Proceedings of the ASME 2015 34th International Conference on Ocean, Offshore and Arctic Engineering

OMAE2015
May 31-June 5, 2015, St. John's, Newfoundland, Canada

OMAE2015-41561

OPTIMIZATION OF THE CEMENT SLURRY COMPOSITIONS WITH ADDITION OF ZEOLITE

FOR CEMENTING CARBON DIOXIDE INJECTION WELLS

Krunoslav Sedić Nediljka Gaurina-Medjimurec Borivoje Pašić

Crosco, Integrated Drilling & University of Zagreb University of Zagreb

Well Services Co., Ltd., Faculty of Mining, Geology and Faculty of Mining, Geology and
Zagrebacka 17, 10313 Graberje Petroleum Engineering Petroleum Engineering
Ivanicko, Croatia; Phone: +385 Pierottijeva 6, 10 000 Zagreb, Pierottijeva 6, 10 000 Zagreb,
91 277 0079; E-mail: Croatia Croatia
krunoslav.sedic@crosco.hr Phone: +38515535825 Phone: +38515535840
nediljka.gaurina- borivoje.pasic@rgn.hr
medjimurec@rgn.hr

ABSTRACT INTRODUCTION

Well integrity related to carbon dioxide injection into depleted oil and
gas reservoirs can be compromised by corrosion which can affect
casing, downhole and surface equipment and well cement. Impact on
well cement can cause overall degradation of set cement and lead to
migration of carbon dioxide back to the surface. Thus, special types of
cements should be used. One of the acceptable solutions is application
of cement blends based on a mixture of Portland cement and
pozzolans. The present paper deals with optimization of the cement
slurry design containing zeolite which is nowadays widely used due to
its high pozzolan activity potential. Cement blends containing 20%,
30% and 40% zeolite clinoptilolite were used. Cement slurries were
optimized for application in slim hole conditions on CO2 injection
wells on Žutica and Ivanić oil fields in Croatia (Europe), where an old
and deteriorated production casing was re-lined with new smaller
sized one. Results obtained by this study suggest that cement slurry
containing zeolite can be optimized for application in well conditions
related to CO2 injection and underground storage, ranging from a
slim hole to standard size casing cement jobs which leads to an
improvement of well integrity related to CO2 injection.
Key words: wells, well cementing, carbon dioxide, underground
storage, EOR, set cement, CO2 corrosion, leakage.
The interest in carbon capture and storage is relatively new, but the
underground injection and effective storage of large quantities of CO2
is not a new technology for oil and gas industry. In the last 10 years,
most of the technologies developed through the last 44 years of CO2
EOR (enhanced oil recovery) experience have been successfully
applied in GS (geologic sequestration) for CCS (carbon capture and
storage) in saline aquifers [1]. To date, the technology as a whole has
only been deployed so far at a few pilot sites around the world such as
the Sleipner field in Norway, Weyburn field in Canada, In Salah field
in Algeria [2, 3]. The majority of locations that are being considered
for carbon dioxide injection and sequestration are typically found in
areas that have a history of oil, natural gas, and/or coalbed methane
production [2, 4, 5, 6]. However, wells in such areas are usually not
completed as corrosion resistant and require new completion design
before they can be used for CO2 underground injection and storage.
Casing and downhole equipment should be made of steel alloys with
high chrome content or should be protected with regular injection of
corrosion inhibitors in case they are made of pure steel. The cement
should contain materials which increase the set cement's resistance to
CO2 corrosion. However, cement slurry design with these materials has
to be optimized for application in well conditions.
One of the solutions is the use of cement blends which contain
pozzolans. Pozzolans are materials which possess little or no
cementitious value but which will in the presence of water react
chemically with calcium hydroxide to form compounds possessing

1 Copyright © 2015 by ASME

cementitious properties [7]. The process of their activity during the
hydration of cement is called secondary binding reaction in which they
react with free calcium hydroxide, formed during the hydration,
thereby reducing its overall content in the set cement. Concurrently,
created compounds fill micro pores within the matrix, resulting in a
reduction in permeability and porosity, and in an increase of the
compressive strength [8].

