Energy Geoscience 2 (2021) 181e188

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Energy Geoscience
journal homepage: www.keaipublishing.com/en/journals/energy-geoscience

Quartz dissolution in a single phase-high pH Berea sandstone via

alkaline injection
Abdullah Musa Ali*, Mohammed Yerima Kwaya, Abubakar Mijinyawa
Department of Geology, Bayero University Kano (BUK), Kano, Nigeria

a r t i c l e i n f o a b s t r a c t

Article history: A common assertion is that alkaline solution aids oil mobilization by generating in situ soap, or by
Received 22 September 2020 lowering interfacial tension (IFT) to ultra-low values in synergy with surfactants. This study takes a
Received in revised form different approach that involves the alkaline dissolution of detrital quartz grains of sandstone reservoirs
23 February 2021
to create pathways for oil migration and accumulation. Quartz dissolution via alkaline injection will
Accepted 4 March 2021
result in changes in permeability and porosity. This study performed high-pH core flooding on Berea
sandstones using core displacement equipment. Silica molybdate spectrophotometry was applied to
Keywords:
measure the amount of dissolved silica. Inlet and confining pressure variations were also observed. The
Alkaline injection
Core flooding
molar concentration of NaOH varied at 0.5 M and 1.0 M. The results show higher initial silica dissolution
Dissolved silica for 0.5 M NaOH (˃200mg/L) compared to 1.0 M NaOH (20 mg/L), which can be attributed to the presence
Quartz of pre-existing dissolved silica and precipitates in the system prior to the first injection phase. None-
Petroleum recovery theless, a steady quartz dissolution rate of 0.4 mg/L/hr for 20 h was only achieved at 1.0 M. Conversely, an
abrupt drop in quartz dissolution to below 0 mg/L was recorded for 0.5 M NaOH after 3 h of dissolution.
At higher molar concentration of injected alkaline solution, both confining and inlet pressures increased
from 8 and 5 bars to 12 and 11 bars as a result of the increased secondary phase of (hydr)oxides or
precipitates in the pores. Thus, it can be inferred that the effect of alkaline solution on quartz dissolution
is strongly dependent on molar concentration.
© 2021 Sinopec Petroleum Exploration and Production Research Institute. Production and hosting by
Elsevier B.V. on behalf of KeAi. This is an open access article under the CC BY-NC-ND license (http://creati
vecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction such techniques is alkaline flooding, which involves the injection of

With the continuous decline in petroleum resources and
increased global energy demand, the oil and gas industry needs to
proffer innovative and economical approaches to residual oil phase
extraction. However, issues such as low porosity and low perme-
ability of reservoirs, as well as high viscosity, high wettability and
high interfacial tension (IFT) of residual oil phase are constraints
that hinder the recovery of petroleum. Therefore, developing
effective recovery techniques to resolve these challenges will help
enhance the recovery of oil from reservoirs (Sun et al., 2015). One of
* Corresponding author.
E-mail address: amali.geo@buk.edu.ng (A.M. Ali).
Production and Hosting by Elsevier on behalf of KeAi
alkaline chemicals such as sodium hydroxide (NaOH), or sodium
carbonate during polymer flooding or water flooding operations. A
common assertion is that alkaline solution aids oil mobilization by
generating in situ soap or surfactant or emulsifiers at the oil/brine
interface (Hornof et al., 2000; Li et al., 2005), or by lowering IFT to
ultra-low values in combined effect with surfactants (Liu et al.,
2006). The alkaline chemicals react with the oil to form surfac-
tants, which in turn reduce the IFT between oil and water and
initiate an increase in oil production. The alkaline solutions can also
reverse the reservoir wettability from oil-wet to water-wet state.
This study takes a different approach by exploring alkaline
dissolution of detrital quartz grains to create pathways for oil
migration and accumulation, with the aim of considerably boosting
recovery and sweep efficiency. The dissolution/leaching of labile
framework grains such as quartz and feldspar has been identified as
the most important porosity-enhancing process (Kassab et al.,
2014). Reaction of the alkaline solution with reservoir minerals
between the injection and production wells can alter porosity and

https://doi.org/10.1016/j.engeos.2021.03.001
2666-7592/© 2021 Sinopec Petroleum Exploration and Production Research Institute. Production and hosting by Elsevier B.V. on behalf of KeAi. This is an open access article
under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
A.M. Ali, M.Y. Kwaya and A. Mijinyawa Energy Geoscience 2 (2021) 181e188

permeability over the flooding path, and hence the extent of re-
covery (Bagci et al., 2000). Generating flow paths and widening
fractures in the reservoir will allow for pore throat expansion,
enhance permeability and porosity, which in turn improve oil
mobility.
Changes in pH, alkaline consumption and aqueous chemistry
have been predicted from alkaline injection in reservoirs
(Kazempour et al., 2012). Dissolution or precipitation of silica
minerals provides information on the change of porosity, perme-
ability, and reaction surface area of siliciclastics. The governing
equations for the dissolution and precipitation rate of the ith silica
mineral (Takeno et al., 2000) are given as follows. The left side of Eq.
(1) is positive for dissolution and negative for precipitation.

