INVESTIGATION OF FORMATION DAMAGE DURING NATURAL

SURFACTANT FLOODING IN SANDSTONE RESERVOIR

BY

JONAH OTUANKEME
UG/17/2675

A PROJECT

SUBMITTED TO THE DEPARTMENT OF PETROLEUM

ENGINEERING, FACULTY OF ENGINEERING IN PARTIAL
FUFILMENT OF THE REQUIREMENTS FOR THE AWARD OF THE
UNIVERSITY’S DEGREE BACHELOR OF SCIENCES (B.Sc).

IN

THE DEPARTMENT OF PETROLEUM ENGINEERING

JULY, 2023

i
 DEDICATION
This research project work is dedicated to God Almighty for his infinite mercies
during the research work.

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 ACKNOWLEDGEMENTS

My profound gratitude goes to God Almighty Who made my academic journey

successful. To him I give all the glory and adoration. My Sincere thanks goes to
my project supervisor Engr. Wilson Omuso pensive for his devoted attention and
contribution to my project.

My gratitude goes to my parents who encouraged, guide, and supported me. To my

friends, who were there for me throughout this journey. I really appreciate your
supports and kindness. May God bless you all, and may you flourish in every area
of your life.

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 TABLE OF CONTENTS
Title Page
Cover Page i
Declaration ii
Certification iii
Dedication iv
Acknowledgements v
Abstract vi
Table of contents vii
List of tables xi

CHAPTER ONE: INTRODUCTION

1.1 Statement of the Problem 2
1.2 Aims of the Study 2
1.3 Objectives of the Study 2
1.4 Scope of the Study 3
1.5 Significance of The Study 3

CHAPTER TWO: LITERATURE REVIEW

2.1 Formation Damage 4
2.1.1 Emulsion Blockage 4
2.1.2 Adsorption and Retention of Surfactants 5
2.1.3 Wettability Alteration 5
2.2 Enhance Oil Recovery 6
2.2.1 Chemical Enhanced Oil Recovery (CEOR) 6
2.2.1.1 Natural Surfactants 7
2.3 Characterization of Surfactants 8
2.3.1 Critical Micelle Concentration 8
2.3.2 Kraft Temperature and Kraft Point 9
2.3.3 Solubilization and Optimum Salinity 10
2.4 Surfactants Adsorption 10
2.4.1 Temperature 11
2.4.2 Salinity 11
2.4.3 PH 11
2.5 Mechanisms of Natural Surfactants Flooding 11
2.5.1 Interfacial Tension Force (ITF) 12
2.5.2 Wettability Alteration 13
2.6 Research Gap 14
CHAPTER THREE: INTRODUCTION

3.1 Research Design 15

3.2 Research Approach 15
3.3 Materials/Equipments 15
3.4 Data Collection 16
3.5 Experimental Procedure 17
3.5.1 Brine Preparation 17

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3.5.2 The Extraction of the Extract from the Leafs of Vernonia Amygdalina
17
3.5.3 Critical Micelle Concentration 18
3.5.4 Preparation and Formulation of Surfactant-Brine Solutions 19
3.6 Data Analysis 20
3.6.1 Density Measurement 20
3.6.2 Viscosity Determination 20
3.6.3 Porosity and Permeability Analysis 20

CHAPTER FOUR: RESULT AND DISCUSSION

4.1 Properties of the Prepared Solutions 23
4.2 The CMC of the Natural Surfactant 24
4.3 Porosity Estimation After Saturation 25
4.4 Hydraulic Conductivity Test 27

CHAPTER FIVE: CONCLUSION AND RECOMMENDATIONS

5.1 Conclusion 33
5.2 Recommendations 33
References
Appendix

v
 LIST OF FIGURES
Figures Titles Pages
2.1 Types of natural Surfactants 8

2.2 Formation of surfactants micelle 9

2.3 Solubility Cruve – CMC Curve 9

2.4 Wettability alteration of reservoir rock. 13

3.1 Displacement Experiment for Single Phase Flow 19

4.1 Bar on the properties of the prepared solutions 24

4.2 The critical micelle concentration for the natural 25

surfactant
4.3 Graphical representation of porosity against the prepared 26
concentrations.

4.4 The graph of flowrate against pressure drop when 1.5%-B was 29
injected into the core sample.

4.5 The graph of flowrate against pressure drop when 29

0.05%-SB was injected into the core sample
4.6 the graph of flowrate against pressure drop when 30
0.1%-SB was injected into the core sample
4.7 The graph of flowrate against pressure drop when 31
0.4%-SB was injected into the core sample

4.8 The graph of flowrate against pressure drop when

0.05%-S was injected into the core sample 31
4.9 Graphical representation of the hydraulic conductivities
against brine and surfactant-brine solutions 32

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 LIST OF TABLES
Tables Titles Pages

Table 4.1.1 Properties of the prepared solutions 23

Table 4.3.1 porosity and core sample characterization 26
Table 4.4.1 Test result obtained from hydraulic conductivity test 27

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 ABSTRACT

In the course of natural surfactant flooding as an EOR technique in

sandstone reservoir, the retention of natural surfactant particles on the pore
spaces of the sandstone reservoir rock can cause a reduction on the porosity
and permeability of reservoir rock leading to formation damage. During
natural surfactant flooding as an EOR technique in sandstone reservoir, as
the reservoir rock minerals are extremely sensitive to chemicals injected in
to the formation, it is important to carry out a critical investigation of
formation damage in other to evade operating cost, reduce the cost of oil
production and improve oil recovery. In this research work, an experimental
investigation was carried out on the porosity and permeability of sandstone
core sample before and after flooding with natural surfactant derived from
vernonia amygdalina leaf. A single phase displacement setup method was
used to carry out the core flooding analysis. The permeability of the core
sample was calculated at the beginning and the end of the flooding by
measuring the pressure deferential across the core holder at deferent flow
rates. The concentration of the natural surfactant was varied in each stage
of the flooding process, and a graph of permeability against surfactant
concentration was plotted to analyses the formation damage of the core
sample. The experimental result reveal that the initial porosity and
permeability before the core flooding were 16.5% and 35622md. The
porosity decreased to 12.5% after carrying out the core flooding with
increasing surfactant concentration. The permeability increased to
42210(md) when the surfactant concentration was 0.05wt%, decreased to
31026md when the concentration was increased to 0.2wt% and increased to
38417md when the surfactant concentration was increased to 0.6wt%. The
analysed results shows that the presence of natural surfactant derived from
vernonia amydalina leaf has a minimal effect on the porosity and
permeability of the sandstone core plug. The porosity reduce as the
concentration of the natural surfactant increases and also have a partial
sinusoidal effect on the permeability of the core sample.

