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CONTRADICTORY TRENDS FOR SMART WATER

INJECTION METHOD: ROLE OF PH AND SALINITY
FROM SAND/OIL/BRINE ADHESION MAPS

Mathilde Didier, Annabelle Chaumont, Thibaut Joubert, Igor Bondino, and Gérald Hamon
TOTAL SA, CSTJF, Avenue Larribau, Pau, France

This paper was prepared for presentation at the International Symposium of the Society of Core
Analysts held in St. John’s Newfoundland and Labrador, Canada, 16-21 August, 2015

ABSTRACT
Smart Water Injection Methods (SWIM) requires a good understanding of the
evolution of wettability not only as a function of salinity but also of pH. In order to
have a better understanding of this parameter, adhesion tests were performed on crude
oil/sand/brine systems. These tests were developed according to an in-house
experimental protocol which guarantees full control of pH during its various stages and
when crude oil/brine/rock are in equilibrium. Fontainebleau and Ottawa sands were
used to understand the effect of pH and salinity on wettability. The brine was
composed of a mixture of NaCl and CaCl2 (ratio 9/1). The salinity varies from 7.9 to
785 mM and pH from 2 to 12.

Firstly, our adhesion tests are in good agreement with previous adhesion maps from the
literature, although the experimental techniques are very different. Moreover our tests
incorporate the effect of divalent ions and long term interactions between oil/water and
the solid, which were not accounted for in previous studies. Our results confirm that at
low salinity and acidic pH (pH < 7), oil adhesion increases for both sands, although
quite more importantly for Fontainebleau. In that respect, our adhesion maps highlight
contradictory results compared to the recent literature regarding the effect of salinity on
wettability.

Secondly we find three distinct oil adhesion areas (for salinity from 0.5 to 50 g/L)
which vary with equilibrium pH: from pH = 2.5 to 6 and pH = 8.5 to 12 showing oil
wettability, pH = 6 to 8.5 showing water wettability. Interestingly it is found that
critical pH thresholds exist in the range pH = 6 to 8.5 at which large variations in the
adhesion between oil and sand are seen. This critical pH might be rock dependent: these
three areas are specifically pronounced for Fontainebleau sand compared to Ottawa
sand where the water wet area is more important (pH = 5.5 to 10). Considering the fact
that both sands are mainly composed of quartz, it would imply that the predominant
mineral species is not an impacting factor on wettability and therefore on SWIM.

INTRODUCTION
SWIM (Smart Water Injection Methods) have been widely investigated in the last 15
years. This is an emerging EOR (Enhanced Oil Recovery) technique highlighted by
Tang and Morrow [1] in Berea sandstone, which is more and more studied due to its
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economical aspect and feasibility. There are in the literature, numerous papers on this
topic in order to understand the mechanism, but at this time, the real mechanism or
combination of mechanisms which lead to the increase of the oil recovery have not
been clearly defined. Several authors have various approaches to explain this effect as
fine migration [2] controlled by clay particles, alkaline-flooding behavior which relies
on interfacial tension reduction caused by pH increase [3], Multiple-Ion-Exchange
(MIE) process [4], pH elevation [5] and formation of water micro-dispersions in the oil
phase [6]. None of these mechanisms on its own can be retained to explain the increase
in oil recovery: rather it is nowadays accepted that a combination of several factors and
a mix of all these mechanisms is behind the SWIM effect [7]. A general consensus is
that low salinity water may induce a change in the wettability towards a more water wet
condition, which would somehow help in releasing additional oil from the pore space.
But this mechanism has not yet been visualized or demonstrated in a convincing
manner.

