Rio Oil & Gas Expo and Conference 2020

ISSN 2525-7579

Conference Proceedings homepage: https://biblioteca.ibp.org.br/riooilegas/en/

Technical Paper

Influence of fluid loss additive on the

characteristics of oil well cement slurries for pre-
salt layer
Bruna Luiza Ferreira Brito 1

Camila Aparecida Abelha Rocha 2

Iolanda Scheibe de Siqueira 3

Vivian Karla Castelo Branco Louback Machado Balthar 4

Caroline Santana Rangel 5

Romildo Dias Toledo Filho 6

Robert Santos 7
Cristina Aiex Simão 8.
1. UNIVERSIDADE FEDERAL DO RIO DE JANEIRO - UFRJ, ENGENHARIA CIVIL, . RIO DE JANEIRO - RJ - BRASIL, brunaluizafer@coc.ufrj.br
2. UNIVERSIDADE FEDERAL FLUMINENSE - UFF / UFRJ (BOLSISTA DO CNPQ - BRASIL, 154343/2018-8), ENGENHARIA CIVIL, . NITEROI / RIO DE JANEIRO - RJ -
BRASIL, camilaabelha@id.uff.br
3. UNIVERSIDADE FEDERAL DO RIO DE JANEIRO - UFRJ, ENGENHARIA CIVIL, . RIO DE JANEIRO - RJ - BRASIL, iolanda@coc.ufrj.br
4. UNIVERSIDADE FEDERAL DO RIO DE JANEIRO - UFRJ, FACULDADE DE ARQUITETURA E URBANISMO, . RIO DE JANEIRO - RJ - BRASIL, vivian@coc.ufrj.br
5. UNIVERSIDADE FEDERAL DO RIO DE JANEIRO - UFRJ, ENGENHARIA CIVIL, . RIO DE JANEIRO - RJ - BRASIL, carolrangel@poli.ufrj.br
6. UNIVERSIDADE FEDERAL DO RIO DE JANEIRO - UFRJ, ENGENHARIA CIVIL, . RIO DE JANEIRO - RJ - BRASIL, romildo@coc.ufrj.br
7. PETROLEO BRASILEIRO SA - PETROBRAS, CIMENTAçãO, . RIO DE JANEIRO - RJ - BRASIL, rlucianls@gmail.com
8. PETROLEO BRASILEIRO SA - PETROBRAS, CIMENTAçãO, . RIO DE JANEIRO - RJ - BRASIL, caies@petrobras.com.br

Abstract

Fluid loss-control agents have been added to well cement slurries for decades, and the industry has long recognized that
they can significantly improve the quality of cement jobs. For cementation in saline areas, such as the Brazilian pre-salt
layer, it is recommended to use cement systems containing salt, to reduce the dissolution of saline rock and the
consequent incorporation of salt in the slurry. However, not too much is known about the long-term behavior and saline
rock dissolution from pastes containing fluid-loss additive. In this way, this article compares two commercial saline paste
systems: one without filtrate control additive and one containing. The evaluated properties were autogenous shrinkage,
creep, thermal expansion and diffusivity, mechanical properties, and salt dissolution, beyond the typical properties, such
as fluid loss, rheology, free-fluid and static sedimentation. The results showed that the slurries have different mechanical,
rheological and creep behavior. However, in the tests of free-fluid, static sedimentation, shrinkage and thermal properties,
the slurries showed similar results. In the filtrate and saline dissolution tests, the saline slurry with fluid loss additive
showed a lesser change in rheological properties due to saline dissolution and a significant decrease in the fluid loss of
filtrate.
Keywords: fluid-loss additive. oil well cement slurry. salt dissolution. mechanical properties. thermal properties

Received: February 28, 2020 | Accepted: Jun 06, 2020 | Available online: Dec 01, 2020
Article Code: 122
Cite as: Rio Oil & Gas Expo and Conference, Rio de Janeiro, RJ, Brazil, 2020 (20)
DOI: https://doi.org/10.48072/2525-7579.rog.2020.122