viii
 CHAPTER ONE

INTRODUCTION

The majority of the world’s energy demand comes from crude oil, making

world highest energy consumers rely on and countries with large revenue

(Energy Information Administration, 2003). Worldwide energy demand is

estimated to increase by 30% in 2040 compared to 2010 (Karatayev et al.,

2019). It is estimated that oil consumption will reach 111.1 Million barrels

per day (Zhang et al., 2020). With the depletion of reservoirs and rise of

energy demand due to population growth. It has become so vital improve oil

recovery from declining reservoirs (Joshi et al., 2015). Oil production

methods are followed by primary depletion, secondary recovery and tertiary

recovery process. It is estimated that about 30-50 percent of the original oil

in place can be produced through the entire life of a reservoir that has been

developed under primary and secondary recovery process (Green &

Willhite, 1998). Considering the fact that the easily recoverable oil is

running out, a significant quantity of crude oil remain unrecovered in the

reservoir after conventional method have been exhausted. This unrecovered

oil is de to the interfacial tension between oil and water and the capillary

forces holding this residual oil in the pore space. Injection of chemicals such

as natural surfactants has played an important role producing this residual oil

by reducing the interfacial tension, resulting in a corresponding increase in

the capillary numbers (Berger & Lee, 2006). Surfactants can also drive the

ix
reservoir wettability towards more water-wet. These can only be achieved

by the proper selection of surfactants according to environmental variables

such as pressure temperature and salinity.

1.1 Statement of The Problem

Despite being one of the most promising methods of EOR process among all

chemical processes, poor selection of surfactants according to environmental

variables such as concentration, salinity, temperature and PH could be

detrimental to the reservoir causing formation damage due to undesirable

wettability alteration, clay swelling possible rock dissolution resulting in a

chemical reaction with displacing fluids and blockage of pore space. It may

also lead to high adsorption. Surfactant adsorption is another major factor

which affects the surfactant flooding process. Therefore any reduction in

surfactants concentration from injected slug may decrease the surfactants

efficiency to reduce oil-water interfacial tension. This will lead the whole

process to economic failure.

1.2 Aims of The Study

The aim of this research is to investigate the formation damages on

sandstone reservoir during natural surfactant flooding.

1.2 Objectives of The Study

the objectives of this study are as follows:

1. to characterize sandstone core samples before and after flooding.

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 2. To vary the effect of the concentration rate of natural surfactant

extract derived from Vernonia amygdalina leaf on the porosity of

the core sample.

3. To vary the effect of the concentration rate of the natural

surfactant extract from vernonia amygdalina on the permeability

of the core sample.

1.3 Scope of Study

This work consider the effectiveness of natural surfactant on the porosity

and permeability of sandstone reservoir. The research is also based on

investigating the possible formation damage caused during natural surfactant

flooding.

1.5 Significance of The Study

The high cost of oil recovery has become a challenging factor in the oil

field. The main aim of every oil company to invest in the oil business is to

make profit thereby trying to minimize the cost of production. However, in

some cases formation damage is one major factor that has contributed to this

high cost of production. Several EOR methods have been employed to boost

the recovery factor, including surfactants. Due to the toxicity and high cost

of conventional surfactants, this study finding, further reveals the

effectiveness of natural surfactants in minimizing the capillary forces

holding the oil in place as a result of reducing the interfacial tension force,

increasing capillary number and improving oil recovery factor. It also entails

xi
the development of experimental and analytic method to investigate, prevent

and to control, and mitigate formation damage. This will play an important

role in reducing the cost of production and improving oil recovery.

xii
 CHAPTER TWO

LITERATURE REVIEW

2.1 FORMATION DAMAGE

Formation damage can be defined as the various damage mechanisms

affecting the properties of the Formation Matrix which alters the transport

efficiency of reservoir fluids. Mostly, it is detected by the changes that occur

in the well performance in terms of infectivity, productivity, and oil

recovery (Harper and Buller, 1998). Formation damage impairs the

permeability of the work matrix which has a direct impact on the cost of oil

recovery. Formation damage mechanisms are classified into four categories,

which are; mechanically, biologically, chemically and thermally induced

(Faergestad, 2016).

During EOR process, several chemicals are injected into the reservoir to

boost the transport efficiency of the reservoir fluids; on the other hand these

chemicals can also cause damage to the formation. These chemically

damaged mechanisms further classified as rock-fluid incompatible and fluid-

fluid incompatible (Bennion, 2023).

The fluid-fluid incompatibles are sale deposition, emulsion blockage and

hydrate formation while the rock-fluid incompatibles are clay swelling,

wettability alteration and surfactant adsorption.

xiii
2.1.1 Emulsion Blockage

Injection of chemicals into the reservoir rock matrix, can sometimes results

to serious blockage of pore throats by emulsion, which impairs the

permeability, especially in low permeability reservoir (Feng et al., 2011).

Oil (mixing surfactant with oil), in a conditions of high-salinity increases the

apparent viscosity of the emulsified fluid which may be higher than that of

the oil. Such change impairs the flowing efficiency of oil towards the

wellbore (Xu et al., 2011).

Allen et al. (1982) showed that structural expansion occurs when excess

water is absorbed between clay layers, hydrophilic materials like smectite

and mixed Layer are hydrated and expand when interacting with Fresh and

Low salinity water severe reduction in permeability can occur when clays

obstruct flow by either expanding to fill pore spaces or entrain the fluid

streams and blocking the pore spaces.

