ensure a
“constant” flow rate;
 initial pressure inside the pipe varying between 100 and 200 bar;
 CO2 temperature equal to the ambient temperature (15°C).
A defect has been considered on the pipe wall, which leads to a leak hole depending on the pressure.

41
Four weather scenarios have been investigated, in order to analyse the influence of atmospheric
conditions on the CO2 dispersion:
 stable conditions with a wind velocity at 10 m of 1.5 m/s: 1.5F;
 unstable conditions with a wind velocity at 10 m of 1.5 m/s: 1.5A;
 stable conditions with a wind velocity at 10 m of 5 m/s: 5F;
 unstable conditions with a wind velocity at 10 m of 5 m/s: 5A.
The numerical results have shown that weather conditions presents only poor effects on CO 2
dispersion in the first meters close to the source and that the stable atmosphere (F) provides longer
dispersion distances than the unstable conditions (A). More in the detail, among the cases simulated,
the 1.5/F is the most critical, providing the longest dispersion distances presented in Table 34. It has
been pointed out that CO2 concentration along the centreline increases with the operating pressure,
while the gas temperature decreases. For all the conditions simulated a distance of 20 m from the
source are necessary to reach a concentration of about 1% and a temperature close to the ambient
value.
On the basis of the above considerations, it is therefore advised to place the sensors within a distance
of 20 m from the release point, with a refinement between 0 and 5 m. As a consequence, a proposal
for the layout of the 36 CO2 sensors is presented in Figure 39.

Case Distance to 1% Distance to 0.5% Distance to 0.2% Distance to 0.1%

(m) (m) (m) (m)
P=100 bar, 1.5/F 10 25 85 130
P=150 bar, 1.5/F 15 40 125 190
P=200 bar, 1.5/F 25 65 180 280
Table 34: Characteristic distances for the leak before break tests of SARCO2

Figure 39: Position of the environmental sensors for the leak before break tests

Task 2.3 Development of HSE requirements for full scale Leak before Break tests
The aim of this task is to provide and interpret modelling data needed to define Health and Safety
and Environment (HSE) Requirements & Loss Prevention Plan to be applied during preparation,
execution and post-test full-scale activities planned in WP2.
Indications concerning the hazard distances from the release point and the inaccessible time of the
test area have been supplied, also based on the results provided by numerical simulations performed
by Phast 6.7 and ALOHA modelling tools, for the leak before break tests.
The ALOHA simulation results for the most critical scenario (1.5/F, 200 bar) are reported in Figure
40, in terms of area in which the ground CO2 concentration is predicted to exceed the levels of 0.5%
(5000 ppm, yellow zone) and 1% (10000 ppm, orange zone), at some time after a release starting.
On the basis of the above considerations, the minimum safety distance from the release point,
referred to 1% CO2 level in air, can be fixed at 128 m. The 1% concentration has been assumed as
reference value for the risk assessment analysis because represents the upper limit of CO 2 in air
which allows staying up to 8 hours with no consequences for human health.

42
 Figure 40: CO2 dispersion footprint as Figure 41: Time evolution of CO2 concentration at
predicted by ALOHA for the most critical 128m from the source, 1.5/F - 200 bar.
scenario

Finally, Figure 41 depicts the time evolution of CO2 concentration at 128 m downwind from the
source, which corresponds to the last point reached by a CO2 level equal to 1%, referred to a release
period of 15 minutes. As can be seen, the inaccessibility time of the test site, defined as the minimum
interval time after the release initiation required for the abatement of CO 2 concentration below 1%
in the entire domain, can be fixed in about 20 minutes.
Starting from these considerations the safety area and the inaccessibility time of the test site has
been defined in conservative way.

Task 2.4 Full-scale leakage tests

In the frame of SARCO2, two full-scale tests were scheduled to evaluate the structural and fluid
dynamic phenomena associated to the CO2 release from a pipe. Pipe geometry for leak test was
12.75in OD x 12.9mm WT. A longitudinally oriented through-wall defect has been manufactured on
the pipe wall and plugged with a stopper until the test target pressure is achieved. At that moment
the stopper is removed and the gas release starts.
The two tests differ in terms of the leak size. In particular:
 test #1: the through wall defect was designed so that to not evolve into a pipe rupture and
the gas outflow through the leak in a steady state condition;
 test #2: the defect size was designed closer to the so called “leak-rupture” boundary. In this
way, the action of the gas outflow could produce a potential crack growth this resulting in a
potential rupture.
To this aim, a criterion is required to establish whether the longitudinally oriented leak is expected
to evolve into rupture or not. Among the available predictive models, most reliable for the material
and operating conditions of interest is the Battelle NG-18 (flow-stress dependent formulation) [18],
which takes into account both the pipe material properties and the gas pressure inside the line. It is
here shown that “rupture” and “leak” regions are discriminated by means of a boundary curve, that
is function of the pipe geometry, the material properties and the axial length of the leak. It is here
shown that high pressure or large axial size promote the rupture, while low operating pressure or
small defects promote the leaking.
Both test#1 and #2 was designed so to reproduce the event of the CO2 decompression taking place
in a real pipeline, where the small size of the leak compared to the large pipeline size allows
considering the mass of CO2 escaping from the hole as negligible to the total amount of gas flowing
along the line. In such conditions, it was expected that the constant thermodynamic conditions
(pressure, temperature) inside the pipeline leads the decompression phenomenon to a stationary
regime. Therefore, the leaking phenomenon may take place indefinitely.
Reproducing such stationary conditions on a pipe of limited length requires an adequate design of
the testing set up (Figure 42) and of the testing parameter. As a matter of fact, the following
specifications are imposed:
 the gas flow rate through the leak has to be constant for the duration of the whole test;
 test duration has to be long enough as to allow the gas expansion through the leak to cool
down the surrounding external pipe wall and (if the case) to produce the potential
embrittlement of the material. This time has been estimated to be 10 minutes minimum.

43
  the total amount of CO2 available for the test is bound to ~1ton.
The test specifications are summarized in Table 35.

PARAMETER VALUE

pressure 130 bar

temperature room, 15-25 °C
CO2 mass to be
1000 kg
released
test duration ~10 min
longitudinal through
leak shape
wall slit

Figure 42: Sketch of leak test rig Table 35: Test data.

By basing upon those test specifications the through-leak flow rate has been designed as well as the
leak size for both test#1 and test#2.
In the following sections, the procedures for the defects design are summarized.

First leakage test

Aim of the test is to evaluate the CO2 behaviour while expanding through a leak defect in steady
state condition for a time of about 20min. Since the total amount of CO2 at disposal is given, the
leak size was designed to assure the adequate flow rate to meet the target test duration.
So, the key point in the leak defect sizing is the definition of the mass flow per unit area, which is
given by the product of the CO2 density and the velocity, both measured at the escaping area. The
total amount of CO2 released through a leak is given by:

𝑀𝐶𝑂2 = (𝜌 ⋅ 𝑣) ⋅ 𝐴 ⋅ 𝑡 Eq. 6

where:

𝑀𝐶𝑂2 [kg] CO2 mass

𝜌 [kg/m3] CO2 local density
𝑣 [m/s] local flow speed
𝜌⋅𝑣 [kg/(m2 s)] mass flow per unit area
𝐴 [m2] cross section area of the leak
𝑡 [s] test time
The total amount of available CO2 was fixed and it is equal to about 1000kg, the test duration was
specified in the range of 10-20min. It results therefore that the leak section (A) is function of the
specific mass flow (ρ ⋅ v):
𝑀𝐶𝑂2 1
𝐴= ⋅ Eq. 7
𝑡 𝜌⋅𝑣

Therefore, as a first step it is essential achieving a good estimate of the mass flow per unit area, that
is function of the initial pressure and temperature conditions. To this aim, Lees equation (Lees, 1996)
for isentropic expansion has been used:

2 (ℎ
𝜌𝑒𝑥𝑖𝑡 ⋅ 𝑣𝑒𝑥𝑖𝑡 = 0.62√2𝜌𝑒𝑥𝑖𝑡 𝑣𝑒𝑠𝑠𝑒𝑙 − ℎ𝑒𝑥𝑖𝑡 ) Eq. 8

where h is the gas enthalpy.

The reliability of the Lees equation has been evaluated, inside the SARCO2 project, against a set of
experimental tests performed by British Petroleum and consisting of a number of tests available in
public literature (DNV, 2012) where supercritical CO2 was released at constant pressure from pipes
with circular holes of different sizes (30-500mm2) and at feeding pressures of 82-158bar. In
particular, a set of 6 tests has been selected among those available which have been performed at
the same initial pressure of ~155bar and at similar initial temperatures. The set is therefore

44
homogeneous in terms of initial conditions, but the tests differ each other in the outflow section (see
Table 36).

PARAMETER RANGE
number 6
pressure 154.4-158.6 bar
temperature 7.8-12.7 °C
outflow hole section 32-507mm2
test duration (release time) 31-184 s
released mass 0.420-3.175 tons
Table 36: Dataset of experimental CO2 release tests. (Data from DNV, 2012)
By analysing the test data it is observed that the experimental value of the mass flow per unit area
is not invariant with respect to the leak size (Figure 43). In other words, though ρv is a parameter
normalized by the area of the outflow hole, it still varies with the leak size. Being the initial
thermodynamic conditions equal, the smaller is the leak size, the higher is the resulting specific mass
flow.
200000
rho v [kg s -1 m-2]

150000

100000

50000

0
0 200 400 600
leak area, [mm2]

Figure 43: Experimental mass flow per unit area.

Such experimental evidence has been compared with the numerical predictions. The ρv values have
been calculated for the set of 6 selected tests by means of the Lees equation.
In this case, no influence of the hole area is accounted as the specific mass flow only depends on the
enthalpy evolution during the decompression. Calculation of the enthalpy variations have been
calculated by using REFPROP, a numerical tool developed by the National Institute of Standards and
Technology (NIST) for calculating the thermodynamic and transport properties of industrial fluids
and their mixtures.

P T leak area rho*v rho*v Error

(exp) (calc)
[bar] [°C] [mm ]
2 -1 -2
[kg s m ]
-1
[kg s m ]
-2 [%]
154.4 12.7 507 80151 89378 -10
155.4 7.8 127 90070 91501 -2
156.7 9.5 32 110517 92066 +20
156.9 9.9 507 80333 92352 -13
158.5 10.4 32 123217 92346 +33
158.6 11.1 127 90857 91985 -1
Table 37: Mass flow per unit area: experimental to numerical comparison.
The theoretical–experimental comparison evidenced that an error is made by using Lees formula,
which is function of the hole size (Eq. 9) as shown in Figure 44 .

𝐸𝑟𝑟% = 𝐸𝑟𝑟% (𝐴) Eq. 9

45
 50

25

rho v error, %
0

-25

-50
0 200 400 600
leak area, [mm2]
Figure 44: Specific mass per unit area: exp-to-theoretical error as function of the leak area.
The considerations made above are based upon the experimental evidences obtained from BP tests
executed at ~150bar while the SARCO2 tests was performed at 130-150bar. However, it can be
reasonably estimated that the percent error made by the Lees equation at 130bar is similar to that
observed at 150bar.
Therefore, referring to the test of interest, the actual mass flow per unit area is estimated by starting
from the Lees formulation corrected by means of the calculated error:
(𝜌 ⋅ 𝑣)𝑒𝑥𝑝 = (𝜌 ⋅ 𝑣)𝐿𝑒𝑒𝑠 ⋅ [1 + 𝐸𝑟𝑟% (𝐴)] Eq. 10

and Eq. 7 becomes:

𝑀𝐶𝑂2 1
𝐴= ⋅ (𝜌⋅𝑣) Eq. 11
𝑡 𝐿𝑒𝑒𝑠 ⋅[1+𝐸𝑟𝑟% (𝐴)]

The resolution of Eq. 11 provides:

𝐴 = 10𝑚𝑚2
The defect has been manufactured as a slit, therefore having a very large longitudinal length if
compared to the circumferential width (Figure 45). However, experimental evidences prove that a
minimum width size of 0.8mm is required to avoid the leak closure as a consequence of the ice
formation during the test.

L
WT w
L

Figure 45: Defect shape. Through wall view (left side) and top view (right side)
So, the final size is:

𝐿 = 12.5𝑚𝑚
𝑤 = 0.8𝑚𝑚
As shown in Figure 46 the application of the Battelle NG-18 leak-rupture criterion to the designed
leak proves that the test lies in the “leak” region at a considerable distance from the “rupture”
boundary. Therefore, even though the material might suffer from embrittlement during the test, the
defect was not envisaged to evolve in a rupture.

46
 Figure 46: Leak-rupture prediction (by Battelle NG-18) Figure 47: Leak test picture.
for the test condition of interest.
A sealing system has been used to close the leak before the achieving the target pressure of CO2
and then removed with the aim to avoid the obstruction of CO2 escape.
In the following pictures the overview of images collected during the test is shown.

Figure 48: Leak test from side Figure 49: Leak test detail of CO2 escape
During the test, gas pressure has been monitored both in the reservoir and in the test pipe following
the transducers layout reported in Figure 50

Figure 50: Pressure transducers layout.

Figure 51: Pressure transducers results.

After an instability period during the first stage of test, the test pressure was constant and very close
to the target pressure for the whole test. This means that the CO2 mixture inside the pipe remained
in dense condition for the test duration. After about 1300 seconds the pig, inside the reservoir,
arrived to the end of accumulator pipe and the test finished with depressurization and phase chance.

47
10 thermocouples have been positioned on external surface of test pipe to monitor the temperature
drop during the test. The TC layout is reported in Figure 52.
TC X Y
1 0 125
2 -300 0
3 -100 0
4 100 0
5 300 0
6 0 -125
7 0 35
8 -45 0
9 45 0
10 0 -35
Figure 52: Temperature transducers layout (mm).
The initial temperature was high due to the fact the pipe was heated from solar radiation, but after
the test onset all the temperatures decreased of about 20°C. After the test finished the pipe surface
temperature decreased again below 0°C.
In fact the expected strong temperatures decrease was not evident during the test but it was more
evident after the test when the CO2 was terminated and the pressure drop down. Moreover there
isn’t a large difference among the TP in the pipe surface, this difference is more evident after the
end of test.
The analysis of the TC results shows that during the phase on which the medium inside remains in
dense phase, the pipe wall temperatures do not change too much due to the fact the temperature
inside doesn’t change. The pipe temperatures start to decrease significantly when line
depressurization starts after the end of test.

Figure 53: Temperature transducers results.

This means that the material cooling during a leak is a local effect very close to the leak as confirmed
by the thermos-camera installed near the pipe.

Figure 54: Thermocamera picture Figure 55: Temperatures monitored with

thermocamera
The temperature evolution monitored by means the thermos-camera is reported in Figure 55.

48
Second leakage test
It was previously discussed that the gas expansion through the leak should lead to a reduction of
the temperature in the material surrounding the leak. If the temperature decrease is sufficient to
lead to a sufficient reduction of the local toughness and if the leak size is large enough an evolution
from leak to rupture might be observed. The second test has been designed as to promote such
behaviour.
To this aim the leak axial length is sized as to meet the leak/rupture boundary curve. Starting from
this “threshold” condition any local embrittlement is expected to produce the enlargement of the
through wall defect along the axial direction.
For this reason, the defect length of the second has been designed longer (the minimum length of a
through wall defect was of L=150mm). Being the slit width of w=0.8mm (as in test#1), it arises that
the cross section of the leak is A=120mm2. However, this size is very large and, it was estimated
that it should lead to a complete release of the CO2 mass in less than one minute.
With the aim to not reduce to much the test duration that is require to achieve the temperature
steady conditions the solution adopted was to reduce the pipe wall thickness maintaining the
representability of pipeline for transporting CO2.
The new pipe wall thickness was reduced to 7mm and the new leak-rupture prediction is reported in
Figure 56. This means that a longitudinal defect with a total length of 40mm is very close to the
border line between leak and break using the toughness dependent model with a Charpy V 2/3 value
of 5J (Charpy V 1:1 value of 7.5J). Moreover, the test pressure was increased to 150bar (maximum
test rig pressure).

Figure 56: Leak-rupture prediction (by Battelle NG-18) for the test#2.
As in the first test a sealing system has been used to close the leak before the achieving the target
pressure of CO2 and then removed with the aim to avoid the obstruction of CO2 escape.
In the following pictures are shown the overview of test images.

Figure 57: Leak test from side test#2. Figure 58: Leak test detail of CO2 escape

During the test, gases pressures have been monitored both in the reservoir and in the test pipe
following the transducers layout reported in Figure 59.

49
 Figure 59: Pressure transducers results (test#2).
Due to the larger defect dimension the test duration was lower respect to the first test (about
3.3min). The CO2 mixture inside the test remained in dense condition for the test duration. After
about 200 seconds the pig, inside the reservoir, arrived to the end of pipe and the test finished with
depressurization and phase chance.
10 thermocouples have been positioned on external surface of test pipe to monitor the temperature
drop during the test. The TC layout is reported in Figure 52.
The initial temperature was about 22°C, but after the test onset all the temperatures decreased of
about 10-20°C. After the test finished the pipe surface temperature decreased again below 0°C.
In fact, as observed in the first test, the expected strong temperatures decrease was not evident
during the test but was more evident after the test. Moreover there isn’t a large difference among
the TP in the pipe surface, this difference is more evident after the end of test.
The analysis of the TC results confirms that during the phase on which the CO2 mixture inside the
pipe remains in dense phase, the pipe wall temperatures do not change too much due to the fact the
CO2 temperature inside doesn’t change. The pipe temperatures start to decrease significantly when
line depressurization starts after the end of test.

Figure 60: Temperature transducers results Figure 61: Liquid CO2 formation after 500s
(test#2) (test#2).
It is evident from thermo-camera picture that after the end of test with the depressurization al low
pressure the formation of liquid CO2 on the bottom of the tested pipe that due to the very low
temperature remains for several minutes (see Figure 61).

Task 2.5 Collect data related to the release of large quantity of CO2 from a leak
Concerning the CO2 dispersion, with the aim to monitor the CO2 concentration in front of leaked pipe,
a set of sensor have been installed as reported in the Figure 39 for both leak tests.
Environmental instrumentation consists of:
 1 CO2 sensor (CO2 to directly measure the CO2 concentration in atmosphere;
 9 Oxygen cells (OC) at 1m height in order to estimate the CO2 levels in atmosphere from the
variations of O2 concentration in air
 7 temperature sensors (TS), to measure the CO2 cloud temperature in correspondence to
each oxygen cell.

50
General weather conditions during the test:
 Atmospheric temperature:18.4°C
 Wind speed: <1m/s
The results of environmental monitoring for the first test are reported in the following. In particular
for the CO2 concentration, as reported in Figure 62, it is very limited to the area close to the pipe. In
fact, the maximum concentration value is at 1 m far from the pipe leak and average value is about
2.5% of CO2 with a maximum value below 3.5%. At 2m far form leak the CO 2 concentration values
decrease at 0.5-1% and become negligible for higher distances.
Also the decrease of temperature in front of leak pipe, as reported in Figure 63, it is very limited to
the area close to the pipe. In fact, the maximum temperature reduction is of about 1°C at 1 m far
from the pipe leak and become negligible for higher distances.

Figure 62: CO2 concentration in front of leak – Figure 63: Environmental temperature in front
Test 1# of leak – Test 1#
The CO2 dispersion in the second test was higher in flow rate (higher defect area) and as a
consequence shorter in time duration.
The results of environmental monitoring are reported in the following. In particular for the CO 2
concentration, reported in Figure 64, it is evident that it is higher than in the first test. In fact the
maximum concentration value is at 1 and 2 m achieve about 9.0% of CO 2 and also the sensors
located at 20m far from the pipe have recorded about 1% of CO2
Also the decrease of temperature in front of leak pipe, as reported in Figure 65, is more evident than
in the first. In fact the maximum temperature reduction is of about 2-3°C at 1-2 m far from the pipe
leak and become negligible for higher distances.

Figure 64: CO2 concentration in front of leak Figure 65: Environmental temperature in
(test#2). front of leak (test#2)

Task 2.6 Development and validation of Leak before Break fracture mechanical model for
CO2 pipeline.
Several models are available in literature but one of the most recognised criterion is the one
developed by Battelle in the’60-’70, known as NG-18 equation [16], which is a failure criterion for

51
pipes containing a through-wall defects subjected to internal pressure loading, developed on the
basis of a large number of full scale tests.
There are two formulations available:
 Toughness dependent: failure criterion for ductile fracture initiation

12
𝐾𝑐2 𝜋 𝐶𝑣 𝐴 𝐸𝜋 𝜋𝑀𝜎𝜃
= = 𝑙𝑛𝑠𝑒𝑐 ( )
̅̅̅2
8𝑐𝜎 ̅̅̅2
8𝑐𝜎 2𝜎̅
 Flow stress dependent: for material characterized by a high toughness level, when failure is
independent by toughness and is mainly due to plastic collapse.