© Copyright 2020. Brazilian Petroleum, Gas and Biofuels Institute - IBP. This Technical Paper was prepared for presentation at the Rio Oil & Gas Expo and Conference 2020, held between
21 and 24 of September 2020, in Rio de Janeiro. This Technical Paper was selected for presentation by the Technical Committee of the event according to the information contained in the final
paper submitted by the author(s).The organizers are not supposed to translate or correct the submitted papers. The material as it is presented, does not necessarily represent Brazilian Petroleum,
Gas and Biofuels Institute’ opinion, or that of its Members or Representatives. Authors consent to the publication of this Technical Paper in the Rio Oil & Gas Expo and Conference 2020
Proceedings.
1. Introduction

During cementation, one of the factors to be controlled is the fluid loss of the slurry for
formation in static or dynamic condition. Therefore, to reduce the rate of fluid loss, additives known
as fluid-loss additives (FLAs) are generally included in the slurry formulation. It helps to control the
leakage of the aqueous phase of a cement system through the rock formations with high permeability
(Nelson & Guillot, 2006; Taiwo A., Joel, O. F., & Kazeem, A. A., 2011). FLAs decrease the filtration
speed by decreasing the cake filter permeability and/or by increasing the aqueous phase viscosity.
The fluid loss leads to slurry dehydration, premature development of mechanical strength, changes in
the physical properties and dissolution of the saline rock formation, in the case of salt reservoir
(Nelson & Guillot, 2006).
API fluid loss values on neat cement slurries (without additive) lie well above 1000 mL. Often,
values below 200 mL are usually preferred. To achieve these values, FLAs must be added (Liska,
Wilson & Bensted, 2019). However, FLAs is one of the most expensive material in the formulation
of oil well cement slurries. FLAs most used by service companies are cellulose-derived polymers. In
the 1950s, carboxymethyl hydroxyethyl cellulose was introduced for fluid loss control first in water-
based drilling fluids and later in oil well cement slurries (Bülichen & Plank, 2011). The most accepted
theories for the polymeric effect in filtrate control include polymeric junction on the particle surface
and the extent of the polymer in the pore space, through which the filtrate must pass.
Due to its extensive use in cement slurries, including for cementation in salt zones, it is
necessary to know the impact of FLAs on properties of long-term beyond fresh state of saline cement
slurries. Therefore, this work aims to study the influence of the fluid-loss additive on the autogenous
shrinkage, creep, thermal expansion and diffusivity, mechanical properties and salt dissolution,
beyond the typical properties API RP 10B (2013) in a cement slurry.

2. Materials

Materials used in this research were: Portland cement CPP class G with high sulfate resistance;
crystalline silica flour with 90% of the particles smaller than 44 µm; deionized water; chloride brine
(36% NaCl concentration); defoamer additive based on polypropylene glycol, particulate
hydrophobic silica, and an aliphatic hydro carbon; Retarder additive based on modified lignosulfonate
with a slight dispersing effect; cement additive designed to help increase slurry stability and control
free water based on a colloidal dispersion of amorphous silica with very high surface area; and fluid-
loss additive.

3. Methodology

3.1. Slurry design

Two commercial cement slurries were analyzed. The first containing 15% NaCl BWOW (by
weight of water), the most common concentration in slurry for cementation in salt zones (Hunter,
Tahmourpour & Faul, 2010; Simão et al., 2012), 35% silica flour BWOC (by weight of cement),
antifoam and retarder, named REF. The second, named FLC, was include fluid-loss and cement
additive, both with the objective of reduce the filtrate. The amount of water and other additives on
the FLC was adjusted to fulfill the API parameters. The amount of retarder was dosed so that the
slurry reached 500 psi of compressive strength measured by ultrasonic cement analyzer (UCA) in less
than 4 hours. After adjusting, water-cement ratio for cement slurries, considering the water present in
additives, were 0.44 for REF and 0.54 for FLC. The mix designs of the slurries are given in Table 1.
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Influence of fluid-loss additive on the characteristics of oil well cement slurries for pre-salt layer

Table 1 - Composition (600ml) and density of cement slurries REF and FLC.
Cement Silica Deionized Chloride Antifoam Retardant Fluid- Cement Theorical density
(g) flour (g) water (g) brine (g) (g) (g) loss (g) additive (g) (lb/gal – g/cm³)
REF 616.7 222.2 168.1 160.7 1.48 4.65 - - 16.6 – 1.99
FLC 552.2 208.5 175.7 167.4 1.32 3.65 13.2 2.7 15.9 – 1.91
Source: produced by the author.