2.1.2 Adsorption and Retention of Surfactants

Surfactant adsorption in sunstone reservoir in certain conditions can results

in formation damage (Panga et al., 2006). The excessive adsorption of

surfactants by phase trapping (Hirasaki et al., 2011) results in the reduction

of porosity and permeability and lower the efficiency of the surfactant to

adsorp into the oil-water interface which reduce the rate of oil recovery.

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2.1.3 Wettability Alteration

Many addictives such as corrosion inhibitors can enter the near wellbore

region and force a change from water wet to oil-wet conditions. Surfactants

precipitation and phase trapping the contact of cationic fluids with anionic

surfactants and minerals in the formation results in loss and precipitation of

surfactants (Stellner and Scamehorn, 1986).

2.2 Enhance Oil Recovery

EOR is defined as a set of production technologies that are used to recover

more oil than that produced by the conventional method (primary and

secondary method) through the injection of energies or fluids into the

formation (Alvarado and Marique, 2010). EOR are generally classified into

four main categories which are thermal, gas, chemical and microbial,

method. Thermal method involves the introduction of heat into the reservoir

to reduce the viscosity of oil, thereby enhancing oil recovery. It is often

applied in heavy oil reservoirs. Microbial process involves the introduction

of micro-organisms into the reservoir, which grows exponentially and their

metabolic products mobilizes the residual oil (Gao and Zerkri, 2011).

Gas methods involves the injection of slug of gases such as Co 2, N2 and flue

gas to induce gas drive mechanisms within the use of chemical solutions

such as surfactants polymers and castic solution to recover oil. Among all

the EOR methods, chemical EOR process has been deemed as the most

xv
promising method due to its higher efficiency technical and economical

feasibilities and reasonable capital cost (Levitt & Pope, 2008).

2.2.1 Chemical Enhanced Oil Recovery (CEOR)

Chemical flooding is a proven enhanced recovery method which is classified

into polymer, surfactants and alkaline flooding. The injection of polymer

results in higher recovery of oil by reducing the mobility ratio and

improving the macroscopic sweep efficiency (Sorbie and Phil, 1991).

Alkaline flooding involves the injection of chemicals such as orthosilicate

(Nasi O4) or sodium carbohydrate (Na2Co3) into the reservoir with water.

The acid in the oil reacts with the alkaline to form surfactants which then

undergoes adsorption that promotes interfacial tension force reduction (ITF)

between oil and water (Abadli, 2012). Surfactant flooding is an important

EOR process. It involves altering the fluid-fluid attraction by reducing the

interfacial tension force (ITF) between oil and brime, fluid rock properties

via wettability alteration of porous medium. The two types of surfactants are

natural and synthetic surfactants. In the recent studies carried out by

researchers on the use of surfactants, natural surfactants are gaining more

attention than industrial (synthetic) surfactants due to their low-toxicity,

environmental friendliness lower cost of production.

xvi
2.2.1.1 Natural Surfactants

Natural surfactants are surface-active chemicals with hydrophobic tail and

hydrophobic head (Georgiou et al., 1992). Natural surfactants are either

extracted directly or synthesized from plants and animal fats, and they have

shown sterling properties for the use of EOR. Several parts of the plants

such as leaves, seeds, roots, oil and flowers have ending on their constituent

components. Examples are almong seed, ziziphus spina-christi, jatropha

curcas, palm tree, soapnut etc. the classification of natural surfactants used

in EOR, is like the classification of chemical surfactants, which are

classified into four types, they are anionic, non-ionic cationic and

atmospheric (Bere & Mandal, 2015). Anionic surfactants have a negative

charge, non-ionic do not ionize in water or acqeous solution because they do

not carry charge. Atmospheric (Zwitterionic) have both positive and

negative charge, cationic are positively charged.

Figur 2.1: Types of natural Surfactants (Osama and Ahmad, 2020).

xvii
2.3 Characterization of Surfactants

It is necessary to characterize natural surfactants before used in any EOR

operations for technical and economic reasons.

2.3.1 Critical Micelle Concentration

When there are sufficient amount of surfactants molecules present in a

solution, they joined together to form structures called micelles. Micelle is a

term that describes the aggregation form of surfactants molecules dispersed

in a liquid colloid (Bhosle et al., 2020, Naseri et al., 2018). The critical

micelles concentration (CMC) is the surfactants concentration above which

micelles can be formed. The CMC of a particular type of surfactant is

dependent on factors like the molecular structures, solution salinity

(Bratovcic and Nazdrajic, 2020), ionic composition, PH, temperature and

others (Harutyunyan and Harutyunyan, 2019), ITF measurement is

commonly used to determine the CMC of surfactants.

FIGURE 2.2. Formation of surfactants micelle (Osama and Ahmad

2020).

xviii
2.3.2 Kraft Temperature and Kraft Point

The kraft temperature is described as the temperature at which surfactants

melts after being hydrated (Roy et al.,; 2014). Micelles cannot be formed

below the kraft temperature at the kraft temperature, the solubility of

surfactants increase sharply and further increase in the temperature will

results in the formation of micelles to attain the CMC level (Marlic and Ali,

2011).

Figure 2.3: Solubility Cruve – CMC Curve (Osama and Ahmad 2020).

2.3.3 Solubilization and Optimum Salinity

Solubilization ratio is the volume of oil or water that solubilized per volume

of surfactants in micro-emulsion phase (Das, et al., 2020; Sharma et at.,

2020). The presence of saline environment has a significant influence on the

performance of surfactants flooding (ionic). At lower level, surfactants are

highly water soluble, and are oil soluble at higher salinity level. Therefore an

optimal salinity should be attained at which equal quantities of oil and water

can be solubilized to form micro-emulsion (Hirasaki et al., 2011; Gao and

Sharma, 2013b). at optimal salinity the oil solubilization ratio will be equal
xix
to the water solubilization ratio (Bera et al., 2011, Hamidi et al., 2015). The

optimum salinity level is the level at which the lowest oil-water interfacial

tension is obtained.