Since wettability is an important parameter which determines the fluids distribution and
has an effect on oil recovery, several authors performed adhesion experiments in order
to understand the interaction between crude oil, brine and rock [8-12]. Usually the
reservoir sandstone rock is represented by crystalline quartz or various glass surfaces
and classically two kinds of experiments are performed: contact angle [9, 10, 12]
measurement and adhesion of a drop of crude oil on the surface [8, 10, 12]. In both
cases, crude oil is surrounded with a brine composed of sodium chloride at various
salinities and with a pH which varies from 2 to 10 and several parameters are normally
tested as pH, Temperature, I (ionic strength), nature of oil, amongst others. From these
results, adhesion maps are built which give a rapid and semi-quantitative means for
characterizing crude oil interactions with a brine/solid system. Most researches have
highlighted three areas in the adhesion map as a function of pH, brine salinity [9, 10]
whose extension depends on crude oil’s nature, brine’s ionic composition, temperature
and nature of solid:

- Adhesion at low pH (pH < 6) and low salinity (TDS < 5.8 g/L)
- Non-adhesion for pH comprised between 6 and 9 at moderate salinity (TDS ≈
50 g/L)
- Adhesion at high pH (pH > 9) and high salinity (TDS > 50 g/L)

Lebedeva and Fogden [13] have shown similar results for kaolinite. It is seen that pH
has a non negligible effect on adhesion. These results also highlight that there is more
adhesion at lower salinity, which is difficult to reconcile with the claim that at low
salinity, the system become more water wet. Nevertheless all these previous
experiments were performed in a very short time for the contact between oil and glass
(less than 10 min) which means that the system equilibrium may not have been reached.
Moreover, no divalent ions were present in surrounding brine and for some authors [14,
16, 24-26], their presence in the brine is essential to observe a low salinity effect.

In this paper, we developed adhesion tests with a home-made protocol which allow the
equilibrium of the system for various pH and salinities. Simple solids were used as pure
SCA2015-005 3/12

sands. This study allows us to evaluate the combined effect of salinity and pH on oil
adhesion to the rock grains.

EXPERIMENTAL PROCEDURES
Materials
Minerals
For this study, two pure sands were used, Fontainebleau (from VWR) and Ottawa
sands (from Fischer Chemical) in order to mimic sandstone reservoirs. These samples
have been chosen for their purity in terms of mineralogy. Both sands are comparable
in terms of mineralogy and are mainly composed of quartz (SiO2) (Table 1).

Table 1: Mineralogy of sands from XRF measurements

Sands SiO2 CaO K2O P2O5 Fe2O3 TiO2 Ba
Fontainebleau 99.914 0.070 0.006 0.014 0.017 0.017 0.045
Ottawa 99.896 0.071 0.013 0.019 0.021 0.007 0.000

These samples were also characterized with a binocular magnifier to evaluate their
external structure (Figure 1). We can remark that the sands have completely different
structure. These sands were also characterized by laser granulometry. Ottawa sand has
bigger particles with a size of 880 μm compared to Fontainebleau which has a particle
size of 260 μm.

Figure 1: Sand observations with the binocular magnifier, Ottawa sand (left) and Fontainebleau
sand (right)
Crude Oil
The same crude oil was used for all the adhesion tests. The oil has been filtered at 40
μm before use. Table 2 highlights its properties.
Table 2: Analysis of crude oil
Property Units Crude oil
TAN mg/g KOH 0.2
TBN mg/g KOH 1.77
Density @ 40 °C kg/m3 834
Density @ 60 °C kg/m3 820
Viscosity @ 40 °C cSt 6.26
Viscosity @ 60 °C cSt 3.94
% Asphaltenes weight % 2.9
TCC* °C 35
*TCC: Critical Temperature of Crystallization
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Brines
Synthetic brine solutions were prepared at various salinities with 90 wt% of NaCl and
10 wt% of CaCl2. NaCl(s) and CaCl2(s) were manufactured by Sigma Aldrich® with a
purity higher than 99.9%. Demineralized water was used. Brine solution pH was
adjusted with HCl(aq) or NaOH(aq) solutions at 0.1 or 1 M. After stirring, all the
solutions were filtered at 0.45 μm, pH varies from 2 to 12 and it was controlled during
manipulation. Tested TDS (Total Dissolved Salts) were 0.5, 1, 3, 7, 11, 15, 25 and 50
g/L. The properties of the brine used in this study are summarized in the Table 3.

