Durability of Oilwell Cement Formulations
Aged in H2S-Containing Fluids
E. Lécolier, A. Rivereau, N. Ferrer, A. Audibert,* and X. Longaygue,** Institut Français du Pétrole (IFP)
Summary
In the next few decades, the production of oil fields with high
contents of associated sour gases will increase. For instance, it is
estimated that 40% of the world’s remaining gas reserves contain
more than 2% of carbon dioxide (CO2) and/or more than 100 ppm
of hydrogen sulphide (H2S). Therefore, investigations on technolo-
gies to produce such fields are of utmost importance. Because of
the presence of corrosive gas, special attention has to be paid to
the design and the selection of materials (steel and cement) used
for well construction. Corrosion of steel caused by acid-gas-
containing brines is well documented in the literature, and to a
lesser extent, data about the degradation by wet CO2 or wet H2S
can be found. For cement-based materials, one can find abundant
literature dealing with deterioration of cement pastes because of
the CO2 environment. Published data on degradation mechanisms
of cement-based materials exposed to H2S environments are more
scarce. This paper addresses the problem of durability of oilwell
cement in different H2S environments.
Different periods of time can be identified in the lifetime of
the wells—the production period (typically between 20 and 40
years), the post-abandonment period (some tens of years following
the permanent well abandonment), and the abandonment period
(several centuries). For each period of time, cementing materials
(primary cementing, plugs) are in contact with different types
of fluids. Therefore, to correctly assess the behavior of oilwell
cement, aging tests have to be carried out in fluids representative
of these different periods of time. In this paper, we present both the
methodology implemented under high-pressure/high-temperature
conditions for testing materials in H2S-containing fluids and the
results obtained on cement-based materials. Main physicochemi-
cal degradation mechanisms of cement-based materials caused
by H2S are identified using various characterization techniques.
Depending on the nature of the fluid in contact with cement
materials, severe degradation can occur with a strong impairment
of macroscopic properties.
Introduction
The major goal of the primary cementing is to provide a complete
and permanent zonal isolation of the well. This means that the
cement sheath must prevent any fluid circulation (gas, oil, brine)
between different rock layers. To achieve this goal, many events
must be successfully addressed from the beginning of the cement-
ing job to the well plugging. Fig. 1 exemplifies the different steps
that must be successful during the lifespan of the well.
This paper focuses on the durability of cement-based materials
used for the cementing of wells that are drilled in fields with high
contents of sour gases. For the authors, durability means keeping
the initial qualities of the cement sheath: mechanical integrity
(absence of mechanical failure) and low hydraulic conductivity
(no increase of porosity and/or connectivity vs. time, which would
facilitate transport of aggressive species and/or pollutants). Modi-
fications of the macroscopic properties of cement materials are
* Now with Total, La Défense (France).
** Now with French Department of Energy, Environment, and Industry.
Copyright © 2010 Society of Petroleum Engineers
This paper (SPE 99105) was accepted for presentation at the IADC/SPE Drilling
Conference, Miami, Florida, 21–23 February 2006, and revised for publication. Original
manuscript received for review 21 December 2005. Revised paper received for review 04
June 2009. Paper peer approved 15 July 2009.
90
generally induced by chemical reactions. Nonetheless, chemical
reactions taking place in the cementing materials could be accept-
able if they do not impair mechanical resistance and/or increase
hydraulic conductivity.
As one can see in Fig. 1, durability concerns both production
and well-abandonment periods. The major differences between