2.4 Surfactants Adsorption

Adsorption of surfactants is the most critical problem that can influence the

success or failure of surfactant flooding (Azam et al., 2014). Surfactant

adsorption may occur on the rock surface due to the electrostatic interaction

and vanderwaals that arise between the surfactant and solid surface (Kamal

et al., 2017).

Surfactants adsorption depends on many factors such as surfactant type,

surfactant concentration, pH, salinity and temperature. These factors can

influence the dissolution behavior of minerals and their force, it will cause

significant changes in the adsorption of surfactants into the rock surface

(Siracusa and Somasundaran 1987).

2.4.1 Temperature

Surfactant flooding is commonly operated under low-temperature and low

salinity conditions.

Anionic and non-ionic Surfactants are favourable to be used in these

conditions. On the other hand, at high temperature and high-salinity

conditions, anionic Surfactants show low slat resistance (Kamal et al.,

2018).

xx
2.4.2 Salinity

High-salinity water is not desirable for anionic Surfactants due to the facts

that it can precipitate, resulting from the interaction between salt ions and

the Surfactant. Increasing the salinity will reduce the repulsive forces

between the anionic Surfactant and the rock Surface (Azam et al., 2013;

Kamal et al., 2017).

2.4.3 Potential of Hydrogen (pH)

Surface charges that exist on the Surfactants as well as the rock surface have

a direct effect on the Surfactant adsorption. At lower pH, Surfactants

solution drive mineral hydroxyl to acquire positive charge which increases

the adsorption of Surfactants by attracting the negative charge molecules to

the rock surface.

2.5 Mechanisms of Natural Surfactants Flooding

The mechanisms of using surfactants is basically to lower the interfacial

tension force (ITF) and to alter the wettability in other to increase the

capillary number towards the producing well (Hirasaki and Zhang, 2004).

2.5.1 Interfacial Tension Force (ITF)

Interfacial tension force is determined as the force of attraction existing

between the interface of two immiscible fluids e.g. (oil & water). The

xxi
interfacial tension force between hydrocarbons and water molecules which

cause an increase in the capillary forces which are responsible for the

trapped hydrocarbons in the pore spaces of the rock matrix. Surfactants

injection is used as an option to lower the interfacial tension force

(Hosseininoosheri et al., 2016).

When natural surfactants are injected into the reservoir formation, due to

their amphilic nature, the hydrophilic head of the surfactants aligns with the

water or brine, while the hydrophobic tail attracts the oil phase which reduce

the ITF between the oil and water (Gbadamosi et al., 2022). A good

solubility of natural surfactants is an important property in lowering the ITF

of oil and water. Numerous studies have shown the effectiveness of natural

surfactants in lowering the ITF of oil and water. Imuetinyan et al. (2022)

demonstrated oil-water interfacial tension, wettability alteration and foaming

studies of natural surfactants derived from vernonia amydalina. The

synthesized surfactants reduced the interfacial tension force between oil and

water from 18mN/m to 0.97mN/m.

Ali et al. (2015) demonstrate the feasibility study of natural surfactants

synthesized from olive leaf. The synthesized natural surfactant decreased the

ITF between kerosene and water from 36.5mN/m to 14mN/m.

2.5.2 Wettability Alteration

Wettability is defined as the tendency of a fluid to adhere on the surface of a

solid in the presence of other immiscible of fluids (Jing et al,, 2019; Yang

xxii
and Zhou, 2020). Natural surfactants have shown a good property in altering

the wettability of a porous media from an oil-wetting condition to more

water-wetting condition wettability alteration alters the contact angle of oil

on the rock surface from an oil-wet state (θ > 900) to water-wet state (θ <

900) which is caused by surfactants.

FIGURE 2.4:. Wettability alteration of reservoir rock. (Gbadamosi et al.,

2018).

Alsabagh et al. (2021) synthesized non-ionic surfactants from waste cooking

oil. The surfactant reduced the contact angle up to 27.5 0 and an incremental

oil recovery of 24.3% and 11.7% was recorded for the non-ionic surfactants

from palm kernel oil and palm oil.

Mehdi et al. (2004) studies the effect of natural derived surfactant on

wettability alteration and interfacial tension in water-oil on his flooding. He

demonstrated that a surfactant solution containing 10% of mulbery could

reduce the contact angle from 62.50 to 48.50.

2.6 RESEARCH GAP

xxiii
To the best of this research’s knowledge and ability, it was determined from

the available articles and publications on the subject that while there are

studies on the use of natural surfactants as a flooding agent in oil recovery,

very few of them have looked into the possibility of formation damage due

to this mode of enhanced oil recovery technique. As a result, the project’s

knowledge contribution and fundamental research gap include the use of

natural surfactants (Vernonia Amygdalina) as a flooding agent while

examining the impact of formation damage on the reservoir.

xxiv
 CHAPTER THREE

INTRODUCTION

This chapter covers the research design, research approach, materials and

equipment used during the process of the practical, data collection,

experimental procedure and data analysis.

3.1 RESEARCH DESIGN

The study made use of a quantitative experimental research design, as it is

useful in identifying causal relations in spite of assigning participants

randomly to different groups for ethical or practical purposes. Instead, with

this research design method, this experimental investigation can place

reliance on pre-existing conditions or existing groups to form comparison

for group of data obtain experimentally. It is also applicable to a much larger

scale with an increasing statistical power of the results due to the fact that

the research focuses on the effect of a locally sourced surfactant (Vernonia

amygdalina Leaf.) on Niger Delta Reservoir formation.