3.2. Preparation and conditioning of slurry

Cement and silica were homogenized and dumped on liquid additives, NaCl solution and water.
Slurries were produced according API RP 10B (2013). When the volume of slurry needed was greater
than 600 ml, the rotation speed of the mixer was fixed, and the mixing time was varied to keep the
same mixing energy in all slurries (Vorkinn & Sanders, 1993). The mixing energy used was 5.9 kJ/kg.
Slurry conditioning was performed according to the procedure P6 (Procelab, 2014). For the
tests at 27 °C, the slurry was conditioned in atmospheric consistometer for 30 min. For the tests at
60 °C, the slurry started conditioned at 27 °C, and increase the temperature in a rate of 1.1 °C/min;
after reaching 60 °C, the slurry was kept homogenizing for another 15 min at this temperature.
Note that, for simplification, temperature rates used for carrying out the tests and conditioning
of the slurries in this study do not include cooling and heating profiles typical of deepwater cementing
of pre-salt scenario (Gannam et al. 2016).

3.3. Rheology, free-fluid, static sedimentation

Rheological properties and free-fluid were determined at 27 °C and 60 °C in a slurry previously

conditioned at same temperature. Rheological test was performed in viscometer according API RP
10B (2013). In free-fluid test, slurry was poured in the cylinder, and after 2 hours on a static surface,
the volume of exuded fluid was measured (Procelab, 2014).
Static sedimentation test, slurry was conditioned at 60°C, and then transferred in two layers to
cylindrical molds, shaking each layer for 45 s and cured in a 60°C bath for 24 hours. After, tubes have
cooled, and the retraction volume of the slurry was measured. The cylinders were demolded, divided
into 4 equal parts, and then the density of each part was determined. Density difference between the
top and bottom part were calculated (Procelab, 2014).

3.4. Fluid loss

The fluid loss was performed at 60°C in conditioned slurry at this temperature. During the fluid-
loss test, the slurry was subjected to an axial pressure of 1000 psi, maintaining the test temperature.
The fluid was collected for up to 30 min or until no more liquid came out. Filter cake was measured,
also checking its consistency.

3.5. Salt core dissolution test

The salt dissolution test measured change in the mass of halite (NaCl) core in dynamic contact
with a cement slurry and its variation in rheology. Dissolution test was performed according
procedures describe for Simão et al (2012). The times evaluated was 0, 20, 40, 60 min.
Constituents of slurry were weighed to obtain 5 volumes of 600 ml for each formulation. Before
starting the test dissolution (0 min), and in times of 20, 40 and 60 min of dissolution, 200 ml of slurry
was removed to perform the rheology test. For the rheology blank test, 400 ml of slurry was separated
in 0 min, homogenized atmospheric consistometer at a temperature of 60 °C during the entire
dissolution test time and finally having the rheological properties measured.

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 Bruna Brito, Camila Rocha, Iolanda Siqueira, Vivian Balthar, Caroline Rangel, Romildo Toledo Filho, Robert Santos,
Cristina Simão

3.6. Compressive strength and elasticity modulus

Cement slurry was poured in two layers in 50 mm x 100 mm molds. Each layer was
homogenized, with the aid of a glass stick, in circular movements for 45 s, to eliminate air bubbles.
The slurries were cured in a humid chamber at 27°C for 24 hours. After this, the specimens were
demolded, vacuum packed and immersed in a bath at 27°C warmed up to 60°C in 90 min and kept at
this temperature for 7 days. After, specimens were cooled slowly, and their surfaces were flattened.
Compressive strength tests were performed a mechanical press with a 200 kN load cell. The
test was performed on four specimens for each formulation at a rate displacement of 0.025 mm/min.
Axial displacements were measured using two electric displacement transducers (LVDT). Secant
elastic modulus (E) was determined according ASTM C 469 (2014). The difference between results
were analyzed statistically by Analysis of Variance (ANOVA) to a confidence interval of 95%.