these two periods of the well life are the following:
• Mechanical loading: Stress variations within the cement sheath
occurring during the production period can be induced by thermal
and/or pressure changes in the well (Thiercelin et al. 1998; Bosma
et al. 1999). After the plugging of the well, a mechanical loading
can still exist, but contrary to what happens during the production
time, the stress changes occur more slowly and last over a very long
period of time (Mainguy et al. 2005; Mainguy et al. 2007).
• Downhole environment: Downhole pressure and temperature,
as well as the nature of the fluids in contact with the cement sheath,
are generally varying with time. Depending on well location and
well type (producer, water injector, gas injector), the thermody-
namic state (gas, liquid, supercritical fluid) and the composition
of the fluid in contact with the cement annular differ over time,
and these changes are able to modify the cement.
Consequently, to correctly assess oilwell cement durability,
aging tests must be carried out with fluids that are representative
of the different life periods of the different types of well. For wells
drilled in areas with high contents of H2S or H2S/CO2 mixture, the
following situations can be considered as critical from a chemical
point of view:
• Primary cementing across the caprock and the reservoir dur-
ing the production
• Primary cementing during an acid-gas injection (in case of
reinjection)
• Primary cementing and plugs after the end of the production
and reinjection operations
In this work, we investigated both chemical evolution and
physical-properties change of cement-based materials in condi-
tions corresponding to those encountered during production and
abandonment periods. We studied low-permeability formulations
[see Dubois et al. (1999), Noïk et al. (1998), and Noïk and Rivereau
(1999) for more details] and compared the results with those
obtained on conventional cement systems.
For the purpose of this investigation, aging tests were per-
formed with a mixture of hydrocarbons, gas, and water that mim-
ics a reservoir fluid in contact with cement during the production
period and just after the well plugging, and a brine saturated with
H2S that is considered to be representative of the equilibrium fluid,
a long time after the end of H2S reinjection.
State of the Art
Alteration of cementing materials in harsh environments [for
instance, sour-gas production or injection (Krilov et al. 2000;
Benge and Dew 2005), brines, hot-fluid injection] has been investi-
gated already. More recently, a concern with acid-gas sequestration
(for example, CO2 geological storage) has been growing. Indeed,
CO2 may alter cement-based materials through two processes:
• CO2 injected underground will form a wet supercritical plume
at the top of the reservoir. This wet supercritical CO2 can induce a
dramatic leaching of the cement material after long-term exposure
(Van Gerven et al. 2004; Barlet-Gouédard et al. 2005).
• When dissolved in brine, CO2 reacts with hydration products
in the cement pores to form different species of calcium carbonate
that can be leached out of the cement matrix because of a prolonged
March 2010 SPE Drilling & Completion
 Fig. 1— Steps of cement-sheath life with some associated operational concerns.
contact with CO2. These reactions lead to an impairment of the
material (Barlet-Gouédard et al. 2005).
Another important problem that will not be addressed here is
the role and behavior of interface between caprocks and cement
on one hand and between cement and casing on the other hand. It
is suspected that interfaces degradation caused by chemical reac-
tions or mechanical stresses occurring during the life cycles of the
well (injection/reservoir compression, abandonment) can lead to
the formation of fluid-migration pathways. In that case, risks of
leakage through these pathways could be much higher than those
expected through bulk-altered cement or corroded steel casing.
Published data on degradation mechanisms of cement-based
materials exposed to pure H2S or H2S/CO2 environments are more