3.2 RESEARCH APPROACH

Quantitative research approach was used and selected to implement the

objective procedures in other to analyze, interpret and collect experimental

data so as to produce and investigate a graphical casual relationships that

will explain, describe, predict and control phenomena of interest primarily.

xxv
3.3 MATERIALS/EQUIPMENTS

This area covers the description and discussed what is been carried out in the

laboratory and the sources of the materials used in this study. The success of

this experimental investigation was achieved by the use of the following

laboratory equipment/materials;

1. A simple separation set-up

2. electronic weighing balance
3. Soxhlet extractor
4. 30×100mm thimbles
5. Heating element (electronic cooker)
6. Filter paper
7. calibrated beakers
8. measuring cylinders
9. Conical flask
10. spatula
11. Mercury thermometer
12. magnetic stirrer
13. viscometer
14. density bottle
15. valves
16. accumulators
17. micro-pump
18. Vanier caliper
19. Accumulator
20. Pipette
21. U-tube manometer
The chemical reagents used for this investigation are: laboratory distilled

water (H2O), Ethanol and the natural surfactant was locally sourced from

Amassoma, Bayelsa state in June 15, 2023. The leafs extract of Vernonia

amygdalina Leaf. were sun-dried for about 6 to 7 days (one wee2k) before

being grinded to some very fine infinitesimal particles in powdered form and

kept in an air tight container. Two cylindrical core samples are obtained

from the Niger Delta reservoir sandstone formation.

xxvi
3.4 DATA COLLECTION

Experimental data collection method was utilized in this research work as it

is a standard data collection method for measuring, obtaining, analyzing and

observing accurate manipulation of the test samples by making a change of

treatment prior to the ascertain data and information. Though, it's time

consuming but it measures and propagate the curse and effect of the

experimental units from the manipulated independent variables. In this

study, the obtained experimental data from the investigation will shear more

light on the formation damage caused by presences of Limestone in the

reservoir.

3.5 EXPERIMENTAL PROCEDURE

3.5.1 BRINE PREPARATION

1.5% brine concentration was prepared by adding 15g of sodium chloride

(NaCl) in 1000ml (1L) of the laboratory distilled water and stirred using the

spatula and magnetic stirrer at room temperature (29-31 oC) for about 60min

to obtain an efficient mix of solute and solvent, and filtered to discard any

filtrate. Density bottle, Ostwald viscometer and PH digital meter where used

to determine the density, viscosity and PH value of the saline solution. The

prepared saline solution in the cylinder is utilized as the control sample.

xxvii
3.5.2 THE EXTRACTION OF THE EXTRACT FROM THE LEAFS

OF VERNONIA AMYGDALINA LEAF.

A rig of the extraction apparatus was build using stands and clamps to

support the extraction apparatus, Following this, measured 250ml of ethanol

was poured into a round bottom flasks that is connected to the soxhlet

extractor and condenser mounted on an heating element (Electric cooker).

Weighed mass of the pulverized leave was loaded into a 30×100mm

cellulose thimble and placed inside the soxhlet extractor. The side arm is

lagged with a cotton wool, the ethanol inside the round bottom flasks was

heated using the heating element which enable the transformation of the

ethanol into vapor, moving through the external tube in the siphon unit to the

condenser, the condensate then drips into the thimble inside the siphon unit.

Once the level of the solvent reaches the siphon it pours back into the flasks

through the orifice and the circle begins again until the pure ethanol was

obtained in the siphon unit.

The mixture of the ethanol and the mineral content is separated using a

simply distillation set up. The obtained mixture was poured into a pyres

flasks mounted on an heating element that is connected to a different

condensing chamber. The heating element heat up the mixture in the flasks,

the boiling point of ethanol is lower than that of the mineral so the ethanol

will first vaporize and fall as liquid droplets into the collector (a covered jar

that is connected to the condenser) after passing through the condensing

xxviii
unit. Once the whole ethanol in the mixture have been vaporized the heating

element is turned off and the mineral remaining in the flasks was poured into

a tray as to expose the remaining ethanol in the mineral to evaporate in other

to obtain the extract using a spatula.

3.5.3 CRITICAL MICELLE CONCENTRATION

The CMC was determined by surfactant physical properties such as density,

surface tension and electrical conductivity. For this research investigation

the electrical conductivity method was utilized. At first the conductivity

detector was calibrated using standard solution and the probe was washed up

with distilled water for accuracy of solutions conductance, the CMC of the

natural surfactant is obtained from the point of inflection from the plot of the

conductivity of the various different surfactant solution against the

surfactant concentration in percentage. The experimental procedures

undertaking to obtain the conductivity of the different surfactant

concentrations is shown below.

 1g of sodium chloride was weighed and added to 1000ml of the

laboratory distilled water (H2O).

 The solution was stirred properly until all the solute particles of NaCl

in the solvent (water) dissolved completely.

 The solution was left to stand at room temperature (30⁰C) for about

ten minutes to obtain a homogeneous solution of 1000ppm brine

solution.

xxix
  250ml of 1000ppm brine solution was poured into a calibrated

beaker.

 0.25g of the natural surfactant in powdered form was weighed and

mixed with the 250ml of the 1000ppm brine solution and left for

24hrs (one day).

The solution was sieved and the calibrated electrical conductivity meter is

used to obtain the conductivity of prepared solutions.

The steps above was repeated with different grams of the natural surfactant.

Nine samples of the natural surfactant solution with different concentrations

are made (1.e 1000ppm, 2000ppm, 3000ppm, 4000ppm, 5000ppm,

6000ppm, 7000ppm, 8000ppm and 9000ppm) and the conductivity of each

of the solutions were obtained.

3.5.4 PREPARATION AND FORMULATION OF SURFACTANT-

BRINE SOLUTIONS

The prepared 1.5% saline solution was kept constant for preparing the five

different surfactant-brine solutions which are 0.05%, 0.1%, 0.2%, 0.4%, and

0.6% surfactant-brine solutions. The viscosity, density and PH value of the

three solutions where measured by Ostwald viscometer, density bottle and

the PH meter at 30oC.

xxx
3.5.5 MACROSCOPIC CORE FLOODING

The constant head permeability test assemble shown below was setup.

Figure 3.1: Displacement Experiment for Single Phase Flow (Gbonhinbor et

al., 2021)

The core sample was saturated with 20,000ppm brine solution in the

saturation chamber for 5min at 29-31oC.

The core sample was then placed in the core holder.

Calibration of the injected fluid (brine) flowrate was done conventionally by

timing the volume of fluid flowing out of the discharge point.

The flowrate was held constant and increased gradually while the

corresponding pressure drop across the core sample was recorded.

xxxi
The above steps were repeated with the different prepared surfactant-brine

solutions (i.e. 0.05%, 0.1%, 0.2%, 0.4%, and 0.6%).