Zeolites are aluminosilicate minerals which are nowadays frequently

used in cement blends due to their pozzolan properties that enable
them to decrease set cement porosity and permeability and increase
compressive strength. Some authors suggest that zeolites can
significantly reduce or completely deplete all available quantities of
calcium hydroxide from set cement matrix after 28 days setting time,
which puts them ahead of other pozzolans [9-12]. Their application as
Portland cement admixture in CO2 resistant cement blends is the
subject of this study.

CARBON DIOXIDE INJECTION WELL DESIGN

The technologies for drilling and equipping CO2 injection wells are
well developed. Most aspects of drilling and completing such wells are
similar or identical to that of drilling and completing a conventional
gas (or other) injection well or a gas storage well, with the exception
that much of the downhole equipment (e.g. casing and tubing, safety
valves, cements, blowout preventers) must be upgraded for high
pressure and corrosion resistance. The well is completed at the surface
by installing a wellhead and “Christmas Tree” that sits on top of the
wellhead and is an assembly of valves, pressure gauges and chokes.
Devices are connected to the “Christmas Tree” that allow the
monitoring of pressure, temperature, and injection rates. The combined
wellhead has casing annulus valves to access all annular spaces to FIGURE 1. SCHEMATIC OF A CO2 INJECTION WELL
measure the pressure between the casing strings and between the
casing and production tubular. Above the Christmas tree, a CO2 Cement and Its Degradation Due to CO2 Injection
injection valve is mounted and an access valve for running wirelines
from the top. The typical components of an injection well that are Portland cement systems are used conventionally for zonal isolation in
relevant to maintaining mechanical integrity and to ensuring that fluids oil or gas production wells. It is thus crucial to study how such cement
do not migrate from the injection zone into USDWs are the casing, behaves at depth in CO2-rich fluids and understand the chemical
tubing, cement, and packer (Fig. 1) [13]. The well components should interactions between injected CO2 and existing cements that could
be designed to withstand the maximum anticipated stress in each potentially lead to leakage. Portland cement is thermodynamically
direction – axial direction (tensile, compressive) or radial (collapse, unstable in CO2-rich environments and can degrade rapidly upon
burst), and include a safety factor. The loading in each of the stress exposure to CO2 in the presence of water [14]. As CO2-laden water
directions should be compared to the strength of the material in that diffuses into the cement matrix, the dissociated acid (H2CO3) reacts
direction. The loadings correspond to the burst, collapse, and tensile with the free calcium hydroxide and the calcium-silicate-hydrate gel.
strengths of the material. The reaction products are soluble and migrate out of the cement
matrix. Eventually, the compressive strength of the set cement
decreases and the permeability and porosity increase leading to loss of
zonal isolation [15].

There are mainly three different chemical reactions involved in

cement-CO2 interaction: (1) formation of carbonic acid, (2)
carbonation of calcium hydroxide and/or cement hydrates, and (3)
dissolution of calcium carbonate (CaCO3) [6, 13, 16].

Cement is important for providing structural support of the casing,

preventing contact of the casing with corrosive formation fluids, and
preventing vertical movement of carbon dioxide. Some of the most
current research indicates that a good cement job is one of the key
factors in effective zonal isolation.