3.7. Autogenous shrinkage

Autogenous shrinkage test was performed on three prismatic specimens for each formulation,
with a cross section of 75 mm x 75 mm and a length of 285 mm. The test was carried out at
temperature of 23.0 ± 2.0 °C and relative humidity of 50 ± 4%. The first phase of the test was molds
preparing by positioning plastic plates on all their faces, to reduce the friction between the specimen
and the mold, and fixing a pin at each end, to allow length measurements. The specimens were
produced according 3.6. After, the molds were sealed to avoid humidity changes and drying
shrinkage.
Specimen longitudinal dimension measurements on external faces pins were started when the
temperature of the slurry started to rise (that is, the cement hydration reactions started). After four
days, the specimens were demolded. Each prism was sealed one more time and positioned above two
rollers on a flat surface, where they remained for the rest of the test period. Tests were conducted for
a period of 60 days. The total autogenous shrinkage was calculated according ASTM C490 (2017).
ANOVA also was performed.

3.8. Creep

Creep in compression were performed on cylindrical specimens of 100 mm in diameter and 200
mm in height, at the age of 9 days until 60 days. Samples were prepared according 3.6 with a
thermocouple and an extensometer inside. After cure, the specimens were sealed and positioned on
the equipment. For each slurry, two specimens were submitted to the loading process until the level
corresponded to 40% of the rupture stress, obtained by compressive strength test, in four specimens
with the same dimensions. In addition, the deformation of two control specimens per slurry was
measured, whose function was to determine the load-free deformations.
The basic creep was determined (Equation 1) by the difference between the total deformation
(obtained with loading) and the autogenous deformation (obtained by the readings of the control
specimens) and thermal deformation (obtained with thermometers inside the specimens). The division
of basic creep by the applied stress provided the specific creep value (Equation 2). ANOVA also was
performed.

 f   t   aut   T (1) (2)

Where: f = creep deformation (); t = total deformation (); aut = autogenous deformation
(); T = thermal deformation ();  = applied loading stress (MPa).

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Influence of fluid-loss additive on the characteristics of oil well cement slurries for pre-salt layer

3.9. Thermal Expansion

Thermal expansion tests were carried out on three prismatic specimens with 75 mm edges and
285 mm length according to ABNT NBR 12815 (2012). The samples were prepared and cured
according 3.6. Sealed specimens were completed coupling two copper plates on two opposite lateral
faces, with 5 cm from the center of the specimen to its edges. The specimens were submitted to
variable strain cycles due to exposure to different temperatures, 23ºC ± 2ºC, 38ºC ± 2ºC e 4ºC ± 2ºC.
The test started with the specimens in the chamber of 23ºC ± 2ºC. After the specimens were
transferred to the chamber of 38ºC ± 2ºC, 23ºC ± 2ºC, 4ºC ± 2ºC, and then, returned to the chamber
of 23ºC ± 2ºC. The transfers of the prisms between the chambers only occurred after their temperature
stabilized, which corresponded to daily displacement measurements for at least 48 hours. A minimum
of three measurements of displacements to each sample per day was done with the Tensotast
Huggenberger. The linear thermal expansion coefficient of each slurry was determined by the
Equation 3. ANOVA was also performed.

(3)

Where:  = linear thermal expansion coefficient (× 10-6/oC); q = deformation measurement in

the chamber of 23ºC ± 2ºC (m/m); f = deformation measurement in the test chamber (m/m); Tq =
temperature of the chamber to stabilization (oC); Tf = temperature of the test chamber (oC).

3.10. Thermal Diffusivity

Thermal diffusivity tests were performed on two cylinders with 200 mm diameter and 400 mm
length according to ABNT NBR 12818 (2012). The molds have an internal hole with 10 ± 1 mm
diameter until half of its height. Each mold was filled by the slurry in three layers, with the filling of
each layer followed by its homogenization on a vibrating table. The specimens were curing according
3.6. After to 9 days of cure, the specimens were sealed. A PVC tube was fixed in the internal hole.
The test was carried out at three different temperatures (20ºC ± 2ºC, 40ºC ± 2ºC and 60ºC ± 2ºC),
with the aid of thermal baths. The temperatures were monitored by a thermocouple, fixed to the
central hole of the specimens, and connected to a Data Logger, which performed a data recording
every 5 min. Subsequently, each cylinder was cooled in an ice water bath maintained in a chamber
with a controlled temperature of 4ºC ± 2ºC. In this way, the test provides the cooling curve of the
specimen from each initial test temperature up to the bath stabilization temperature of 4ºC
(ANDRADE, 1997). The thermal diffusivity (m2/h) were obtained according ABNT NBR 12818
(2012). ANOVA was also performed.