3.6 DATA ANALYSIS

3.6.1 DENSITY MEASUREMENT

To determine the density of the solutions prepared, the of an empty dry,

clean flask (density bottle) and liquid filled must be recorded. The ratio of

the differences between mass of the empty flask and liquid filled flask, to the

volume of the density bottle was adopted to quantitatively analyze the

density of the solutions.

3.6.2 VISCOSITY DETERMINATION

To measure the viscosity of the various prepared brine and surfactant-brine

solutions, the surfactant-brine solution or the brine is first held within the

two reference marks for the liquid volume (brine or surfactant brine

solution). The liquid is then allowed to flow through the capillary section

while simultaneously recording the time taken (efflux time). Then the

dynamic and kinematic viscosity of the liquid is calculated in accordance

with a deduction made by poiseuille’s law to laminar fluid flow in a

capillary tube.

3.6.3 POROSITY AND PERMEABILITY ANALYSIS

The two core samples were weighed using the electronic weighing balance

and saturated in the 1.5% brine solution for about 20min in the saturation

xxxii
chamber. The pore volume of the cores was calculated using equation (1),

the calculation is based on the weight different between dry and wet core

100% saturated with a brine of known density.

Wsat−Wdry
Vp =
Pbrine
……………………………………………………………………………..(1)
2
πd
Vb =
4
………………………………………………………………………………
………(2)
Vp
ɸ =
Vb
………………………………………………………………………………
………...(3)
where:
Vp= pore volume (cc)
Vb= bulk volume of the core sample (cc)
Wdry= dry weight of the core sample (g)
Wsat= saturated weight of the core sample (g)
Pbrine = density of the brine (g/cc)
ɸ = porosity of the sample (%)
L= length of the core sample (cm)
D= diameter of the core sample (cm)
The core samples where 100% saturated with brine by leaving it in the

saturation chamber for 20min. The permeability of the core samples was

calculated using a single phase displacement set up by measuring the

pressure difference along the core holder at different flow rates (1cc/min to

5cc/min). The cores were individually loaded into the core holder and then

the end-stems where connected at the inlet and outlet of the core holder.

xxxiii
1.5% brine solution was then flowed through the cores at a constant flow

rate of 1cc/min to 5cc/min. The selected flow rates were used because it is in

the range of laminar flow and the flow rate remains proportional to the

pressure gradient. The pressure drops across the cores were recorded with a

U-tube manometer and the volume of the brine produced were collected in a

graduated beaker and their values recorded. The above scenario was

repeated for 0.05%, 0.1%, 0.2%, 0.4%, and 0.6% surfactant-brine solutions

to investigate the formation damage.

qµL
K = …..
A∆P
………………………………………………………………………………
…..(4)
Where:
q = flowrate (cc/s)
A = area extent (cm2)
µ = viscosity of the fluid (cp)
∆ P = pressure drop across section (atm)

L = length of the porous medium (cm)

K = absolute permeability (D)

xxxiv
 CHAPTER FOUR

RESULT AND DISCUSSION

The most imperative objective of this research experimental work was to

investigate the impact of how locally sourced surfactant (I.e., Vernonia

amygdalina Leaf.) Influences the two major petrophysical properties

(porosity and hydraulic conductivity) of Niger Delta reservoir core sample.

This chapter focus on the result and discussion of the obtained result from

characterization of the leave extract and core flooding experiment

conducted.

4.1 PROPERTIES OF THE PREPARED SOLUTIONS

The viscosity, pH values and specific mass (density) results of the prepared

brine and surfactant-brine solutions obtained from the investigation

experimentally is tabulated below.

Table 4.1 Properties of the prepared solutions.

C(%) ρ(g/cc) pH υ(cp)

1.5-B 1.0895 6.5 0.0887
0.05- 1.0906 6 0.0931
SB
0.1-SB 1.091 5.5 0.09422
0.2-SB 1.0943 5.3 0.0973
xxxv
 0.4-SB 1.0952 5.1 0.0988
0.6-SB 1.1008 4.9 0.1005

4 C (%)
ρ (g/cc)
3 PH
υ (cp)
2

0
1 2 3 4 5 6

Figure 4.1: Bar chart representation on the properties of the prepared

solutions

The results presented from table 4.1 and figure 4.1 above showed an a

decline in pH value while the viscosity and density increases as the

concentrations increases meaning that the addition of surface active agent to

a saline solution will definitely enhance the properties of the prepared saline

solutions.

4.2 THE CMC OF THE NATURAL SURFACTANT

CMC of natural surfactant sample is indicated on a plot in Fig. 4.2 The CMC

for test surfactant was found to be 0.25%. The conductivity rises linearly

with increasing surfactant concentration until it reaches a specific point

beyond which conductivity changes its slope and increases linearly with

xxxvi
lower slope. The point on the graph where conductivity changes its slope is

the CMC of the test surfactant.

Figure 4.2 the critical micelle concentration for the natural surfactant

(Vernonia amygdalina Leaf.)

From the graph above it s clear that as the concentration of the solution

increases, monomers of the surfactant are aggregately adsorbed and tend to

form micelles concentration. This aggregation can form one or two layer(s),

and the hydrophobic interaction of the surfactant molecules leads to level of

critical micelle increase in the adsorption (Azam et al., 2013 and Wu et al.,

2017). According to Tagavifar et al. (2018) surfactant properties such as pH,

ionic strength, temperature, and adsorbent concentration can affect the

adsorption of surfactant and have the influence in the behaviours of the

dissolution of the mineral and surfactant precipitation.

xxxvii
4.3 POROSITY ESTIMATION AFTER SATURATION

The absolute porosities of the obtained reservoir core sample after been

saturated one hundred percent in a vacuum saturation assembly with the

control sample (15,000ppm brine) and various prepared surfactant-brine

solutions were calculated by taking the difference between the wet mass and

dry mass of the core plug divided by the bulk volume (volume of the

cylindrical core), the core which were experimented on could have a

substantial absolute porosity due to inter-connected throat in the reservoir

core sample. The table below shows estimated result quantitatively.

Table 4.2 porosity and core sample characterization.