𝜎𝜃 = 𝑀−1 𝜎̅
M is defined as the Folias factor, and several formulations are available in literature:
A two terms asymptotic expression applicable to short defect, most conservative respect to the other
two formulations:

2
2𝑐
𝑀 = √1 + 0.40 ( )
√𝑅𝑡
A two terms revised formulations applicable to longer defects

2
2𝑐
𝑀 = √1 + 0.26 ( )
√𝑅𝑡
A three terms equation which is in the same validity range of the two terms revised but is slightly
more conservative than the above mentioned one.

2 4
2𝑐 2𝑐
𝑀 = √1 + 0.314 ( ) − 0.00084 ( )
√𝑅𝑡 √𝑅𝑡
The model has been validated in several past activities where a large number of full scale tests have
been carried out [16]. This validation has demonstrated a good prediction of the model reported in
Figure 66 in particular for the toughness dependent formulation.

Figure 66: NG18 model validation [16]

This model has been considered for the SARCO2 project as model to predict the evolution of a leak
into a break. In particular, the toughness dependent formulation permits to take into account the
reducing in toughness due to the pipe wall temperature during the test. The results obtained by the
leak full scale activity have shown that this model is valid also for the CO2 medium even if the number
of tests is limited as reported in Figure 67.

52
 Figure 67: NG18 model validation with SARCO2 tests
In particular, the second leak test, designed to verify if a premature break could be happened due
to the cooling effect for the CO2 decompression, has demonstrated that the leak was maintained as
predicted by the NG18 model. Additional tests should be required to improve the statistical reliability
of this statement, but the analysis performed during the test have demonstrated that the pipe wall
temperatures do not decrease a lot if the pressurizing medium conditions are maintained in dense
phase. In this condition the applicability of the proposed model is possible.

Figure 68: NG18 model for different valued of Charpy-V energy

In fact this formulation permits to have different border line between leak and break condition
changing the level of toughness that can be identified from the Charpy-v energy material transition
curve (see Figure 68). The differences between toughness dependent and flow stress dependent
models tend to disappear for toughness values greater than 50J (2/3 sample).

Task 2.7 Analysis of dispersion results and comparison between experiments and modelling
results.
The experimental conditions are reported in Table 38. The physical system was simulated with the
CFD code by means of a 3D domain composed of 1,000,000 cells, with a center plane of symmetry
passing per the slot and schematised in Figure 69.

53
 Symmetry plane

0.8 x
Slot size (mm x mm) centerline
12.5
Slot position (height, m from 20 m
1
ground)
Pressure (bar) 130
Dispersed CO2 total amount (kg) 1200
Temperature at leakage slot(°C) 15
20
Test duration (min)
min 1m

1m
Table 38: Experimental conditions for the first Figure 69: Sketch of the domain simulated
test and subsequently simulated with CFD
code
The description was multiphase, with species transport approach, and pressure outlet at ambient
conditions – air entrapment and ambient temperature were imposed at lateral wall, surface and end
plane opposite to that where leak occurs (see Figure 69).
The CFD simulations were carried out and the results are reported in the following pictures.

1m 2m 10 m 20 m

Figure 70: Numerical modelling: concentration map at Figure 71: Numerical modelling: temperature
centerplane map (°C) at centerplane

Figure 72: Comparison between numerical calculation data and experimental data.
Figure 72 reports the comparison between the numerical simulation performed using Ansys Fluent
CSD code and the range of measured values acquired during the test. The comparison is very good
also considering the fact that in the full scale test the wind was very low, but it could affect slightly
the jet direction with respect to centre line where there was a line of sensors.
As a consequence of the successful validation shown with experimental data, the CFD model can be
reasonably considered reliable for the description of such type of physical scenario and it is
recommended for short and medium range description of leakage phenomena and in general of
dispersion material occurrence especially as refers to environmental impact issues.

54
WP3: Fracture propagation control
The activity foreseen in the WP3 is mainly related to two full scale fracture propagation tests on a
pipe section of 24in outside diameter. The tests have been carried out using dense phase CO2
mixtures.

Task 3.1 Mechanical characterization of steel pipes selected for the fracture propagation
full-scale tests
A specific mechanical characterization, additional to that performed in WP1, was carried out to
evaluate the material capability in arresting ductile running fracture. In particular Crack Tip Opening
Angle (CTOA) test has been carried out.
The two specimens method, as the name implies, consists of testing of two specimens to derive one
CTOA value. The specimens differ in notch depth; one has a machined notch of 10mm and the second
specimen of 38 mm depth. In this case the CTOA values are derived based on the assumption that
there is a linear relationship between the total specific energy absorbed by an impact specimen and
the length of the specimen ligament. The results are given in Table 39 and Table 40.

Pipe no. Pipe type CTOA in degree

125740 UOE 18,35
125728 UOE 12,33
125734 UOE 13,43
LYO 973/1 HFI 25,97
LYO 970/7 HFI 20,09
Table 39: CTOA values for pipes of first test (two specimen method)
Pipe no. Pipe type CTOA in degree
125740 UOE 18,35
7950 17/4 HFI 18.6
7953 17/7 HFI 18.1
7960 18/4 HFI 20.9
LYO 970/7 HFI 20,09
Table 40: CTOA values for pipes of second test (two specimen method)

Task 3.2 Definition of dispersion instrumentation and its layout for the fracture propagation
full-scale tests
This task is aimed at the definition of specific instrumentation to measure CO 2 concentration for the
fracture propagation full-scale tests. A possible layout of the sensors location has been defined, based
also on the results provided by numerical simulations performed by Ansys Fluent, ALOHA and Phast
6.7 modelling tools, for the propagation rupture tests. The CO2 dispersion in the atmosphere has
been evaluated for possible scenarios of WP3 full-scale tests, characterized by:
 200 m long with 24” outer diameter pipeline;
 operating fluid is a mixture of CO2 with 4.0-6.0% of N2;
 initial pressure inside the pipe equal to 130 bar;
 mixture temperature equal to 10-20 °C
The rupture has been generated at the centre of the test line and the fracture can propagate along
the whole test line.
Only one weather condition has been considered, characterized by:
 neutral stability class: D;
 wind velocity of 5 m/s.
The results of the numerical simulations performed by the different codes are reported in Table 41,
in terms of maximum dispersion distances from the source reached by the 1% CO2 cloud during the
rupture propagation tests. This concentration has been assumed as reference value because
represents the upper limit of CO2 in air which allows staying up to 8 hours without consequences for
human health. The distances predicted are different depending on the code used.
Results from Phast 6.7, which present the lowest distances, have been used to place the CO2 sensors.
They must not be placed too close from the pipe not to deteriorate them during the rupture. National
Grid provides 36 sensors for these tests. A layout of sensors positioning is presented in Figure 73.
All sensors are installed at the same height, which is suggested equal to 10 m.

55
 Code Height (m) Width (m) Length (m)
ALOHA - 750 >1000
ANSYS Fluent 50 500 570
Phast 6.7 70 140 200
Table 41: Characteristic distances for the leak before break tests of SARCO2

Figure 73: Lay-out of CO2 sensors positioning for the rupture propagation tests.

A picture of a typical environmental instrumentation station with all the sensors installed a cabled is
reported in Figure 74.

Figure 74: environmental instrumentation station.

Task 3.3 Development of Health, Safety and Environment requirements for the fracture
propagation tests
The two full-scale fracture propagation tests, which has been performed by CSM at the test site
located in Nettuno (military range of Nettuno, UTTAT), caused the dispersion in atmosphere of
relevant quantitative of anthropogenic CO2 (~ 60 ton), released in short time from a high pressure
pipeline subjected to a long running fracture. The research activity included in this task has been
focused at the study of the physics involved in such realistic scenario with the aim to identify safety
area and to produce the safety procedure for the correct execution of test. The activities have been
performed according to the following operating phases:
 identification of the specific aspects, definition of the test parameters and analysis of the
different environmental variables associated to the test execution;
 study of the fluid dynamic phenomena which guide the CO2 release and dispersion in
environment. Several commercial numerical codes have been used in order to predict the
56
 evolution of the contaminant concentration in air, taking into account the influence of
different atmospheric conditions;
 analysis of the consequences deriving from the CO2 release, in terms of both impact on the
environment and abatement of CO2 concentration in atmosphere.
200
Fro Time = 1s Front view
nt v
iew
1200 1000 800 600 400 200
400
Wind
200

Distance [m]
ew
vi 0
p
To nt
i 200
e po
le as 5% CO2 - hmax = 14 m
Re
400
Top view 1% CO2 - hmax = 15 m
Distance [m]
200 200
Time = 20s Front view Time = 60s Front view

1200 1000 800 600 400 200 1200 1000 800 600 400 200
400 400
Wind Wind
200 200
Distance [m]

Distance [m]
0 0

200 200

5% CO2 - hmax = 37 m 400 5% CO2 - hmax = 9 m 400

Top view 1% CO2 - hmax = 49 m Top view 1% CO2 - hmax = 32 m
Distance [m] Distance [m]
200 200
Time = 160s Front view Time = 300s Front view

1200 1000 800 600 400 200 1200 1000 800 600 400 200
400 400
Wind Wind
200 200
Distance [m]

Distance [m]
0 0

200 200

5% CO2 - hmax = 0.8 m 400 5% CO2 - hmax = 0 m 400

Top view 1% CO2 - hmax = 9 m Top view 1% CO2 - hmax = 2.2 m
Distance [m] Distance [m]
Figure 75: Time and space evolution of the CO2 clouds corresponding to the concentrations of 1%
and 5%. Wind velocity 5 m/s- CFD output.
The full scale tests represent a pipeline section at operating conditions typical of the anthropogenic
CO2 transport, on which the fracture is properly initiated. The fluid dynamics analysis has been
focused on the interaction between the CO2 jet and the atmosphere and on the prediction of CO 2
concentration in air, at different time instant and spatial positions. The final goal is to perform a risk
assessment analysis as a support for the test planning and execution. Indications about the hazard
distances from the release point and about the inaccessible time of the test area has been supplied
with reference to the possible CO2 levels that are foreseen in atmosphere. The safety limits included
in the risk assessment analysis, have been determined considering the CO2 thermo-fluid dynamics
and the consequences on human health deriving from exposition to different CO 2 concentration
levels.
This analysis has been focused on the following topics:
 Identification of CO2 health issues due to the fact CO2 is an asphyxiating substance whose
toxicity follows its concentration from safe levels for humans up to potentially deadly values.
 Description of fluid dynamic of the release and dispersion, in particular with a focus both on
the fluid release, which occurs inside a spatial region of few meters close to the source, and
the dispersion phenomenon which is led by the atmospheric conditions (in particular wind
intensity and direction) and could transport the contaminant to long distances (several
kilometres) from the release point.
 Use of numerical codes for the prediction of CO2 concentration in time and space (see Figure
75. In this work, the consequences of the fracture propagation in a CO2 pipeline have been
57
 studied using the CFD commercial code Ansys Fluent and the Gaussian code ALOHA 5.4
(Areal Location of Hazardous Atmospheres) [17], [18], [19].
In more detail, CFD codes represent the state of the art for the numerical resolution of fluid dynamic
phenomena, which allow obtaining complete maps of the fluid dynamic variables (pressure, velocity
and temperature) as well as concentrations levels of dispersed contaminant, in time and space. On
the other hand, the Gaussian codes are based on simplified dispersion models and presents simplicity
usage as well as fast computational time. For these characteristics, Gaussian codes are used for the
evaluation of chemical release, primarily for rapid deployment by responders, as well as for use in
emergency pre-planning.
Several numerical simulations have been performed with both the CFD and Gaussian codes, in order
to analyse the influence of the atmospheric conditions (ABL) on CO2 dispersion in environment.
Among the different ABL considered, in terms of stability class and wind velocity, the one which
shows the longer dispersion distances from the source has been chosen as the most critical for the
risk analysis. For this scenario, the CFD code provided a more conservative prediction respect to the
Gaussian code, resulting in a more extended dispersion area for the same CO2 concentration level.
Focusing on the consequences on human health due to the exposition at different CO2 concentrations,
the analysis has been oriented on a CO2 level in air equal to 5%, which results below the toxicity
level (SLOT) for long exposition periods (beyond 1 hour), as reported by the Health and Safety
Executive United Kingdom and accepted by Det Norske Veritas (DNV).
In more detail, the following considerations have been pointed out about the dispersion at the
different atmospheric conditions simulated:
 CO2 concentration higher than the toxicity level has been predicted within 200 m from the
source. However, a safety CO2 concentration value is expected in about 5 minutes after the
release initiation;
 between 200 and 600 m from the release point, the CO2 concentration in air decreases with
the distance, down to acceptable levels (5%) for long exposure time at around 600 m. The
safety conditions are reached in 5 minutes;
 beyond 600 m the CO2 presence in air is below 5% and it is acceptable for long exposure
period, as reported by DNV-RP-J202;
 at 1200 m from the source the CO2 concentration remains below 1% and no effect on human
health are expected up to 8 hour of exposition;
 the CO2 concentration is expected to decrease below 1% in all the domain within 310 s (less
than 6 minutes);
The undisturbed conditions in the environment are recovered in about 13 minutes after the release
starting. This information has been used for the definition of safety procedure for the test, in
particular to identify the minimum distance for the control room and for the waiting time before the
inspection of test site.

Task 3.4 Full scale propagation tests

The two full scale propagation tests have been carried out by CSM in the Military Shooting Range of
Nettuno, located 60km south of Rome where it was authorized the execution of full scale propagation
test (see Figure 76 and Figure 77).

Figure 76: Nettuno military shooting range Figure 77: SARCO2 test area
location
The test was initially foreseen in Sardinia inside the CSM full scale laboratory located in the
Perdasdefogu military shooting range. At the beginning of 2013 the military activities and also the

58
civil ones were stopped due to investigation on presence of possible the environmental pollutants in
the area for military activities. For this “force majeure” reason CSM worked to identify a different
location for the tests execution. Several sites in Europe were taken into account for the propagation
tests, at the end the only site with all the requirements for a safe execution of the test was the
military shooting range located in Nettuno. Due to the fact the site is not very large the test area
was located near to the sea with the scope to have a safe distance from the border of the military
area (>2km).
This change in test site resulted in a strong addition effort for CSM due to the fact the Nettuno site
was not equipped for this type of tests as Perdasdefogu were CSM operate since many years. In
particular, some of additional activities are here reported:
1. reclamation of ordnances from the assigned area before digging
2. area preparation
3. preparation of fence
4. trench preparation
5. installation of acquisition bunker
6. installation of workman offices
7. new design and construction of line anchor blocks for the line considering a sand soil
8. dismantling, transport and reassembly of pressurizing and acquisition devices from
Perdasdefogu and Nettuno
This was the main reason of CSM request of project extension from 3 to 4 years and the additional
costs in charge to CSM.

Figure 78: New 24in full scale propagation test line construction phases.
In the Table 42 are reported the main test parameters for both tests.

1st FSFP TEST 2nd FSFP TEST

pipe nominal outside diameter 24in 24in
pipe nominal wall thickness 12.7mm Europipe 12.5mm Corinth Pipeworks
13.7mm SMLP 12.7mm Europipe
13.7mm SMLP
test section length 48m 48m
total line length 220m 220m
(test section + reservoirs)
API 5L steel grade X65 X65
ground backfill 1.4m soil: compacted to 1.2m soil: compacted to
reproduce real in-field reproduce real in-field
conditions conditions
pressurizing medium CO2 mixture (3.8% N2 + CO2) CO2 mixture (6.0% N2 + CO2)
target pressure 129.5barg 127.0barg
target saturation pressure 59barg 72barg
test hoop stress 68% SMYS - Europipe 68% SMYS - Corinth Pipeworks
63% SMYS - SMLP 68% SMYS - Europipe
63% SMYS - SMLP
average test temperature +13°C +17.8°C
test initiation explosive shaped charge on the upper generatrix of the
initiation pipe
Table 42: SARCO2 X65 full scale fracture propagation tests main parameters and conditions.

59
First full scale propagation tests
The objective of the full scale fracture propagation test is to evaluate the effectiveness of 24” outer
diameter line pipe made of ISO3183 L450M (API 5L X65) grade steel in arresting a running ductile
fracture.
Test pipes were 24in outer diameter X65 grade steel pipes manufactured by Europipe (12.7mm wall
thickness) and by Salzgitter Mannesmann Line Pipe (SMLP, 13.7mm wall thickness). Test section
was made of 5 pipes (1 initiation pipe and 4 test pipes) for a total length of about 48m; 2 longitudinal
welded SMLP pipes were placed at the South side and 2 longitudinal welded Europipe pipes at North
side.
CO2 based mixture (3.8% N2 plus CO2) was used as pressurizing medium at a pressure of 129.5barg
this resulting in a different hoop stress depending on the local pipe wall thickness, that is:
− 304MPa (0.68 SMYS) for the Europipe pipes and
− 282MPa (0.63 SMYS) for the SMLP pipes.
Given line geographical orientation and the position of the onset explosive charge, the two branches
of the line are identified as North-side and South-side. The two sections mainly differ in the typology
of pipes installed, that is:
 10m long, 24inOD x 12.7mm thick pipes longitudinal welded pipes from Europipe are located
along the North side.
 10m long, 24inOD x 13.7mm thick pipes longitudinal welded pipes from Salzgitter
Mannesmann are located along the South side;
Test conditions
In order to allow the decompression of the gas to occur as in a real pipeline, two reservoirs of 24in
diameter were placed at both ends of the test section. Additional X65 pipes were also installed
between test line end and the reservoirs. These pipes host two crack arrestors to ensure that the
fracture is arrested before achieving the concrete blocks, thus protecting the line setup from severe
damages. Both the South and the North reservoirs are 86m long. See Figure 79

onset
North side South side

TEST ID N2 N1 I S1 S2
PRODUCER Europipe Europipe Europipe SMLP SMLP
PRODUCER ID 125740 125728 125734 LYO 973/1 LYO 970/7
type LSAW LSAW LSAW HFI HFI
GEOMETRICAL PROPERTIES

outer diameter [in] 24 24 24 24 24

nominal wall thickness [mm] 12.7 12.7 12.7 13.7 13.7
actual wall thickness [mm] 13.0 12.9 12.8 13.7 13.8
actual pipe length [mm] 10.5 10.5 6 10.5 10.5

TENSILE TEST (TRANSVERSE) ROUND-BAR SPECIMEN TEST @ ROOM TEMPERATURE

Rt0.5 [MPa] 500 543 549 462 496
Rm [MPa] 596 624 629 580 592
Rt0.5/Rm [%] 84 87 87 80 83

CHARPY V-NOTCH 10X10 CV SPECIMEN @ +20°C

absorbed energy [J] 258 173 135 321 320
DWTT PRESSED NOTCH DWTT energy @ +20°C
total energy [J/cm2] 942 681 622 1381 1390
propagation energy [J/cm2] 647 450 443 977 971

Table 43: 1st SARCO2 X65 full scale fracture propagation test layout.
Pipes along the South side (Europipe) were disposed according to the traditional “telescopic layout”
(see Table 43): pipes with higher toughness were placed at increasing distance from initiation, so
that crack faced pipes of increasing fracture resistance while propagating along the line. Pipe on
South side (SMLP pipes) were disposed according to the “even toughness” configuration.

60
 Figure 79: Scheme of the 1st SARCO2 X65 full scale fracture propagation test line.
The fracture propagation in a CO2 transporting pipeline is heavily influenced by the pressure level at
which the expanding fluid is subjected to a phase change. In particular fracture propagation is
promoted by the saturation pressure. Therefore, the test gas mixture composition, the initial pressure
and temperature were established to assure a saturation pressure of at least 59 bar.
Target operating conditions included a gas mixture containing 96.2 mol% CO 2 and 3.8 mol% N2 at a
pressure of 129.5barg and at a temperature of 13°C. More details about main test parameters and
conditions are resumed in Table 42.
Instrumentation
The measurement of the parameters of interest was carried out by using the following
instrumentation for both tests:
− timing wires (TW) to measure the fracture speed;
− pressure transducers (TP), to measure the test pressure and monitor the pressure decay
during the fracture propagation event;
− thermocouples (TG and T), to measure both the gas and the pipe wall temperature
respectively.
In order to increase the reliability of the measurements, each transducer was monitored and sampled
by two independent Data Acquisition Systems (DAS). The sampling system was developed and set
up by CSM and it is based upon Personal Computer (PC), National Instruments Data Acquisition
Boards and National Instruments Analysis Software (LabVIEW). A sampling rate of 10kHz was used
for all acquisition channels.
The consequences of the line rupture and the subsequent gas dispersion in the environment were
also evaluated. This was achieved by means of dedicated sets of transducers:
− CO2 sensors to directly measure the CO2 concentration in atmosphere;
− Oxygen cells in order to estimate the CO2 levels in atmosphere from the variations of O2
concentration in air;
− a set of temperature sensors, to measure the CO2 cloud temperature.
The atmospheric conditions before and during the test have been measured by means of the following
instrumentation:
− ultrasonic anemometers to measure the wind speed and direction;
− pyranometers for the measurements of the solar irradiance;
− barometric pressure sensors for the atmospheric pressure.
Fracture propagation test preparation and execution
The test was prepared and carried out according to CSM detailed internal full scale fracture
propagation test procedures.
The following steps were carried out:
1. Trench preparation;
2. Test pipes laying and welding;
3. Hydraulic testing;
4. Instrumentation;
5. Soil backfilling and explosive shaped charge placement;
6. Gas pressurization and analysis;
7. Test execution.
First fracture propagation test results
The test line was pressurized with CO2 based mixture (96.2% CO2) up to a pressure of 129.5barg.
The pipe wall temperature at test was of about +13°C, that is recognized to be high enough to ensure
fully ductile fracture propagation on the pipe material.