4. Results and discussion

4.1. Rheology, free-fluid, Static sedimentation

The flow curves of the slurries at 27°C and 60°C are shown in Figure 1. In the curves the
ascending and descending readings are present. REF slurry presented a lower descending curve at
27°C than the ascending curve, the difference between the readings in some points was greater than
12 Pa. The REF curves are adapted to the Herschel-Bulkley model, so the REF yield stress and plastic
viscosity were calculated from this model.
Flow curves obtained for FLC slurry at 27°C and 60°C did not show difference between the
upward and downward readings. The FLC curves behave like a Bingham fluid, so the FLC yield

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 Bruna Brito, Camila Rocha, Iolanda Siqueira, Vivian Balthar, Caroline Rangel, Romildo Toledo Filho, Robert Santos,
Cristina Simão

stress and plastic viscosity were calculated according to this model. Table 2 shows the rheological
parameters and initial and final gels of the slurries.

Figure 1 - Flow curves at 27°C (a) and at 60°C (b).

80 150
FLC FLC
REF REF
120
60
Shear Stress (Pa)

Shear stress (Pa)

90
40
60

20
30

0 0
0 100 200 300 400 500 0 100 200 300 400 500
Shear rate (1/s) Shear rate (1/s)

(a) (b)
Source: produced by the author.

Table 2 - Rheological parameters and free- fluid of REF and FLC slurries at 27°C and 60°C.
Temperature
Yield stress Plastic viscosity Initial gel Final gel Free-fluid
(°C)(Pa) (cP) (Pa) (Pa) (%)
REF 29.2 208.4 14.0 19.9 0.36
27
FLC 11.8 132.4 7.4 14.6 0.44
REF 19.9 15.0 8.2 14.3 1.02
60
FLC 14.6 7.9 3.1 4.9 1.72*
Source: produced by the author.

The temperature changed the yield stress and the plastic viscosity more considerably, but the
initial and final gel also had their values reduced. The decrease in the rheological parameters of neat
cement slurries with the increase in temperature was already expected, as this thinning is common for
most slurries (Ravi & Sutton, 1990). The same was observed for the FLC, as well as in the work of
Abbas, Irawan, Kumar & Elraya (2013).
The FLC slurry is less viscous than the reference and has a lower yield stress. It is not possible
to distinguish whether this fact occurred using the filtrate controlling additive or by the increase of
the water-cement ratio in the FLC slurry. However, it can be concluded that the filtrate control
mechanism of this slurry does not occur due to an increase in the viscosity of the aqueous phase, but
probably due to a decrease in the porosity of the cake.
As can be seen in Table 2, in the free-fluid test at 27°C, there was no difference in the volume
percentage of the supernatant phase without cementing characteristic, even FLC slurry has a higher
w/c ratio. At a temperature of 60°C, there was a difference, but the heated free fluid assay for the
FLC slurry cannot be considered (*), because in two hours the slurry was still very fluid, and cannot
guarantee that the free fluid did not contain slurry.
The results of the static sedimentation test are shown in Table 3. The cement slurries showed
variations in density between the bottom and top sections ( ) equal. The difference values were less
than 0.5 lb/gal and the lowering of the top of the slurry less than 5 mm. Although slurry with FLA
has a higher w/c ratio, it did not show greater sedimentation than the REF slurry, and both slurries
can be considered stable by the static sedimentation test. Observing the experimental values of
density, they are slightly higher, about 2%, than the theoretical ones.

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Influence of fluid-loss additive on the characteristics of oil well cement slurries for pre-salt layer

Table 3 – Values of density and lowering of sedimentation essay.

IV
I (top) II III (IV-I) Lowering Average density
(bottom)
(lb/gal) (lb/gal) (lb/gal) (lb/gal) (mm) (lb/gal – g/cm³)
(lb/gal)
REF 16.80 16.95 16.97 17.08 0.28 2 16.95 – 2.03
FLC 16.06 16.17 16.15 16.34 0.28 2.6 16.18 – 1.94
Source: produced by the author.