Table 3: Salinity, molar concentration and ionic strength of used brines

TDS(g/L) 0.5 1 3 7 11 15 25 50
C (mM) 7.85 15.7 47.1 11 17.3 23.6 39.3 78.5
I* 0.019 0.036 0.11 0.25 0.40 0.55 0.91 1.82
*: Ionic Strength

Experimental Protocol
Sand Cleaning
In order to eliminate all contaminations, mainly by iron, the sand was washed
beforehand with an acid solution (HCl(aq), 1M), then neutralized with sodium
bicarbonate (NaHCO3(aq), 1M), rinsed thoroughly with demineralized water and
finally oven dried at 60°C for 24 h.

Protocol of Adhesion Tests

The test tube experiment is a fast screening of sand/oil/brine interactions permitting to
focus on the effect of one parameter at the time. These batch experiments use a static
procedure which is described below.

1. Prepare brine at the chosen salinity.

2. Place a known mass of cleaned sand in contact with a known volume of brine.
The brine has to be in excess compared to the sand.
3. Add HCl(aq) at C = 0.1 M or 1 M or NaOH(aq) at C = 0.1 M to adjust the pH
to the chosen value.
4. Leave the solution at 60°C during 24h for equilibration; regularly shake
manually to homogenize the sand/brine system.
5. Measure the pH.
If the target pH is not reached, repeat the steps 3 and 4 to eliminate the
buffering effect of sand.
6. When the target pH is reached and is seen to be stable, mark this pH as initial
pH (pHi). Now add a known volume of oil to the system.
7. Shake manually the glass vial to free the oil that is trapped under the weight of
the sand and not actually adhering to it.
8. Leave the system at 60°C during 48 h under continuous stirring.
9. Observe wetting state at equilibrium at T = 60°C. The wetting state is the
evaluation of the oil quantity which is in adhesion on and in the sand compared
to the oil which stays above the brine phase (Figure 4 for example). Three
states were defined; adhesion, transition and non-adhesion. When the oil
quantity in the sand is higher than in the brine, then there is adhesion. If there is
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quite the same quantity of oil in the sand and in the brine phase, then it is
transition state. Finally when no oil adheres in the sand, then it is non-adhesion
state.
10. Shake manually, wait for equilibrium and observe the wetting state. As
previously, manual shake makes the system more homogeneous and helps to
estimate visually the actual sand and oil adhesion by freeing the oil that is
trapped under the weight of the sand.
11. Measure the final pH (pHf) after filtration at 0.45 μm of the brine in the system.
12. Report the observed wetting state at fixed pH in an adhesion map
13. Perform this protocol for another initial pH until the adhesion map is complete
with all the tested salinity and initial pH

Remark: Equilibrium was estimated with tests at various experiment durations. It was
estimated that after 48h of stirring, the interaction between oil, sand and brine stays the
same even after more hours of stirring at temperature.

This protocol allows removal of the buffering effect of the sand (which can be quite
important) and to control the initial and final pH of the system. The key parameter in
this study is the control of pH. The final pH could be estimated with the pHi-pHf
diagram of the used crude oil (Figure 2). We can remark in this graph that the
evolution of pH is the same at low salinity (1 g/L) as at high salinity (50 g/L). For this
studied oil, when initial pH is comprised between 4 and 10, the final pH is between 6
and 8. This oil is mainly a basic one.

Figure 2 : pHi-pHf diagram of the tested crude oil at 45°C in NaCl/CaCl2 brine at low and high
salinity (TDS = 1 and 50 g/L)
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RESULTS AND DISCUSSIONS

The adhesion map of Fontainebleau sand is displayed in Figures 3a and 3b.

Figure 3a: Adhesion map of Fontainebleau sand

Figure 3b: Adhesion map of Fontainebleau sand (zoom on low salinity (TDS<10 g/L))
SCA2015-005 7/12

The information in this map can be approximated by three main adhesion areas
roughly situated at:

- 2 < pH < 6 : oil adheres to grains

- 6 < pH < 8 : oil does not adhere to grains
- 8 < pH < 12 : oil adheres to grains

An example of test tube experiments is displayed in Figure 4 to illustrate this adhesion

map at 7 g.L-1. In this example, adhesion occurs at final pH equal to 5.42 and at higher
pHf (10.17), whilst non-adhesion is seen for pHf = 7.23.