Niger delta reservoir sandstone core sample

C Ρ L = 6.94cm D = 3.83cm
(%) (g/cc) Mdry Mwe Vp Vb Φ
(g) (g) (cc) (cc) (%)

1.5-B 1.0895 146.17 160.5492 13.19800 79.9874 16.5

0.05-SB 1.0906 146.17 159.4199 12.14927 79.9874 15.19

0.1-SB 1.091 146.17 159.25999 11.99816 79.9874 15

0.2-SB 1.0943 146.17 158.5599 11.32230 79.9874 14.16

0.4-SB 1.0952 146.17 158.4199 11.18517 79.9874 13.98

0.6-SB 1.1008 146.17 157.2199 10.03815 79.9874 12.55

xxxviii
 THE GRAPH OF POROSITY AGAINST THE
18
BRINE AND SURFACTANT-BBRINE SOLUTION
16 f(x) = − 0.0525 x⁵ + 0.91583333 x⁴ − 6.04083333 x³ + 18.6341667 x² − 27.0366667 x + 30.08
14
12
10
φ (%)

8
6
4
2
0
0 1 2 3 4 5 6 7
C (%)

Figure 4.3: Graphical representation of porosity against the prepared

concentrations.

As shown from figure 4.3 above which is a bar chat representation of how

the various solutions affect the ability of Niger delta subsurface reservoir

core sample to accumulate hydrocarbon, the laboratory test result obtained

and analyzed quantitatively verifiers that surfactant-saline solutions have an

infinitesimal effect on the pivoted petro physical property (porosity) of the

Niger delta porous and permeable formation core sample.

4.4 HYDRAULIC CONDUCTIVITY TEST

This is an experimental technique that measures the absolute permeability by

pumping the fluid of interest (brine and surfactant-brine solutions) with

known viscosity horizontally via the ascertained cylindrical core sample.

The flowrate was unaltered, while the corresponding difference between the

xxxix
 inlet and outlet capillary pressure was recorded and tabulated in table 4.4

Consequently, the absolute permeability is deduced using Darcy’s equation.

Table 4.3 Test Result Obtained From Hydraulic Conductivity Test

15,000PPM BRINE SOLUTION

S/N P1 P2 ΔP ΔP V T Q Q
(mmH2O) (mmH2O) (mmH2O) (atm) (cc) (s) (cc/s) (cc/min)
1 5 5 10 0.0009678 0.60 152 0.003947 0.2368
2 6 6 12 0.0011614 0.65 137 0.00474 0.28467
3 7 7 14 0.0013549 0.62 100 0.00620 0.37200
4 9 9 18 0.0017421 0.90 110 0.00818 0.49091
5 11 11 22 0.0021292 1.30 150 0.00867 0.5200
6 12 12 24 0.0023228 1.00 90 0.0111 0.66667
7 13 13 26 0.0025516 0.95 81 0.011728 0.70370
8 15 15 30 0.0029035 1.00 80 0.01250 0.75000
9 18 18 36 0.0034842 1.30 70 0.01857 1.11429
500PPM SURFACTANT-BRINE SOLUTION
1 5 5 10 0.0009678 1.10 190 0.00597 0.34727
2 6 6 12 0.0011614 0.80 130 0.00615 0.36923
3 7 7 14 0.0015985 1.20 140 0.00857 0.514286
4 9 9 18 0.0017421 1.40 160 0.0875 0.52500
5 11 11 22 0.0018195 1.00 100 0.0100 0.60000
6 12 12 24 0.0019357 1.00 90 0.01111 0.66667
7 13 13 26 0.0021290 1.63 80 0.020375 1.22250
8 15 15 30 0.0023230 1.60 60 0.026667 1.60000
9 18 18 36 0.0029035 2.00 70 0.02857 1.714285
1,000PPM SURFACTANT-BRINE SOLUTION
1 11 11 22 0.001219 0.50 100 0.00500 0.30
2 12 12 24 0.0023228 0.70 105 0.00667 0.40
3 13 13 26 0.0025164 0.60 75 0.00800 0.48
4 14 14 28 0.0028067 0.50 50 0.01000 0.60
5 15 15 30 0.0029035 1.00 75 0.01333 0.80
6 16 16 32 0.0030971 1.23 70 0.01757 1.05
7 19 19 38 0.0036778 1.20 40 0.03000 1.53
8 21 21 42 0.0040649 1.30 39 0.03333 2.00
9 23 23 46 0.0044521 0.90 20 0.04500 2.70
2,000PPM SURFACTANT-BRINE SOLUTION
1 3 3 6 0.000581 0.65 167 0.003890 0.233533
2 4 4 8 0.000774 0.80 150 0.005330 0.32000
3 5 5 10 0.000967 0.60 100 0.006000 0.36000
4 6 6 12 0.0011614 0.80 120 0.006667 0.40000
5 7 7 14 0.0013597 0.82 80 0.010250 0.61500
xl
6 9 8.5 17.5 0.0016937 0.62 50 0.012400 0.74400
7 10.5 10.5 21 0.002032 0.85 60 0.014167 0.85000
8 11 11 22 0.0021293 1.10 65 0.016920 1.01538
9 13 13 26 0.002516 0.97 40 0.024250 1.45500
4,000PPM SURFACTANT-BRINE SOLUTION

1 6 6 12 0.001161 0.80 130 0.006154 0.36923

2 11 11 22 0.002129 0.60 90 0.006667 0.40000
3 12 12 24 0.0023228 0.60 70 0.0085714 0.51428
4 13 13 26 0.002516 0.62 60 0.0103333 0.62000
5 15 15 30 0.0029035 1.00 80 0.0125000 0.75000
6 16 16 32 0.003097 0.82 55 0.014909 0.89454
7 17 17 34 0.0032906 0.80 40 0.020000 1.20000
8 19 19 38 0.003678 0.85 30 0.028333 1.70000
9 22 22 44 0.004258 0.95 25 0.0.03800 2.28000
6,000PPM SURFACTANT-BRINE SOLUTION
1 10 10 20 0.001935 0.40 60 0.006667 0.40000
2 11 11 22 0.002129 0.50 50 0.010000 0.60000
3 14 14 28 0.002709 0.42 30 0.014000 0.84000
4 174 17 34 0.003290 0.60 40 0.015000 0.90000
5 19 18 37 0.003550 0.42 19 0.022111 1.32632
6 23 22 45 0.004355 0.80 25 0.032000 1.92000
7 24 24 48 0.004646 0.65 18 0.036111 2.16667
8 26 25 51 0.004936 0.70 16 0.043752 2.62500
9 28 27 55 0.005330 0.95 21 0.045240 2.71428