scarce (Krilov et al. 2000; Jacquemet et al. 2005). Jacquemet et al.
(2005) investigated the durability of cement paste aged in brine
with acid gas (66% molar H2S + 34% molar CO2) at 50 MPa and
200°C. They conducted experiments in carefully controlled con-
ditions (pH, Eh) providing reliable results for chemical reactions.
They showed that the initial tobermorite phase has been converted
into a calcium-depleted one. The released calcium from calcium
silicate hydrates (CSHs) was combined with carbon aqueous spe-
cies to form calcite. Pyrite formation is observed because of the
reaction between H2S, C4AF, and steel. Nonetheless, the authors
did not study the evolution of the microstructure (pore-size dis-
tribution for instance) or the physical properties (such as water
permeability) of their degraded cement pastes. Aging in sour gas
(150 ppm of H2S and 22% of CO2) brine has been studied by Krilov
et al. (2000). It is generally observed that carbonation occurs on the
TABLE 1—COMPOSITION OF THE AGING FLUID
Hydrocarbons (diesel type II)
47% parafins
50% vol
32% naphtens
11% alkylbenzene
Brine (sea water)
4 g/L Na 2S04
20% vol
11 g/L MgCl 2
1 g/L CaCl 2
Gas
85% CH 4
30% vol
5% CO2
10% H2S
March 2010 SPE Drilling & Completion
cement surface through a time-dependence phenomenon and may
induce a decrease of compressive strength. Experimental results
are difficult to interpret because several minerals can dissolve or
precipitate simultaneously, but a severe depletion of calcium on
the outer layer is generally observed. Recently, it was shown that
the formation of a layer rich in calcium carbonate may retard the
leaching phenomenon but does not stop it (Barlet-Gouédard et al.
2005; Duguid et al. 2005).
When in contact with acidic aqueous solutions, acid attack of
cement-based materials takes place. In the course of acid attack,
H3O+ ions penetrate within the cement matrix and dissolve solid
hydration products. Experimental works have shown that the
alteration of the cement-based materials depends on the chemical
composition of cement as well as the pH of the acid solution. The
rate of the degradation is strongly linked to acid concentration
and to the type and amount of hydrated phases involved in the
reactions. For example, dissolution of ferrite or aluminate phases
and the induced leaching of Fe3+ and Al3+ is slower and occurs at
lower pH values than the depletion of Ca2+ from portlandite. As
the pH decreases, portlandite (pH stability equal to 12.6), CSH
(pH stability ≈ 10–11), calcium aluminate, and ferrite hydrates
are successively dissolved. The ultimate material is a silica gel
when pH is les than approximately 2. For pH ranging between 4
and 6–7, depleted-calcium hydrates remain with residual aluminate
and ferrite hydrates.
Experimental
Aging of Cementitious Materials in a Reservoir Fluid. In this
experiment, the aging fluid corresponds to API fluid specification
16 (i.e., a mixture of seawater, hydrocarbon, and gas, as detailed
in Table 1). Aging tests were performed in IFP facilities close to
Lyon. This area was specifically designed for H2S safety environ-
ment. Tests were performed at 120°C and 7 MPa in an agitated
vessel so that gas/liquid contact is maintained during aging. A
photograph of the aging vessel is given in Fig. 2. Similar aging
tests were performed in lime-saturated water for comparison.
Three cement systems have been tested: a high performance
cement, named Cement I; a classical mortar (which is a blend of
cement powder and sand); and an ordinary oilwell-cement slurry
(water/cement weight ratio of 0.44). The latter two are used for
comparison. The composition of the Cement I system is detailed in
Table 2. Cement I is a low-permeability material, and its properties
were described previously (Dubois et al. 1999; Noïk et al. 1998).
Aging tests lasted from 1 to 12 months. More than 200 cement
specimens have been tested. For each exposure time, different mea-
surements were performed: variation of sample weight, variation
91
 TABLE 2—COMPOSITION OF THE CEMENT I SYSTEM (g)
Cement 1
Silica fume 0.25
Crushed sand 1.1
Dispersant 0.044
W/C 0.15