5.42 7.23 10.17 6.38 7.11 7.74

Figure 4: Glass vial adhesion map Figure 5: Glass vial adhesion map
results at fixed salinity (7 g.L-1) results at fixed salinity (3 g.L-1) and
and for three pH (pHf) values. for three pH (pHf) values. From
From left to the right: adhesion, left to the right: non-adhesion,
non-adhesion, adhesion. transition, non-adhesion.

By decreasing the pH, whatever the salinity, a greater adhesion of oil on the
Fontainebleau sand is visible, a result in agreement with the work of Yang et al. [10]
and Drummond et al. [9]. Oil adhesion is systematic for pH below 5 as well as for pH
higher than 10. In addition, at low salinity (TDS < 3 g/L), the zone of oil adhesion
extends towards higher pH. In this area (6 < pH < 8) small variations of salinity for a
given pHf can create very different adhesion results (Figure 5).
This observation is very important since pH values expected at reservoir conditions
would cover the interval 5 < pH < 7 [22]: wettability being so sensitive in these pH-
salinity ranges, could create an important variability of outcomes and would render
SWIM performance not trivial to assess.

In conclusion, the result obtained for Fontainebleau shows that the rock becomes more
oil wet when salinity decreases, in contradiction to comments in literature on smart
water techniques ([14-17]) where when decreasing the salinity, the water wetness of
the solid increases, leading to the increase of oil recovery.

In Figure 6 the adhesion map for Ottawa sand is displayed. There are three main areas
of adhesion, mainly controlled by pH, as for Fontainebleau, but here there is much less
influence of salinity. The oil adheres when pH decreases (pH < 5) and for low salinity
(TDS < 10 g/L) as well as for basic pH (> 11) for all salinities. The last area in this
adhesion map shows water wet condition.
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Figure 6: Adhesion map of Ottawa sand

Since both sands share a very similar mineralogy, then we would conclude that for this
case sample mineralogy does not have an important effect on wettability.
The three areas in the adhesion maps of Fontainebleau and Ottawa sands could be
partially explained by adsorption of oil components on sand and electrostatic
repulsion, at least at low pH (Figure 7).

Figure 7: Interpretation of adhesion maps. Continuous and dotted green curves show the transition from
water-wet to oil-wet for Fontainebleau and Ottawa sand respectively

The results of this study could be compared with those from Bondino et al. [18], where
the authors used similar experimental setup to evaluate oil adhesion on sand. They
highlighted also oil adhesion at high and low salinity conditions (TDS = 1 and 50 g/L)
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and for acidic pH (pHi < 5). Water wetness is observed at basic pH (pH > 7) and for
low salinity. Nevertheless the main difference between the two studies is that in [18],
the pH was not controlled and measured at the end of the experiment (therefore the pH
discussed in the paper happens to be the initial one). Regarding our results, we
demonstrate pH is a key parameter in wettability variation and has to be controlled and
measured all along the experiment.

These results are comparable with those from the literature [8-12] where adhesion
maps highlight also three areas which depend on pH and salinity range. Oil adhesion
occurs also for low pH (< 6) and high pH (> 9) and non-adhesion for intermediate pH
(6< pH < 10) and salinity (≈ 50 g/L). Transition zone for low salinity (TDS < 5.8 g/L)
is located for pH close to 6 and 8, as observed in this paper. This pH area is therefore
critical and pH seems to be a key parameter in oil adhesion. This study confirms these
previous contradictory results where oil adhesion increases for low salinity range.
Nevertheless the test tube experiments presented in this paper seem to be more
representative of SWIM compared to the previous adhesion tests. Indeed, compared to
the results of [8-12], duration of experiments is longer and led to equilibrium within
the system oil/brine/sand. Moreover brines were composed of mono and divalent ions
as Ca2+ which is favourable for low salinity effect [4, 16] compared to brines with only
monovalent ions in the cited literature.

Adhesion maps (Figures 3 and 6) could be explained by electrostatic interaction

between oil and sand. The isoelectric point of quartz is estimated to be close to 2.5
([19, 20]) which means that quartz (Qz) is negatively charged for pH higher than 2.5
(Figure 8). Usually, acid and base components of oil are simplified by RNH2, RCOOH
and Quinoline. pKa of these redox couples are illustrated in Figure 8. At low pH
(< 4.9), oil components are essentially positive and inversely at basic pH (> 8.1).