61
 1.0s 2.0s 4.0s

8.0s 14.0s 30.0s

Figure 80: CO2 dispersion pictures sequence
The fracture was successfully initiated by means of the explosive charge and propagated on the
upper pipe generatrix along both longitudinal directions (referred as North side and South side
according to the geographical position of the line). On site measurements after the test revealed that
fracture deviated from the straight trajectory after 0.8m of propagation along the North side and
after 0.4m along the South side.
Gas decompression behaviour was as expected according to its chemical composition and
thermodynamic condition. Few seconds after initiation, CO2 cloud started to be dispersed in
atmosphere as shown in Figure 80.
The following sections provide a detailed description of the fracture propagation test event including
a deep analysis of the signals acquired by the installed instrumentation.
Crack speed and fracture path
A general overview of the test result is given in Figure 81, where both ends of the fracture
propagation are shown and the deformed shape of the initiation pipe is clearly depicted. The detailed
analysis of the appearance of fracture surface revealed that crack propagated in fully ductile manner
(see Figure 82).

north side

south side

Figure 81: Test result - overview.

62
 Figure 82: Fracture surface appearance along the axial propagation.
By basing upon the pipe appearance after the test execution, the fracture path was inferred as in
Figure 83. The plot shows that after a short axial propagation, fracture was redirected and arrested
within the initiation pipe.
However, it is anticipated that the fracture redirection and arrest are driven by the inherent fracture
resistance properties of the initiation pipe. Those were evidently sufficient to contrast the crack
driving force generated by the gas escaping. In other words, the observed arrest, though very short,
is a “good” arrest and provides reliable indications about the material effectiveness in controlling a
running ductile fracture. This is well in accordance with the fact that the toughness properties of the
initiation pipe (CharpyV abs.en.: 135J) is overabundant with respect to the minimum energy
requirement for assuring a safe arrest, as estimated through the Battelle Two Curve Method (i.e.
85J).

S1 initiation pipe N1
Figure 83: Fracture path.
Gas decompression
The time evolution of the pressure is reported in Figure 84, showing that at burst onset, the test
pressure (average value) was 129.5barg. Both signals exhibit a good agreement with the expected
trend. As the test starts, decompression waves start running along the line from the initiation down
to both ends.
After arriving at the line end caps, the pressure wave is reflected and returns back thus being
detected again by the transducer. This latter passage is detected as a slope change in the pressure
trend.
In order to provide a first indication about the reliability of the sampled data, the pressure versus
decompression velocity curve has been compared to that predicted by using GASMISC. The code,
developed by CSM, is able to calculate the one-dimensional decompression behaviour of gas on the
basis of its initial chemical composition, pressure and temperature.
The experimental-to-numerical comparison has been performed for TP2 that was located along pipe
S2 (South side, at 22.83m from initiation). Results are given in Figure 85, which allows making some
considerations:
 The measured values exhibit a good agreement with GASMISC prediction, thus revealing that
during the decompression phase no unexpected factors regarding the gas affected the regular
pressure vs. decompression speed and further confirming that the CO2 mixture was well
mixed inside the line.
 The signal is reliable since consistent with the typical decompression trend in a gas
transmission line during ductile fracture propagation.
 The decompression code underestimated the initial value of the waves speed (about 30m/s
slower than the experimental velocity, corresponding to 513m/s) and predicted a saturation
pressure which is slightly lower (~2bar) than the observed value (i.e. 61barg).
 The plateau of the decompression curve predicted by GASMISC develops at constant pressure
of 59barg, while the experimental plateau decreases with the wave speed. This behaviour
has been experimentally observed in decompression curves measured in other experimental
tests involving CO2 mixtures.
 The experimental decompression curve interrupts at 51barg (for a velocity of 34m/s). This
pressure level was detected by TP2 after about 750ms (see Figure 84), corresponding to the
time at which the first expansion wave to return at the TP2 position after being reflected by
the reservoir end cap.
63
 wave arrival

42ms 209ms

~750ms

arrival of the
reflected wave

Figure 84: Pressure signals on TP1 and TP2 Figure 85: Decompression velocity curve,
(South side) experimental to numerical comparison

At the burst onset the gas and pipe wall temperatures were:
 Gas temperature on the test line (average): +13.0 °C.
 Pipe wall temperature (average): +16.0°C;

Second full scale propagation tests

The second test has been carried out on same pipe geometry 24in outer diameter and X65 grade
steel pipes manufactured by Corinth Pipeworks (12.5mm wall thickness), Europipe (12.7mm wall
thickness) and by Salzgitter Mannesmann Line Pipe (SMLP, 13.7mm wall thickness).
Test section was made of 5 pipes (1 initiation pipe and 4 test pipes) for a total length of about 48m;
the two external pipes Europipe and SMLP of the first test has been reused for the second test. The
three pipes in the middle of test line were replaced with Corinth Pipeworks pipes.
Main test design parameters are summarized in Table 42.

Test conditions
With the experience gained in the first test a more severe test condition has been decided for the
second test. The aims were:
 to have longer propagation in particular in the mid-section of test line,
 to reach the natural arrest in one of the higher toughness pipes,
 to test the capability of designed crack arrestor to arrest the ductile fracture.
The best test parameter to calibrate the severity of the test is the gas mixture, because small
difference in amount of impurities (N2) permits to change a lot the test conditions. The same
behaviour is not possible changing the test initial pressure and the test temperature fixed by
environmental conditions.
Moreover, the second test layout, in terms of toughness, is more or less “even” toughness (not
telescopic toughness layout) if the Charpy-V energy is considered and lightly telescopic toughness
layout if the DWTT energy is considered. To this information it important to add the differences in
wall thicknesses (12.5, 12.7 and 13.7mm). This means that a simple comparison of the toughness
energy is not enough to establish the tougher pipe but the use of model BTC is required to evaluate
the arrest capability as done in next paragraph related to the Task 3.6.
The test line was pressurized with CO2 based mixture (94.0% CO2) up to a pressure of 127.0bar
with that aim to have a target of saturation pressure of about 72bar that was the requirement to
achieve the above mentioned test aims.
The pipe wall temperature at test was of about +17.8°C, that is recognized to be high enough to
ensure fully ductile fracture propagation on the pipe material.

64
 onset
North side South side

TEST ID N2 N1 I S1 S2
PRODUCER Europipe Corinth Corinth Corinth SMLP
PRODUCER ID 125740 7950 17/4 7953 17/7 7960 18/4 LYO 970/7
type LSAW HFI HFI HFI HFI
GEOMETRICAL PROPERTIES

outer diameter [in] 24 24 24 24 24

nominal wall thickness [mm] 12.7 12.5 12.5 12.5 13.7
actual wall thickness [mm] 13.0 12.5 12.5 12.6 13.8
actual pipe length [m] 10 10 8 10 10

TENSILE TEST (TRANSVERSE) ROUND-BAR SPECIMEN TEST @ ROOM TEMPERATURE

Rt0.5 [MPa] 500 465 468 441 496
Rm [MPa] 596 591 605 578 592
Rt0.5/Rm [%] 84 79 77 76 83

CHARPY V-NOTCH 10X10 CV SPECIMEN @ +20°C

absorbed energy [J] 258 260 296 271 320
DWTT PRESSED NOTCH DWTT energy @ +20°C
total energy [J/cm2] 942 810 702 729 1390
propagation energy [J/cm2] 647 501 415 467 971

Table 44: 2nd SARCO2 X65 full scale fracture propagation test layout.
The line instrumentation layout was the same of the first test with timing wires (TW) to measure the
fracture speed; pressure transducers (TP) to measure the test pressure and monitor the pressure
decay during the fracture propagation event and thermocouples (TG and T) to measure both the gas
and the pipe wall temperature respectively.
Also in this case the test preparation followed the same steps of the first test.
The fracture was successfully initiated by means of the explosive charge and the fracture propagated
on the upper pipe generatrix along both longitudinal directions (referred as North side and South
side according to the geographical position of the line).
The following sections provide a detailed description of the fracture propagation test event including
a deep analysis of the signals acquired by the installed instrumentation.

Figure 86: Second propagation test burst

65
 Figure 87: CO2 dispersion pictures sequence
Crack speed and fracture path
A general overview of the test result is given in Figure 88, where it is clear the ejection of line after
the test end. The detailed analysis of the appearance of fracture surface revealed that crack
propagated in fully ductile manner (see Figure 89).

north side

south side
Figure 88: Test result: overview.

Figure 89: Fracture surface appearance along the axial propagation.

By basing upon the pipe appearance after the test execution, the fracture path was inferred as in
Figure 90. The fracture, initiated straight on top generatrix, run for the whole initiation pipe in both
directions.
The timing wires positioned along the line permitted to evaluate the fracture speed during the test,
the results is reported in Figure 91 on which it is clear a stable crack propagation non both sides up
to the entrance in the pipes 2S.
66
In North side the fracture run in the top generatrix in fully ductile manner in the first pipe after
initiation pipe and also in the second pipe at constant speed (~110m/s) arresting in the composite
CA. The arrest in the CA was clear and quite rapid (10-15cm) without generating severance on the
line demonstrating the good design of the CA.
In South side the fracture run in the top generatrix in fully ductile manner in the first pipe after
initiation pipe at constant speed (~120m/s) and arrested in the second pipe after 4,3m. The arrest
in this pipe was clear and with a classical spiral path before arrest, also in this case without generating
severance on the line.
The ejection of line occurred after the test was concluded, due to the strong driving force and the
pour resistance of trench (sand soil), not affecting the results. The demonstration of the good
execution of the test and of the fact that the test line was ejected after that the fracture stopped on
both sides is due to the analysis of timing wires that was acquired up to the fracture arrest on both
sides. In fact even only a small line movement, before the fracture arrest, would produce an
anticipation of the timing wire rupture that is not present on the crack speed diagram (Figure 91).
On the contrary the crack speed diagram is clean and sensors ruptures are clearly correlated with
the crack speed and positions.

Figure 90: Fracture path.

Figure 91: Crack speed diagram.

The constancy of the crack speed is due to the fact the large plateau in mixture decompression force
the crack tip to maintain a minimum level of speed even if material properties can change a little
from pipe to pipe.
The image of the arrest on the composite crack arrestor is reports Figure 92 a) where is clear that
the running fracture stopped in a short path without producing severance. This result is very
promising due to the fact the use of crack arrestors could be mandatory in all of cases on which the
CO2 transporting conditions are very severe (e.g very high level of impurities). In these cases, the
toughness requirements to achieve a natural arrest can be out of reach and the presence of crack
arrestor is the only solution to arrest the fracture.
In this specific case the design of composite crack arrestor permits to arrest the fracture propagation
in the pipe but also, considering the shape of the crack arrestor that it is made by a composite layer
that increase its thickness from the border to the centre part, it permits a gradual decrease of fracture
speed down to arrest that avoid the ring off of the line.
On the other side of the test line the fracture arrested in natural way by means the toughness of the
material as evident in Figure 92 b). In this case the fracture started to turn in spiral path that is
typical of unstable behaviour.

67
 a) Arrest on composite CA b) Natural arrest
Figure 92: Arrest on composite crack arrestor and natural arrest.
Gas decompression
In order to provide a check about the reliability of the sampled data, the pressure versus
decompression velocity curve has been compared to that predicted by using GASMISC.
The experimental-to-numerical comparison has been performed for TP3 and TP6 that was located
respectively on pipe S1 and N1. Results are given in Figure 93, which allow making some
considerations:
 The measured values exhibit a good agreement with GASMISC prediction, thus revealing that
during the decompression phase no unexpected factors regarding the gas affected the regular
pressure vs. decompression speed and further confirming that the CO2 mixture was well
mixed inside the line.
 The signal is reliable since consistent with the typical decompression trend in a gas
transmission line during ductile fracture propagation.
 The plateau of the decompression curve predicted by GASMISC develops at constant pressure
of ~72barg, while the experimental plateau decreases with the wave speed.

Figure 93: Decompression velocity curves, experimental to numerical comparison

At the burst onset the gas and pipe wall temperatures were:
 Gas temperature on the test line (average): +17.8 °C.
 Pipe wall temperature (average) : +17.3°C;

Task 3.5 - Collection of data related to the release of very large quantity of CO2 from
broken pipeline
After the rupture, the CO2 escaped from the pipeline and was subjected to a rapid (quasi-isenthalpic)
expansion, from chocked to atmospheric pressure, thus leading to a temperature decrease. Phase
changes can take place during the expansion with the possible formation of solid and/or liquid CO 2.
The consequent dispersion is guided mainly by the atmospheric phenomena and takes place along a
prevalent direction determined by the wind blowing, but also it diffuses in all the other directions
because of the atmospheric turbulence contribution.
In Figure 94 and Figure 95 the wind speed and wind direction are reported for the first test, showing
that:
− the wind was blowing at an average speed of about 4.7m/s.
− the average direction is equal to 143° that is from south. This observation which differs from
that expected on the base of the statistical meteorological data, that is from east.
68
Further meteorological data measured during the test are reported in Figure 96 (solar radiation) and
in Figure 97 (atmospheric pressure).

Figure 94: wind speed. Figure 95: wind direction.

Figure 96: solar radiation. Figure 97: atmospheric pressure.

In the second test the atmospheric conditions were:
− the wind was blowing at an average speed of about 5.4m/s.
− the average direction is equal to 260° that is from south.
In order to evaluate the evolution of the CO2 concentration in atmosphere and of the temperature of
the dispersing cloud, a number of transducers have been displaced in the surroundings of the line.
They consist of:
 2 CO2 sensors (CO2) to directly measure the CO2 concentration in atmosphere;
 Oxygen cells (OC) in order to estimate the CO2 levels in atmosphere from the variations of
O2 concentration in air:
o 31 oxygen cells at 1m height;
o 5 oxygen cells at 2m height;
 a set of temperature sensors (TS), to measure the CO2 cloud temperature in correspondence
to each oxygen cell.
The data acquired by the sensors are discussed in the following sections.
The signal of all the sensors (oxygen cells and CO2 sensors) were properly sampled and stored, thus
allowing the CO2 dispersion in environment to be reconstructed. The time evolution of the CO 2
concentration in atmosphere detected by the oxygen cells at the height of 1m above the ground is
shown in Figure 98 for both tests. On the basis of those data, it is observed that:
− the absolute maximum CO2 concentration value was of about 8% in the first test and 25%
in the second test (see Figure 98). The difference is essentially due to the atmospheric
conditions with particular influence of wind direction.
− CO2 concentrations over 1%, which was considered a sort of safety level for humans in case
of long exposure time (up to 8 hr), are only observed within the first 200s after the pipe
rupture on both tests.

69
Figure 98: CO2 concentration measured by oxygen cells at 1m height above the ground for the first
(left) and second (right) propagation tests
Figure 99 and Figure 100 show a comparison among the CO2 concentrations detected by the oxygen
cells and by the IR sensors at the some locations (50m and 100m from the fracture onset section).
The comparison shows that the response of the two sensors is similar and both detect the arrival of
the CO2 cloud in the same time instant. Moreover, the CO2 concentration values measured by the IR
sensors are in good agreement with those that are provided by the oxygen cells.

Figure 99: Comparison between the oxygen Figure 100: Comparison between the oxygen
cells and the IR sensor CO2 measurements cells and the IR sensor CO2 measurements

A set of 31 thermocouples were installed to measure the temperature on the CO 2 dispersing cloud.
All the sensors correctly acquired the temperature values and the signals were properly sampled and
stored.
The time evolution of the CO2 cloud temperature measured by the thermocouples at the height of
1m above the ground is shown in. It is possible to observe that, the minimum temperature reached
after the expansion of the CO2 in environment corresponded to +2°C for the first tests and about
+5°C for the second propagation test.

Figure 101: CO2 temperature measured at 1m height above the ground for the first (left) and
second (right) propagation tests

70
Task 3.6 Validation and final set-up of ductile fracture propagation models for CO2 pipeline

The most recognized model for the identification of minimum toughness requirements Battelle Two
Curve Method (BTC) due to the fact the key point of this model is that the decompression behaviour
of gas is taken into account using the decompression curve of the used gas. This is the reason why
its application can be extended to the CO2 pipeline transport.
As anticipated in the Task 1 of present report, in case of rupture in a CO2 pipeline, the CO2 initially
decompresses rapidly as a liquid. The decompression path then crosses the phase boundary and
enters in the two phases zone on which the decompression is much slower. The discontinuity in the
decompression curve occurs when the decompression path crosses the phase boundary; the pressure
at which the mixture crosses the phase boundary is the saturation pressure Ps.
The saturation pressure of the pipeline (in the transporting condition) is the key parameter for
identify the minimum toughness requirement for the linepipe material. For this reason, it is possible,
using the BTC model, to prepare a prediction chart that reports on the axes both the saturation
pressure and also the minimum toughness requirement.

Figure 102: BTC model chart

With the aim to validate the BTC model two tests have been carried out inside the present project.
Moreover other three tests has been carried out in the same period and these data are available in
public literature [1] [2]. This permits to have a set of five tests to be used for assessing the predictive
capability of the existing design approaches. The tests used for the calibration of model are reported
in Table 45 with relevant information on test data.

Test
1 2 3 4 5
Test name SARCO2 #1 SARCO2 #2 NG #1 NG #2 NG #3
Diameter (in) 24 24 36 36 24
Wall thickness (mm) 12,7-13,7 12,5-13,7 25,4 25,4 19,1
Test pressure (bar) 129,5 127,7 148,3 150,6 150,2
Test Temperature (°C) 13 17 13,1 10,5 15,0
Gas composition CO2: 96.2% CO2: 94.0% CO2: 90.9% CO2: 93.7% CO2: 90.3%
N2: 3.8% N2: 6.0% H2: 1.0% H2: 1.1% H2: 1.1%
N2: 4.0% N2: 3.4% N2: 6.6%
O2: 1.8% O2: 0.0% O2: 0.0%
CH4: 2.2% CH4: 1.8% CH4: 2.0%
Saturation pressure (bar) 61 72 80,6 73,8 73,8
Table 45: CO2 full scale tests results available.
In the following is reported the application of the model for the previous test taking into account the
evaluation of the flow stress parameter, required for the BTC model, using the actual values of tensile
properties.

71
 Figure 103: BTC approach for the 1st SARCO2 test – Europipe Initiation pipe

2N pipe Europipe 1N pipe Corinth Pipeworks I pipe Corinth Pipeworks

1S pipe Corinth Pipeworks 2S pipe SMLP

Figure 104: BTC approach for the 2nd SARCO2 test

72
3W pipe 2W pipe 1W pipe

I pipe 1E pipe 2E pipe

3E pipe 4E pipe
Figure 105: BTC approach for the 1st NG test

3W pipe 2W pipe 1W pipe

73
 I pipe 1E pipe 2E pipe

3E pipe
Figure 106: BTC approach for the 2nd NG test

2W pipe 1W pipe I pipe

1E pipe 2E pipe
Figure 107: BTC approach for the 3rd NG test

The analysis of charts from Figure 103 to Figure 107 shows that the application of BTC “as it is” is
strongly un-conservative for the application to CO2 transmission pipelines. In fact it is evident in

74
Figure 108 that there are propagations also for pipes that exhibit toughness values up two times the
BTC prediction without correction factor.

Plotting the arrest/propagation results for all the tests considered here, it is evident that it is not
possible to obtain a unique correction factor (that is the ratio between the toughness value of the
pipe which actually arrested the fracture in the test and the toughness value predicted for having an
arrest by BTCM); looking at Figure 108 a range can be, however identified, that is between 1.6 and
2.2. This range is bounded by an upper and lower line, the first one is the conservative limit on which
all the obtained propagations are avoided.