TABLE 3—COMPOSITION OF THE BRINE (g/L)

NaCl 143.7
Na2SO4 4.3

TABLE 4—COMPOSITION OF THE CEMENT II SYSTEM (g)

Cement 1
Silica fume 0.24
Crushed sand 0.20
Fig. 2 — Pressurized vessel used for aging with H2S-containing Dispersant 0.018
fluids. W/C 0.27

of sample volume, variation of compressive strength, and variation
of flexural strength and water permeability.
Aging of Cementitious Materials in an H2S-Saturated Brine. In
this experiment, aging fluid is a brine pressurized with H2S. The
composition of the brine is given in Table 3.
Experiments were carried out in pressurized cells of the type
shown in Fig. 2. Two cement-based materials have been tested.
The first one is a conventional portland oilwell-cement slurry with
a water/cement weight ratio equal to 0.44. No additives, except a
defoamer, were incorporated in the formulation. The second tested
formulation, named Cement II hereafter, is a high performance
cement whose composition is given in Table 4.
All the samples were cured at 80°C and 7 MPa. Tests were per-
formed at 120°C and 15 MPa in a nonagitated cell. All the cement
specimens were immersed in H2S-saturated brine. Specimens were
cylinders 2.5 cm in diameter and 5.0 cm in height. During the first
hours, a decrease of the pressure was observed because of the
solubilization of H2S in the brine. The pressure of H2S was then
adjusted to maintain a value of 15 MPa.
These samples were aged for 7 and 21 days. The ratio of the vol-
ume of fluid to the volume of cement specimens was approximately 2.
The fluid was not renewed during the aging, but the control of H2S
pressure maintained a constant pH (≈ 4) throughout the test. Only
the results of the 21-day aging are presented in this paper.
Results and Discussion
Aging of Cement-Based Materials in a Reservoir Fluid. As can
be seen in Fig. 3, diesel is absorbed into the different materials and
especially into those presenting the higher permeability. Diesel is
even desorbing from the mortar specimen after its removal from
the aging vessel. This observation is correlated with the increase

Fig. 3 —Weight variations of Cement I and mortar vs. time.

92 March 2010 SPE Drilling & Completion

 400

350 Mortar
Cement I

Compressive strength (MPa)

300 Cement Paste

250

200

150

100

50

0
0 2 4 6 8 10 12
Time (month)

Fig. 4 —Variations of the compressive strength of Cement I, mortar, and cement paste vs. time.

showing that, even after 1 year, some anhydrous cement grains

TABLE 5—RESULTS OF THE PERMEABILITY
MEASUREMENTS (C3S) have not been fully hydrated. For the mortar and the con-
ventional-oilwell-cement system, compressive strength is constant
Sample Permeability (darcy) even after 1 year of aging in deionized water or in seawater.
Time Cement Slurry Aging of Cementitious Materials in an H2S-Saturated Brine.
(months) (W/C = 0.44) Mortar Cement I After 21 days of aging in the H2S-saturated brine, specimens
0 6 10
–6
1 10
–5
3 10
–6 were removed from the pressurized vessel and analyzed by X-ray
3 5 10
–6
3 10
–7
3 10
–9 tomography to evidence an alteration front. Indeed, X-ray tomog-
–5 –11
raphy is a nondestructive technique allowing investigation of the
12 – 2 10 < 10 internal structure of material. Photographs of cross sections of
one cylinder of the cement slurry and one cylinder of Cement II
are given in Fig. 5. Dark areas correspond to low X-ray absorp-
of the sample weight, which is, respectively, 3% for the mortar tion zones (i.e., in the present case, to higher-porosity areas).
and 1% for Cement I (Fig. 3). However, variations in volume are Sound zones appear as bright ones on the image. Thanks to X-ray
quite low (i.e., less than 1%, whatever the cement system). From tomography, the degradation front in the cement materials is eas-
surface observations, it also seems that H2S has reacted within ily evidenced. Examination of Cement II shows that the degraded
the material pores and especially within the mortar. This may be layer is approximately 11 mm thick. Observation of the ordinary
linked to a higher pore connectivity allowing a higher reactivity of cement paste shows that the cylinder is homogeneously degraded.
H2S solubilized in the water phase. Whatever the cement material, Therefore, the cement paste was severely attacked by the H2S-
mechanical properties are affected slightly after aging (Fig. 4). saturated brine. This observation is in accordance with the results
Similar results are observed for the evolution of water permeability of Krilov et al. (2000) and of Jacquemet et al. (2005). The porosity
(Table 5). of the cement samples has been measured by mercury intrusion
When comparing aging results in various water compositions porosimetry. While the initial porosity was equal to 27%, the
(Noïk and Rivereau 1999), an increase of the mechanical properties porosity of degraded areas reached 64%. The initial porosity has
for Cement I was generally observed related to its microstructure been multiplied by a factor 2.5 after the 21-day aging in H2S-rich

Fig. 5 —X-ray tomography images of an ordinary cement slurry (left) and Cement II (right) after aging in H2S-saturated brine.