2 Copyright © 2015 by ASME

The proper placement of the cement is critical, as errors can be
difficult to fix later on. Failing to cement the entire length of casing,
failure of the cement to bond with the casing or formation, not
centralizing the casing during cementing, cracking, and alteration of
the cement can all allow migration of fluids along the wellbore. If
carbon dioxide escapes the injection zone through the wellbore
because of a failed cement job, the injection process must be
interrupted to perform costly remedial cementing treatments. In a
worst case scenario, failure of the cement sheath can result in the total
loss of a well.
During the injection phase, cement will only encounter dry CO2.
However, after the injection phase and all the free CO2 around the
wellbore had been dissolved in the brine, the wellbore will be attacked
by carbonic acid (H2CO3). The carbonic acid will only attack the
reservoir portion of the production (long string) casing, therefore
special consideration of CO2 cement needs only to be considered for
the reservoir, the primary seal and a safety zone above the reservoir.
Regular cement should be placed over the CO2-resistant cement.
However since two different cement slurries will be used, CO2-
resistant cement that is compatible with regular Portland cement has to
be used to prevent flash setting. The cement must be able to maintain a
low permeability over lengthy exposure to reservoir conditions in a
CO2 injection and storage scenario. Long-term carbon sequestration
conditions include a contact of set cement with supercritical CO2 (>31
°C at 7.3 MPa) and brine solutions at increased pressure and
temperature and decreased pH [17].
3 Copyright © 2015 by ASME
WELL INTEGRITY
One of the main CO2 injection candidates may be new wells, or old
wells that are active, closed or abandoned. In all cases, it is critical to
ensure that the long-term integrity of the storage wells is kept; in
others words wellbore integrity is one of the key performance criteria
in the geological storage of CO2 as well as in CO2 EOR projects.
Underground gas storage operations and CO2 sequestration in aquifers
rely on both proper wellbore construction and sealing function of the
cap rock. The potential leakage paths are the migration CO2 along the
wellbore due to poor cementation and flow through the cap rock. The
permeability and integrity of the cement will determine how effective
it is in preventing leakage. The integrity of the cap rock is assured by
an adequate fracture gradient and by sufficient cement around the
casing across the cap rock and without a micro-annulus.
Well integrity has been identified as the biggest risk contributing to
leakage of CO2 from underground storage sites. Wellbore represents
the most likely route for the leakage of CO2 from geologic carbon
sequestration. Abandoned wells are typically sealed with cement plugs
intended to block vertical migration of fluids. In addition, active wells
are usually lined with steel casing, with cement filling the outer
annulus in order to prevent leakage between the casing and formation
rock.
Several potential leakage pathways can occur along active injection
well (Fig. 2a) and/or abandoned well (Fig. 2b). These include leakage:
through deterioration (corrosion) of the tubing (1), around packer (2),
through deterioration (corrosion) of the casing (3), between the outside
of the casing and the cement (4), through deterioration of the cement
in the annulus (cement fractures) (5), leakage in the annular region
between the cement and the formation (6), through the cement plug
(7), and between the cement and the inside of the casing (8) [13].
 FIGURE 2. POSSIBLE LEAKAGE PATHWAYS IN AN ACTIVE CO2 WELL (A) AND ABANDONED WELL (B)
The permeability and integrity of the cement in the annulus and in the
wellbore will determine how effective the cement is in preventing fluid
leakage.
The greatest risk for the escape of CO2 may come from other wells,
typically for oil and gas, which penetrate the storage formation. Such
wells need to be properly sealed in order to ensure that they do not
provide pathways for the CO2 to escape into the atmosphere. Planning
for geologic storage must take such wells into account. The escaping
of CO2 through water wells is much more unlikely since water wells
are usually much shallower than the storage formation.
In injection wells, the presence of CO2 may lead to corrosion of those
parts that get in contact with CO2, which normally means the
production tubing and part of the production casing below the packer.
Corrosion may be limited by: the selection of high alloy chromium
steels, resistant to corrosion, and by inhibitor injection, if using carbon
steel casing.
CO2 CORROSION RESISTANT CEMENT SYSTEMS
WITH ADDITION OF ZEOLITE
Research encompassed optimization of cement slurry compositions
based on cement blends of Portland cement and zeolite clinoptilolite in
4 Copyright © 2015 by ASME
order to determine several designs which could be used for cementing
CO2 injection wells. Previous studies on application of zeolites in
cement blends indicated that they had a high pozzolan activity
potential, which means that they can significantly reduce or even
completely deplete calcium hydroxide during the hydration and
consequently decrease calcium migration out of the set cement matrix.
Moreover, pozzolan reactions will form new cementitious compounds,
which will fill micro pores within the matrix, resulting in a decreased
porosity and permeability and in an increased compressive strength
[8]. This type of cement blends could provide an improved solution
against CO2 corrosion.
The chemical reactions start with the decomposition of zeolite
structure in alkaline environment [18-20] which occurs in cement
during the hydration process as a consequence of increased content of
Ca2+ and OH- ions. Zeolite reacts with OH- ions which causes its
decomposition and creation of new ions, [SiO(OH)3]- and [Al(OH)4]-.
These ions react with Ca2+ forming new hydrated calcium silicates
(C-S-H) and aluminates which ultimately results in an improved set
cement microstructure [11].
Case study
Well conditions were determined according to well data of the existing
wells on two oilfields in Croatia, Žutica and Ivanić, where carbon
dioxide is injected underground during the Enhanced Oil Recovery
project.