Figure 108: Evaluation of correction factor for BTC model in the CO2 mixture transportation

Although the correction factor range is not so wide some tests (see test 4 in Figure 108) exhibited
unexpected results if compared with the others. In any case, due to the small number of tests
available, further investigations and tests are necessary before to considered as reliable the previous
correction factors, in particular because just some testing conditions have been taken into account
and also because these results exhibit a not negligible level of inherent scatter. As basis for
comparison for the natural gas transportation there exist more the 150 full scale propagation tests
available in public literature.
In fact, the Recommended Practice DNV-RP-J202 state that:
“The Battelle TCM is an empirically derived parametric model validated for Natural Gas and
liquids by large scale tests. Even though a number of tests has been performed for liquids
resembling liquid state CO2, at the time of publication of this RP it has not yet been
sufficiently validated with CO2 as test medium for the design of new CO2 pipeline the
execution of a full scale propagation test on the operating conditions.”
The SARCO2 tests and the other ones available permit now to have a more clear framework of the
limits of the application of BTC model to the CO2 transportation, moreover these tests permit to
state that a correction factor it is mandatory to be more confident to reach the arrest. A range of
correction factor has been identified even is the statistical relevance of this data is limited to five
tests.
The obtained results will be useful for the preliminary design of a new CO2 transporting pipeline in
particular for operating conditions close to those used for the validation of model (Table 47). In any
case due to the fact the set of tests used for the identification of the correction factor is limited in
particular in terms of pipe geometry (medium diameters) it remains recommended, as suggested by
the ISO 3183 in its specific annex for requirements to resist to ductile fracture propagation, the
execution a full scale burst test in particular in case of very severe conditions (approach 5, annex G,
ISO 3183).
It is important to note that the mixture composition and the operation condition (mainly operating
temperature and chemical composition) can affect strongly the saturation pressure of the CO2
mixture generating toughness requirements extremely high that are not achievable with present
metallurgical technologies. This means that in case of very high values of toughness requirement the
use of external devices as crack arrestors could be the unique solution to overcome the problem of
running fracture.
The experimental activities carried out in this project confirm that the crack arrestors can arrest the
fracture also in linepipes where the natural arrest (using just the toughness of material) is not
achievable. A carful design can assure both the arrest of fracture and also the integrity of the line

75
after the arrest (no severance). Moreover, as demonstrated in the present project the dimension of
the crack arrestor can be reduced with the aim to reduce the impact on costs.
A further important point is related to the brittle/ductile behaviour during the fracture propagation
in a CO2 transporting pipeline. In fact, in both tests the pipe wall temperature has been monitored
during the test and the results showed that the rapid CO2 decompression is not able to affect the
material temperature in the time on which the fracture propagation occurs. A slow decrease trend of
pipe wall temperature happens in the seconds and minutes after the fracture arrests. This means
that no additional requirements to the tradition Battelle 85% shear area criterion is required to ensure
the ductile behaviour of the fracture propagation in a CO2 pipeline.

Task 3.7 Analysis of dispersion results and comparison between experiments and modelling
results

The data arising from the experimental test were compared with the Computational Fluid Modelling
simulation results achieved. The code is based on a finite-volume approach for structured and
unstructured grids (mesh), by subdividing the geometrical domain into a discrete number of
computational volumes (cells), allows to solve transient or steady state problems, compressible or
incompressible, laminar and turbulent flows and the dispersion model adopted is the species
transport without reaction. Here, the code evaluates the cell local mass (Y) of CO 2 dispersed into
atmospheric air by a particular form of the conservation equation accounting for passive scalar
convection and diffusion:

 (Y) 
   (vY)  S m  J
t
where J is the diffusion flux due to the concentration gradients, Sm represents the source term of the
mass added to the continuous phase from the dispersed second phase; ρ is the total fluid density

and v is the flow velocity.

The analysis involved the CO2 concentration measured with probes allocated as in Figure 109. The
measured values are shown together in Figure 98. The wind conditions under which the experimental
test was performed are shown in Figure 94 and Figure 95 respectively for speed and direction.

Figure 109: Probes allocation.

As a reference, Figure 98 shows the CO2 concentration vs time at the measurement point 8,
corresponding to 50 m from the release, compared with the results of the model in form of snapshots
at different times corresponding to the same location. A more detailed analysis is shown in the Figure
111 and Figure 112, respectively as regard to probe 8 and probe 13, located at 100 m from the CO 2
source. The analysis is made along a shorter period, within 2 min from the release onset. The markers
correspond to points resulting from the CFD calculation under the same conditions.

76
 CO2 concentration at the measurement point 8 (50 m from the release)
3.5

3.0

2.5

CO2 concentration [%]

2.0

1.5

1.0

0.5

0.0
0 200 400 600 800 1000
Time [s]

Figure 110: CO2 concentration vs time (probe8) compared with snapshots of the model results.

Figure 111: CO2 concentration vs time (probe8) compared with model results (markers).

Figure 112: CO2 concentration vs time (probe13) compared with model results (markers).
From previous figures, a reasonable agreement is found between experimental data and model
results. Both the order of magnitude of the concentration values and some features of the trend are
found. For example, a good correspondence is found for the data within the first 20 s. The subsequent
values are in reasonable agreement; nevertheless, the uncertainties in the measurement related to
the wind speed variation can result in a noise on the values measured as long as the emission is
produced. In any case, for the higher emission values, the model can be considered so far reliable,
and this is of outmost importance as far as the risk analysis issues are concerned.

77
WP4: Corrosion and stress corrosion control

Task 4.1 Corrosion and stress corrosion behaviour of steel pipes and welded joints working
in anthropogenic CO2 environment: upgrade of actual state of the art
In this task an upgrade of the actual state of the art has been performed regarding the corrosion and
stress corrosion behaviour of steel pipes working in anthropogenic CO2 environment for the duration
of SARCO2 project.
This literature review and gap analysis, on the likely internal corrosion phenomena relevant to CCS
fluids transportation pipelines, revealed that control of carbon steel CO 2 corrosion in pipelines has a
very significant industrial background in the Oil & Gas industry: mechanisms, modelling, factors
affecting (main of them being: CO2 pressure, temperature, fluid flow regime, water content, water
pH, water chemistries related to its scale tendency, H2S content, carbon steel metallurgy, solids
particles, corrosion inhibitors) and prevention of corrosion are covered extensively.
Main corrosion types/scenarios covered by the Oil & Gas domain’s background are:
 Uniform and/or localised corrosion including pitting or mesa corrosion, as well as erosion
corrosion, preferential corrosion at welds (girth or seam welds), typical of carbon steel in
contact with CO2 containing wet gas and hydrocarbons fluids, including the effect of typical
water soluble impurities such as H2S, O2, organic acids (mainly acetic acid), methanol and
glycol.
 Sulphide stress corrosion cracking and related phenomena associated with the presence of
H2S.
 Stress corrosion cracking related to the simultaneous presence of CO, CO2 and water (this
background coming mainly from the” town gas” industry background).
In contrast, little attention has been paid to corrosion fatigue, most probably because the
phenomenon is not relevant to the operating conditions typical of current (“ordinary”, i.e. except
specific locations subjected to abnormal mechanical loading for any reason) sections of pipelines in
the present Oil and Gas industry domain.
Corrosion management by means of corrosion inhibition has been essentially studied and applied, in
the present Oil and Gas industry domain, for equipment subjected to wall loss corrosion damage, i.e.
uniform and localised corrosion damages (including pitting corrosion, mesa corrosion and flow
induced localised corrosion i.e. erosion-corrosion).
There is relatively little background regarding pipeline CO 2 corrosion control by internal coatings.
This way of corrosion management has not been traditionally in use for internal CO 2 corrosion control
of steel pipelines in the Oil & Gas industry.
In the Oil and Gas domain, most frequently, two main philosophies are adopted for pipelines’ internal
corrosion management and there is a substantial background regarding fundamental knowledge,
corrosion prediction and mitigation practices for their practical implementation. Both rely on the use
of bare steels:
 Wherever possible, the first one consists in operating the pipeline under “dry conditions”,
monitoring the actual water level and over-sizing the pipe design wall thickness (corrosion
allowance) so that some corrosion damage may be allowed to a limited extent, this enabling
to cope with exceptional water upsets.
 The second one consists in operating under wet conditions, either without any inhibitor
treatment (usually where free water corrosivity is low) or with an inhibitor treatment,
together with the use of corrosion monitoring, pipe wall thickness over-sizing (corrosion
allowance) according to the fluid corrosivity, and periodic pipeline inspection, in order to
contain the integrity, throughout pipeline lifetime.
In the CCS context, these two philosophies, and most of the existing corrosion background, should
basically also be applicable. Nevertheless, with regards to the anthropogenic CO 2 transportation, the
range of operating factors covered by this Oil & Gas background is to some extent limited, particularly
as regards two factors, broadly speaking:
 CO2 partial pressure: The high CO2 pressure range involved in the dense or supercritical CO2,
typical of CCS context, which exceeds by far the 0-20 bar range typical of the Oil & Gas
domain, leads to lower water pH, in the range of 3.1 to 3.4, in absence of any other acidic
or alkaline compound, this range being outside the water pH range typically dealt with in the
Oil & Gas domain.
 Nature and concentration of impurities: Depending on the captured CO2 fluid treatment
(before introduction into the pipeline) philosophies adopted in the various CCS projects, some
specific impurities not traditionally encountered in Oil & Gas domain, and particularly the
78
 acidic impurities such as NOx, SOx, HNO3, HCl – which, depending on their concentration
levels in the actual CO2 stream, may lead to water phase pH values lower, or even far lower,
than 3. Furthermore, CO may be present in the CO2 streams.
Generally speaking, the water content level is a primary corrosion factor and these two main
differences raise three kinds of topics, when considering the internal corrosion concern of CO 2
carrying pipelines, under operating conditions relevant to the CCS projects:
 Under “liquid water free” conditions: Whereas, in the Oil & gas domain, corrosivity of the CO2
phase toward steel (and whatever the corrosion scenario) is considered as insignificant when
no free liquid water is present, some experimental evidences showed that in presence of the
highly acidic impurities relevant to CCS projects (depending on the treatment philosophies)
the critical water content level for significant corrosion may be far lower than the water
saturation level. Hence, - as the review revealed that a lack of data, as regards the impact
of impurities on this critical water content level for corrosion, does exist -, this first topic
raises two questions:
o how is the critical water content influenced by the nature and level of the acidic
impurities relevant to the CCS projects
o and how are the corrosion scenarios, mechanisms and rates influenced by the
water level, when this one is in between the critical water content level and the
water saturation level?
 When free liquid water is present: The second topic is related to the impact the water pH,
and more generally the water chemistry, have on the corrosion scenarios, mechanisms and
rates, when dealing with the range of high CO 2 pressure and of impurities composition
relevant to the CCS projects (including the impurities commonly found in the oil & Gas
domain, such as H2S, oxygen).
 Whatever the water level: A third topic has also been raised in the literature, though it seems
less consensual. It is related to the impact the high CO 2 pressure and the specific physical
state of the CO2 (dense liquid or supercritical) might have on the corrosivity of the CO 2 phase,
and the free liquid water phase, and, by extension, on the corrosion scenarios, mechanisms
likely triggered by these specific conditions, as well as on corrosion modelling of these
scenarios.
The very significant industrial background related to the E.O.R. or Acid Gas re-injection projects is
of limited help with respect to these topics, since corrosion threat has been traditionally controlled
in the pipelines related to these domains by adopting operating philosophy requiring very stringent
constraints as regards to the maximum allowed water content of the CO2 mixture operated (very low
“relative humidity” with regard to water saturation), and since the range of impurities usually dealt
with in these projects is more restricted than the one to be considered in CCS projects.

Critical water level for significant corrosion:

Critical water content for significant corrosion is obviously a main topic when considering the “dry
conditions” operating philosophy in the CCS content. The review revealed some significant recent
works addressing this “critical water content level for corrosion” topic. From old and recent
experimental evidences, there is now no doubt that under pure water-CO2 streams (or in presence
of very low levels of additional impurities) the critical water content is very near from the water
saturation level. These results justify, a posteriori, the maximum water level (in the range of 500-
600 ppm-vol. which, depending on the nominal pipeline operating conditions, corresponds to ca. 40-
50 % of the water saturation level) adopted nowadays in the E.O.R. projects.
In contrast, from the limiting amount of experimental results (a few recent works only) addressing
this topics, it is clear that the presence of acidic impurities specific to the CCS projects such as NOx,
SOx and HCl significantly lowers the critical water content. The review revealed that there is a lack
of data regarding the “safe” water level that has to be specified in presence of these specific
impurities, and how the level is affected by each impurity content. In addition, as the literature
review revealed that the oxygen impurity tends to segregate to the CO 2 rich phase, there is a need
to complementary address the “critical water content” topic in presence of acidic impurities together
with oxygen impurity. At last the possible impact, on corrosion rates, of minor contaminations such
as solids particles or specific mineral contamination (such as chlorides), is not reported in the
literature and should deserve some consideration.
The outcomes of the review and gap analysis, with regards to the other topics and their implication
for CCS pipeline internal corrosion management are subsequently summarised, with specific analysis
for each corrosion types / scenarios.

79
Uniform and or Localised corrosion
The review revealed a clear need to better substantiate the impact of NO x, SOx, HNO3, O2, H2S
impurities and their concentration levels on uniform/localised (i.e. pitting, mesa or flow induced
localised) corrosion rate of carbon steel exposed to high pressure (dense or supercritical) CO 2
saturated free liquid water, as well as to high pressure “humid” CO 2 when the water level is higher
than the critical water content, but lower than the water saturation level. The impact of these specific
impurities on the corrosivity of dense or supercritical CO2 mixtures is poorly known.
These data are needed in order to allow a safe identification of the required corrosion allowance
values, whether the CCS pipeline operating philosophy retained is the “dry conditions”, or one or the
“wet conditions” one, with or without inhibitor treatment.
Some works revealed that the uniform or localised corrosion mechanisms (such as pitting corrosion,
mesa corrosion, flow induced localised corrosion), in the range of operating variables typical of the
CCS domain are very similar to the one identified in the context of the Oil & Gas domain, particularly
with regards to the impact of the iron carbonate layer properties on the actual corrosion behaviour
(i.e. localised or uniform pattern) and corrosion rate. Impact of parameters, such as ferrous ions
content in the liquid water, temperature, liquid water pH, water velocity, on the iron carbonate layer
properties, and on the actual corrosion morphology appeared to be similar in both domains.
Nevertheless, corrosion data revealed that the currently existing corrosion predictive models
(prediction of corrosion pattern and of ranges of corrosion rate) developed in the context of the Oil
& Gas industrial domain cannot be directly transferred to the CCS context. It has been found that
models may be over- or under-conservative depending on the range of operating parameters. In
addition, existing models do not account for the influence of impurities such as the acidic ones
relevant to the CCS context (NOx, SOx, HCl) considered.
Hence this context clearly reinforces the need to further develop experimental data and analysis, so
as to back up the needed extension and refinement of the existing models.
Very few experimental works have covered the impact of fluid velocity on the corrosiveness of high
pressure dense liquid or supercritical wet CO2 streams, and this topic would deserve further
experimental work and analysis, if the “wet philosophy” of internal corrosion management is to be
selected.
It is not clear whether or not, the dense liquid or supercritical “wet” CO 2 streams may trigger the so-
called “top of the line corrosion” (or a phenomenon alike) in case of unusual negative heat transfer
from the external environment (cold spots) at the pipe wall surface. No specific experimental data,
or theoretical analysis, have been found in the open literature, regarding the possible corrosion
impact of high water condensation rates at inner pipe wall surface in the CCS pipeline context.
Only very few experimental works have been dedicated to corrosion inhibition of high pressure dense
liquid or supercritical wet CO2 streams. This topic should deserve further consideration in the future
corrosion research activities, if the “wet philosophy” of internal corrosion management is to be
selected.
No particular work dedicated to preferential corrosion at welds (girth or seam welds) has been found
in the public literature consulted and this topic should deserve some limited experimental work, at
least in order to check the relevance of the knowledge on this topic, coming from the Oil and Gas
background.
No particular work dealing with the impact on corrosion phenomena and rates of solids particles
contamination in the free liquid water on the CO2 stream corrosivity, in the context of the operating
condition of the CCS pipelines.
At last the review revealed that, owing to different partitioning coefficients of the different impurities
relevant to the CCS context, between the CO2 liquid phase and the CO2 gas phase, segregation of
impurities in one of the two phases may occur during the pipeline depressurisation events, and this
may significantly impact the corrosivity of the CO2 or of the free water phase during these transient
events. Few experimental data have been found in the literature, regarding this phenomenon and its
impact on corrosivity of the CO2 streams.

Stress corrosion cracking

H2S:
Sulphide related cracking phenomena and mechanisms are relatively well described and there is no
particular argument which could advocate that this background cannot be applied to the CCS context.
In the context of E.O.R. and acid gas reinjection projects, substantial experimental works and
significant field feedback experience give grounds to these assertions. The extensive existing

80
background regarding the phenomena, and the way to practically control them, is embedded in
industrial standards such as the ISO 15156-1,2,3/NACE MR01-75 standard and the related ones.
The ranges of the expected “actual” pH of the aqueous phase associated with CO 2 fluids in the event
of free water break out, as well as of the expected H 2S partial pressure likely to be operated in the
CCS context, are more or less covered by the existing ISO 15156-1,2,3/NACE MR01-75. However,
most of the field experiences and the laboratory tests supporting this knowledge refer to rather low
partial pressure of CO2, typically lower than 30 bar. Moreover, impact of some impurities, “exotic” to
the oil and gas domain, such as the acidic impurities SO x and NOx, has not been experimentally
investigated. In addition, if the CCS pipeline adopted operating philosophy leads to allow relatively
“high” levels of these acidic impurities, the free water pH may range far lower than the typical range
of pH experienced in the Oil & Gas domains, including the E.O.R. and the acid-gas reinjection
projects, and this even more in specific cases of transients free water pH values that might be
associated to pipe depressurisation events. Hence, in any CCS project where significant amounts of
H2S impurity is currently expected in the transported CO2, careful consideration must be paid to the
actual water chemistry and pH, and systematic use of fit for purpose tests accounting for the actual
composition of the CO2 streams should be recommended, at least, considering the present status of
knowledge of the H2S cracking damage scenario under operational conditions relevant to the CCS
pipelines. In the context of the SARCO2 project, a prudent approach is recommended, consisting in
performing at least some “checking” experimental tests, in order to verify the consistency of the
results with regards to the general knowledge framework.
CO:
Requiring the simultaneous presence of CO, CO2 and free water, the stress corrosion cracking
damage, attributed to an inhibitive effect of CO linked with the characteristic of its adsorption to the
steel surface, is a well-recognised phenomenon that occurred in the sixties, particularly in vessel
steels and town gas pipelines. The studies performed at that period showed that, basically, the
phenomenon requires a “balance” between the inhibitive effect of CO and the oxidative power of the
medium. So that the domain of occurrence is depending on factors such as CO2 partial pressure,
temperature, CO partial pressure, presence of impurities, particularly those behaving as oxidant
towards steel.
Considering the literature analysed, it can be assumed that under the typical composition of the CO2
fluids transported, with the high CO2 partial pressure, CO-CO2-water stress corrosion cracking
should be rather unlikely whatever the carbon capture route considered, even in case of the pre-
combustion route where the CO partial pressure in the CO2 stream will be the highest.
Indeed with the high CO2 pressure typical of the transport pipeline in the CCS project, and with the
low CO content expected, even when considering the pre-combustion carbon capture route (<0.4 %
vol. CO), the balance between the corrosive property of CO2 and the inhibitive property of CO should
be in favour of the wall loss corrosive side, rather than on the opposite side, comparing with the
typical conditions relevant to the town gas pipelines or vessel steels that suffered from the cracking
phenomenon.
However, no experimental evidence of this assertion can be found in the public literature relevant to
this report: tests related to the laboratory studies dedicated to the CO-CO2-water SCC have been
performed up to around 16 bar CO2 partial pressure, up to around 42 bar total pressure and down
to water pH values in the range of pH = 4 to 5, with no particular study of the impact of some minor
impurities relevant to the CCS context such as NOx, SOx.
In addition, in case of implementation of corrosion inhibition in CCS pipeline, it may be conceivable
that the balance between dissolution of the steel, promoted by the CO2 content of the transported
fluid, and the inhibition of the corrosion, promoted by the CO component in conjunction with the
added corrosion inhibitive species, might be modified.
Hence inferring, by extrapolation of the knowledge acquired from the existing background on the
CO-CO2-water SCC of carbon steel, that CCS conditions are innocuous towards this phenomenon,
whatever the operating conditions of the pipeline, may be challenged.
Within the SARCO2 consortium, a prudent approach of this topic is suggested, consisting in
performing some limited laboratory experiments aimed at checking that the new and unprecedented
conditions (lower water pH, occurrence of “exotic” impurities such as NOx and SOx) do not alter the
general framework of knowledge and confirmed the (generally assumed) innocuousness of the CCS
CO2 streams with regards to the CO cracking phenomenon.
Corrosion fatigue:
No particular fatigue corrosion data relevant to the CCS context has been found in the public
literature. With consideration to the operation envelope of the CCS pipelines, this supports the
decision of the SARCO2A JIP consortium to experimentally address this topic in the framework of the
full scale corrosion tests programme.
81
Internal anticorrosion coatings:
The review revealed that only some limited experimental laboratory work has been performed on the
resistance of internal anticorrosion coating towards dense liquid or supercritical CO2 fluids relevant
to the CCS pipelines. These works proved that internal coating can be a viable corrosion management
technology. However, data and guidelines are still lacking for the proper selection of coatings systems
and their appropriate application procedures, including the field joint coatings. There is practically
few or no experimental data regarding the impact of actual pipelines conditions on anticorrosion
internal coatings resistance and durability.
This situation triggered the decision of the SARCO 2–A JIP consortium to experimentally shortly
address this “internal coating resistance” topic in the framework of a full scale corrosion tests
programme.

