Microfluidic Analysis of Pore-Scale Petroleum Recovery in ......Microfluidic Analysis of Pore-Scale...

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Microfluidic Analysis of Pore-Scale Petroleum Recovery in Steam Assisted Gravity Drainage Abdul Haseeb Syed A thesis submitted in conformity with the requirements for the degree of Master of Applied Science Graduate Department of Mechanical Engineering University of Toronto © Copyright 2015 by Abdul Haseeb Syed

Transcript of Microfluidic Analysis of Pore-Scale Petroleum Recovery in ......Microfluidic Analysis of Pore-Scale...

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Microfluidic Analysis of Pore-Scale Petroleum

Recovery in Steam Assisted Gravity Drainage

Abdul Haseeb Syed

A thesis submitted in conformity with the requirements for the degree of Master of Applied Science

Graduate Department of Mechanical Engineering University of Toronto

© Copyright 2015 by Abdul Haseeb Syed

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Abstract

Microfluidic Analysis of Pore-Scale Petroleum Recovery

in Steam Assisted Gravity Drainage

Abdul Haseeb Syed Master of Applied Science

Graduate Department of Mechanical Engineering University of Toronto

2015

Steam Assisted Gravity Drainage (SAGD) is an in-situ method of extracting bitumen and involves the

injection of steam into the oil sands reservoir through a horizontal well pair. The formation of a steam

chamber and heat transfer to the bitumen allows gravity drainage and production. There is presently a

lack of understanding concerning the specific mechanisms of bitumen mobilization and drainage at the

pore-scale within the SAGD process. This thesis focuses on developing and utilizing microfluidic

platforms to allow the experimental observation and characterization of the interface morphology at

the edge of the steam chamber.

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Acknowledgements

I would like to express my sincere gratitude to my supervisor, Professor David Sinton, who offered me

this wonderful opportunity to conduct my Master’s research in the very exciting and innovative field of

microfluidics. Professor Sinton’s insightful expertise, his support and advice helped me greatly to

achieve this work.

I would like to thank all the members of the team, in particular I would like to thank Nader Mosavat who

helped me during my experimental work and shared his valuable knowledge. My special thanks goes out

to Pushan Lele for his friendly collaboration and the many interesting conversations we had on a wide

range of topics, I also extend my gratitude to Seven Qi who spent many long hours helping me with the

very involved process of microchip fabrication. My thanks to Ryan Mendell who helped me understand

how to design reliable devices and demystify the fine details mechanical design. I would like to thank

Jason Riordon, Huawei Li, Bo Bao, Phong Nguyen, Tom Burdyny for providing their support whenever I

needed. I would like to thank Percy Graham, Matt Ooms and Scott Pierobon for their input.

I would like to thank my family immensely for giving me unlimited support!

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Table of contents

Abstract ................................................................................................................................ ii

Acknowledgements .............................................................................................................. iii

Table of Contents ..................................................................................................................iv

List of Figures ........................................................................................................................vi

1.0 Foreword ......................................................................................................................... 1

1.1 Motivation ................................................................................................................................. 1

1.2 Thesis Overview ........................................................................................................................ 2

2.0 Introduction to Microfluidics & Oil Sands ......................................................................... 4

2.1 The Potential of Microfluidics in Petroleum Research ............................................................. 4

2.2 Review of Oil Sands Resources & Extraction Technologies ...................................................... 5

2.2.1 Characteristics of Oil Sand Reservoirs ....................................................................... 6

2.2.2 Steam Assisted Gravity Drainage (SAGD) .................................................................. 8

2.2.3 Theoretical Model of SAGD and Research Topics ................................................... 10

2.2.4 Effect of IFT, Viscosity & pH on Petroleum Recovery .............................................. 14

2.3 Fluid Mechanics in Microfluidic Context ................................................................................ 15

2.4 Glass Micromodel Fabrication Method .................................................................................. 19

3.0 Micromodel Analysis of Pore-Scale SAGD Recovery ........................................................ 19

3.1 Experimental Apparatus & Platform Development ................................................................ 19

3.1.1 Experimental Apparatus ....................................................................................... 19

3.1.2 Micromodel Design ............................................................................................... 20

3.1.3 Manifold Design .................................................................................................... 22

3.2 Pore-Scale Analysis of Additive Effect on SAGD Interface ...................................................... 23

3.2.1 SAGD Micromodel Recovery ................................................................................. 23

3.2.2 Physical Morphology of Steam-Bitumen Interface ............................................... 27

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3.2.3 Thermal Morphology of Steam-Bitumen Interface .............................................. 35

3.2.4 Pore-Scale Fluorescence Imaging of Steam-Bitumen Interface ........................... 40

3.2.5 Key Findings on the Nature of Pore-Scale Steam Front Dynamics ....................... 42

3.3 Bitumen Displacement from Gasification of Reservoir Liquid ................................................ 46

3.4 Emulsion Analysis & Segmentation Algorithm ....................................................................... 49

4.0 Conclusion & Future Directions ..................................................................................... 53

Appendix A: PEEK Manifold CAD Drawings .......................................................................... 54

Appendix B: Glass Fabrication Standard Operating Procedure ............................................. 56

Appendix C: Semi-Automated Emulsion Analysis Standard Operating Procedure ................. 65

Bibliography ....................................................................................................................... 80

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List of Figures

Figure 1 - Distribution of bitumen, water and sand grains within the oil sands deposits ............................ 6

Figure 2 – (A) Cross sectional view of Idealized SAGD steam chamber (B) Pore-scale SAGD recovery at

the interface (C) Side view of injection (red) and production (blue) horizontal wells in SAGD ................. 10