The standard for well design applied to the existing wells on the Žutica
oil field consist of: surface casing 339.7 mm (13 3/8”), intermediate
casing 244.5 mm (9 5/8”) and production casing 139.7 mm (5 1/2")
[21]. Whereas the standard well design of the existing wells on Ivanić
oil field consist of: intermediate casing 244.5 mm (9 5/8”) and
production casing 139.7 mm (5 1/2") [22]. However, these existing
wells will have to be modified to resist the corrosion caused by CO2.
Requirements specified in EOR project regarding well design include
the following:
- cement, casing, tubing, packers and all other downhole and
surface equipment which will be in contact with injection fluid
have to be CO2 corrosion resistant,
- production casing has to be pressure tested to 200 bar.

However, since the cement and production casing in these existing

wells are not CO2 corrosion resistant and that production casing
pressure testing to 200 bar could lead to severe damage, and taking
into account it’s the deteriorated condition after 50 years of oil
production, it has been decided that the design of the injection wells
will be modified by re-lining the existing production casing with a
new, smaller casing. New re-lining (production) casing will be
corrosion resistant and cemented with CO2 resistant cement. The size
of the re-lining casing was determined to be either 101.6 mm (4”) or
88.9 mm (3 1/2"). Figures 3. and 4. illustrate the standard well design
of the injection wells on Žutica and Ivanić oil fields after re-lining.

FIGURE 4. STANDARD WELL DESIGN OF INJECTION WELL

ON IVANIĆ OIL FIELD AFTER RE-LINING [22]

Although re-lining with new casing has many benefits related to CO2
corrosion resistance and overall well stability, there are some
unwanted consequences as a result which primarily concerns clearance
between the two casings. Namely, the inside diameter of the existing
production casing 139.7 mm (5 1/2") is 124.3 mm while the outside
diameter of the re-lined casing is 101,6 mm (4“). The clearance
between them is only 11.35 mm (0.447”) which differs significantly
from the well design recommended value of 19.1 mm (3/4“) [23].
Consequently, the dynamic pressure during cement job is increased
which increases the overall annular pressure and the risk of fracturing
the formation accordingly. Therefore, cement job has to be optimized.
This can be done by optimizing the rheological properties of the
cement slurry and flow rate. In this study, optimization was carried out
using well cementing simulation software.

Properties of cement slurry and set cement required for re-lining

casing cementing are specified by mining projects of hydrocarbon
production on Žutica and Ivanić oil fields [21, 22] and presented in the
table 1.

FIGURE 3.STANDARD WELL DESIGN OF INJECTION WELL

ON ŽUTICA OIL FIELD AFTER RE-LINING [21]