Task 4.2 Corrosion and stress corrosion behaviour of steel pipes and welded joints working
in anthropogenic CO2 environment: development of needed new experimental data
The girth welded joints, object of this work, are three as reported in Table 25 and Table 26. These
joints have been made with different welding technique (GMAW and SMAW).
The following tests were originally planned at the beginning of the project.
Corrosion tests. Autoclave corrosion testing under stagnant conditions and simulated flow in
rotating cage and rotating disc test set-up by using various chemical compositions of
anthropogenic CO2. Compositions have been established in agreement with the specific
needs arisen from WP1 and from the gap highlighted in WP4.1. Transfer and verification of
the usability of corrosion inhibition concepts has been updated from the above state-of-the
art-review.
Stress corrosion tests at constant stress level. SSC four-point-bend tests of the selected
welded joints by using various chemical compositions of anthropogenic CO2 according to EFC
16.
Stress corrosion tests at variable stress level. Slow-strain-rate (SSR) and cyclic SSR tests,
simulating realistic transport environment conditions (anthropogenic CO2 in dense phase and
supercritical conditions) and pressure changes or pipeline vibration in case of subsea re-
injection. The chemical composition of anthropogenic CO2 has been fixed in agreement with
the specific needs arisen from the WP1.
Due to the fact that the state of the art review, about CO2 related corrosion, highlighted that corrosion
issues are more relevant to be examined in depth than corrosion fatigue itself during the course of
the project it was agreed to focus the effort on corrosion, enlarging the corrosion testing program
instead performing small scale corrosion tests under variable amplitude loading. Moreover there
exists an in progress Joint Industrial Project (SARCO2A) addressing fatigue corrosion issue at full
scale level. Such results will be available in a short time frame (within 2017) and, once published,
will contribute in clarifying definitely the importance of fatigue corrosion in CO 2 environment.
For the stress-corrosion testing activity only, which originally envisaged stress-corrosion tests under
constant and variable amplitude loading, some changes have been done for the part at variable
amplitude loading. In particular in this part, it was envisaged slow strain rate (SSR) and cycling slow
strain rate tests. The first tests have been regularly executed the latter ones have been substituted
enlarging the corrosion and stress-corrosion testing program.
Autoclave testing under stagnant conditions
The tests were performed on three different weld joints of carbon steel material. Three welded
materials were investigated:
 GMAW Corinth (GMAW-C)
 SMAW MLP (SMAW)
 GMAW Vallourec (GMAW-V)
Weight Loss Coupons (WLC) was machined from the inner weld and, as reference, from the base
material of each joint. The sketch of the sample is reported in Figure 113.

82
 Figure 113: Weight Loss Coupon – Base Material and Welded (see the red line)

The test conditions for this activity have been defined as reported in Table 46.
Test Pressure Temperature CO2 mixture Water content Inhibitor Exposure
no. (MPa) (C°) (ppm) time (h)
1 10.0 70 Post-Combustion like 600 No 168
2 10.0 70 Post-Combustion like 6000 No 168
3 10.0 70 Oxy-fuel like 6000 No 168
4 10.0 70 Post-Combustion like 6000 Yes 168
Table 46: Test program for autoclave testing under stagnant conditions
Duplicate WLC for both, Welded and Base Material, were utilised for each test.
Post-test examination consisted as follow:
 Weighting of coupons were performed before and after tests in order to determine the mass
loss of the samples.
 Stereo microscope examination (max 40 times magnification) were carried out in order to
evaluate localised corrosion attack.
 3D optical microscope (OM) analysis to evaluate the pits morphology and dimensions (depth
and width).

Test 1
Main results are reported in Table 47
Post Test N° T(°C) Total Pressure (bar) Time (hours)
Combustion 1 70 100 168
Non uniform
H2 O Corrosion Rate Pitting
ID Sample Material corrosion attacks
(ppmv)
mm/y Average Yes/No Dimensions
GMAW_C1 0.002 No Max. Depth =16 µm;
Base Material 600 0.006
GMAW_C2 0.009 No Width = 195 µm
GMAW_C9 Weld 0.001 No Max. Depth =14 µm;
600 0.001
GMAW_C10 material 0.001 No Width = 225 µm
SMAW-1 0.002 No Max. Depth =8 µm;
Base Material 600 0.003
SMAW-2 0.003 No Width = 76 µm
SMAW-9 Weld 0.007 No
600 0.004 -
SMAW-10 material 0.001 No
GMAW_V1 0.001 No
Base Material 600 0.004 -
GMAW_V2 0.007 No
GMAW_V9 Weld 0.004 No
600 0.003 -
GMAW_V10 material 0.001 No
Table 47: Post Combustion conditions – Summary of Results Test N°1
General corrosion was observed on all the specimens. Non uniform general corrosion was observed,
mainly on the base material samples. An example of this corrosion attack is illustrated in Figure 114.

83
 Figure 114: Detail of the surface appearance – GMAW-C
3D OM analyses have been performed in order to evaluate the morphology and size of the corrosion
attacks. A typical example of the output is reported in Figure 115.

Figure 115: 3D Optical Microscope Analysis – GMAW Corinth (Test N°1)

Both base material and welded specimens did not suffer of localised corrosion. The base materials of
GMAW-Corinth and SMAW-MLP suffered of non-uniform general corrosion attack.
Test 2
Main results are reported in Table 48.
Post Test N° T(°C) Total Pressure (bar) Time (hours)
Combustion 2 70 100 168
Non uniform
H2 O Corrosion Rate Pitting
ID Sample Material corrosion attacks
(ppmv)
mm/y Average Yes/No Dimensions
GMAW_C3 <0.001 No
Base Material 6000 <0.001 -
GMAW_C4 <0.001 No
GMAW_C11 Weld <0.001 No
6000 <0.001 -
GMAW_C12 material <0.001 No
SMAW-3 <0.001 No
Base Material 6000 <0.001 -
SMAW-4 <0.001 No
SMAW-11 Weld <0.001 No
6000 <0.001 -
SMAW-12 material <0.001 No
GMAW_V3 <0.001 No
Base Material 6000 <0.001 -
GMAW_V4 <0.001 No
GMAW_V11 Weld <0.001 No
6000 <0.001 -
GMAW_V12 material <0.001 No
Table 48: Post Combustion conditions – Summary of Results Test N°2
A general corrosion attack was mainly present on the specimens’ surface. After Test N°2, the base
material and welded samples did not suffer of localised corrosion. Moreover, after the autoclave
exposure, all the specimens showed an increase of the weight. This increase was mainly due to the
scale formation on the surface.

84
Test 3
Main results are reported in Table 49.
Test N° T(°C) Total Pressure (bar) Time (hours)
Oxyfuel
3 70 100 168
Non uniform
H2 O Corrosion Rate Pitting
ID Sample Material corrosion attacks
(ppmv)
mm/y Average Yes/No Dimensions
GMAW_C7 0.143 Yes Max. Depth =40 µm;
Base Material 6000 0.215
GMAW_C8 0.287 Yes Width = 400 µm
GMAW_C13 Weld 0.297 Yes Max. Depth =64 µm;
6000 0.314
GMAW_C14 material 0.331 Yes Width = 250 µm
SMAW-5 0.222 Yes Max. Depth =26 µm;
Base Material 6000 0.271
SMAW-7 0.321 Yes Width = 250 µm
SMAW-13 Weld 0.345 Yes Max. Depth =68 µm;
6000 0.348
SMAW-14 material 0.351 Yes Width = 160 µm
GMAW_V5 0.320 No
Base Material 6000 0.292 -
GMAW_V6 0.264 No
GMAW_V15 Weld 0.355 Yes Max. Depth =28 µm;
6000 0.293
GMAW_V16 material 0.230 Yes Width = 50 µm
Table 49: Oxyfuel conditions – Summary of Results Test N°3
The presence of a scale on the specimen surfaces was generally observed. On all the specimens, the
localised and general corrosion was observed by stereo microscope, up to 20x magnification (see
Figure 116).

Figure 116: SM Analysis – Test N°3

3D OM analyses have been performed in order to evaluate the morphology and size of the corrosion
attacks. An example of the typical output s reported in Figure 117.

85
 Figure 117: 3D Optical Microscope Analysis – GMAW Corinth Welded Material (Test N°3)
In Test N°3 conditions, all the specimens (base and welded material) suffered of general and localised
corrosion.

Test 4
Main results are reported in Table 50. In this test a corrosion inhibitor (Hexadecyl-trimethyl-
ammonium bromide-HTABr) in concentration of 10 ppm, was used.

Post Test N° T(°C) Total Pressure (bar)

Time (hours) Inhibitor
Combustion 4 70 100 168 Yes9
Non uniform
H2 O Corrosion Rate Pitting
ID Sample Material corrosion attacks
(ppmv)
mm/y Average Yes/No Dimensions
GMAWC_5 < 0.001 No
Base Material 6000 < 0.001 -
GMAWC_6 < 0.001 No
GMAWC_15 Weld < 0.001 No
6000 < 0.001 -
GMAWC_16 material < 0.001 No
SMAW-6 < 0.001 No
Base Material 6000 < 0.001 -
SMAW-8 < 0.001 No
SMAW-15 Weld < 0.001 No
6000 < 0.001 -
SMAW-16 material < 0.001 No
GMAW_VM_7 < 0.001 No
Base Material 6000 < 0.001 -
GMAW_VM_8 < 0.001 No
GMAW_VM_13 Weld < 0.001 No
6000 < 0.001 -
GMAW_VM_14 material < 0.001 No
Table 50: Post Combustion conditions – Summary of Results Test N°4
All the specimens (base and welded material) did not suffer of localised corrosion. After the Test N°4
autoclave exposure, an increase of the weight was observed on all the samples. Also in this case,
the increase was associated to the scale formation on the surfaces.
Table 51 summarises the results of the whole tests performed. The Oxyfuel condition was the worst
and all the specimens (base and welded material) suffered of general and localised corrosion.
The inhibitor (HTABr) did not influence the corrosion rate for the Post Combustion condition.

9
Hexadecyl-trimethyl-ammonium bromide (HTABr) – 10ppm

86
 Corrosion Rates (mm/y)
Water
Test Gas Content Inhibitor GMAW-C SMAW GMAW-V
(ppmv)
Weld BM Weld BM Weld BM
Post Combustion 600 No 0.001 0.006 0.004 0.003 0.003 0.004
Post Combustion 6000 No <0.001 <0.001 <0.001 <0.001 <0.001 <0.001
Oxyfuel 6000 No 0.314 0.215 0.348 0.271 0.293 0.292
Post Combustion 6000 Yes <0.001 <0.001 <0.001 <0.001 <0.001 <0.001
Table 51: Results (BM = Base Material)
Autoclave testing under simulated turbulent flow
All three weld joints typologies have been tested. For each of them 1 base material specimen and 3
weld specimens have been tested.
A sketch of the setup of the testing device is reported in Figure 118.

Liquid
CO2

Figure 118: Set-up for rotating cage test

The test programme is reported in Table 52. Three of the conducted tests were carried out in post-
combustion CO2 with water content either in the range of the postulated critical value (600 ppmv) or
the tenfold value representing a pipeline transport scenario with presence of a free water phase. The
latter condition is also used to investigate the effect of a dedicated inhibitor substance, whereby the
inhibition effect in expected moderate corrosive conditions is addressed. The fourth test studies the
corrosion behaviour of the three girth welded joints in the more corrosive Oxy-fuel CO2-mixture,
again against the background of a transport scenario with presence of a free water phase.
Test no. Temperature Pressure Gas mixture Water content Inhibitor
(°C) (MPa) (ppmv)
1 70 10 post-comp. 600 no
2 70 10 post-comp. 6000 no
3 70 10 oxy-fuel 6000 no
4 70 10 post-comp. 6000 HTABr
Table 52: Test conditions
Testing of inhibitor effect is conducted using Hexadecyltrimethylammonium bromide (Cetrimonium
bromide, HTABr) as a model inhibitor substance. The concentration of the inhibitor is set to 150 ppm
based on the water content.
Specimens taken from the girths weld are tested with the face representing the inner pipe wall in
original condition without further machining of the surface. Thus, these faces not only feature a quite
rough surface texture, but also remainder from the pipe manufacturing and welding processes as
well as some corrosion products formed after welding (Figure 119). Complete removal of these
residua before the corrosion tests without machining is impossible. Hence, determined weight loss
and consequently corrosion rates might over assess general corrosion on the weld specimens, since
part of these residua might be removed during pickling.
All shown specimens have been selected as representative for the corresponding test results.
Generally, specimens from the same weld or all base material specimens tested under identical
conditions show analogue appearance with only minor differences.
Qualitative analyses of layer compositions were conducted in terms of EDX-determination and some
wet-chemical tests. Because of the low accuracy of the EDX-method for light elements and the

87
reciprocal interference of various ions during wet-chemical analyses, a precise determination of layer
composition is not possible.

Figure 119: Inner surfaces of girth welded joints (root pass) in condition upon delivery
(GMAW-C, SMAW and GMAW-V)
General corrosion
The observed corrosion rates are given in Table 53.

Corrosion Rates (mm/y)

Water
Test Gas Content Inhibitor GMAW-C SMAW GMAW-V
(ppmv)
Weld BM Weld BM Weld BM
Post Combustion 600 No 0.08 0.04 0.21 0.04 0.15 0.04
Post Combustion 6000 No 0.28 0.26 0.35 0.24 0.30 0.23
Oxyfuel 6000 No 0.12 0.08 0.43 0.09 0.32 0.08
Post Combustion 6000 Yes 0.31 0.21 0.34 0.18 0.22 0.14
Table 53: Results of rotating cage tests
In case of the base material specimens, testing in the post-combustion CO2-mixture with water
content of 600 ppmv leads to a corrosion rate of 0.04 mm/a independent of the deployed pipe
material. Even though the rate is higher than the one observed on the base material specimens, also
the GMAW-C weld specimens show a corrosion rate below 0.1 mm/a, a value generally accepted to
be tolerable. The corrosion rates observed on specimens from the two other weld types slightly
exceeded this value.
Testing in the post-combustion CO2-mixture with 6,000 ppmv water leads to the expected increase
of the corrosion rates. All specimens have weight losses corresponding to a corrosion rate in the
range of some 0.28 mm/a. Again, weld specimens show slightly higher corrosion rates, with values
increased by similar figures as with the 600 ppmv test, corroborating the theory that the increased
values are caused by additional removal of manufacturing or welding residua.
The corresponding test with 6,000 ppmv in the oxy-fuel CO2-mixture leads to corrosion rates on the
base material specimens just under the critical value of 0.1 mm/a. Hence, corrosion rates are below
the values for the respective test in post-combustion CO2. On the other hand, SMAW and GMAW-V
weld specimens show slightly higher corrosion rates than the ones tested in the post-combustion
CO2-mixture. Again, this effect might be caused by removal of residua, in the present case possibly
assisted by the acidic nature of the test gas, etching the scales from the manufacturing and welding
processes.
Investigation of the inhibitor effect in combination with the test conditions of test no. 2 reveals an
exiguous impact of HTABr. On the base material specimens, corrosion rates are reduced by 20 to 40
%, whereas the effect on the weld specimens is small or even negligible. The somewhat small effect
could be explained by the relatively small inhibitor amount. Possibly, the applied amount of substance
was insufficient for a complete covering of the specimen surfaces. Combined with the only temporary
and locally confined contact between water rich phase and specimen surface, the exiguous effect
might be explained.
Layer formation and localised corrosion
The precise identification of the corrosion product layers on the tested specimens is difficult.
Corrosion products formed under test conditions are not necessarily stable under standard ambient
conditions. Removal of the specimens from the autoclave after test requires a certain time period,
since depressurisation takes time because of the extreme cooling effect of the test gas release. Thus
specimens are exposed to undefined conditions, eventually including access of air, before any
88
investigation on the layer composition can be conducted. In this phase formed corrosion products
can undergo a change of conformation, modification or derivatisation to other compounds.
Post-combustion CO2-mixture with 600 ppmv water
Testing in the post-combustion CO2-mixture with 600 ppmv water leads to formation of an extremely
thin cover with rubiginous corrosion products, discontinued by some grey spots on the surfaces
placed on the outside of the rotating cage (Figure 120). The specimen surfaces placed on the inner
side of the rotating cage show a comparably thin, light grey (base material) to dark grey (weld
specimens) layer of corrosion products after the test. The darker colour of the weld surfaces is most
likely evoked by the aforementioned residua (c.f. Figure 119). Analyses of the layers reveal that iron
carbonate represents the principal component of the layer.

Figure 120: Specimens after ageing in post-combustion CO2 with 600 ppmv water
(from left to right GMAW-C, SMAW and GMAW-V; for each sample: machined weld material outer
face of cage, weld inner face and base material inner face)
Removal of the corrosion products by pickling reveals no localised corrosion on the machined
specimen surfaces (Figure 121). This applies to both base and weld material on the three machined
sides of the specimens. In case of the un-machined specimen side, the surfaces show a pitted
appearance on the original pipe material, whereas the welded joints themselves show no localised
corrosion. Generally, the pitted surface was already present before the corrosion test, but,
nevertheless, depths of the pits might be increased during the test, because of crevice corrosion
conditions between metal and residua on the surface.

Figure 121: Specimens after ageing in post-comb. CO2 with 600 ppmv water in pickled condition
(from left to right GMAW-C, SMAW and GMAW-V; for each sample: machined weld material outer
face of cage, weld inner face and base material inner face)
Post-combustion CO2-mixture with 6,000 ppmv water
After ageing of the specimens in the post-combustion CO2-mixture with 6,000 ppmv water, all
machined specimen surfaces are covered with a porous, almost homogenous rubiginous layer of
some 25 µm thickness. Layers on the machined sections of the weld material, especially on the
GMAV-V weld, show a somewhat more porous structure. In case of the un-machined weld surfaces,
the rubiginous corrosion products only occur localised at spots between the residua (Figure 122).
The corrosion products consist predominantly of iron carbonate and iron hydroxide.

89
 Figure 122: Specimens after ageing in post-combustion CO2 with 6,000 ppmv water
(from left to right GMAW-C, SMAW and GMAW-V; for each sample: machined weld material outer
face of cage, weld inner face and base material inner face)
After pickling, none of the machined specimen surfaces except for the GMAW-V weld shows signs for
localised corrosion (Figure 123). In case of the GMAW-V weld material a number of shallow pits are
observable, none of them with a depth of more than 15 µm. This attack is restricted to the 2nd layer
of the weld, i.e. the hot pass and possibly parts of the first filling pass, while the root pass shows no
signs of localised corrosion. As after testing with 600 ppmv water, the un-machined weld surfaces of
the specimens show a pitted appearance on the pipe material with no pits on the welds themselves.
Again, the GMAW-V weld is an exception to this with few shallow pits on the weld as well.

Figure 123: Spec. after ageing in post-comb. CO2 with 6,000 ppmv water in pickled condition
(from left to right GMAW-C, SMAW and GMAW-V; for each sample: machined weld material outer
face of cage, weld inner face and base material inner face)
Figure 124 shows microsections of the three weld surfaces in original state and after ageing in post-
combustion CO2 with 6,000 ppmv water. The pitted surfaces in the original state become apparent
for all three welded joints. In case of the GMAW-C and SMAW welded joints pits have a depth of up
to 100 μm, whereas the GMAW-V weld shows pits of merely some 10 μm in the un-machined part.
After ageing, similar pit depths are observed for GMAW-C and SMAW, while pit depth slightly
increased on the GMAW-V weld. All surfaces show signs of superficial corrosion attack, possibly
intensified by accumulation of corrosive compounds beneath the residua scales.

Figure 124: Microsections of original states (top) and pickled surfaces aged in post-combustion
CO2 with 6,000 ppmv water (bottom) of welded joints GMAW-C, SMAW and GMAW-V (left to right)
90
Oxy-fuel CO2-mixture with 6,000 ppmv water
The test in the oxy-fuel CO2-mixture with 6,000 ppmv water causes formation of a thin greyish layer
of corrosion products on all surfaces. The porous layer shows weak adhesion and consists mainly of
iron nitrate and sulphite. On the original pipe material, layer formation occurs only locally (Figure
125).

Figure 125: Specimens after ageing in oxy-fuel CO2 with 6,000 ppmv water
(from left to right GMAW-C, SMAW and GMAW-V; for each sample: machined weld material outer
face of cage, weld inner face and base material inner face)
Removal of the corrosion product by pickling reveals no localised corrosion on the machined surfaces,
but first indications of a non-homogeneous attack (Figure 126). The original pipe surfaces show the
described pitted appearance with no localised corrosion on the welded joints. Any possible non-
homogeneous attack on the welds themselves is masked by the irregular surface of the weld.

Figure 126: Specimens after ageing in oxy-fuel CO2 with 6,000 ppmv water in pickled condition
(from left to right GMAW-C, SMAW and GMAW-V; for each sample: machined weld material outer
face of cage, weld inner face and base material inner face)
Post-combustion CO2-mixture with 6,000 ppmv water and inhibitor
Ageing of the specimens in the post-combustion CO2-mixture with 6,000 ppmv water and HTABr
leads to formation of very thin greyish corrosion product layers. Adhesion of the scales consisting
mainly of iron carbonates is poor. In case of the original pipe surfaces layer formation is confined to
areas where the primal scales are spalled.
Pickling reveals no signs of localised corrosion on the base material and the machined GMAW-C- and
SMAW-specimen surfaces (Figure 127). In case of the machined GMAW-V surfaces, part of the weld
material shows a slight heterogeneous attack without formation of pits. As with the benchmark test
without inhibitor use, this attack is restricted to the 2 nd layer of the weld, i.e. the hot pass and
possibly parts of the first filling pass, while the root pass shows no signs of localised corrosion. Again,
the original pipe surfaces show the pitted appearance with no localised corrosion on the welded joints
including the GMAW-V weld. Any possible non-homogeneous attack on the welded joints themselves
is masked by the irregular surface of the weld.