 
vmH4 SiO4 A Q
¼ kþi i 1  (1)
vt M Ki

Q ¼ mH4 SiO4 (2)

where m is the molality of aqueous silica species, t is the time, kþi is

the dissolution rate constant of ith silica mineral, Ai is the reaction
surface area of ith silica mineral, M is the mass of solution, and Ki is
the solubility constant of ith silica mineral.
The quartz grains grow or dissolve, relating fluid chemistry to
permeability changes. In a subgrid-scale grain model based on a
spherical close pack of grains, dissolution or overgrowth occurs on
the grain faces exposed to the fluid with a local spherical close pack
Fig. 1. Schematic illustration of NaOH interaction with quartz in sandstone (Dove and
radius (R0). Differences in volume and surface area occluded during
Elston, 1992).
such growth or dissolution yield an effective local grain radius, RN
(slightly larger than R0, both in meter). Thus, quartz dissolution can
be explained by the rate of change of effective grain radius with 2. Methodology
time as shown in Eq. (3) (Bolton et al., 1999):
Two sets of alkaline dissolution experiments were performed:
static dissolution using the batch bottle system, and alkaline in-
vRN jection using the core displacement equipment system. The alka-
¼  V q kq A c (3)
vt line injection experiment was performed on the Berea sandstone
core as depicted in Fig. 2. The petrophysical properties of the Berea
where t denotes time (in sec), kq is a kinetic rate term (in mole *m-
2  sandstone were characterized by mercury microporosimetry. Data
*sec-1), V q is the molar volume (in m3 of quartz/mole), and Ac is on porosity, pore volume, and pore size distribution of the sand-
unity. stone were obtained utilizing the non-wetting properties of mer-
During the NaOH interaction with a-quartz in sandstone, surface cury through mercury porosimetry. The surfaces of the NaOH-
complexes are sorbed onto the quartz surface. The cation-sorbed
complexes or ligands include SiOH, SiO-, SiONa (Dove and Elston,
1992) as illustrated in Fig. 1. Several experiments have been per-
formed on quartz dissolution in alkaline (Yanina et al., 2006; Dove
and Han, 2007; Zhang and Liu, 2014; Nangia and Garrison, 2008;
Rimstidt, 2015; Ali et al., 2017). However, these studies were con-
ducted on pure quartz, with not much consideration given to ma-
trix materials (clays) and secondary minerals such as (hydr)oxides
of iron and aluminum. Hence, the effect of alkaline dissolution on
porosity, permeability and ultimately oil recovery in sandstones is
not fully elucidated. This is imperative, as Ali et al. (2020) have
shown that the energy for NaOH interactions with reservoir
sandstone was considerably higher than that of a single quartz
crystal, due to the variability between isotropic deformation of a
single crystal and anisotropic deformations of adjacent quartz
grains in sandstone. Moreover, the dynamic flow of the caustic
solution through sandstone has not been considered. Therefore,
this study presented both empirical data on quartz dissolution in
both static and dynamic (core flooding) conditions with respect to
variation in alkaline concentration, and the effect of quartz disso-
lution on oil recovery. In addition, changes in pressure condition
with quartz dissolution were also presented. Fig. 2. Berea sandstone plug (with the arrow and dotted lines illustrating fluid flow).