4.2. Fluid loss

The results of filtrate volume (Q30) and cake height are shown in Table 4. The Q30 of the REF
slurry was ten times higher than the FLC slurry, in an average of 20 s REF had already lost its entire
liquid phase. The final volume of filtrate and the height of cake of the slurries was practically the
same, the difference was the time in which the slurry took to dehydrate. The value found for the FLC
slurry is classified as cement slurry with regular filtrate loss (Freitas, 2010) and follows the
requirements of Petrobras standards that require that slurry for isolation of permeable regions have
Q30 between 80 and 120. Thus, as expected, the FLAs was highly effective in reducing the filtrate,
even with a much higher w/c ratio than the reference slurry.

Table 4 - Values of filtrate volume, in their respective time, height of plaster and Q30.

Volume (mL) Time (min) Q30 Cake filter (mm)

REF 57 0.33 1082 43
FLC 59.5 30 119 45
Source: produced by the author.

4.3. Salt core dissolution test

The results of the salt dissolution test are shown in Table 5. Figure 2 and Figure 3 show the
dissolution of the saline core samples after immersion in REF and FLC slurries, respectively. Both
samples suffered a reduction in mass and dimensions, thus indicating that the salt cores were
dissolved by contact with cement slurry and its incorporated salt.

Table 5 – Values of mass and dimensions of salt cores during the test.

REF FLC
Time Mass (g) Volume (cm³) Mass (g) Volume (cm³)
0 min 857.3 157.4 859.3 157.7
20 min 821.0 155.2 812.2 156.6
40 min 781.8 148.7 787.4 152.8
60 min 759.5 147.5 760.9 148.5
(0 – 60 min) (%) 11.4 6.3 11.5 5.9
Source: produced by the author.

The results showed that there was no difference between the slurries in the reduction of mass
and volume of saline rock samples after immersion and agitation. The dissolution of the salt cores
results was higher than those obtained in Simão et al. (2012) research, who studied the saline
dissolution of slurries with different concentrations of NaCl. This can be associated with different
formulations and rheological properties of the slurries in both researches.
Through the rheology test in slurry after dissolution test it was observed that there was a change
in the characteristics of the slurry due to salt incorporation and evolution of hydration reactions, as
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 Bruna Brito, Camila Rocha, Iolanda Siqueira, Vivian Balthar, Caroline Rangel, Romildo Toledo Filho, Robert Santos,
Cristina Simão

can be observed in Table 6. The rheological properties were, in general, increasing over time and core
dissolving. This effect was more pronounced for the reference slurry.

Figure 2 – Salt core immersed for 0, 20, 40 e 60 min in REF slurry.

Source: produced by the author.

Figure 3 - Salt core immersed for 0, 20, 40 e 60 min in FLC slurry.

Source: produced by the author.

Table 6 - Values of yield stress and plastic viscosity during salt dissolution test.
REF FLC
Time
Yield stress (Pa) Viscosity (cp) Yield stress (Pa) Viscosity (cp)
0 min 20.7 180.7 4.5 102.6
20 min 22.0 188.6 6.5 90.7
40 min 13.8 276.4 5.1 97.1
60 min 25.1 328.2 4.7 142.6
Blank 18.8 157.9 4.7 86.2
(%)
(60min – blank) 33.3 107.9 -0.4 65.3
Source: produced by the author.

4.4. Compressive strength and modulus of elasticity

The mean values and coefficient of variation of compressive strength (fc), axial deformation
(e) and modulus of elasticity (E) are shown in Table 7.

Table 7 – Mechanical properties of slurries and their respective coefficients of variation (CV).
fc CV fc CV  CV E CV
(MPa) (%) (psi) (%)  (%) (GPa) (%)
REF 48.02 1.64 6964.4 1.64 6842 4.30 14.32 6.72
FLC 32.57 1.84 4724.2 1.84 6485 5.05 11.04 2.20
Source: produced by the author.
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 Influence of fluid-loss additive on the characteristics of oil well cement slurries for pre-salt layer

Statistically significant differences in compressive strength were found between slurries. The
FLC showed lower compressive strength and modulus of elasticity than REF. The reference samples
also had higher deformation until their failure. This reduction in compressive strength and modulus
of elasticity to FLA occurred mainly due to the higher w/c ratio of this slurry.