91
 Figure 127: Spec. after ageing in post-comb. CO2 with 6,000 ppmv water and HTABr in pickled
condition
(from left to right GMAW-C, SMAW and GMAW-V; for each sample: machined weld material outer
face of cage, weld inner face and base material inner face)
In conclusion, with respect to general corrosion, no substantial differences are found for the three
tested circumferential welded joints in the rotating cage tests. With a water content of 600 ppmv
corrosion rates remain below or in the vicinity of 0.1 mm/a. Water contents of 6,000 ppmv lead to
corrosion rates above this critical value, independent of the applied CO2-mixture. For all investigated
test conditions corrosion rates are generally independent of the welding procedure. The effect of the
tested inhibitor model substance was exiguous, not leading to significant decrease of the corrosion
rates compared to the benchmark test. At large there is also no significant difference between base
material and weld concerning the corrosion rates. Determination of corrosion rates on specimens
with retained original inner pipe wall is hindered by residua on the test specimens. During pickling
and possibly testing part of these residua might be removed simulating higher corrosion rates. On
the other hand these residua might evoke higher corrosion rates by facilitating formation of crevice
corrosion conditions beneath the original scales.
Localised corrosion was not observed on machined surfaces of the GMAW-C and SMAW welded joints.
Testing in the Oxy-fuel CO2-mixture led to a heterogeneous attack without formation of pits. In the
Post-combustion CO2-mixture, certain localised attack in form of shallow pits was observed in the
range of the hot pass area of the GMAW-V weld. The roots pass, i.e. the surface exposed to CO 2 in
a pipeline, is not affected.
Stress corrosion testing at constant stress
Four Point Bent Beam (FPB) specimens, loaded at 90%-72% AYS, were used to assess the stress
corrosion cracking issue.
The FPB were machined from the inner weld joint in the longitudinal direction (see Figure 128).

Figure 128: Four Point Bent Beam Specimen

The surface was prepared to a consistent repeatable finish with a Ra value of 0.8 μm. The test
specimens were machined carefully at an appropriate rate to avoid overheating and undesired cold
working of the surface, in accordance to EFC16.
The FPB specimens were loaded prior to test at ambient temperature. The values of the strain
corresponding to 90% - 72% of AYS were obtained from the stress/strain curve of the base materials,
performed at 70 °C and 23°C by tensile specimens.
To achieve the correct stress values calibration tests were always performed, using a combination of
tensile test data and four points bent beam specimens instrumented with strain gauge. Examples of
stressed four point bent beam specimen in test jigs are shown in Figure 129: Examples of stressed
Four Point Bent Beam specimen used for calibration.

92
 Figure 129: Examples of stressed Four Point Bent Beam specimen used for calibration.
For the specimens loading, the strain at 90% and 72% AYS was converted into a displacement.
The results obtained are summarised in the Table 54, where the values of AYS, the relevant strains
and displacements are shown.

Girth Displacement to
Temperature AYS% (MPa) Strain με
welded apply (mm)
(°C)
Joints 90 % 72 % AYS 90% AYS 72% AYS 90% AYS 72%
70 °C 409.5 327.6 2620.9 1839.4 1.16 0.82
GMAW-C
23 °C 435.6 348.5 2952.6 2019.0 1.31 0.90
70 °C 510.3 408.2 3252.5 2485.6 1.42 1.11
SMAW
23 °C 471.6 377.3 3158.1 2174.1 1.38 0.98
70 °C 406.8 325.4 1782.7 1385.2 0.83 0.65
GMAW-V
23 °C 421.2 337.0 1993.4 1555.6 0.93 0.73
Table 54: Loading condition in the FPB testing

Table 55 reports the tests conditions.

Temp. Pressure H20 Exposure time

N° Environment Inhibitor AYS%
(°C) (bar) (ppmv) (h)
90
1 Pre-Combustion* 25 100 6000 No 720
72
90
2 Pre-Combustion* 70 100 6000 No 720
72
*for gas mixture composition see Table 56

Table 55: Test conditions – Four Point Bent Beam

Table 56 describes the Pre-Combustion composition:

Pre-Combustion Composition
H2 O
CO O2 NO2 SO2 CH4 N2 Ar H2 S H2 CO2
(ppm)
Vol-% 0.4 - - - 0.08 0.6 0.2 3.4 1.8 Bal. 6000
Table 56: Pre-Combustion Composition

Duplicate FPB specimens were utilised for each test at two stresses, 90% and 72% AYS.
The Environments were refreshed each 360 hours (15 days).
Post-test examination consisted as follow:

Stereo microscope (SM) examination up to 40X magnification to determine the presence of
cracks or localised corrosion.
 Cross section analysis in order to assess crack morphologies by means of Optical Microscopy
(OM). Sections were taken at 1/3 and 2/3 of the sample width.
Table 57 shows the overall results.

93
 Temp. Exposure
Test N° Envir. Material AYS% SCC Note
(°C) time (h)
90 No
GMAW Blistering Pitting attack in the Side A
72 No
Pre- 90 No
1 25 720 SMAW MLP Incipient cracks
Combustion 72 No
90 No
GMAW V&M Incipient cracks
72 No
90 No -
GMAW
72 No -
Pre- 90 No
2 Combustion 70 720 SMAW MLP Incipient cracks
72 No
90 No
GMAW V&M Incipient cracks
72 No
Pressure 100 bar – 6000 ppm H2O
Table 57: Summary of results – Stress Corrosion testing
An example of blistering is reported in Figure 130, while Figure 135 shows example of pitting detected
on the surface under stress. Finally Figure 132 Figure 133 shows examples of incipient cracks
detected.

Figure 130: FPB Spec.(GMAW-C) appearance after autoclave exposure (Test N°1 - 90%AYS)

Side A: Surface under stress; Side B: Surface under compression

Figure 131: OM images of the FPB cross sections (GMAW-C) after the test N°1 (90% AYS).

94
 Figure 132: OM images (Side A) of the FPB cross sections (SMAW) after Test N°1 (72% AYS)

Figure 133: OM images (Side A) of the FPB cross sections (SMAW) after Test N°1 (90% AYS)
Assessment of susceptibility to SCC in Slow Strain Rate tests
Slow Strain rate tests have been conducted according to NACE TM0198-2011 on round bar
specimens. This standard is actually developed for CRAs, but can also be used for a good basic
assessment of the SCC susceptibility of low alloyed or carbon steels. Tests were conducted in a CO 2
gas mixture, representing CO2 captured with the pre-combustion technique. The composition of the
gas mixture is given in Table 56. Impurities in CO2 from this process show the greatest probability
to evoke SCC on carbon steels either by the H2S/H2O- or by the CO2/CO/H2O-mechanism. After
carrying out the test specimens were examined for any ductility loss and indication of SCC according
to TM 0198.
Based on results published in the literature two possible SCC-mechanisms might occur in connection
with pre-combustion CO2 impurities. First, a combination of H2S and H2O might lead to SCC. For
differentiation from other SCC mechanisms, this phenomenon is referred to as sulphide stress
cracking (SSC), when occurring at room temperature and SCC when operating at higher
temperatures. For this mechanism to work, sulphide layers - hence the designation SSC - on the
steel act as a promoter for the uptake of atomic hydrogen. This causes embrittlement and in
combination with tensile stresses failure of the material. The second mechanism is based on the
simultaneous presence of CO, CO2 and H2O and was identified as the course for SCC in carbon steel.
Since both mechanisms require the presence of water, additional 6,000 ppmv water were added to
the CO2 mixture.
Generally, independent of the assumed SCC-triggering mechanism, one could expect stronger effects
of the impurities at higher partial pressures. Even though CCS CO2 pipelines might be operated with
higher pipeline pressures, for the test programme, the pressure had to be limited to 10 MPa, because
of technical limitations of the autoclaves used.
Tests for this study were conducted at 5 and 70 °C, in the range of likely lower and upper limits for
standard pipeline operations. The lower temperature could possibly aggravate the H 2S/H2O-
mechanism, while any occurring CO/CO2/H2O-mechanism could potentially be intensified at the
higher temperature.
Tests have been conducted on samples taken from the selected three different girth welded joints.
Specimens were sampled at mid-wall position in longitudinal direction of each of the two joined pipe
rings pairs, perpendicular to the circumferential weld. The round bar specimens were machined with
a gauge section diameter of 6.55 mm and a shoulder section diameter of 10 mm. Other dimensions
are according to NACE TM0198. The weld region of the samples was placed at the middle of the
specimen gauge section. The gauge sections of the specimens were finally electropolished to a
diameter of 6.35 mm.
95
Tests were carried out using an autoclave made of Alloy 625 with a volume of 750 ml mounted in a
test machine of 5 t capacity, both concordant with the NACE TM0198-2011 requirements. The
specimens were degreased and mounted in the autoclave. Insulation from the autoclave and the
machine was achieved by use of ceramic disks.
For every girth weld a set of three specimens was tested under the two test conditions. One of the
specimens of every set is used as reference for evaluation and tested in pure nitrogen at the given
temperature.
For the specimens tested in CO2, after mounting, the autoclave was rinsed with gaseous CO2 for two
hours. Subsequently, the required amount of de-ionised water was added in deaerated condition
under CO2 counter flow. For testing at 70 °C, following sealing of the autoclave, calculated amounts
of pure H2S and N2 as well as a CO2-based concentrate containing the impurities CO, H2 and Ar are
pressed on from gas cylinders. Finally, liquid CO2 is added. Subsequently, the autoclave was heated
to the target temperature. The added CO2 and impurity quantities were calculated in such a manner
that the target conditions are attained after temperature adjustment. In case of testing at 5 °C, the
autoclave was cooled down before the test gas mixture was added. In this case the target amounts
of substances were added directly.
For testing of the reference specimens, the autoclave was rinsed with nitrogen for 30 min after
sealing and then heated or cooled to the designated temperature.
Subsequently, the specimens were preloaded to 2 kN and the slow strain rate test was started. The
load was increased at a crosshead speed of 2.5*10-5 mm / s corresponding to a strain rate of
1.0*10-6 s-1.
After test completion specimens tested in the CO2 mixture were visually inspected for SCC-indications
under a low-power optical microscope at a magnification of 40X and classified according to TM0198
(Table 58). As mentioned above, NACE TM0198 is actually intended for CRAs, so that the determined
classification should not be overrated. Furthermore, the ductility parameters “specimen elongation”
and “reduction in area” were determined. Resulting values are related to the corresponding values
of the specimens tested in the inert atmosphere, allowing grading of the test atmosphere effect on
the material.

Classification Description

1 Normal ductile behaviour with no indication of SCC

Ductile behaviour with slight loss of ductility. Fissures in necked region. No indication of
2
SSC
3 Substantial loss of ductility. Fissures in necked region. No indication of SCC
4 Evidence of SCC on fracture surface. Secondary cracking
Table 58: Summary of classification according to TM0198

In some cases, specimen fracture occurred on the gauge section but outside the weld area part.
These outlying fractures could not totally be excluded, since the three investigated welded joints
show widths of some 13 (GMAW-C), 16 (GMAW-V) or 20 mm (SMAW) and specimens were machined
with identical dimensions for comparisons sake.
The results of the specimen evaluation according to TM0198 are summarised in Table 59. Pictures of
the specimens are shown in Figure 134, Figure 135 and Figure 136.
Two of the specimen fractures on sample GMAW-C occurred outside the actual weld area. All other
fractures on specimens from this sample occurred on the weld, but on the border area to the base
material (HAZ). In case of the GMAW-V sample also three fractures in the border area (HAZ) were
observed, while on sample SMAW all fractures occurred in the weld metal area.
At a temperature of 5°C specimens of all three samples showed an impact of the pre-combustion
CO2 mixture. In case of the GMAW-C sample necking of the specimens is slightly reduced compared
to the reference specimen tested in the inert atmosphere. A similar, somewhat stronger effect is
observed for the specimen fracture elongation, which is also reduced compared to the reference
specimen. Finally, the specimen with fracture inside the weld area shows an appearance to be
classified into class 2 according to NACE TM0198.

96
Sample Test Temperature Fracture Necking Necking Elongation Fracture Fracture Classification
Atmosphere (°C) location % Ratio % elongation elongation acc.to TM0198
% % ratio %
inert WM,HAZ 84.39 7.5 24.19
CO2 Mix 5 BM 80.33 95.19 7.0 22.58 93.33 1
GMAW-C CO2 Mix WM,HAZ 82.64 97.93 6.8 21.94 90.67 2
inert WM,HAZ 78.5 6.3 20.32
CO2 Mix 70 BM 73.96 94.22 6.3 20.32 100 1
CO2 Mix WM,HAZ 66.72 84.99 5.1 16.45 80.95 2
inert WM 81.92 7.3 23.55
CO2 Mix 5 WM 36.33 44.35 5.1 16.45 69.86 4
SMAW

CO2 Mix WM 37.38 45.63 4.9 15.81 67.12 4

inert WM 83.34 6.8 21.94
CO2 Mix 70 WM 49.38 59.25 4.5 14.52 66.18 4
CO2 Mix WM 35.87 43.04 5.0 16.13 73.53 3
inert WM 85.16 7.3 23.55
CO2 Mix 5 WM 28.58 33.56 4.5 14.52 61.64 4
GMAW-V

CO2 Mix WM,HAZ 47.36 55.61 5.8 18.71 79.45 4

inert WM,HAZ 88.03 6.5 20.97
CO2 Mix 70 WM,HAZ 50.02 56.82 5.3 17.10 81.54 4
CO2 Mix WM 54.82 62.27 5.7 18.39 87.69 4
Table 59: Test results according to TM0198
The specimens of the two other investigated samples show a somewhat stronger impact of the CO 2
mixture. For both welded joints a considerable reduction of necking and elongation on fracture is
observed, whereat the effect is approximately equal on the specimens from both samples.
Furthermore, all specimens not only show fissures in the necked region as with the GMAW-C
specimens, but also some minor SCC indications on the fracture surfaces, leading to a class 4 rating.
For testing at 70 °C similar results were observed with all three samples showing an impact of the
CO2 mixture. The ductility parameters of the of the GMAW-2 specimen are worse than the ones
observed at 5 °C, but the SCC rating is still class 2.

Figure 134: GMAW-C spec. after testing: left 5 °C and right 70 °C. Reference specimen on top.

Figure 135: SMAW spec. after testing: left 5 °C and right 70 °C. Reference specimen on top.

Figure 136: GMAV-V spec. after testing: left 5 °C and right 70 °C. Reference specimen on top.
In case of testing on the other two weld samples at higher temperature, the heat effect is reverse.
The specimens show higher necking and fracture elongation ratios than observed at 5 °C, but
nevertheless the determined values are still lower than the results obtained for the corresponding
97
GMAW-C specimen. Furthermore, at 70 °C one specimen of sample SMAW is only rated class 3 with
no indications of SCC on the fracture surface. However, the three other specimens show signs of SCC
leading to a class 4 categorisation.
The aggravation of ductility loss and, where applicable, certain increase of SCC indications at 5 °C
for the SMAW and the GMAW-V specimens or at 70 °C for the GMAW-C specimens could be an
indication for a preponderance of the H2S/H2O-mechanism on the SMAW and GMAW-V welded joints
and the CO/CO2/H2O-mechanism on the GMAW-C weld. Nevertheless, the above-mentioned
temperature effect is derived from the oil and gas industry with CO 2 being only a minor component
of the fluid. In case of CO2-based gas mixtures, solubility of the crack initiating compounds in a
water-rich or in a CO2-phase might be completely shifted, leading to completely different effects of
the fluid temperature so that only a temperature dependence of the SCC susceptibility of the three
investigated welded joints can be stated.
In conclusion all the three different tested girth welded joints show certain SCC susceptibility in the
pre-combustion CO2 mixture. The ductility parameters in the slow strain rate tests decline compared
to the reference specimens tested in the inert atmosphere and several specimens show SCC
indications on the fracture surfaces at test end.
In case of the GMAW-C weld, the effect is somewhat less pronounced than on the other two welded
joints. Regarding the test temperature, the susceptibility of the GMAW-C weld is slightly higher at
70 °C. The two other welded joints show a reverse temperature dependency of the SSC susceptibility,
with better ductility parameters at 70 °C.

98
WP5: Project Management, Procedure Deliverables and Result Dissemination

Task 5.1 Project Management

Several project meetings have been organized:
 1st meeting hosted by CSM in Rome on June 18th -19th, 2011
 2nd meeting hosted by Europipe in Mülheim on January 30th -31st, 2012
 3rd meeting hosted by CSM in Rome on July, 5th, 2012.
 4th Web-Conference meeting on January 30th, 2013
 5th meeting hosted by CSM in Rome + Web-Conference meeting on September 26th, 2013
 6th Web-Conference meeting on June 5th, 2014
 7th Web-Conference meeting on March 3rd, 2015
Moreover, several web-conferences have been held for specific issues between sub-groups of project
partners with the aim to define the activities and sharing the results of work.
A web-site, “project room”, dedicated to the project has been designed and opened in order to
facilitate the sharing of documents and information among the partners. This web site, accessible
from CSM web page, permits a secure access to the project information. Moreover, it permits to
upload documents and files directly in the shared area.
Each partner has received own user name and password for the access to the project room and a
guide to use it.
CSM has also managed the request of change of project duration due to the cause of force majeure
for the impossibility to continue the full scale activities inside the Sardinian military shooting range.
To complete the test program CSM identified a new site (Nettuno military shooting range)

Task 5.2 Definition of procedures

A fundamental prerequisite for CO2 pipeline transport is the achievement of suitable safety levels, so
the possibility to anticipate/reduce major accident scenarios. In this respect running ductile fracture
control is a crucial issue in CO2 pipelines as well as in gas pipelines generally, but CO2 pipelines (and
in particular those gathering anthropogenic CO2) show significantly different physical behaviour for
the transportation process. Compared to natural gas, the most relevant differences for structural
integrity issues are:
 Higher susceptibility to long-running ductile fracture propagation than natural gas pipeline
operating at comparable material usage factor; as a matter of fact, the CO2 decompression
curve is more severe. As a consequence, the resulting driving force is stronger and the crack
arrest conditions can be reached only using steel pipes with very high toughness, by external
mechanical devices (crack arrestors) and/or using innovative ultra-high “equivalent
toughness” reinforced pipes.
 The likelihood to reach lower temperatures during service operation, as during line venting
(temperature down to -20 °C) or in the case of unlikely event such as a leakage (temperature
down to -80 °C), due to the significant Joule Thomson cooling effect [4]. This results in
lowering pipe material toughness so that steel may exhibit local brittle behaviour and also
important local residual stress can arise which can encourage the leak-to-break transition
and the running fracture propagation onset. The potential risk that a leak may evolve into a
break for CO2 pipeline has to be investigated. This forces the definition of more stringent
requirements in terms of minimum service temperature for both base material and welded
joints in anthropogenic CO2 pipeline, compared to that in natural gas pipeline: -5°C ÷ -10°C
are typical values of onshore natural gas European pipelines grid, while -25°C ÷ -30°C are
the values adopted for the minimum service temperature in the CO2 “Cortez” pipeline made
recently in USA. Such lower design service temperature reflects in more demanding
requirements for welding consumables and in the need for specifically developed Welding
Procedure Specification (WPS) which should guarantee girth welded joints with good
toughness also at such low service temperature.
 Increased pipe wall corrosion and/or stress corrosion susceptibility when free water phase is
present within the CO2 mixture. About this issue, laboratory studies utilising CO2 at high
pressure and corresponding field experiences suggest that corrosion on carbon steel in pure
and dry CO2 is negligible. But it is well known that at low to medium carbon dioxide partial
pressures severe corrosion damage will occur if a water-enriched phase is present. Economic
considerations in the power plant sequestration process require a minimum degree of
humidity. Moreover, stress corrosion cracking and corrosion fatigue issues can arise due to
the presence of gases like H2S, CO, SOx, NOx and probably even hydrogen assisted cracking
due to H2. Even, a possibility exists to have a spec-off period at the capture unit when CO2
purity can be allowed to be outside limits over a limited time span (that needs to be studied
99
 and quantified). The likelihood and severity of these different corrosion mechanisms depend
on several parameters.