182
A.M. Ali, M.Y. Kwaya and A. Mijinyawa
dissolved sandstone grains were characterized using field emission
scanning electron microscopy (FESEM) attached with energy
dispersive X-ray spectroscopy (EDX).
2.1. Batch bottle system
The static dissolution experiments were performed on sand-
stone chips taken from the Berea core using the batch bottle sys-
tem, which involves the use of sealed polyethylene bottles (50 mL
each) containing the weighed sample and dissolving solvent
(NaOH). The bottles were preheated for 10 min to adjust to the
temperature of the water bath, and then immersed in a water bath
placed on a stirring hot plate. The dissolution temperature is sup-
posed to be maintained at 80e90  C under atmospheric pressure
conditions, and the rotating speed regulated at approximately
50 rpm. After 14 h of continuous dissolution, the silica content of
the solution was measured using silica molybdate spectropho-
tometry. The weights of the samples were checked intermittently
to measure changes in mass with time, as well as to observe the
development of pores. The morphological characterization of the
samples was performed using a high-resolution FESEM (Carl Zeiss
Supra 55VP; operated at 5e20 kV).
2.2. Alkaline injection using the core displacement equipment
system
Alkaline injection experiments were performed using core
displacement equipment at an injection rate of 0.1 ml per minute.
The core flooding experiment was performed using core displace-
ment equipment located at Universiti Teknologi PETRONAS (UTP),
Fig. 3. Depiction of the core flooding equipment.
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Energy Geoscience 2 (2021) 181e188
an institute of hydrocarbon recovery. The system design as depicted
in Fig. 3 consists of storage tanks (pressure vessels) that contain the
oil and brine solutions, which are connected to the inlet of the core,
the Berea sandstone core and core holder, as well as collection
tanks to receive fluids from the outlet of the core. The system is
jointly controlled by the control panel programmable logic
controller (PLC) and touch screen display. The back-pressure con-
trol system controls the pore pressure in the system as well as
provides a means to measure the rates of fluid flow in the core.
Two different NaOH concentrations were used (0.5 M and
1.0 M). The core was first saturated with brine to create imbibition,
followed by oil injection into core to form the residual hydrocarbon
phase. The volumetric ratio of oil and water was set at 40:60. It
should be noted that the focus of the injection was on porosity
increase and amount of dissolved silica through quartz dissolution,
instead of recovery. Nonetheless, the volume of displaced oil via
alkaline injection was compared to that by brine injection. The
amount of dissolved silica in the displaced fluid was measured
using silica molybdate spectrophotometry. The confining and inlet
liquid pressures were monitored in the course of the injection. The
quartz grains were examined using FESEM after injection to
determine surface morphological variations in the quartz under
dissolution. All reagents were of analytical grade and used without
further treatment. The pH of solution was monitored in all titration
and ageing experiments using a pH meter (EUTECH, Model:
Cyberscan). Dilute sodium hydroxide (NaOH) and hydrochloric acid
were used as neutralizing agents in the titration process to adjust
the pH value.
3. Results and discussion
3.1. Porosity characterization using mercury intrusion porosimetry
(MIP)
Based on the plot of cumulative pore volume vs. pore diameter
(nm) obtained from the MIP data as shown in Fig. 4, the measured
porosity of the Berea sandstone was 28.17%, with an average pore
diameter of 13.5 mm, median pore diameter of 24.1 mm and modal
pore diameter of 23.9 mm. The plot of pore size distribution shows a
Fig. 4. Cumulative pore volume vs. pore diameter (nm) showing micropores the
dominant pore type.
A.M. Ali, M.Y. Kwaya and A. Mijinyawa Energy Geoscience 2 (2021) 181e188

nearly variable pore distribution. The cumulative pore volume in-

dicates micropores are the dominant pore type in the core,
accompanied by relatively lower presence of nanopores.

3.2. Alkaline dissolution

3.2.1. Static dissolution experiment

Changes in mass (g) and dissolved silica variation were
measured with time for different NaOH concentrations (0.5 M and
1.0 M). Fig. 5 shows the cumulative amount of dissolved silica is
higher at 1.0 M NaOH (9.4 mg/L) compared to 0.5 M NaOH (˂2 mg/L).
Similarly, at 0.5 M NaOH, the weight of the Berea chip decreased by
about 0.04 g after 14-h dissolution. On the other hand, the chip
decreased by approximately 0.10 g at 1.0 M NaOH as shown in Fig. 6.
The starting pH values for the 0.5 M and 1.0 M NaOH solutions were
11 and 12, respectively. The surface of the sandstone chip was
observed pictorially before and after dissolution as seen in Fig. 6.
Surface defects in terms of dissolution etch pits (depicted as dark
hollow spots) emerge after the dissolution process as shown in
Fig. 6b and c. These pits represent the development of new pores
and mesopores transformed from nano- and micro-pores under
dissolution.