Figure 3 - Schematic representation of heat transfer & fluid flow at the steam chamber interface based

on the assumptions for the Butler equation (Author’s reproduction of figure from *22+) ........................ 11

Figure 4 - Glass chip fabrications steps with image of fabricated chip ...................................................... 18

Figure 5 – Schematic of experimental apparatus for SAGD micromodel ................................................... 19

Figure 6 – (A) Pore-scale SAGD recovery at the interface (B) Pore network pattern in micromodel ........ 20

Figure 7 – Unit cell of pore network pattern prior to etching (photomask, left) and after etching .......... 20

Figure 8 – Distribution of post and of pore throat within a single the unit cell of the pore network ........ 21

Figure 9 – Steel manifold is shown on the left and PEEK manifold on the right. ....................................... 22

Figure 10A – Time-lapse progression of Steam (0ppm additive) injection test ......................................... 24

Figure 10B – Time-lapse images of steam + 200pppm additive injection test ........................................... 24

Figure 10C - Time-lapse images of steam + 2000pppm additive injection test .......................................... 25

Figure 11 – Bitumen Recovery vs. Time ...................................................................................................... 26

Figure 12 - Final Recovery vs. additive concentration in ppm .................................................................... 26

Figure 13 – Steam chamber interface for steam (0 ppm), 200ppm, 2000ppm additive

(A – In-situ bitumen, B – Leading Edge, C – Lagging Edge, D – Steam Chamber) ....................................... 28

Figure 14 – Bitumen recovery through droplet generation at the interface (Time-lapse: 2 sec) .............. 30

Figure 15 – Finger Displacement of bitumen (Time-lapse: 1 min) ............................................................. 31

Figure 16 – Non-directional Gravity Drainage at the top of steam chamber (Time-lapse: 5min) .............. 31

Figure 17 – Emulsion generation under limited bitumen drainage rate at outlet port ............................. 32

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Figure 18A – Steam vapor bubble invasion & trapping into lagging edge ................................................. 33

Figure 18B – Maximum extent of steam invasion into lagging edge (steam test) .................................... 34

Figure 19A – Trapped Steam bubble condensation (Time-lapse: 2min) ................................................... 34

Figure 19B – Size of condensing trapped steam droplet vs. Time .............................................................. 35

Figure 20 - Time-lapse thermal images over the 160 minute duration of the tests .................................. 36

Figure 21 – Thermal & Physical Steam Chamber Comparison: Lagging edge acts as barrier to steam

chamber expansion .................................................................................................................................... 37

Figure 22 – Temperature profile at the interface ...................................................................................... 38

Figure 23 – Comparison of the rate of advance of leading & lagging edge of steam chamber ................ 39

Figure 24 – Fluorescent (bitumen = green) & Brightfield (bitumen = black) post-run microscope images .... 41

Figure 25 – Small water droplets are observed in the bitumen ahead of the leading edge ..................... 41

Figure 26 – Bitumen droplets drainage ahead of the interface ................................................................. 42

Figure 27 – Physical model allows evaluation of validity of interface assumptions .................................. 45

Figure 28 – Gasification of liquid volume over 45 minutes leads to 35% bitumen displacement ............. 47

Figure 29 – Pore-scale view of gas expansion (left) and liquid finger region (right) .................................. 47

Figure 30 – Fluorescence microscope images of bitumen displacement in gas & liquid region ................ 48

Figure 31 – (Top) Original image of emulsion (Bottom) Semi-automated analysis ................................... 50

Figure 32 – Semi-automated analysis particle size distribution (corresponding to Figure 31) .................. 51

Figure 33 – Automated image segmentation of the SAGD interface ......................................................... 52

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1.0 Foreword

1.1 Motivation

Petroleum is a major component of the world’s energy supply. Petroleum is an energy dense, highly

portable fuel and is of particular importance for transportation. The ability to economically transport

people and freight over long distances is a key enabler of modern trade and economic activity. It was

estimated that in 2012, the combustion of petroleum fuels provided 92% of the energy used for

transportation in the United States [1]. Energy demand has grown 51.8% from 1985 to 2013 from 60,083

to 91,195 thousand barrels per day and is expected to climb further commensurate with an increase in

population and economic development in emerging economies [2, 3].

Recent data shows that conventional oil discoveries peaked in the 1960s with a steady decline in

subsequent decades, very few giant oil fields have been found since the early 1980s and 261 of the 507

known giant oil fields are already in their decline phase [4]. On the other hand, the volume of

conventional oil consumed has increased commensurate with industrialization and economic

development. The widening gap between the forecast demand and conventional productions means

that unconventional resources may have to be developed to meet demand. Some factors affecting the

future demand for petroleum includes the price of oil (with lower prices encouraging consumption) and

the development of alternatives to petroleum for transportation (with electric vehicles, ethanol-based

fuels lowering petroleum demand).

Due to the slowdown in new discoveries of large conventional oil fields and the continued increase in

petroleum demand, there has been increased interest in developing unconventional petroleum

resources. Greater development has taken place in terms of shale gas, heavy oil, carbonate reservoirs

and oil sands. However, extraction from the unconventional reservoirs presents a host of complex

technical challenges and significant investment has been made in research work to better understand

these new resources. Canada holds a large reserve of unconventional petroleum in the form of oil sands

with 169 billion barrels of proven reserves amounting to 98% of total Canadian reserves and giving the

country the 3rd largest petroleum reserves after Saudi Arabia and Venezuela. However, numerous

technical and environmental challenges must be overcome in order to develop the oil sands in a

sustainable manner [5].