March 2010 SPE Drilling & Completion 93

 TABLE 6—RESULTS OF THE PERMEABILITY
MEASUREMENTS
Sample Permeability (darcy)
Time (months) Cement Slurry (W/C = 0.44) Cement I
–7 –9
0 4.6 10 6.5 10
–5 –5
21 4.4 10 1.0 10
brine. With such high porosity values, one can expect high perme-
ability levels. Table 6 summarizes the results of water-permeability
measurements for the tested materials.
As expected, the increase of water permeability after H2S
exposure is very high. The permeability of degraded cement slurry
is increased by two orders of magnitude, and the permeability of
the degraded Cement II is multiplied by 104. Although the initial
permeability of Cement II is very low, its final value is similar to
that of the degraded cement slurry. The increased porosity and per-
meability are probably linked to strong chemical modifications of
the matrix. Therefore, the mineralogy of degraded cement systems
has been investigated by X-ray diffraction (XRD). Phase identifica-
tion showed the presence of pyrite, ettringite, and calcium sulfates.
Peaks of very low intensity corresponding to calcium carbonate
(CaCO3) (aragonite, calcite) were also observed; the presence of
CaCO3 is caused by a partial carbonation of the samples occurring
during the specimen handling. The diffuse peak at 0.27–0.31 nm
corresponding to CSHs still exists, but its intensity is very low.
This low-intensity and diffuse peak probably means that CSHs are
leached and amorphous silica gel is formed. XRD did not reveal the
presence of anhydrous phases (for instance C2S or C4AF), nor port-
landite and hydrogarnet, also named katoite [Ca3Al2(SiO4)(OH)8].
The absence of peaks corresponding to these crystallized phases
indicates that the matrix has been severely leached. This explains
the very high porosity and permeability values observed.
Although Cement II specimens were not homogeneously
degraded, uniaxial-compressive-strength measurements have been
performed on the two tested cement systems. The results are given
in Table 7.
We can notice a sharp decrease of the mechanical resistance
of the degraded samples. The compressive strength of the cement
paste is divided by 23.5, and the compressive strength of Cement
II by only 9. The impairment of mechanical integrity of Cement II
is lower compared to that of the ordinary-cement paste.
To summarize, the aging of Portland-cement-based materials
in H2S-saturated brine under pressure and temperature is critical.
Portlandite and katoite are dissolved. The weakening of the materials
is related to calcium leaching (dissolution of Portlandite and decalci-
fied CSH), inducing a high porosity increase. The impairment of the
properties of the cement system cannot be explained by strength ret-
rogression occurring above 120°C. Indeed, Cement II incorporating
silica fume for impeding strength retrogression (Le Saoût et al. 2004)
appears also highly degraded. Therefore, the severe deterioration of
Portland-cement-based materials properties is a direct consequence
of the calcium leaching of the matrix. However, it is worth noticing
that the aging tests were performed at pH ≈4, which is a very low
value, probably much lower than expected in the field.
Conclusions and Perspectives
Laboratory results show that the production period should not be
critical from a chemical point of view for the integrity of cement
annulus located in the reservoir. Even when sour gases are present,
the limited amount of water should impede deleterious chemical
reactions inducing a degradation of Portland cement. However,
these conclusions should be confirmed on a longer time scale
and/or for higher content of sour gases. Indeed, presence of acid
gases dissolved in water should lead to the degradation of the
Portland-cement matrix. But in the conditions tested during this
work, the acid attack is less obvious than the degradation occurring
in acidic aqueous solutions (typically brine saturated with sour
gases). The aging behavior of the Cement I system is better than
94
TABLE 7—RESULTS OF MECHANICAL TESTS
Compressive Strength (MPa)
Ageing Duration Cement Slurry
(days) (W/C = 0.44) Cement II
0 47 196
21 2 22
that of conventional cement materials (oilwell-cement slurry and
mortar) because of the very low porosity impeding the transport
of aggressive species within the cement matrix.
Conditions prevailing after the abandonment of H2S-injector