3.2.2. Alkaline injection

Upon injection of alkaline solution, 0.5 pH difference between
inlet and outlet pH was observed. This is an indication of weak pH
buffering capacity of this rock during NaOH flooding. Only small
amounts of silica were produced during this experiment, which
might have been due to the low dissolution rate of quartz in the
rock. Quartz dissolution rates were directly calculated from the
experimental data. It is imperative to note that by increasing the
molar concentration of NaOH injection, the amount of silica in the
aqueous phase varied, favourable for chemical EOR processes. At
0.5 M, the initial rate of dissolution in the first 3 h was high
(218 mg/L), which can be attributed to the removal of fines and
plastered silica. However, the dissolution declined drastically af-
terwards to 0 mg/L in the following hours, as shown in Fig. 7a. With
the increase in molar concentration of NaOH to 1.0 M, the con-
centration of dissolved silica was approximately 20 mg/L in the first
3 h, until a steady state of dissolution was achieved at the rate of
0.4 mg/L/hr as seen in Fig. 7b. Therefore, the initial rate of silica
dissolution is dependent on in situ mineralogy (i.e., quartz ligands,
silica flakes, and dissolved silica), rather than concentration of the
alkali. However, steady rate of silica dissolution in reservoir in-
creases with the alkaline concentration on the rise. At 0.5 M, steady
Fig. 6. (a) Plot of mass loss against time for sample dissolved in 1.0 M NaOH; (b)
Sandstone chip before dissolution; (c) Sandstone chip after dissolution showing the
formation of surface defects (etch pits).
state dissolution was not attained; or rather the amount of dis-
solved silica was erratic before dropping to zero (0). In contrast, a
steady silica dissolution rate of 0.4 mg/L/hr was achieved following
the relatively higher initial rate as seen in Fig. 7c.
3.2.3. Pressure analysis
The confining and inlet pressure measurements show variations
with difference in NaOH concentration. At 0.5 M, the confining
pressure varied between 8 and 9 bars, and between 11 and
12 bars at 1.0 M. Similar results were recorded for inlet pressure
measurement. The confining reservoir pressure increases with the
increase in molar concentration of injected alkaline. Thus, the
higher pressure at higher concentration of NaOH indicates
increased concentration of fines in the pores, which increases the
amount of pressure needed to maintain flow in the Berea sand-
stone. Fig. 8 shows that rock-fluid interactions via alkaline injection
depend strongly on the concentration of alkaline solution. The
amount of dissolved silica at 0.5 M was then plotted against inlet
pressure (see Fig. 9). As observed, the drastic drop in the concen-
tration of dissolved silica coincided with the highest inlet pressure
recorded (with a shift in pressure from approximately 4.8 bars to
5.8 bars). . Afterwards, the steady rate of dissolution was consistent
with unwavering inlet pressure. It can be deduced that pressure
difference during core flooding experiments is a marked response
to the variable dissolution rate.

3.3. Oil recovery

Fig. 5. Plot of dissolved silica against time for (a) 0.5 M NaOH, and (b) 1.0 M NaOH. The The impact of quartz dissolution on oil recovery was also
amount of dissolved silica shows increase with higher molar concentration of NaOH. measured. Two separate cores with similar petrophysical
184
A.M. Ali, M.Y. Kwaya and A. Mijinyawa
Fig. 7. (a) Plot of dissolved silica against time in 0.5 M NaOH; (b) Plot of dissolved silica against time in 1.0 M NaOH; (c) Cross-plot of dissolution in 0.5 M and 1.0 M NaOH, indicating
that molar concentration is more effective at initial rate of dissolution.
Fig. 8. Plots of (a) confining pressure against time and (b) inlet pressure against time, indicating that molar concentration of NaOH during alkaline injection affects both the inlet
and confining pressures.
properties were used for this part of the experiment. The sandstone
core has a length of 30 cm and volume of 212 cm3 with a porosity of
approximately 28%. The first core (Core 1) was subjected to brine
flooding after saturation with oil, whereas the second core (Core 2)
underwent brine flooding after alkaline (NaOH) injection. The
volume of oil in each core, referred to as original oil in place (OOIP),
was set at 77 ml after irreducible water saturation was achieved. For
Core 1, the volume of displaced oil was 48.3 ml with a confining
pressure of 10.6 bars, after flooding with 200 ml of brine. On the
other hand, after flooding with 200 ml of brine, the volume of
displaced oil in Core 2 was 64.5 ml with a confining pressure of
6.50 bars. This implies that the residual/remaining oil in place
(ROIP) after brine flooding is 28.6 and 12.5 for Core 1 and Core 2,
respectively. The recovery factor (displacement efficiency) was
calculated from Eq. (4):
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Energy Geoscience 2 (2021) 181e188
 