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Approximately 20% of the Canadian oil sands reserves can be extracted through mining as the deposits

are close to the surface but the remaining 80% require in-situ methods for recovery. Steam assisted

gravity drainage (SAGD) is an important extraction technique enabling in-situ recovery from oil sands

formations. SAGD essentially involves the injection of steam into the underground reservoir to heat the

bitumen and allow recovery through gravity drainage [6].

Research into the SAGD process has mostly occurred in the form of simulation studies or core flood

experiments. A significant limitation of core flood tests is the inability to visualize exactly what is

happening at the advancing steam interface; furthermore it is difficult to reproduce consistent

experimental conditions due to core changes through chemical deposition or permeability damage.

Simulation models require some level of simplification of the process since it is difficult to model multi-

phase flow while also accounting for heat transfer, phase change, steam condensation and a moving

steam front. Solving simulation models may take a long time and it is also be difficult to history match

simulation results with field data, specifically at the pore scale.

Microfluidic pore-scale models provide an important tool to study oil recovery beyond simulations and

core floods. The micromodel provides a platform for direct experimental observation and

characterization of the specific mechanisms associated with oil recovery from the reservoir at the pore-

scale. The objective of our work is to develop and use a microfluidic platform to investigate the

mechanisms of bitumen displacement and drainage at the pore-scale within the context of the SAGD

process. The effect of alkaline additive on the bitumen recovery was also investigated.

1.2 Thesis Overview

Chapter 1 begins by presenting the motivation for this work followed by an overview of the thesis.

Chapter 2 is an introduction to microfluidics and oil sands. A review of oil sand characteristics and the

steam assisted gravity drainage (SAGD) process is provided, along with a review of relevant microfluidic

concepts and glass micromodel fabrication methods.

Chapter 3 discusses the experimental apparatus as well as the characteristics of the pore network in the

micromodel. Section 3.2 presents the main study conducted on the pore-scale analysis of the SAGD

interface and the effect of alkaline additive at various concentrations. A second study of bitumen

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displacement through porous media as a result of gas generation from a trapped liquid volume is

presented in section 3.3. Semi-automated methods for image and emulsion analysis developed during

the course of the research are discussed in section 3.4.

Chapter 4 explains future directions that could be pursued based on the high temperature-pressure

micromodel developed in this work.

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2.0 Introduction to Microfluidics & Oil Sands

2.1 The Potential of Microfluidics in Petroleum Research

Microfluidics is a multi-disciplinary field of research that focuses on the manipulation and study of small

volumes of fluids, typically 10-9 to 10-18 liters, at small scales. A microfluidic device typically consists of a

portable chip that contains a network of channels, junctions and components with a geometry that

allows the processing of injected fluids. Microfluidic devices represent a miniaturization of fluid handling

systems that allow accurate fluid metering, transport, mixing, and separation. These devices have been

manufactured from a range of materials including glass, polymer (PDMS, PMMA, and Teflon), silicon,

paper and even carbonates. [7-10].

Inkjet printers in the 1950s marked an important milestone in the accurate handling of small volumes of

fluid; the precursor to modern microfluidics was the gas chromatograph technologies of the 1970’s

which allowed for the first time very high resolution and sensitivity measurements [11, 12]. Microfluidics

today is used as a platform for research in a wide variety of fields ranging from molecular biology to

solubility analysis to cooling of integrated circuits [13, 14]. Microfluidics research can either focus on

developing new capabilities in terms of small scale fluid handling or on studying the science of fluid

behavior at the small scale. Microfluidics devices provide an effective platform to investigate research

topics on the behavior of fluids at the micrometer or nanometer scale.

Microfluidics technology has the potential to play an important role in the petroleum sector in the

context of both laboratory research and field applications. Oil samples are a valuable resource and there

are economic and logistical benefits in reducing the sample fluid volume required in petroleum research

and testing. Microfluidics provides an ideal solution to allow the extraction of meaningful data from

small volumes of oil using an inexpensive and portable device.

For instance, Hossein et al developed a microfluidics device to perform CO2 diffusivity measurements in

bitumen and reduced the time required for these measurements from days to 10 minutes and the fluid

requirements from 0.5L to 1nL [14].

Some commercialization of lab-scale microfluidic equipment has already taken place. One example that

is relevant for the petroleum industry is the measurement of asphaltenes. Crude oil is a complex mixture

of a wide variety of hydrocarbon fractions and one of the heaviest and most aromatic fractions in

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petroleum is the asphaltene fraction. The manual method for asphaltene measurement is prone to

human error since fluids are dispensed manually and asphaltene precipitation is observed by eye. A

compact and portable microfluidic device was developed by Fraunhofer for asphaltene analysis. The

device is able to dispense precise volumes of fluid and uses multi-wavelength imaging techniques to

identify asphaltene precipitation and is able to remove subjectivity from the process [53].

An important aspect of microfluidics is the ability to fabricate chips that incorporate a complex network

of pores from transparent materials while retaining the ability of the device to withstand high

temperatures and pressures. Due to the steady depletion of previously established oil fields, new

ventures in petroleum extraction are increasingly tapping into unconventional petroleum resources with

complex micro-scale geometries including shale gas, heavy oil, carbonate reservoirs and oil sands.

The precise mechanism of oil recovery at micrometer scales within porous media in unconventional

reservoirs is not well understood and microfluidics can be a useful tool in this context since it allows

direct visual observation of oil recovery throughout the model.