SARCO2 project, through the extensive experimental activity performed including full scale burst
tests, allowed to collect a comprehensive set of information related to anthropogenic CO2 large
diameter pipeline critical issues, and to give a contribution to the update of the existing standards
and to the ones under development.
With the aim to highlight the contribution to the present project to the revision of existing CO2
pipeline standard a table has been prepared with the aim to compare the actual standard
requirements of the most recognized and specific for CO2 pipeline transportation code (DNV-RP J202)
and the evidence of the results obtained in the SARCO2 project activity.
Item
relevant to
Recommendations/Requirements
Materials Findings from SARCO2 Project
of DNV-RP-J202 Apr. 2010
and Pipeline
design
Initiation, Accidental release of CO2 from an In SARCO2 project two full scale leak tests have
Leak initial liquid state to ambient been carried out in operation conditions, that
conditions involves decompression means simulating, for the test duration, the
and expansion of the released maintenance of dense phase condition due to the
medium with a corresponding drop in presence of very large quantities of CO2 (long
temperature of the released medium pipeline).
and remaining inventory. CO2 differs The acquisition of temperatures around the defect
from decompression of hydrocarbons has demonstrated that the temperature decrease
with respect to that the release may is not so high as expected from the literature
appear as a combination of gaseous information, in fact if the test is carried out in
and solid state CO2. operating conditions the pipe wall temperature
[…] decreases in negligible way that doesn’t affect the
The temperature reduction through actual toughness of the pipe.
the crack/opening at the leak point A higher decrease of pipe wall temperature
may however not be significantly happens when the pressure inside the line
more pronounced than for volatile decrease down to the saturation pressure due to
hydrocarbons. the fact the mixture inside the line is finishing. In
this phase the temperature is low, and as a
consequence the pipe toughness could be lower,
but also the internal pressure decreased reducing
the risk of change from leak to break.
This effect has been noted in both tests performed
with low and higher flow rate due to the defects
dimensions.
Both tests, and in particular the second one,
performed in borderline condition between leak
and break evolution, have maintained the leak
configuration without moving into a break.

Ductile Fracture control plan
Fracture A fracture control plan should be
established, and should consider
fracture initiation control and fracture
propagation control. The latter should
be considered a second barrier, while
the former should be a first barrier.
Evaluation of fracture propagation
An evaluation route for a rough
assessment of fracture arrest can be
performed with a 3-step procedure:
1. determine fracture arrest pressure
based on pipeline design
2. determine critical pressure based
on CO2 stream composition
3. If pressure in step 1 is higher than
pressure in step 2, fracture arrests.
This approach may be non-
conservative for a CO2 stream
containing a significant fraction of
SARCO2 Project confirmed that the best model for
the identification of minimum toughness
requirements is the Battelle Two Curve Method
(BTC) due to the fact the key point of this model
is that the decompression behaviour of gas is
taken into account using the decompression curve
of the target gas mixture.
The decompression behaviour of CO2 is the key
point for the identification of the minimum
toughness requirements due to the presence of
very large plateau that happens when the mixture
crosses the phase boundary and enters in the two
phases zone on which the decompression is much
slower.
The pressure at which it crosses the phase
boundary is the saturation pressure Ps. The
evaluation of this parameter can be done by
means thermodynamic codes that, even if they
are not able to describe very well the first part of

100
 Item
relevant to
Recommendations/Requirements
Materials
of DNV-RP-J202 Apr. 2010
and Pipeline
design
non-condensable gases, such as H2.
In such cases, a two curve model
approach, like the Battelle TCM,
should be alternatively applied. In
doing this, decompression speed and
fracture propagation speed needs to
be taken into account.
Determination of decompression
speed for CO2 streams can be
performed using transient multiphase
solvers simulating a pipeline rupture.
The simulation set-up needs to be
able to sufficiently account for the
rapid transients occurring during the
rupture scenario.
The fracture propagation speed may
be obtained from several methods,
including empirical correlation to
Charpy-V Notch (CVN) impact or Drop
Weight Tear tests at operating
temperature (accounting for a de-
rating term for measured CVN>95J),
full scale burst testing or FEM
simulations. FEM simulations should
be used with great care, and it is
recommended it is recommended to
carry out mesh sensitivity studies and
to ensure that conservative
assumptions are made both for the
mechanical properties of the pipeline
and the gas pressure.
Fracture arrestor
In case neither fracture initiation
control nor fracture propagation
control is ensured by other means,
fracture arrestors should be installed.
This is considered standard practice in
CO2 pipeline operating in the USA.
The feasibility and type of fracture
arrestors should be documented.
Spacing of fracture arrestors should
be determined based on safety
evaluations and cost of pipeline
repair. However, the safety risk
associated with a running ductile
fracture may not necessarily be
significantly worse compared to a
local guillotine rupture; safety risk
assessment needs to be performed to
assess this.
101
Findings from SARCO2 Project
the decompression curve (dense phase), they are
good enough to identify the saturation pressure.
The analysis of full scale propagation tests carried
out inside the SARCO2 project, plus those tests
available in public literature, shows that the
application of BTC “as it is” is strongly un-
conservative for the application to CO2
transmission pipelines. This means that a
correction factor for the application to the CO2
transporting pipeline is required.
The set of these available tests is not enough to
identify a unique correction factor that is able to
predict correctly all the tests even if a correction
factor in the range between 1.6 and 2.2 is strongly
recommended for the arrest of running ductile
fracture in CO2 pipeline.
Although the correction factor range is not so wide
some tests exhibited unexpected results if
compared with the others. In any case, due to the
small number of tests available, further
investigations and tests are necessary before to
consider as “statistically” reliable the previous
correction factors.
The obtained results will be useful for the
preliminary design of a new CO2 transporting
pipeline in particular for operating conditions close
to those used for the validation of model. In any
case due to the fact the set of tests used for the
identification of the correction factor is limited in
particular in terms of pipe geometry (medium
diameters) it remains recommended, in particular
for application in severe conditions (as suggested
by the ISO 3183 in its specific annex for
requirements to resist to ductile fracture
propagation approach 5, annex G, ISO 3183) the
execution a full scale burst test.
It is important to note that the mixture
composition and the operation condition (mainly
operating temperature and chemical composition)
can affect strongly the saturation pressure of the
CO2 mixture generating toughness requirements
extremely high that are not achievable with
present metallurgical technologies. This means
that in case of very high values of toughness
requirement the use of external devices as crack
arrestors could be the unique solution to
overcome the problem of running fracture.
The experimental activities carried out in this
project confirmed that the crack arrestors are able
to arrest the fracture also in CO2 transporting
linepipes where the natural arrest is not
achievable. A carful design can assure both the
arrest of fracture and also the integrity of the line
after the arrest (no severance). Moreover, as
demonstrated in the present project the
dimension of the crack arrestor can be reduced
with the aim to reduce the impact on costs.
 Item
relevant to
Recommendations/Requirements
Materials
of DNV-RP-J202 Apr. 2010
and Pipeline
design
Dispersion The effect on modelling results of
modelling solid CO2 formation within the release
stream is not validated and results
must therefore be handled with care.
It is expected that the effect is larger
for large leaks and full bore ruptures
than for small releases. When the cold
stream of CO2 hits the ground, a
small release will be heated by the
surface, however, if the leak is large
and/or long lasting, less of the gas will
be heated by the surface and the
effect of solid CO2 is expected to be
larger.
Internal Corrosion rates
Corrosion For a carbon steel pipeline, internal
corrosion is a significant risk to the
pipeline integrity in case of
insufficient dewatering of the CO2
composition. No reliable models
available for prediction of corrosion
rates with sufficient precision.
Presence of other chemical
components such as H2S, NOx or SOx
will also form acids which in
combination with free water will have
a significant effect on the corrosion
rate
Corrosion control
As primary strategy for corrosion
control, dewatering of the CO2 at the
inlet of the pipeline should be
sufficient.
Corrosion protection
For mechanical protection, shorter
pipeline sections internal
polyethylene (PE) liners may be used
102
Findings from SARCO2 Project
All the tests analysed have shown stable
propagation at quite low speed. If this issue is not
usual for the natural gas pipelines, it is more
evident for CO2 pipelines due to the presence of
large plateau that is able to “push” steadily the
crack tip also a very low speed.
A further important point is related to the
brittle/ductile behaviour during the fracture
propagation in a CO2 transporting pipeline. In fact,
in both tests the pipe wall temperature has been
monitored during the test and the results showed
that the rapid CO2 decompression is not able to
affect the material temperature in the time on
which the fracture propagation occurs. A slow
decrease trend of pipe wall temperature happens
in the seconds and minutes after the fracture
arrests. This means that no additional
requirements to the tradition Battelle 85% shear
area criterion is required to ensure the ductile
behaviour of the fracture propagation in a CO2
pipeline.
The dispersion measurements carried out during
the full scale tests have demonstrated that CO2
after the dispersion tends to expand on ground
even if with low-medium concentrations.
The modelling of CO2 dispersion by means CFD
codes is very accurate even if requires long
calculation time. The evaluation with Gaussian
and integral codes are less precise but the results
can be compared and in case used with
conservative factors.
Corrosion rates
The results of the activities performed for the girth
weld material in the SARCO2 project have
demonstrated that the corrosion rates were
influenced by the concentration of the impurities
(H2S, H2O, NOx , or SOx ).
In stagnant condition, the Oxyfuel environment
was the worst and all the specimens (base and
welded material) suffered of general and localised
corrosion.
In rotating cage setup, the Post-combustion CO2-
mixture (6000 ppmv H2O), certain localised attack
in form of shallow pits was observed in the range
of the hot pass area of the GMAW-V weld. The
roots pass, i.e. the surface exposed to CO2 in a
pipeline, is not affected.
The rotating cage setup results more severe that
in stagnant condition and probably more
representative of the actual pipeline condition. In
any case rotating cage setup is to prefer even if to
 Item
relevant to
Recommendations/Requirements
Materials
of DNV-RP-J202 Apr. 2010
and Pipeline
design
for corrosion protection. The annulus
between the PE liner and the outer C-
steel pipe must be vented to avoid
collapse of the PE liner in a pressure
reduction situation.
For chemical protection, no evidence
support that CO2 corrosion rates in
case of free water can be controlled
using pH stabilization, hence this
approach should not be applied
without extensive qualification.
Corrosion allowance
The system should be operated such
that internal corrosion is avoided
through operational control, i.e.
dewatering of CO2.
Findings from SARCO2 Project
avoid the stratification of impurities and water
contents.
Corrosion protection
For chemical protection, the Hexadecyl-trimethyl-
ammonium bromide (HTABr) inhibitor was used,
but its effect was exiguous, in fact not leading to
significant decrease of the corrosion rates
compared to the benchmark test.
Stress Corrosion
Concerning the stress corrosion tests although on
all the specimens, no evidence of cracks was
observed by Stereo Microscope, incipient cracks
were observed on the cross sections of GMAW
V&M and SMAW on some samples.
At 25°C the GMAW samples show a blistering and
pitting attack on the surface.
The results obtained in the project are very
promising even if not enough to complete the
frame of the stress corrosion issues in the CO2
pipeline also due to the very small quantity of data
in public literature.

Task 5.3 Dissemination and discussion of results

Dissemination of the SARCO2 project results has been regularly carried out during the whole project
execution, thanks to the large participation of European Companies to the project. Just to remember
EPRG was involved since the beginning and the majority of EPRG members (namely Eni, Shell,
Corinth, SZMF, SMLP, Europipe, etc.) actively participated to meetings where SARCO2 results were
presented and discussed. Also DNV was deeply involved before and after major testing activities and
in the results discussion as well.
In addition to that a specific workshop on fracture propagation and CO2 main topics has been
organized in May, 2015, in coincidence with the EPRG-PRCI-APGA Joint Technical Meeting on Pipeline
Research held in Paris. In that occasion SARCO2 results were presented, discussed and compared
with R&D results on similar topics coming from other world institutes. Participants were in fact not
only from Europe but also from USA (PRCI10 members) and Australia (APGA11 and Energy Pipelines
CRC12 members) in addition to worldwide recognised experts (e.g. Andrew Cosham from Atkins)
representing both operator, pipe maker and standardization body points of view.
Main items touched during the workshop were:
 Linepipe production - Verify the capability of current linepipe production originally designed
for gas transmission to safely transport supercritical CO2; SARCO2 results confirmed this in
line with the general consensus on the matter. No specific linepipe material design is needed
but just additional material requirements for taking into account supercritical CO2 specific
features.

 Decompression - How to correctly model the CO2 decompression behaviour during leak and
break events; SARCO2 experience and results were compared with findings from other
European and non-European projects (USA, Australia). Gas decompression models used in
SARCO2 proved to be able to correctly predict the decompression behaviour.

 Fracture control - How to correctly predict minimum fracture toughness for having an arrest.
SARCO2 test results provided fundamental data for deriving fracture arrest guideline,
including crack arrestor design.

10 Pipeline Research Council International, http://prci.org/index.php/about/

11 Australian Pipelines and Gas Association Ltd, www.apga.org.au/about/
12 Energy Pipelines CRC, http://epcrc.com.au/about
103
  Dispersion – SARCO2 modelling based on CFD tool proved to be able to correctly predict the
CO2 dispersion around the pipeline after a leak/break.

 Coating - Main topic under discussion was if currently used internal coating for gas
transmission pipeline could be safely used for supercritical CO2 transmission, and this was
generally confirmed by both SARCO2 project and other projects results.

Within the EPRG-PRCI-APGA Joint Technical Meeting on Pipeline Research held in Paris, a dedicate
paper on results of the first full scale propagation test have been presented the references of paper
are reported in [20].
The complete list of papers produced during the project is reported:
1. C. Spinelli, G. Demofonti M. Di Biagio, “Requirements for safe and reliable CO2 transportation
pipeline CO2 Forum - 3rd Int. Forum on Transportation of CO2 by pipeline, Newcastle, UK
2012
2. M. Di Biagio, G. Demofonti, A. Lucci and C. Spinelli, “Research Fund for Coal & Steel SARCO2
Project, Full Scale Fracture Propagation Testing on Dense Phase CO2 Pipeline,” in EPRG-
PRCI-APGA Joint Technical Meeting on Pipeline Research, Paris, France, 2015.
3. M. Di Biagio, A. Lucci, E.Mecozzi, C.M.Spinelli, “Fracture Propagation Prevention on CO2
pipelines: Full Scale Experimental Testing and Verification Approach,” in EPRG-PRCI-APGA
Joint Technical Meeting on Pipeline Research , Colorado Springs, USA, May 2017.
4. M. Di Biagio, A. Lucci, E.Mecozzi, C.M.Spinelli, “Fracture Propagation Prevention on CO2
pipelines: Full Scale Experimental Testing and Verification Approach,” in PTC Pipeline
Technology Conference, Berlin, Germany, May 2017.
5. M. Di Biagio, A. Lucci, E. Mecozzi, C.M.Spinelli, “Fracture Propagation Prevention on CO2
pipelines: Full Scale Experimental Testing and Verification Approach,” in 3R International -
Technical journal for piping system integrity and efficiency. Special issue 1/2017, pages 27-
37, ISSN 2191-9798.

104
Conclusions
SARCO2 project has produced a large set of information concerning different topics related to the
safe CO2 transportation. A critical analysis of existing know-how is now available including specific
focuses in-depth examinations on:
 evaluation of potential impurities for each capture technology;
 selection and evaluation of the physical models and computer codes to calculate the
thermodynamic properties of CO2 mixtures
 description of available models for the assessment of fracture initiation and propagation events.
 analysis of existing models for the prediction of leak vs. break evolution of a pipeline defect.
 state of Recommendations and Standardization for CO2 transportation via pipeline.
 database of existing pipeline/project for CO2 transportation around the world.

The two full scale leak tests have been correctly executed and in both cases the defect didn’t evolved
in break. The acquisition of temperatures around the defect has demonstrated that the temperature
decrease is not so high as expected from the literature information, in fact if the test is carried out
in operating conditions the pipe wall temperature decreases in negligible way that doesn’t affect the
actual toughness of the pipe. A higher decrease of pipe wall temperature happens when the pressure
inside the line decrease down to the saturation pressure due to the fact the mixture inside the line
is finishing. In this phase the temperature is low, and as a consequence the pipe toughness could be
lower, but also the internal pressure decreased reducing the risk of change from leak to break. This
effect has been noted in both tests performed with low and higher flow rate due to the defects
dimensions.
NG18 model, used to describe the evolution of a defect from leak to break, has been used for the
prediction of the leak test behaviour. Even if the number of tests were low the model results able to
describe also the evolution of defect in presence of CO2 decompression.
The releasing data have been compared with Ansys Fluent CFD code simulations. The comparison
results are very good demonstrating that the developed model is able to correctly describe all the
decompression phases of CO2.
Two full scale propagation tests have been successfully carried out. The results of the two tests have
been used for the validation of the most recognized model for the identification of minimum
toughness requirements (Battelle Two Curve Method - BTC). The analysis of these tests shows that
the application of BTC “as it is” is strongly un-conservative for the application to CO2 transmission
pipelines and a correction factor is required. The results of the two SARCO2 tests was compared with
other three tests carried out in the same period and all these tests have been used for the evaluation
of a correction factor. This analysis shows that it is not possible to obtain a unique correction factor
(that is the ratio between the toughness value of the pipe which actually arrested the fracture in the
test and the toughness value predicted for having an arrest by BTCM); however, a correction factor
in the range between 1.6 and 2.2 has been identified.
Although the correction factor range is not so wide some tests exhibited unexpected results if
compared with the others. In any case, due to the small number of tests available, further
investigations and tests are necessary before to considered as reliable the previous correction factors,
in particular because just some testing conditions have been taken into account and also because
these results exhibit a not negligible level of inherent scatter.
The SARCO2 tests and the other ones available permit now to have a more clear framework of the
limits of the application of BTC model to the CO2 transportation, moreover these tests permit to
state that a correction factor it is mandatory to be more confident to reach the arrest.
The obtained results will be useful for the preliminary design of a new CO2 transporting pipeline in
particular for operating conditions close to those used for the validation of model. In any case due
to the fact the set of tests used for the identification of the correction factor is limited in particular in
terms of pipe geometry (medium diameters) it remains recommended, as suggested by the ISO
3183 in its specific annex for requirements to resist to ductile fracture propagation, the execution a
full scale burst test in particular in case of very severe conditions (approach 5, annex G, ISO 3183).
It is important to note that the mixture composition and the operating conditions (mainly operating
temperature and chemical composition) can affect strongly the arrest/propagation prediction. This
means that the presence of not negligible amount of impurities in the CO2 mixture can increase the
value of saturation pressure generating toughness requirements extremely high that are not
achievable with present metallurgical technologies (300-350J). On this particular conditions the use
of external devices as crack arrestors could be the unique solution to overcome the problem of
running fracture.
The experimental activities carried out in this project confirm that the crack arrestors can arrest the
fracture also in CO2 linepipes where the natural arrest (using just the toughness of material) is not
achievable. A carful design can assure both the arrest of fracture and also the integrity of the line
105
after the arrest (no severance). Moreover, as demonstrated in the present project the dimension of
the crack arrestor can be reduced with the aim to reduce the impact on costs.
A further important point is related to the brittle/ductile behaviour during the fracture propagation
in a CO2 transporting pipeline. In fact, in both tests the pipe wall temperature has been monitored
during the test and the results showed that the rapid CO2 decompression is not able to affect the
material temperature in the time on which the fracture propagation occurs. A slow decrease trend of
pipe wall temperature happens in the seconds and minutes after the fracture arrests. This means
that no additional requirements to the tradition Battelle 85% shear area criterion is required to ensure
the ductile behaviour of the fracture propagation in a CO2 pipeline.
Concerning the corrosion issue an exhaustive review of all corrosion topics have been carried out
and a specific experimental activity have been carried out on girth welded joints where there exists
a lack of information. The results of the corrosion activities performed for the girth weld material in
the SARCO2 project have demonstrated that the corrosion rates were influenced by the concentration
of the impurities (H2S, H2O, NOx or SOx). The rotating cage setup results more severe that in
stagnant condition and probably more representative of the actual pipeline condition. In any case
rotating cage setup is to prefer even if to avoid the stratification of impurities and water contents.
Concerning the stress corrosion tests although on all the specimens, no evidence of cracks was
observed by Stereo Microscope, incipient cracks were observed on the cross sections of GMAW-V and
SMAW on some samples. The results obtained in the project are very promising even if not enough
to complete the frame of the stress corrosion issues in the CO2 pipeline also due to the very small
quantity of data in public literature.
The outcomes of the SARCO2 project have been collected in indications and comments to supply
support for future releases of actual standard requirements concerning the CO2 transportation.

106
Exploitation and impact of the research results
The Carbon Capture Transportation and Sequestration (CCTS) approach is mandatory to reduce fossil
fuel power plant emissions down to acceptable levels and technical solutions have to be found very
timely. Pipelines can efficiently transport supercritical CO 2 and most of the know-how already
available from natural gas transportation system could be used. This approach has already been
adopted is the remote areas (USA, Canada, Algeria, Norway) mainly for pure CO2 in EHR (Enhanced
Hydrocarbons Recovery) applications.
The project activity supplied several information to contribute to cover the gaps existing between
the traditional design approach for the natural gas pipelines and the design of CO 2 pipelines. In
particular, for example, with the results of full scale tests those are required to validate the most
recognized models available for the pipeline design.
As an example the two full scale propagation tests performed in the SARCO2 project strong
contribution to the small set of tests (5) available in public literature. We are far from the number of
test available for natural gas pipelines (>150) but they are enough to supply first strong indications
for a more reliable design.
Additionally, the two full scale leak tests carried out at constant pressure (representative of a real
long line) have been useful for the understanding of the actual behaviour of CO2 decompression from
a leak and its influence on the pipe wall temperature changes in the defect area.
At the end it is possible to affirm that this project has brought a very innovative know-how and
experimental data about the specific issues of the safe transportation of anthropogenic CO2 by
pipeline.
The interest on SARCO2 project results has been confirmed to the participation of European
Companies to the project. Just to remember EPRG was involved since the beginning and the majority
of EPRG members (namely Eni, Shell, Corinth, SZMF, SMLP, Europipe, etc.) actively participated to
meetings where SARCO2 results were presented and discussed. Also DNV was deeply involved before
and after major testing activities and in the results discussion as well with the aim to use the project
results in the new release of standard when they will be published.