5 Copyright © 2015 by ASME

 TABLE 1. PROPERTIES OF CEMENT SLURRY AND SET TABLE 2. CEMENT SLURRY COMPOSITIONS
CEMENT SPECIFIED BY MINING PROJECTS OF
HYDROCARBON PRODUCTION ON ŽUTICA AND IVANIC OIL CS 20 CS 30 CS 40
Composition:
FIELDS [21, 22] Concentration (% BWOC)
Cement Class G Class G Class G
Properties Values Water 46.00 53.00 65.33
Density (kg/m3) 1 558 – 1 650 Friction reducer 1.00 1,00 1.00
Free fluid content (ml/250 ml) 0.5 Fluid loss additive 0.50 0.50 0.50
Retarder 0.35 0.35 0.35
< 80 ml
Fluid loss (ml) Antisettling agent 0.10 0.20
(@ 6.9 MPa)
Latex 22.53 22.53 22.53
Compressive strength after 24 h (MPa) > 12 0.35 0.35 0.35
Defoamer
Glass microspheres 3.00 2.00
Zeolite 20.00 30.00 40.00
Research was commenced with cement slurry composition marked as
CS 50 containing 50% zeolite BWOC. However, slurries with this
content of zeolite could have not been mixed with laboratory mixing
devices. Consequently, further tests were dismissed and investigation
TABLE 3. CEMENT SLURRY AND SET CEMENT
continued on cement slurries containing 40% zeolite BWOC (marked
as CS 40). This content indicated the possible applicability at PROPERTIES
downhole conditions and therefore optimization of water and additives
content was performed as well in order to achieve the cement slurry CS 20 CS 30 CS 40
and set cement properties specified by mining projects. Further on, Density (kg/m3) 1 650 1 650 1 650
optimization of cement slurries with addition of 20% (marked as CS Free fluid content
0.0 0.0 0.0
20) and 30% (marked as CS 30) zeolite were carried out resulting in (ml/250 ml)
two more slurry designs containing zeolite that could have been used API Fluid loss (ml) 142 128 146
for cementing CO2 injection wells on Žutica and Ivanić oil fields. Thickening time (min) > 240 > 240 > 240
Optimization of these slurries was carried out in a manner that the Compressive strength 15.29 17.28 15.27
proportion of water and other additives in the slurry composition after 72 h, MPa (psi) (2 217) (2 506) (2 215)
changes as the least possible in relation to the composition of the
cement slurry with addition of 40% zeolite. An attempt was made to Cement slurries were optimized to decrease the dynamic pressure as
design three cement slurries with different content of zeolite, which much as possible and in the same time to cover wide range of slurry
according to the proportion of other additives were as similar as types. However, software simulation of cement job indicated that
possible, while in the same time applicable in well conditions. optimization of cement slurries will not be enough to decrease the
However, water content could have not been successfully optimized pressure below the formation fracturing pressure. Thus, flow rate
entirely due to substantial decrease of zeolite content which optimization had to be done as well. Flow rate on Žutica wells was
proportionally caused an increase of water content in relation to the decreased from 400 dm3/min to 100 dm3/min just before the expected
total amount of solid particles in the slurry. This resulted in density pressure increase due to slurry entering the annular. Flow rate on
reduction and excess water in composition, which decreased the Ivanić wells had to be decreased twice, from 400 dm3/min to 100
viscosity and caused the sedimentation. Therefore, to optimize the dm3/min and then to 50 dm3/min, because formation fracturing
compositions with addition of 30% and 20% zeolite, water content had pressure on this field is considerably lower (15 kPa/m) [24] than on
to be changed which caused the changes in settling agent content as Žutica field (16 kPa/m) [25]. Appendices 1 – 6 illustrate simulation of
well. Furthermore, glass microspheres were added to correct the annular pressure development during re-lining casing cement job on
density of cement slurries. Cement slurry compositions are presented Žutica and Ivanić injection wells. Input data used for simulation are
in table 2. Properties of cement slurry and set cement are presented in presented in table 4.
the table 3.

6 Copyright © 2015 by ASME

 TABLE 4. INPUT DATA FOR SIMULATION OF CEMENT JOBS ON WELLS ŽU-111 AND IVA-70
Well data
Žu-111 Iva-70
Total depth (m) 2 129 1 772
139.7 mm (5½”); 25.5 kg/m; J-55; 139.7 mm (5½”); 25.5 kg/m; J-55;
Old production casing
0 – 2 125 m 0 – 1 770 m
101.6 mm (4”); 14,1 kg/m, 101.6 mm (4”); 14.1 kg/m,
Material: Material:
New re-lined casing
0 – 1 960 m: carbon steel R-95 0 – 1 620 m: carbon steel R-95
1 960 – 2 074 m: duplex Cr25 1 620 – 1740 m: duplex Cr25
Fracturing pressure (kPa/m) 16 15
Pore pressure (kPa/m) 9.8 9.8
Bottom hole static temperature (BHST) (°C) 108 100
Flow rate (dm3/min) 400  100 400  100  50
Cement slurry data
CS 20 CS 30 CS 40
Yield point,Pa) 0.99 1.69 1.65
Flow behavior index, n (-) 0.935 1.014 0.968
Consistency index, K (Pasn) 0.35 0.16 0.12
Density, ρ (kg/m3) 1650 1650 1650