1.2 Graph of q Vs Δp for 15,000ppm-B

1
flowrate (cc/min)

0.8

0.6

0.4

0.2

0
0.0005 0.001 0.0015 0.002 0.0025 0.003 0.0035 0.004
pressure drop (atm)

Figure 4.4 The graph of flowrate against pressure drop when 1.5%-B was

injected into the core sample.

xli
 1.8 Graph of q Vs Δp for 500ppm-SB
1.6 f(x) = 820.852377483199 x − 0.672322427206687

1.4
1.2
flowrate (cc/min)

1
0.8
0.6
0.4
0.2
0
0.0005 0.001 0.0015 0.002 0.0025 0.003 0.0035
pressure drop (atm)

Figure 4.5: The graph of flowrate against pressure drop when 0.05%-SB was

injected into the core sample.

Graph of q Vs Δp for 1000ppm-SB

3

2.5
flowrate (cc/min)

2 f(x) = 773.129436723541 x − 1.22901272184112

1.5

0.5

0
0.001 0.0015 0.002 pressure
0.0025 drop 0.003
(atm) 0.0035 0.004 0.0045 0.005

Figure 4.6: the graph of flowrate against pressure drop when 0.1%-SB was

injected into the core sample.

xlii
 Graph of q Vs Δp for 2000ppm-SB
1.6
1.4
flowrate (cc/min)

1.2 f(x) = 578.901697318229 x − 0.184083546503646

1
0.8
0.6
0.4
0.2
0
0 0.0005 0.001 0.0015 0.002 0.0025 0.003
pressure drop (atm)

Figure 4.7: the graph of flowrate against pressure drop when 0.2%-SB was

injected into the core sample.

Graph of q Vs Δp for 4000ppm-SB

2.5

2
f(x) = 644.248715726606 x − 0.84527289012136
flowrate (cc/min)

1.5

0.5

0
0.001 0.0015 0.002 pressure
0.0025 drop (atm)
0.003 0.0035 0.004 0.0045

Figure 4.8: the graph of flowrate against pressure drop when 0.4%-SB was

injected into the core sample.

xliii
 Graph of q Vs Δp for 6000ppm-SB
3

2.5 f(x) = 698.797758040555 x − 1.05380003159705

slowrate (cc/min)

1.5

0.5

0
0.0015 0.002 0.0025 0.003 0.0035 0.004 0.0045 0.005 0.0055 0.006
pressure drop (atm)

Figure 4.9: the graph of flowrate against pressure drop when 0.05%-SB was

injected into the core sample.

Table 4.4 Hydraulic conductivity test result estimation

Niger delta reservoir sandstone core sample

L = 6.94cm A = 11.52556cm D = 3.83cm

C(%) υ(cp) Δq/Δp K (mD)

(cc.atm/min)

1.5-B 0.0887 725.883 35622

0.05-SB 0.0931 820.85 42210

0.1-SB 0.09422 773.13 41437

0.2-SB 0.0973 578.9 31026

0.4-SB 0.0988 644.25 35029

0.6-SB 0.1005 698.8 38417

xliv
 A graph of absolute permeabities against the prepared
45000 surfactant
42210
solutions
40000 f(x) = − 545.083333 x⁵ + 9273.29167 x⁴ − 57682 x³ + 159636.708 x² − 190749.917 x + 115689
41437
38417
35000 35622 35029
30000 31026
25000
K (mD)

20000
15000
10000
5000
0

C(%)

Figure 4.10: Graphical representation of the hydraulic conductivities against

brine and surfactant-brine solutions.

The analyzed result shows that surfactant-brine solutions have a minimal

effect on the petro physical property (permeability) of the subsurface

sandstone core sample, as showed from figure 4.10 a partial sinusoidal

relationship was established as the surfactant-brine concentration increase.

Normally, the formation particles present in sandstone core plug reacted

with the injected fluids of interest (naturally sourced surfactant) as such

migration and trapping of the particles was activated. As seen in the plot of

permeability against control sample and surfactant-brine solutCOions.

xlv
 CHAPTER FIVEE

CONCLUSION AND RECOMMENDATION

5.1 CONCLUSION

The investigation of permeability and porosity were carried out

experimentally to evaluate the effects of natural surfactant on sandstone core

sample. Based on how important the results of this research work, a series of

experiments, such as saturation test, and constant head permeability test

were conducted at surface condition to verify the distinctive petrophisical

impairment. In summary, these following conclusions can be deduced from

the test results:

1) Addition of natural surfactant (Vernonia amygdalina Leaf.) to a saline

solution decreases the pH-value of the solution.

2) The viscosity and density of the saline solutions increases as the content

of natural surfactant (Vernonia amygdalina Leaf.) increases showing a direct

proportionality.

3) The presence of Vernonia amygdalina surfactant extract-solution in Niger

Delta reservoir core sample reduces the porosity of the sandstone core plug,

as the concentration increases.

4) surfactant flooding have a partial sinusoidal effect on the permeability of

the core sample.

xlvi
5.2 RECOMMENDATION

The following recommendations are made from this research work:

 The whole investigation was carried out at room temperature (30oC)

while the temperature at the reservoir condition is very high.

Therefore temperature investigation should be conducted to obtain an

in-depth knowledge of the impact of natural surfactant (Vernonia

amygdalina Leaf.) on Niger Delta reservoir formation.

 More studies should be conducted both qualitative and quantitative in

other to obtain an in-depth knowledge of natural surfactant (Vernonia

amygdalina Leaf.) for surfactant flooding.

xlvii
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