The value of microfluidic tools is that they provide a smaller, transportable, inexpensive method for

petroleum testing with much lower sample volume requirements. Microfluidics can especially useful as

a screening tool for more comprehensive tests, leading to significant reduction in the misallocation of

time and capital.

2.2 Review of Oil Sands Resources & Extraction Technologies

Canadian oil sands are a massive resource with an estimated 1.8 trillion barrels of bitumen in-place of

which 168.7 billion barrels are considered to be reserves that can be economically recovered using

current technology. Canada also initially had 18 billion barrels of conventional oil reserves of which 16.5

billion barrels has been produced and a further 1.5 billion remains to be produced [15, 16]. The oil sand

deposits are largely located in northern Alberta; the largest fields are Athabasca, Peace River and Cold

Lake.

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2.2.1 Characteristics of Oil Sand Reservoirs

Petroleum deposits are formed by the decomposition of organic matter at a suitable depth and

temperature over geological time scales. The oil sands in Alberta are thought to have been formed by

the same geological processes that lead to the formation of the Canadian Rocky Mountains. The exact

process by which the oil sands were formed is a matter of debate, one possibility is that the rise of the

Pacific tectonic plate over the North American tectonic plate may have caused the deep burial of the

sedimentary rock layers of the Alberta plains and the subsequent conversion of kerogen into light oil

and natural gas took place due to the high temperatures. The light oil then migrated up through hydro-

dynamic transport and microbial action near the surface resulted in the degradation of the light oil into

bitumen [17, 18].

Oil sands deposits consist of highly viscous bitumen hydrocarbons trapped in the porous volume

between unconsolidated sand grains in underground formations. A schematic representation of oil

sands is provided in Figure 1, showing also the presence of small pockets of trapped water between

grains. Fine clusters of clays are also present but not shown in the figure. Various studies suggest the

existence of a thin connate water film, of approximately 10 nm, surrounding the sand grains [19, 23-25].

Figure 1 – Diagram of distribution of bitumen, water and sand grains within the oil sands deposits

The oil sand deposits are found at a depth of up to 700 m, with reservoir temperature between 8˚C and

20˚C and the initial reservoir pressure is on the order of 300 to 500 kPa [21, 27]. The bitumen-rich

region of the oil sands deposit that is viable for extraction is known as the pay zone and the pay

thickness is on the order of 10 to 40 m, with a minimum thickness of 10 m for a field to be considered

economically viable [26].

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The quality of the oil sands ore can vary significantly between fields. Typical ore will consist of 85 wt%

sands grains and fine particulates, 12 wt% bitumen and 3 wt% water. The quartz grains are angular in

shape and range from 160 µm to 250 µm in diameter [21, 47]. There are also clusters of fine particles

including kaolinite, smectite and illite that are generally less than 2 µm in diameter. Lower grade oil sand

ore may contain more than 20 wt% of fine clays while higher grade ore will have less than 5 wt% [22].

Typical oil sands porosity varies between 30-35% and permeability is typically on the order of 1 to 6 D

[27, 21]. Most in-situ bitumen contains some amount of dissolved natural gas and there are also small

pockets of gasses within the reservoir [22]. The study of oil sand characteristics is complicated by the

difficulty in analyzing the ore underground and the tendency for changes to occur within the ore when it

is removed from the reservoir and disturbed by depressurization [20, 21].

Various studies have suggested the presence of water in the oil sands deposits, which may exist

between the sand grains, within clusters of fine clays or as a thin film of connate water over the surface

of the quartz grains. The connate water layer is estimated to be approximately 10nm thick but is

sufficient to ensure no direct contact between the bitumen and quartz. This layer of water, combined

with the hydrophilic nature of the quartz, plays an important role in enabling the easy recovery of

bitumen since the sand is not oil-wet. It should be noted that oil sands reservoirs exhibit significant

heterogeneity. Frequent variations in reservoir geometry and bitumen properties complicate field-scale

recovery.

The form of oil found in the oil sands is an extremely viscous hydrocarbon substance known as bitumen.

While properties vary between fields, typical bitumen will have an elemental composition of

approximately 83.2% Carbon, 10.4% hydrogen, 0.94% oxygen, 0.36% nitrogen and 4.8% Sulphur. The

viscosity of in-situ bitumen in the reservoir typically exceeds 1x106 cP and can in certain locations go

higher than 6x106 cP [28]. Bitumen density is on the order of 1.01 g/cm3 at room temperature and

pressure. The very high viscosity of the bitumen is one of the primary factors making bitumen recovery

and processing more difficult [21, 29].

API gravity is an important measure for the classification of oil. The API gravity, standardized by the

American Petroleum Institute, represents the relative density of a substance compared to the density of

water. API gravity has no units but is expressed in degrees. Oil with an API gravity of more than 10˚ will

float in water and less than 10˚ will sink in water. API gravity is used to categorize oil into light (>31.1˚),

medium (22.3 ˚ - 31.1 ˚), heavy (10 ˚- 22.3 ˚) and extra-heavy (<10 ˚). Bitumen from Canadian oil sands

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formations has API gravity ranging from 6 to 12 and is considered a form of extra-heavy oil [30, 31]. The

equation for API gravity is as follows:

˚API = API gravity SG = specific gravity

The constituent components of bitumen are often separated, on the basis of chemistry, into saturates,

aromatics, resins and asphaltenes. Saturates include non-polar linear, branched and cyclic saturate

hydrocarbons, aromatics contain aromatic rings and are more polar, resins and asphaltenes are large

aromatic molecule. Asphaltenes precipitate out of the oil in excess pentane (C5 asphaltenes) or heptane

(C7 asphaltnenes).