Figure 8: pKa of oil components (RNH2, RCOOH, Quinoline) and isoelectric point of Quartz (Qz)

Figure 7 summarizes adhesion maps with adhesion areas for Fontainebleau and
Ottawa sands. In Area 1, adhesion occurs at low pH (2.5 < pH <5) due to reduction of
electrostatic interaction between sands negatively charged and oil components
positively charged (R+NH3, Quinoline positively charged). In Area 2, non adhesion
occurs at higher pH (pH > 4.9) due to repulsion between sands still negatively charged
and neutral (RNH2, Quinoline) and negative (CH3COO-) oil components. However,
when salinity increases in Area 1, oil adhesion occurs at lower pH for Fontainebleau
sand but not for Ottawa sand. One hypothesis is the influence of roughness and
granulometry which could increase specific surface area of sand grains and therefore
increase the probability of adhesion. The roughness of Fontainebleau sand seems
higher than Ottawa’s, therefore its specific surface area could be higher and this will
increase the probability of oil adhesion. Similar observations were already highlighted
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in the literature [21]. In the Area 3, oil adhesion at very basic pH (pH > 10) is more
difficult and complex to explain: further investigations are ongoing.

This variation of adhesion with pH suggests also that not only the final pH is
necessary to know, but also the initial pH of the system. If there is a pH evolution
during the waterflooding experiment in the system rock/brine/oil, we could have a
change of wettability which could have an impact on the recovery.

This study could be useful for understanding spontaneous imbibitions tests, as

adhesion maps were elaborated with test tube experiments without dynamic aspect. In
the literature, some authors highlight high response variability for spontaneous
imbibitions tests with various carbonates rocks [22] or various type of oil on Berea
sample [23] for example. Romanuka et al. [22] show various wettability modification
in function of rock samples or ionic composition of injected water. Suijkerbuijk et al.
[23] found very different oil recovery during spontaneous imbibitions with ten
different oils on Berea sandstones. Adhesion tests as described in this study could be
useful screening tests for understanding the variability in response of SWIM
spontaneous imbibitions experiments.

CONCLUSIONS
In this paper, test tubes experiments were performed in order to implement adhesion
map for crude oil/sand/brine system. A home-made protocol allows the system to
reach equilibrium at temperature with full control of the pH. Indeed, pH appears to be
an essential parameter in wettability, more than the salinity. Adhesion map of
Fontainebleau sand highlights oil adhesion at low salinity (TDS < 3 g/L) in reservoir
pH area (6 < pH < 8) and non adhesion for a salinity higher than 3 g/L in this pH area.
Moreover, this domain is very sensitive to pH variation. A little variation in pH will
change drastically the wettability. This highlight that pH has to be well monitored
during waterflooding experiments.

The fact that low salinity increases the oil wettability is contradictory to what is
expected in the literature for SWIM, where low salinity waterflooding is seen to
increase water wetness and then the oil recovery. In light of these results, we think that
it would be more appropriate to state that oil recovery depends from the transition
from some initial to some final state, and not simply from a system becoming more
water wet.

It was rather interesting to note that Ottawa and Fontainebleau highlight different
adhesion maps despite the fact that their mineralogy is quite similar. Therefore the
mineralogy may not always be a determinant parameter in low salinity effect.
Moreover both sands have various roughness, which could be an important parameter
for adhesion behavior. The effect of surface roughness and granulometry is currently
under investigation. Finally electrostatic interactions between acid and base
components of the oil seem to control the adhesion on the solid.
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ACKNOWLEDGEMENTS
The authors would like to gratefully acknowledge TOTAL SA for funding this project
and for the technical support.

NOMENCLATURE
SWIM Smart Water Injection Methods I Ionic Strength
EOR Enhanced Oil Recovery wt% Weight %
TCC Critical Temperature of Crystallization C Molar Concentration
TDS Total Dissolved Salts M mol/L

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