CONCLUSIONS REFERENCES

The following conclusions can be drawn:
1. Zeolite clinoptilolite can be used as an admixture to Portland
cement for application in well conditions related to CO2
injection and underground storage, ranging from a slim hole
to standard size casing cement jobs. However, zeolite and
water content ratio has to be optimized because decrease of
zeolite content can proportionally cause an increase of water
content in relation to the total amount of solid particles in
the slurry. This can result in density reduction and excess
water in composition which can decrease the viscosity and
cause sedimentation.
2. Re-lining existing production casings with new ones in CO2
injection wells offers a good solution for old oil and gas
fields which generally have wells with damaged and
deteriorated production casings. Nevertheless, all casing and
downhole equipment which comes into contact with CO2
saturated fluid should be made of steel alloys with high
chrome content or should be protected with regular injection
of corrosion inhibitors in case they are made of pure steel.
3. Cement slurry design, especially rheological properties of
cement slurry and flow rate, has to be optimized to decrease
the dynamic pressure in narrow annular spaces as much as
possible to avoid fracturing of the formations.
ACKNOWLEDGMENT
This study was financially supported by Crosco, Integrated Drilling &
Well Services Co., Ltd. We thank Crosco for allowing us to use their
lab facilities and we also thank Professor Krešimir Pavelić, PhD for
providing the supply of zeolite for this study.
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APPENDIX

Legend for Appendix 1 to 3

Dynamic pressure curve:

1 Bottom plug dropped
2 Top plug dropped
3 Packer fluid entering the annular
4 Pressure decrease due to annular flow rate decrease
5 Beginning of displacement
6 End of a free fall effect
7 Flow rate decrease from 400 dm3/min to 100 dm3/min
8 Beginning of a new free fall effect due to flow rate decrease
9 Cement slurry entering the annular
10 End of a new free fall effect
11 Job completed

Hydrostatic pressure curve:

12 Cement slurry entering the annular
13 End of a new free fall effect
14 Job completed
APPENDIX 1. ANNULAR PRESSURE DURING RE-LINING
CASING CEMENTING ON THE WELL ŽU-111 USING
CEMENT SLURRY WITH ADDITION OF 20% ZEOLITE

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 Legend for Appendix 4 to 6

Dynamic pressure curve:

1 Bottom plug dropped
2 Packer fluid entering the annular
3 Top plug dropped
4 Pressure decrease due to annular flow rate decrease
5 Beginning of displacement
6 End of a free fall effect
7 Flow rate decrease from 400 dm3/min to 100 dm3/min
8 Beginning of a new free fall effect due to flow rate decrease
9 Cement slurry entering the annular
10 End of a new free fall effect
11 Flow rate decrease from 100 dm3/min to 50 dm3/min
12 Job completed

Hydrostatic pressure curve:

13 Cement slurry entering the annular
14 End of a new free fall effect
APPENDIX 2. ANNULAR PRESSURE DURING RE-LINING
15 Flow rate decrease from 100 dm3/min to 50 dm3/min
CASING CEMENTING ON THE WELL ŽU-111 USING
16 Job completed
CEMENT SLURRY WITH ADDITION OF 30% ZEOLITE

APPENDIX 4. ANNULAR PRESSURE DURING RE-LINING

CASING CEMENTING ON THE WELL IVA-70 USING
APPENDIX 3. ANNULAR PRESSURE DURING RE-LINING CEMENT SLURRY WITH ADDITION OF 20% ZEOLITE
CASING CEMENTING ON THE WELL ŽU-111 USING
CEMENT SLURRY WITH ADDITION OF 40% ZEOLITE

9 Copyright © 2015 by ASME

APPENDIX 5. ANNULAR PRESSURE DURING RE-LINING APPENDIX 6. ANNULAR PRESSURE DURING RE-LINING
CASING CEMENTING ON THE WELL IVA-70 USING CASING CEMENTING ON THE WELL IVA-70 USING
CEMENT SLURRY WITH ADDITION OF 30% ZEOLITE CEMENT SLURRY WITH ADDITION OF 40% ZEOLITE
(*Point 6 was excluded from the diagram because in this case, the free
fall effect did not end before the flow rate was decreased.)

10 Copyright © 2015 by ASME