The tendency of asphaltenes to precipitate on process equipment due to high temperatures or changes

in composition (such as addition of saturates) presents significant operational challenges in the

transport and processing of bitumen. Athabasca bitumen will typically consist of 14wt% saturates,

34wt% aromatics, 38wt% resins and 12wt% asphaltenes [30, 32].

2.2.2 Steam Assisted Gravity Drainage (SAGD)

Mining of the oil sands ore is viable only for fields located at a depth of less than 70m from the surface.

From the 169 billion barrels of bitumen in reserve, only 20% can be recovered through mining and the

remainder must be produced by in-situ methods [5, 33].

In-situ recovery of bitumen has been a practical engineering problem with substantial economic

implications. Conventional water flooding is not viable since bitumen has a viscosity in excess of

1,000,000 cP at reservoir conditions. Furthermore, even in heavy oil reservoirs, the injected water has a

tendency to exhibit significant fingering displacement, resulting in a large portion of residual oil

remaining in the reservoir [42].

A major development enabling the economical extraction of Alberta oil sands on a large scale was the

development of horizontal wells and steam injection. Roger M. Butler developed the process of steam

assisted gravity drainage (SAGD) in the 1970’s and participated in the pilot plant testing of SAGD in 1978

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in the Cold Lake deposit. The SAGD process has since been applied on a commercial scale and in 2009

accounted for 242,000 barrels per day of production (18% of the total production) and is expected to

increase in the future as minable reserves are depleted [22, 34].

Steam assisted gravity drainage is a thermal extraction process that begins with the drilling of two

horizontal wells vertically aligned with each other inside the pay zone, steam is injected through the top

well leading to the formation of a steam chamber after an initial start-up period. The steam condenses

at the edge of the chamber resulting in the transfer of the latent heat of condensation to the bitumen

and the subsequent drainage of the lower viscosity heated bitumen due to gravity; Figure 2 illustrates

this process. As the as the bitumen is drained and produced, the empty pore space becomes filled with

steam. The steam chamber grows upwards and sideways over time. A large number of factors affect

SAGD and can broadly be separated into three categories: reservoir properties, bitumen characteristics

and steam parameters. Reservoir and bitumen properties are discussed in more detail in 2.2.1.

The high energy requirements associated with steam generation are a major cost of the SAGD process

and there is strong interest in reducing the energy intensity of SAGD. The steam-oil-ratio (SOR) is a key

measure of efficiency that compares the barrels of water (turned into steam) required for the recovery

of one barrel of bitumen. SOR can be between 4 to 5 during the initial start-up phase of the SAGD

process and can drop down to 2-3 a few years into production [35].

The SOR can be measured as either Cumulative steam-oil ratio (CSOR) averaging the volume of steam

required per barrel over the lifetime of the SAGD process or Instantaneous steam-oil ratio (ISOR) which

measures the number of barrels of water required at any given time to produce a barrel of oil. The SOR

will be high during the initial phases of the SAGD project due to the start-period that requires the

injection of steam to create the steam chamber prior to production [34].

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Figure 2 – (A) Cross sectional view of Idealized SAGD steam chamber (B) Pore-scale SAGD recovery at the

interface (C) Side view of injection (red) and production (blue) horizontal wells in SAGD

2.2.3 Theoretical Model of SAGD and Research Topics

As stated earlier, Roger M. Butler developed the process of SAGD in the 1970’s and established the basic

model and theory. The Butler equation forms the basis for the theoretical understanding of the SAGD

process and will be discussed in this section. Many modifications of Butler’s equation exist but the focus

will be on the original form of the equation since it provides a good starting point for the exploration of

SAGD models. The full derivation of the Butler equation can be found in Thermal Recovery of Oil and

Bitumen, chapter 7, only a brief overview will be provided below [22].

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Due to the hot steam rise, the chamber is expected to initially grow faster in the upward direction,

however the morphology of the typical reservoir as an elongated layer would cause the upwards growth

to be stopped by the overburden and the sideways growth of the chamber to become the dominant

aspect. Figure 3 shows a schematic view of a small section at the interface as defined in the context of

Butler’s equation, the steam chamber is on the left with the in-situ bitumen on the right.

Figure 3 - Schematic representation of heat transfer & fluid flow at the steam chamber interface based

on the assumptions for the Butler equation (Author’s reproduction of figure from *22+)

The steam is at temperature Ts and the reservoir initial temperature is Tr. Steam is condensing on the

interface which is inclined at angle θ. The interface temperature is equal to the steam temperature Ts

and heat flux due to conduction occurs into the bitumen. The interface is moving into the reservoir at a

velocity of U as a result of the difference in oil flow into section (from upstream drainage along the

interface) and the flow out of the section (due to bitumen drainage). The advance of the interface gives

rise to oil production of Q.

The full derivation of the equation can be found in [22]. The basic framework is that Darcy’s law is used

to obtain an equation describing the rate of drainage of oil, dQ, with respect to the element dξ. A

second relationship is established between the flow of oil and the interface velocity by considering the

material balance at the interface. The two equations together are used to eliminate the unknown terms

and yield the Butler equation for oil recovery for SAGD:

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Q = oil production rate

φ=porosity

∆S0 = initial oil saturation - residual oil saturation

νs =oil kinematic viscosity

m = dimensionless factor between 3-5 (based on viscosity-temperature relationship of the oil)

It is interesting to note that all of the terms in the numerator of the Butler equation are equally

weighed, meaning that the porosity, permeability, gravitational force, thermal diffusivity and reservoir

height are all equally important to bitumen drainage according to this model.