wells are dramatic for the integrity of Portland-cement-based
materials. Ordinary Portland-cement slurry and the Cement II
system are rapidly and highly damaged. The very-acidic condi-
tions explain such a behavior. Hydrated phases present in the
cement matrix are leached: Portlandite is totally dissolved from the
ordinary cement paste, and silicate calcium hydrates are severely
decalcified. Both phenomena induce a sharp increase of the poros-
ity and the mechanical weakening of the materials. Because of the
extreme environmental conditions tested, the kinetics of the deg-
radation observed in the laboratory is undoubtedly overestimated
when compared to an actual in-situ alteration rate. However, the
evidenced degradation state of the cement will occur in the well
after a certain time. Future research projects should be initiated to
determine the time scale at which this degradation state will appear,
implying that, at that time, Portland cement will no longer play
its barrier role. Finally, to ensure the long-term confinement of
reinjected H2S, alternative cementing materials have to be designed
to plug and abandon wells successfully.
Acknowledgments
The authors would like to thank Elisabeth Rosenberg and Corinne
Fichen for X-ray tomography experiments and Jean-François Pillot
for his help in preparing samples and measuring the mechanical
properties. They are also grateful to Joseph Martin, Frederic Hil-
lion, Pascal Clermont, and Denis Bonnet for having performed
aging tests in IFP-Lyon.
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SI Metric Conversion Factors
ft × 3.048* E–01 = m
°F (°F–32)/1.8 = °C
in. × 2.54* E–02 = m
psi × 6.894 757 E–02 = bar
psi × 6.894 757 E–03 = MPa
*Conversion factor is exact.
March 2010 SPE Drilling & Completion
Eric Lécolier earned a PhD degree in colloidal science in 1998
at the University of Orléans (France). He joined IFP in 1999 as a
research engineer working in the Drilling Fluids and Cementing
Materials group. Lécolier’s main technical interests include
various aspects of the cement-based materials for wellbore
cementing. He currently manages the Well Integrity Project at
IFP. Alain Rivereau is a research engineer at IFP. He has more
than 30 years’ experience from research and development
in drilling and well cementing. Rivereau has authored numer-
ous SPE papers as well as patents, and his expertise and inter-
ests are in the area of well cementing technology, cements
aging in various conditions and development of new cement-
based materials. Nathalie Ferrer joined IFP in 1988 and worked
on petrochemical procedures in the Kinetics and Catalytic
Department. She joined, in 2004, as research technician chem-
ist with the Drilling Fluids and Cementing Materials Group. Ferrer
is involved in studies dealing with degradation of the steel-
cement interfaces in acid corrosive environment, specifically
for CO2 geological storage. Annie Audibert-Hayet is a petro-
leum architect in charge of development studies in the head-
quarters of Total. She has more than 28 years of experience in
E&P managing research programs and teaching, working in
EOR, formation damage, drilling fluids and cements, and more
generally in colloids science. Author of many technical papers
and holding numerous patents, Audibert-Hayet holds a chemi-
cal engineering degree from Ecole Nationale Supérieure de
Chimie de Paris and a PhD degree from the University of Rouen
in France. Xavier Longaygue is presently working as a visit-
ing expert at the French Ministry of Environment, Energy, and
Sustainable Development. After a first experience in the iron
and steel industry, he joined IFP in 1995 as a metallurgist and
has essentially worked in research and development, first as a
research engineer dealing with corrosion problems, and then
became a project manager in the field of materials behav-
ior for upstream oil and gas applications. Longaygue’s main
domain of expertise is the materials behavior and degrada-
tion in oilfield conditions as well as remediation and monitoring
techniques. He holds an MS degree in engineering in mate-
rials science from Université de Technologie de Compiègne
(UTC), with a specialization in Structural Metallurgy, and a PhD
in Materials Science and Engineering from Institut National
Polytechnique de Grenoble (INPG).
95