4.5. Autogenous shrinkage

The medium curves of autogenous shrinkage versus time of cement slurries are shown in Figure 4
and the average values results and their respective standard deviations in some test ages are shown in
Table 8.

Figure 4 – Autogenous shrinkage curves of REF and FLC Table 8 - Autogenous shrinkage at different ages.
slurries.
400 Autogenous Shrinkage (Standard Deviation) ()
REF
200 FLC Age (days) 0.5 1 3 7
Autogenous Shrinkage ()

0 20.2 -30.9 -21.3 -135.3

0 10 20 30 40 50 60 70 REF
-200
(36.0) (106.7) (104.3) (74.3)
116.1 198.3 134.5 -15.0
-400 FLC
(68.2) (81.3) (79.1) (95.0)
-600 Age (days) 14 21 30 60
-265.5 -361.9 -487.1 -808.4
-800 REF
(87.8) (89.7) (84.5) (83.2)
-1000 -198.3 -280.4 -466.6 -779.9
Age (days) FLC
(88.4) (93.9) (100.0) (135.9)
Source: produced by the author. Source: produced by the author.

The results indicate that, in the first hours of testing, the both evaluated slurries showed
deformations by expansion, with the highest result achieved by FLC slurry at 15 hours of test
(Specimen 2 - 322.6 ). From the statistical analysis of results, it is possible to conclude that, after
24 hours of testing, REF and FLC presented results of autogenous shrinkage equal at each age
evaluated. As shown in Table 8, at 60 days age, the REF and FLC reached a maximum values of
autogenous shrinkage, respectively equal to 808.7  and 779.9 , considered equal by statistical
analysis. Although the FLC slurry has a higher w/c ratio, it presented an autogenous shrinkage curve
like the REF.

4.6. Creep

The typical creep curves of REF and FLC are shown in Figure 5. The results are presented
considering the elastic deformations of the slurry together with the deformations by specific creep.
The average values of elastic modulus and maximum specific creep are presented in Table 9, for both
the loading phase and the unloading phase. The elastic modulus is noted as Ecreep. Specific creep was
obtained for the age of 97 days, while residual creep was determined at the age of 180 days.
When comparing the results of specific creep in the loading phase of the FLC slurry with the
REF slurry, the slurry FLC had an increase of 74.8% in this property. In the unloading phase, the
irreversible creep of the FLC slurry was 79.0% higher than the value achieved by the REF slurry.
Regarding the elastic modulus, when comparing the results of this property between REF and FLC
slurries, it is possible to observe that the FLC slurry presented reductions, equal to 8.8% in the loading
phase and 19.2% in the unloading phase. Lastly, the residual creep of the FLC slurry was 79.0%
higher than the value obtained by the REF slurry. The change in these properties probably occurred
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 Bruna Brito, Camila Rocha, Iolanda Siqueira, Vivian Balthar, Caroline Rangel, Romildo Toledo Filho, Robert Santos,
Cristina Simão

because the higher w/c ratio of the FLC slurry, which presented greater porosity and consequently
greater mobility of water in its microstructure, favoring the creeping.

Figure 5 – Creep curves of REF and FLC slurries. Table 9 - Elastic modulus and creep results for
300
loading and unloading phases.
Elastic Strain plus Creep (x10 /MPa)

Age: 9 days REF

250 FLC
Loading Phase
-6

200 Slurry Ecreep (GPa) Specific Creep (x 10-6/MPa)

150 REF 13.5 102.0
FLC 12.3 178.3
100
Unloading Phase
50
Slurry Ecreep (GPa) Residual Creep (x 10-6/MPa)
0 REF 13.0 70.9
0 50 100 150 200
Time (days) FLC 10.5 126.9
Source: produced by the author. Source: produced by the author.

4.7. Thermal Expansion

The linear thermal expansion coefficients () and the averages specimens temperature variation
(TM) at each temperature range evaluated, as well as the average final thermal expansion coefficients
(F) and its respective standard deviation (SD) are shown in Table 10. Results indicate that the fluid
loss additive did not significantly promote variation on this property.

Table 10 – Thermal expansion results.