The ∆S0 term must be computed in order to solve the equation above. Butler’s theory states that the

viscosity of the residual bitumen in the steam chamber is very low, leading to continued drainage and a

lower fraction of residual oil remaining in the reservoir. The initial oil saturation would be known (from

reservoir geological assessment) and the residual oil saturation could be found using:

(

) ⁄

Sor = average residual bitumen saturation after time t νs = oil kinematic viscosity

φ = porosity k = permeability

g = gravitational force Z = drainage height

b = exponent in Cardwell and Parson's relative permeability equation

h = Net pay thickness

α = reservoir thermal diffusivity

g = gravitational force

k = permeability

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With b set to a typical value of 3.5 and Z set to equal h (the maximum possible value of Z):

(

)

The various theoretical models of SAGD (including the Butler equation) make assumptions regarding the

conditions at the interface of the steam chamber. The current understanding of the SAGD process is

limited and a number of concerns remain with the basic model. One aspect under scrutiny is the

assumption that conduction is the dominant means of heat transfer and that convection plays a minimal

role. Studies by Ito et al and Farouq-Ali et al [38, 39] suggest that convection from the flow of

condensates at the interface does in fact play a significant role in bitumen production and that assuming

heat transfer to occur exclusively through conduction is not viable. Studies by Edmunds et al and Irani et

al [36, 37, 40] indicate that the contribution of convection to bitumen recovery is minimal.

The mechanics of bitumen drainage from the top of the steam chamber are another point of debate.

The morphology of steam rise through the reservoir and the counter-current bitumen drainage is not

well understood [49, 48]. The role of condensate flow in the bitumen drainage is not clear and a

simulation study by Ito et al claims that the condensate flow adjacent to the bitumen is a major factor in

encouraging bitumen recovery [39]. Geomechanics of the steam chamber expansion is another

significant area of research, the high pressure and temperature of the steam chamber has an impact on

the rock remaining within it. Studies estimate that shear failures of sand grains due to stresses within

the steam chamber leads to increases in permeability and promotes continued chamber growth [41].

As discussed above, many of the uncertainties pertaining to the dynamics of bitumen recovery from

SAGD stem from the lack of understanding of the specific interface morphology between the advancing

steam front and the bitumen. Our micromodel work with SAGD would help to get a better

understanding about the specific dynamics of steam-condensate-bitumen interactions at the steam

chamber edge and would help to evaluate the validity of assumptions made in various models. The

experimental data from our physical model could eventually lead to improved simulation of the steam

chamber interface.

Micromodels have previously been applied in the context of petroleum recovery for carbonate

reservoirs [10], CO2 EOR [42], petroleum asphaltenes deposition [43] as well as SAGD [44, 45, 46].

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However, the limitation of the previous work was that either the pore sizes were not representative (at

1mm+), the reservoir fluid was not representative of Alberta bitumen or that the steam parameters

were not representative (due to steam injection at 100˚C and atmospheric pressure). Our present work

ensures reservoir-relevant geometries, since our micromodel grain sizes of 260 µm to 380 µm

correspond with average grain sizes in the field of 160 µm to 250 µm [21, 47]. Our study included

significant platform development that allowed the injection of steam at higher temperatures of more

than 150˚C and pressures on the order of 340 kPa.

2.2.4 Effect of IFT, Viscosity and pH on Petroleum Recovery & Emulsion Formation

At the interface between two immiscible liquids, the imbalance in molecular interactions between

dissimilar fluids gives rise to an accumulation of free energy at the interface known as the interfacial

tension (IFT). The IFT is measured in units of dynes/cm or mN/m, where 1 dyne/cm = 1mN/m, and

represents the amount of work that needs to be done to expand the interface between the two phases

isothermally. Therefore, a larger value for IFT signifies that there is a stronger tendency for the interface

between the immiscible liquids to be minimized. IFT can be measured while the interface between the

phases exists in a transient state, termed as dynamic IFT, or while the interface exists in a steady

equilibrium. [54,55]

Since IFT is a measure of the work required to expand or disturb the interface, a lowering of IFT enables

easier displacement of the oil from the pore network as the interface is less resilient to perturbation.

Another important aspect is that for gravity drainage to occur, IFT must be lowered such that capillary

forces in the pores become less significant in relation to gravitational forces. Reducing IFT between the

bitumen and the condensate leads to improved gravity drainage. [54, 55]

A surfactant consists of a single molecule with a polar head and non-polar tail works to reduce the free

energy at the interface by aligning between the water and oil phases. The polar component is oriented

into the water while the non-polar component, often consisting of hydrocarbon chains, aligns with the

oil phase. The presence of a surfactant reduces the imbalance of forces felt at the interface and reduces

the interfacial tension. An important aspect of surfactant dynamics is the critical micelle concentration

(CMC) which indicates the concentration of surfactant that is required to saturate the interface and

above which significant micelle formation in the bulk phase. A low CMC denotes high efficiency of the

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surfactant in saturating the interfaces. The reduction in surface tension is less pronounced with

increased surfactant concentration beyond CMC. [56-60]

Alkaline additives can be injected into the reservoir in order to react with the acidic components within

the oil and produce surfactants, lowering IFT. The acid content in petroleum is measured by the Total

Acid Number (TAN) which corresponds to the mass of potassium hydroxide (in miligrams) that is

required to neutralize the acid in one gram of oil and is expressed in units of mg/g. The TAN in