Sor2
1  100 (4)
Sor1
where Sor1 indicates ROIP after brine injection and Sor2 denotes
OOIP. The recovery factor values for Core 1 and Core 2 are 63% and
84%, respectively. Table 1 presents the variable oil volumes and
recovery factors. The beakers holding the displaced oil are shown in
Fig. 10. It is evident there is increased recovery of oil via brine
flooding after an initial dissolution process. In addition, the
confining pressure drastically declined with alkaline flooding,
which indicates improved porosity and permeability.
3.4. Quartz surface morphology after dissolution
Although quartz has a relatively non-reactive surface, it can
A.M. Ali, M.Y. Kwaya and A. Mijinyawa Energy Geoscience 2 (2021) 181e188

sites such as edges, pits and fracture sites. Thus, dissolution of

Fig. 9. Plots of dissolved silica concentration against inlet pressure.
serve as a medium for the precipitation and adsorption of authi-
genic materials, which hinders permeability. The agglomeration
and occlusion of particles are more likely to occur at high-energy
quartz grains in sandstone reservoirs will decrease pore throats and
create pathways for oil mobility. Scanning electron microscopy
(SEM) was employed to characterize the quartz grains before and
after dissolution. The microscopic images show the development of
nano-pores in the form of etch pits (see Fig. 11b). This dissolution
process concomitantly dissolves the clays and other matrix mate-
rials that fill the pores, thus enhancing pore diameters. The creation
of pathways in sandstone reservoirs via quartz dissolution is cata-
lyzed or inhibited by secondary phases.
Cross sectional slices of the dissolved grains were obtained to
further elucidate the morphological impact of alkaline injection.
The FESEM images depict rounded to subrounded grain structure
with extensive edge deterioration as shown in Fig. 12a. Fig. 12b
shows the presence of irregular micro-fissures and minute crevices
along the quartz grain boundaries, which indicates the formation of
etch pits by the dissolution process. EDX analysis was applied as
shown in Fig. 12c. The cross-sectional EDX shows a drop in
elemental composition of Si and O in the micro-fissures as shown in
Fig. 12d, which suggests outward diffusion of silica by dissolution.
The micro-fissures become pathways for preferential mineral
leaching, mineral interdiffusion and transformation of nano-pores
into micro-pores.

Table 1
Core flooding parameters indicating fluid saturation and displacement volume, and recovery factors.

OOIP (ml) Volume of displaced oil (ml) ROIP after brine injection (ml) Recovery factor (%)

Core 1 77 48.4 28.6 63

Core 2 77 64.5 12.5 84

Fig. 10. (a) Brine flooding; (b) Brine flooding after alkaline injection.

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A.M. Ali, M.Y. Kwaya and A. Mijinyawa Energy Geoscience 2 (2021) 181e188

Fig. 11. (a) Quartz grain before dissolution; (b) Quartz grain surface showing the formation of etch pits after dissolution.

Fig. 12. Cross sectional analysis showing (a) subrounded quartz (Q) grains with deteriorated grain edges (GE); (b) closer look at the grain edge showing microfissures; (c) EDX line
distribution of the grain edge; (d) EDX line analysis showing a dip in silicon and oxygen distribution at the grain edge indicating leaching of these minerals.

4. Conclusion Declaration of competing interest

Single-phase high-pH core flooding was performed on Berea
sandstone using core displacement equipment. The amount of
dissolved silica and pressure variation within the core were
measured at NaOH molar concentrations of 0.5 M and 1.0 M. The
amount of dissolved silica in the system was comparably higher at
1.0 M than 0.5 M. Inlet and confining injection pressures were
found to increase with molar concentration of injected alkaline
solution. Steady rate of silica dissolution increases in alkaline
concentration, despite the risk of creating more precipitated silica.
The ascent of alkaline concentration leads to the increase of the
amount of dissolved silica in the injected aqueous fluids, which
suggests improved porosity and permeability. The empirical study
shows that the volume of displaced oil increases by approximately
24% with alkaline injection. Thus, alkaline injection during EOR can
enhance the volume of recovered hydrocarbon.
The authors declare that they have no known competing
financial interests or personal relationships that could have
appeared to influence the work reported in this paper.
Acknowledgments
We would like to express our utmost gratitude to Universiti
Teknologi PETRONAS (UTP), Malaysia for providing excellent
research facilities. Our gratitude also goes to Prof. Norhana Yahya
for facilitating the research under the Alpha Matrix research group,
UTP (Cost Centre: 015LC0-149).
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