107
List of Figures
Figure 1: Composite Crack Arrestor for the test line. ................................................................ 5
Figure 2: Leak test from side test#2. ..................................................................................... 6
Figure 3: Temperature transducers results ............................................................................. 6
Figure 4: Comparison between numerical calculation data and experimental data. ...................... 7
Figure 5: First propagation test execution. ............................................................................. 8
Figure 6: Second propagation test, line after the test. .............................................................. 9
Figure 7: Evaluation of correction factor for BTC model in the CO2 mixture transportation............ 9
Figure 8: leak-rupture development...................................................................................... 17
Figure 9: Fracture control scheme ........................................................................................ 18
Figure 10: Decompression curves for Pure Methane, Natural Rich Gas and Pure CO2 .................. 19
Figure 11: Interaction between gas decompression and fracture velocity curves. ........................ 21
Figure 12: CO2 decompression curve .................................................................................... 21
Figure 13: Saturation pressure Ps and arrest pressure Pa ........................................................ 21
Figure 14: Isentropic decompression path [12] ...................................................................... 22
Figure 15: Pipes for full scale activity. ................................................................................... 27
Figure 16: Composite Crack Arrestor. ................................................................................... 27
Figure 17: Minimum requested composite reinforcement thickness to assure a fracture arrest ..... 27
Figure 18: Winding patterns with 70 % O (circumferential) and 30 % B (±20 ° inclined) ............. 27
Figure 19: WPS for GMAW girth welding of X65M 323.9 mm pipe ............................................. 32
Figure 20: Orbital welding system. ....................................................................................... 33
Figure 21: Sketch of the sampling points, girth weld QK.......................................................... 33
Figure 22: Macrograph of girth weld QK, X65, 3 o´clock position .............................................. 33
Figure 23: Hardness ranges of the root and cap area as a function of the position. ..................... 33
Figure 24: Orbital welding system ........................................................................................ 34
Figure 25: GMAW girth welding of X65M 24’’ pipe ................................................................... 34
Figure 26: Macrograph of girth weld. .................................................................................... 34
Figure 27: pWPS for GMAW girth welding of X65M 24’’ pipe. .................................................... 35
Figure 28: Microstructure near the weld cap: WM (left) and HAZ (right). ................................... 36
Figure 29: Microstructure near the weld root: WM (left) and HAZ (right). .................................. 36
Figure 30: Hardness profiles on transversal section. ............................................................... 36
Figure 31: SMAW girth welding of X65M 24’’ pipe ................................................................... 37
Figure 32: SMAW girth welding of X65M 24’’ pipe ................................................................... 37
Figure 33: Irregular inner WM profile .................................................................................... 37
Figure 34: Macrograph of girth weld. .................................................................................... 37
Figure 35: pWPS for SMAW girth welding of X65M 24’’ pipe. .................................................... 38
Figure 36: Microstructure near the weld cap: WM (left) and HAZ (right). ................................... 39
Figure 37: Microstructure near the weld root: WM (left) and HAZ (right). .................................. 39
Figure 38: Hardness profiles on transversal section. ............................................................... 39
Figure 39: Position of the environmental sensors for the leak before break tests ........................ 42
Figure 40: CO2 dispersion footprint as predicted by ALOHA for the most critical scenario ............ 43
Figure 41: Time evolution of CO2 concentration at 128m from the source, 1.5/F - 200 bar. ......... 43
Figure 42: Sketch of leak test rig ......................................................................................... 44
Figure 43: Experimental mass flow per unit area. ................................................................... 45
Figure 44: Specific mass per unit area: exp-to-theoretical error as function of the leak area. ....... 46
Figure 45: Defect shape. Through wall view (left side) and top view (right side)......................... 46
Figure 46: Leak-rupture prediction (by Battelle NG-18) for the test condition of interest. ............ 47
Figure 47: Leak test picture. ................................................................................................ 47
Figure 48: Leak test from side ............................................................................................. 47
Figure 49: Leak test detail of CO2 escape .............................................................................. 47
Figure 50: Pressure transducers layout. ................................................................................ 47
Figure 51: Pressure transducers results................................................................................. 47
Figure 52: Temperature transducers layout (mm). ................................................................. 48
Figure 53: Temperature transducers results. ......................................................................... 48
Figure 54: Thermocamera picture......................................................................................... 48
Figure 55: Temperatures monitored with thermocamera ......................................................... 48
Figure 56: Leak-rupture prediction (by Battelle NG-18) for the test#2. ..................................... 49
Figure 57: Leak test from side test#2. .................................................................................. 49
Figure 58: Leak test detail of CO2 escape .............................................................................. 49
Figure 59: Pressure transducers results (test#2). ................................................................... 50
Figure 60: Temperature transducers results (test#2) .............................................................. 50
Figure 61: Liquid CO2 formation after 500s (test#2). ............................................................. 50
Figure 62: CO2 concentration in front of leak – Test 1# .......................................................... 51
Figure 63: Environmental temperature in front of leak – Test 1# ............................................. 51
Figure 64: CO2 concentration in front of leak (test#2). ........................................................... 51
Figure 65: Environmental temperature in front of leak (test#2) ............................................... 51
108
Figure 66: NG18 model validation [16] ................................................................................. 52
Figure 67: NG18 model validation with SARCO2 tests ............................................................. 53
Figure 68: NG18 model for different valued of Charpy-V energy ............................................... 53
Figure 69: Sketch of the domain simulated ............................................................................ 54
Figure 70: Numerical modelling: concentration map at centerplane .......................................... 54
Figure 71: Numerical modelling: temperature map (°C) at centerplane ..................................... 54
Figure 72: Comparison between numerical calculation data and experimental data. .................... 54
Figure 73: Lay-out of CO2 sensors positioning for the rupture propagation tests. ....................... 56
Figure 74: environmental instrumentation station. ................................................................. 56
Figure 75: Time and space evolution of the CO2 clouds corresponding to the concentrations of 1%
and 5%. Wind velocity 5 m/s- CFD output. ............................................................................ 57
Figure 76: Nettuno military shooting range location ................................................................ 58
Figure 77: SARCO2 test area ............................................................................................... 58
Figure 78: New 24in full scale propagation test line construction phases. .................................. 59
Figure 79: Scheme of the 1st SARCO2 X65 full scale fracture propagation test line. .................... 61
Figure 80: CO2 dispersion pictures sequence ......................................................................... 62
Figure 81: Test result - overview. ......................................................................................... 62
Figure 82: Fracture surface appearance along the axial propagation. ........................................ 63
Figure 83: Fracture path. .................................................................................................... 63
Figure 84: Pressure signals on TP1 and TP2 ........................................................................... 64
Figure 85: Decompression velocity curve, experimental to numerical comparison ....................... 64
Figure 86: Second propagation test burst .............................................................................. 65
Figure 87: CO2 dispersion pictures sequence ......................................................................... 66
Figure 88: Test result: overview. .......................................................................................... 66
Figure 89: Fracture surface appearance along the axial propagation. ........................................ 66
Figure 90: Fracture path. .................................................................................................... 67
Figure 91: Crack speed diagram. .......................................................................................... 67
Figure 92: Arrest on composite crack arrestor and natural arrest. ............................................ 68
Figure 93: Decompression velocity curves, experimental to numerical comparison ..................... 68
Figure 94: wind speed. ....................................................................................................... 69
Figure 95: wind direction. .................................................................................................... 69
Figure 96: solar radiation. ................................................................................................... 69
Figure 97: atmospheric pressure. ......................................................................................... 69
Figure 98: CO2 concentration measured by oxygen cells at 1m height above the ground for the first
(left) and second (right) propagation tests ............................................................................ 70
Figure 99: Comparison between the oxygen cells and the IR sensor CO2 measurements ............. 70
Figure 100: Comparison between the oxygen cells and the IR sensor CO2 measurements ........... 70
Figure 101: CO2 temperature measured at 1m height above the ground for the first (left) and second
(right) propagation tests ..................................................................................................... 70
Figure 102: BTC model chart ............................................................................................... 71
Figure 103: BTC approach for the 1st SARCO2 test – Europipe Initiation pipe ............................ 72
Figure 104: BTC approach for the 2nd SARCO2 test ................................................................ 72
Figure 105: BTC approach for the 1st NG test ........................................................................ 73
Figure 106: BTC approach for the 2nd NG test ....................................................................... 74
Figure 107: BTC approach for the 3rd NG test........................................................................ 74
Figure 108: Evaluation of correction factor for BTC model in the CO2 mixture transportation ....... 75
Figure 109: Probes allocation. .............................................................................................. 76
Figure 110: CO2 concentration vs time (probe8) compared with snapshots of the model results. . 77
Figure 111: CO2 concentration vs time (probe8) compared with model results (markers)............ 77
Figure 112: CO2 concentration vs time (probe13) compared with model results (markers). ......... 77
Figure 113: Weight Loss Coupon – Base Material and Welded (see the red line) ......................... 83
Figure 114: Detail of the surface appearance – GMAW-C ......................................................... 84
Figure 115: 3D Optical Microscope Analysis – GMAW Corinth (Test N°1) ................................... 84
Figure 116: SM Analysis – Test N°3 ...................................................................................... 85
Figure 117: 3D Optical Microscope Analysis – GMAW Corinth Welded Material (Test N°3) ............ 86
Figure 118: Set-up for rotating cage test .............................................................................. 87
Figure 119: Inner surfaces of girth welded joints (root pass) in condition upon delivery .............. 88
Figure 120: Specimens after ageing in post-combustion CO2 with 600 ppmv water .................... 89
Figure 121: Specimens after ageing in post-comb. CO2 with 600 ppmv water in pickled condition 89
Figure 122: Specimens after ageing in post-combustion CO2 with 6,000 ppmv water ................. 90
Figure 123: Spec. after ageing in post-comb. CO2 with 6,000 ppmv water in pickled condition .... 90
Figure 124: Microsections of original states (top) and pickled surfaces aged in post-combustion CO2
with 6,000 ppmv water (bottom) of welded joints GMAW-C, SMAW and GMAW-V (left to right).... 90
Figure 125: Specimens after ageing in oxy-fuel CO2 with 6,000 ppmv water ............................. 91
Figure 126: Specimens after ageing in oxy-fuel CO2 with 6,000 ppmv water in pickled condition . 91
Figure 127: Spec. after ageing in post-comb. CO2 with 6,000 ppmv water and HTABr in pickled
condition ........................................................................................................................... 92
109
Figure 128: Four Point Bent Beam Specimen ......................................................................... 92
Figure 129: Examples of stressed Four Point Bent Beam specimen used for calibration. .............. 93
Figure 130: FPB Spec.(GMAW-C) appearance after autoclave exposure (Test N°1 - 90%AYS) ...... 94
Figure 131: OM images of the FPB cross sections (GMAW-C) after the test N°1 (90% AYS). ........ 94
Figure 132: OM images (Side A) of the FPB cross sections (SMAW) after Test N°1 (72% AYS) ..... 95
Figure 133: OM images (Side A) of the FPB cross sections (SMAW) after Test N°1 (90% AYS) ..... 95
Figure 134: GMAW-C spec. after testing: left 5 °C and right 70 °C. Reference specimen on top. .. 97
Figure 135: SMAW spec. after testing: left 5 °C and right 70 °C. Reference specimen on top. ...... 97
Figure 136: GMAV-V spec. after testing: left 5 °C and right 70 °C. Reference specimen on top. ... 97

110
List of Tables
Table 1: Pipe production for the project ................................................................................. 5
Table 2: full scale fracture propagation tests general design parameters .................................... 8
Table 3: Environment Conditions .......................................................................................... 11
Table 4: Results in under Stagnant conditions (BM = Base Material) ......................................... 12
Table 5: Results of rotating cage tests .................................................................................. 12
Table 6: Results of the SCC corrosion tests............................................................................ 12
Table 7: Results of the Slow Stress Rate Tests ....................................................................... 13
Table 8: Expected impurities in CCTS stream from different capture technologies. ...................... 15
Table 9: EOS implemented in most diffused decompression codes. ........................................... 16
Table 10: difference in measured and predicted saturation pressure. ........................................ 17
Table 11: Database of existing CO2 pipelines ......................................................................... 25
Table 12: Information concerning the chemical compositions ................................................... 26
Table 13: Pipe production for the project ............................................................................... 26
Table 14: Crack Arrestor Design ........................................................................................... 27
Table 15: Seamless pipes tensile properties........................................................................... 28
Table 16: pipe “1” – Charpy-V energy results. ....................................................................... 28
Table 17: pipe “2”–Charpy-V energy results. ......................................................................... 28
Table 18: Battelle drop weight tear test results ...................................................................... 28
Table 19: UOE pipes tensile properties. ................................................................................. 29
Table 20: Europipe Pipes toughness properties. ..................................................................... 29
Table 21: SMLP pipes tensile properties. ............................................................................... 30
Table 22: SMLP pipes toughness properties. .......................................................................... 30
Table 23: Corinth Pipeworks pipes tensile properties. .............................................................. 30
Table 24: Corinth pipes toughness properties. ....................................................................... 30
Table 25: Girth welded joints produced for the project ............................................................ 31
Table 26: Summary of WPS parameters ................................................................................ 31
Table 27: Transverse weld joint tensile test results (cap removed) of girth weld QK, X65. ........... 33
Table 28: Impact test results at -20°C, girth weld QK, X65. ..................................................... 33
Table 29: Tensile test results. .............................................................................................. 36
Table 30: Impact test results at room temperature and -40°C. ................................................ 36
Table 31: Tensile test results. .............................................................................................. 39
Table 32: Impact test results at room temperature and -40°C. ................................................ 39
Table 33: CTOD result on V&M pipes..................................................................................... 41
Table 34: Characteristic distances for the leak before break tests of SARCO2 ............................. 42
Table 35: Test data. ........................................................................................................... 44
Table 36: Dataset of experimental CO2 release tests. (Data from DNV, 2012) ........................... 45
Table 37: Mass flow per unit area: experimental to numerical comparison. ................................ 45
Table 38: Experimental conditions for the first test and subsequently simulated with CFD code .... 54
Table 39: CTOA values for pipes of first test (two specimen method) ........................................ 55
Table 40: CTOA values for pipes of second test (two specimen method) .................................... 55
Table 41: Characteristic distances for the leak before break tests of SARCO2 ............................. 56
Table 42: SARCO2 X65 full scale fracture propagation tests main parameters and conditions. ...... 59
Table 42: 1st SARCO2 X65 full scale fracture propagation test layout. ...................................... 60
Table 45: 2nd SARCO2 X65 full scale fracture propagation test layout. ..................................... 65
Table 46: CO2 full scale tests results available. ...................................................................... 71
Table 47: Test program for autoclave testing under stagnant conditions.................................... 83
Table 48: Post Combustion conditions – Summary of Results Test N°1 ...................................... 83
Table 49: Post Combustion conditions – Summary of Results Test N°2 ...................................... 84
Table 50: Oxyfuel conditions – Summary of Results Test N°3 .................................................. 85
Table 51: Post Combustion conditions – Summary of Results Test N°4 ...................................... 86
Table 52: Results (BM = Base Material) ................................................................................ 87
Table 53: Test conditions .................................................................................................... 87
Table 54: Results of rotating cage tests ................................................................................ 88
Table 55: Loading condition in the FPB testing ....................................................................... 93
Table 56: Test conditions – Four Point Bent Beam .................................................................. 93
Table 57: Pre-Combustion Composition ................................................................................. 93
Table 58: Summary of results – Stress Corrosion testing......................................................... 94
Table 59: Summary of classification according to TM0198 ....................................................... 96
Table 60: Test results according to TM0198 ........................................................................... 97

111
List of Acronyms and Abbreviations
A% Percentage elongation after fracture
ABL Atmospheric Boundary Layer
Ac Fracture surface area
Ag% Percentage elongation at maximum load
AISI American Iron and Steel Institute
API American Petroleum Institute
ASME American Society of Mechanical Engineers
AWS American Welding Society
AYS Actual Yield Strength
b Repulsive factor of cubic EOS
BDWTT Battelle Drop Weight Tear Test
BM Base Metal
BTC Battelle Two Curve
BTCM Battelle two-curve model
BWRS Benedict-Webb-Rubin-Starling
C Constant accounting for backfill constraint
CA Crack Arrestor
CCS Carbon Capture and Sequestration
CCTS Carbon Capture Transportation and Sequestration
CFD Computational Fluid Dynamics
CPA Cubic Plus Association, cubic real gas EOS
CTOD Crack Tip Opening Displacement
CV/A Specific CV energy
CVN Charpy-V Upper Shelf energy
DEP Design and Engineering Practice
DNV Det Norske Veritas
DWTT Drop Weight Tear Test
E steel elastic modulus
EHR Enhanced Hydrocarbon Recovery
EN European Standards
EOR Enhanced Oil Recovery
EOS Equation of State
EPRG European Pipeline Research Group
FL Fusion Line
FPTT Fracture Propagation Transition Temperature
GERG Group European de Recherches Gazieres
GMAW Gas metal arc welding
HAZ Heat Affected Zone
HFI High Frequency Induction welded pipe
HFW High Frequency Welded
HSE Health, Safety and Environment
HTABr Hexadecyltrimethylammonium bromide
ISO International Organization for Standardization
JIP Joint Industry Projects
J-T Joule-Thomson effect
LKP Lee-Kesler Plöcker, virial real gas EOS
M Folias factor
MinOP minimum operating pressure
MOP maximum operating pressure
NACE National Association of Corrosion Engineers
NDT NonDestructive Testing
NIST National Institute of Standards and Technology
OC Oxygen Cell
OD Outside Diameter
p Pressure
Pa arrest pressure
PC Pulverized Coal
ppmv parts per milion in volume
PR Peng-Robinson
PRCI Pipeline Research Council International
Ps Saturation Pressure
r pipe radius
R material resistance to fracture
RANS Reynolds-averaged Navier–Stokes equations

112
ReH Upper yield strength
ReL Lower yield strength
RFCS Research Fund for Coal and Steel
RM Tensile strength
Rp0.2 0.2% offset yield strength
RT Room Temperature
Rt0.5 0.5% extension under load yield strength
SA Shear Area
SAWL Longitudinal submerged arc welding
SMAW Shielded metal arc welding
SMIRK Shell Modified and Improved Redlich Kwong, cubic real gas EOS
SMYS specified minimum yield stress
SRK Soave-Redlich-Kwong, cubic real gas EOS
SSR Slow-strain-rate
t pipe wall thickness
T Temperature
T Thermocouples
TC Thermocouple
TG Thermocouples for Gas
TP Pressure Transducer
TS Temperature sensor
TW Timing Wire
UNIFAC UNIversal Functional Activity Coefficient
UOE U-Ing, O-Ing and Expanding, LSAW pipe
V Volume
Vc fracture velocity
vdW Van der Waals, real gas equation of state
Vm decompression velocity
WM Weld Metal
WPS Welding Procedure Specifications
Z Compressibility factor
𝜎̅ flow stress

113
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117
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 KI-NA-28-918-EN-N
The Carbon Capture Transportation and Sequestration approach is mandatory to
reduce fossil fuel power plant CO2 emissions down to acceptable levels.

Pipelines can efficiently transport supercritical CO2 but some specific issues
have to be investigated due to specific nature of transported fluid.

The general aim of this RFCS project was to develop specific requirements
and design criteria of steel pipes for anthropogenic CO2 transportation pipeline
systems.

The specific programme objectives of this project are the following:

• to improve the know-how and experimental data about toughness

requirements for steel pipes to control initiation and propagation event;
• to collect release dispersion data from a suddenly fractured pipeline;
• to improve existing safety and reliability predictive tools available on the
public domain for natural gas onshore pipelines for tailored anthropogenic
CO2 pipelines.

A huge numerical and experimental testing campaign, including full-scale tests,

has been carried out, that allowed to obtain relevant information to support the
future development of guidelines and recommendation on CO2 transportation
via pipeline.

The project data permitted to have important information on the topics

investigated in the project, in particular on:
• corrective factor for the evaluation of minimum toughness requirement to
arrest the fracture
• development of reliable models for predicting the CO2 dispersion around
fractured CO2 pipeline
• understanding of temperature and pressure evolution of leaked CO2
pipeline
• corrosion and stress-corrosion behaviour of weld joints in CO2 environment

All this information will supply a knowledge contribute for new revision of
international standard on CO2 transportation (e.g. DNV-RP-J202).

ISBN 978-92-79-77023-4
doi:10.2777/205449