Athabasca bitumen typically ranges from 4 to 5.5 mg KOH/g. [61, 62]

A study has found that the surfactant-producing effect of alkaline flooding, within the context of

petroleum extraction, is generally observed at pH ranges above 9 and that a higher acid number may

not correlate directly with increased in-situ surfactant production. The precise nature of the acidic

components present within the oil determines the effectiveness of the produced surfactant in lowering

the interfacial energy. For instance, asphaltenes or resin molecules may have carboxylate functional

groups that cannot be extracted into the aqueous phase. Furthermore, short chain acids may not

produce effective surfactants because they are too hydrophilic since the short hydrocarbon chain

cannot effectively align with the non-polar phase. [63, 64] The naphthenic acids in bitumen are

predominantly cycloaliphatic carboxylic acids, comprising 10 to 16 carbons, and form an important

surfactant-generating component. [65]

2.3 Fluid Mechanics in Microfluidic Context

Reynolds Number

The Reynolds number is a ratio of the inertial forces acting on a fluid to the viscous forces. A fluid or

geometry that results in a larger Reynolds number is more likely to exhibit turbulent flow because the

effect of the inertial forces acting on the fluid will dominate. A Reynolds number less than 2300 signifies

laminar flow, and greater than 4000 will correspond to turbulent flow. Reynolds numbers between 2300

and 4000 result in a transient regime. In the context of microfluidics, the channel dimensions will

typically be on the order of tens to hundreds of microns and most fluid flow within microfluidic devices

will be laminar. The Reynolds number for flow in a channel is computed as:

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Re = Reynolds number A = Cross sectional area

μ = dynamic viscosity ν = kinematic viscosity

ρ = density v = mean velocity

DH = hydraulic diameter Q = Volumetric flow rate

Capillary Number

The capillary number represents a ratio of viscous forces to surface tension on a gas-liquid interface. The

capillary number is important in understanding the behavior of gas-liquid interfaces in micro-channels.

For a flowing liquid, a capillary number much larger than 1 indicates that viscous forces are dominant.

However, if the capillary number is much lower than 1 then viscous forces are negligible compared to

the interfacial forces.

Ca = Capillary Number μ = dynamic viscosity

V = characteristic velocity γ = surface tension

Darcy’s Law

Darcy's law describes the flow of a fluid through porous media of known permeability. Darcy's law is

valid only when the flow is laminar, under steady-state flow conditions and the porous media is

saturated. Another assumption is that the fluid is homogenous, isotherm and incompressible. Kinetic

energy is neglected which is acceptable for low fluid velocities.

Q =Volumetric flow K = Permeability

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A = Cross sectional area μ = dynamic viscosity

dP/dx = Pressure gradient

Bond Number

The bond number is a ratio of gravitational force to surface tension. A large value for the bond number

indicates that the role of the interfacial tension is minimal while a bond number of less than one

signifies that interfacial tension plays an important role in the system. Experimental studies have shown

that a large bond number has a positive effect on petroleum recovery through gravity drainage [50, 51].

g = gravitational acceleration ∆ρ = density difference between phases

L2 = characteristic length σ = interfacial tension

2.4 Glass Micromodel Fabrication Method

The main steps involved with the fabrication of the glass micromodel are detailed in Figure 4.

Fabrication of devices with a large area of micro-scale features is challenging and requires a very high

degree of care in the handling of the glass, even a small force is sufficient to damage the micron-scale

pores during the fabrication process. A comprehensive standard operating procedure was developed in

order to ensure maximum success rate during fabrication (see Appendix A). Pre-coated square Borofloat

33 glass slides of 10 cm x 10 cm x 2.25 mm in thickness were obtained from Telic.

Step 1 in Figure 4 shows the original glass is polished and pre-coated with a 300 nm thick chrome layer

and the photoresist AZ1500 is coated above it to a thickness of 5300 Angstrom. A photomask is also

printed with the desired pore pattern on a transparent polymer sheet. Step 2 involves the exposure of

the pattern whereby the portion of the photoresist not covered by the photomask is damaged. AZ400K

developer is used to remove the damaged photoresist (step 3) and the chip is baked on a hot plate at

130˚C for 30 minutes to harden the photoresist.

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Step 4 shows that the glass is then immersed in de-chromer in order to remove the exposed chrome.

After this step, the glass itself will be unprotected in the pattern of the pore space while the photoresist

and chrome will cover and protect the area corresponding to the grains.

Step 5 involves the etching of the glass using hydrofluoric acid solution prepared from a 1:3:5 ratios of

49% HF: HNO3: H2O. As displayed in the figure, the etching occurs in an isotropic manner, meaning that

the exposed glass is etched both in depth and sideways. This will result in a shrinking of the grains in the

pore network and the mask must be designed to accommodate this effect.

The etched glass is then cleaned with piranha solution (1 H2O2: 2 H2SO4), which will remove the

photoresist. The exposed chrome is also removed with de-chromer (step 6) and piranha cleaning is

repeated. The etched glass is then taken to an optical profilometer in order to measure the exact

etching depth. The bottom left corner of Figure 4 shows an optical profilometer measurement. The

target etch depth is 50 µm for our micromodel this is achieved within +/-5%. The final step involves the

thermal fusion bonding of the cover glass on top of the pore network at 645°C for 10+ hours. An image

of a fabricated chip is shown at the bottom right.