Temperature
~23°C to~38°C ~38°C to ~23°C ~23°C to ~4°C ~4°C to ~23°C FSD
Cycles
TM  TM  TM  TM 
Slurry (×10-6/°C)
(°C) (×10-6/°C) (°C) (×10-6/°C) (°C) (×10-6/°C) (°C) (×10-6/°C)
REF +14.9 14.4 -15,6 15.8 -19.2 12.3 +20.3 22.0 16.1 – 0.6
FLC +16.9 17.3 -16,8 17.6 -19.8 11.1 +20.1 20.5 16.6 – 1.2
Source: produced by the author.

The results achieved by REF and FLC are according with Andrade (1997), that reports a
variation of the linear thermal expansion coefficient of cement slurries between 11.0 × 10-6/oC e 16.0
× 10-6/oC. Other reference of the thermal property was obtained by Balthar (2010), that studied
lightweight high development slurries and achieved results of the linear thermal expansion coefficient
between 16.6 × 10-6/oC e 19.8 × 10-6/oC.

4.8. Thermal Diffusivity

The cooling typical curves of diffusivity tests of REF and FLC slurries are shown in Figure 6a
(Ti = 20oC), Figure 6b (Ti = 40oC) and Figure 6c (Ti = 60oC). The Tn/Ti ratio corresponds to the
relationships between the temperatures of the specimen during the test, in each interval of 5 min (Tn)
and starting from the initial specimen temperature (Ti). The average thermal diffusivities of the
slurries at each evaluated temperature are shown in Table 11.
Cooling curves in all temperatures evaluated (20oC, 40oC e 60oC) of REF and FLC slurries are
presented in Figure 6 and thermal diffusivity are presented in Table 11. There were no significant

Rio Oil & Gas Conference, 2020. | ISSN 2525-7579 9

Influence of fluid-loss additive on the characteristics of oil well cement slurries for pre-salt layer

differences between the results obtained for both slurries, although the FLC slurry has a higher w/c
ratio and probably has greater porosity.

Figure 6 – Cooling curves of diffusivity tests: (a) Ti = 20oC; (b) Ti = 40oC; (c) Ti = 60oC
1.2 o
1.2 o
1.2 o
Temperature: 20 C REF Temperature: 40 C REF Temperature: 60 C REF
1.0 FLC 1.0 FLC 1.0 FLC

0.8 0.8 0.8

Tn/Ti ( C)

Tn/Ti ( C)
Tn/Ti ( C)

o
o

0.6 0.6 0.6

0.4 0.4 0.4

0.2 0.2 0.2

0.0 0.0 0.0

0 50 100 150 200 250 0 50 100 150 200 250 0 50 100 150 200 250
Age (minutes) Age (minutes) Age (minutes)
(a) (b) (c)
Source: produced by the author.

Results of REF and FLC slurries are in accordance with values of the thermal diffusivity
indicated by Andrade (1997), which vary between 0.025 m2/day and 0.039 m2/day for conventional
cement slurries (w/c ratios between 0.3 and 0.8).

Table 11 – Thermal diffusivity results.

Thermal Diffusivity (m2/day)

Slurry
T = 20oC T = 40oC T = 60oC
REF 0.0337 0.0326 0.0333
FLC 0.0327 0.0318 0.0296
Source: produced by the author.

5. Conclusions

 Regarding the rheological properties, on both temperatures 27°C and 60°C, slurry with
FLAs (FLC) presented lower values of yield stress and plastic viscosity then the reference
slurry (REF) mainly due the highest w/c ratio of FLC slurry.
 Although FLC has a higher w/c ratio and different rheological properties comparing with
REF slurry, these slurries did not present significant difference in free water and static
sedimentation.
 As expected, the FLAs was highly effective in reducing the filtrate, even with a much
higher w/c ratio and lower plastic viscosity than the REF.
 FLC did note promote difference in dissolution of the saline core, but promoted change in
slurry rheology by the salt incorporated.
 Compressive strength was significantly lower, and creep was significantly higher in the
FLC slurry, mainly due the high porosity promoted by the high w/c of this slurry.
 There was no significant difference in autogenous shrinkage, thermal expansion, and
thermal diffusivity in the studied slurries.

6. Acknowledgments

The authors acknowledge Petrobras for sponsoring this project.

Rio Oil & Gas Expo and Conference, 2020. | ISSN 2525-7579 10
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