Figure 4 - Glass chip fabrications steps with image of fabricated chip

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3.0 Micromodel Analysis of Pore-Scale SAGD Recovery

3.1 Experimental Apparatus & Platform Development

3.1.1 Experimental Apparatus

A schematic of the experimental apparatus is shown in Figure 5. A Teledyne-ISCO pump is used to feed

the water into the steam generator at a controlled pressure or flow rate. The steam generator produces

steam at a constant set temperature which is then fed into the micromodel through 1/8 inch stainless

steel tubing. The steam flows from the injection port at the top of the model towards the outlet port at

the bottom. A bitumen trap is located between the outlet and the back-pressure regulator (BPR) in

order to prevent bitumen clogging of the small membrane. There is also a bypass line in order to allow

the establishment of a stable steam temperature and pressure prior the injection into the chip.

Figure 5 – Schematic of experimental apparatus for SAGD micromodel

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3.1.2 Micromodel Design

A glass micromodel is used in this study due to the requirements for the model to withstand high

temperatures and pressures while also being optically transparent. The microfluidic pattern, shown in

Figure 6, on the right side, was used to approximate the sand grain and pore network from the oil sands

reservoir. As shown in Figure 7, the basic unit cell of the pattern consists of a double-hexagon

arrangement of circular posts where there is a significant variation in the sizes of the posts in order to

create a range of pore sizes.

Figure 6– (A) Pore-scale SAGD recovery at the interface (B) Pore network pattern in micromodel

Figure 7 – Unit cell of pore network pattern prior to etching (photomask, left) and after etching

(micromodel, right) Red text signifies post diameters and grey text for pore sizes (dimensions in µm)

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Circular posts were chosen to allow the even filling of the bitumen. The pattern was obtained by tiling

the double-hexagon unit cell and changing the orientation of the internal posts at random, thus

preventing directional permeability bias while maintaining a homogenous pore network. The posts and

pore size distributions are shown in Figure 8. The posts range in size from 260 to 380 µm with an

average of 336 µm being comparable to the average grain sizes in the field of 160 µm to 250 µm [21,

47]. Pore sizes range from 112 µm to 170 µm with an average of 134 µm. Every point on the micromodel

is etched to a depth of 50 µm and this is the smallest dimension occurring within the model. Therefore,

in addition to the pore and post geometry, the etching depth of 50 µm plays an important role in

defining fluid dynamics and the physics within the micromodel.

As described in the fabrication section 2.4, a photosmask is used to expose the pattern on the

photoresist and this pattern is later etched isotropically in hydrofluoric acid solution. The highest

printing resolution for the photomask allows a minimum feature size of 10 µm. The smallest pore on the

photosmask is 11.6 µm and isotropic etching to a depth of 50 µm causes the widening of the initial pore

by 100 microns laterally, the final dimension of this pore in the fabricated micromodel is 111.6 µm.

Figure 7 illustrates the pore expansion due to etching of the unit cell. Isotropic etching is the primary

limitation of glass micromodels, thus channels and pores cannot have a large aspect ratio. However,

glass was found to be the only suitable material for this study due to the need for an optically

transparent model that could tolerate high temperatures and pressures.

Figure 8 – Distribution of post sizes (expressed as diameter) and of pore throat sizes (rounded to the

closest µm) within a single the unit cell of the pore network

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The micromodel has a porosity of 50% which is significantly higher than literature data of up to 35% in

oil sands reservoirs. Within the context of isotropic glass etching, a lower porosity could be achieved via

a large increase in the size of the posts; however the posts (simulating sand grains) would not be

comparable to oil sands reservoir geometry if their size was increased. Moreover, it is not practical to

reduce the porosity by reducing the etching depth since a very thin micromodel would not allow for

gravity drainage and not would be representative of the reservoir. The pore network design used for this

model was selected on the basis of minimizing porosity while maintaining reservoir-relevant grain and

pore sizes.

3.1.3 Manifold Design

A significant amount of platform development was required on this project. Most of the engineering

challenges arose from the need to handle steam while maintaining a constant temperature and pressure

as well as working with bitumen. A custom manifold was designed to allow for the exchange of fluids

with the microfluidic chip.

The first version of the manifold was fabricated from stainless steel and extensive insulation was used

during the test in order to minimize heat loss. However, significant heat loss to the steel occurred due to

close contact with the glass. A polymer-based manifold was developed to allow steam injection with

minimal heat loss. Polyether ether ketone (PEEK) was selected since it has good mechanical properties

and can withstand high temperatures. The PEEK manifold, combined with extensive insulation, enabled

the injection of steam into the chip with minimal heat loss.

Figure 9 – Steel manifold is shown on the left and PEEK manifold on the right.

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Another challenge encountered was the need to fill bitumen into the micromodel. Bitumen is a very

thick fluid with a viscosity in excess of 1,000,000 cP at room temperature, and the micromodel has a

depth of 50 μm. The chip-filling with bitumen was achieved by immersing the glass chip in 80°C water

and injecting bitumen slowly at the elevated temperature. The front of the apparatus can be insulated

using a Calcium Fluoride (CaF2) window that allows transmission in both the IR and optical spectrum.

Also, the glass micromodel was initially fabricated from 1.1 mm thick glass, which was not able to

withstand the test pressures. Thicker 2.25 mm thick glass was subsequently utilized.

3.2 Pore-Scale Analysis of Additive Effect on SAGD Interface

The microfluidic platform shown in Figure 5 was used to investigate the effect of an alkaline steam

additive on SAGD interface morphology and recovery profile. The name of the additive cannot be

disclosed due to confidentiality. Three solutions of DI water and the alkaline additive are prepared with

different concentrations of 0 ppm (pure DI water), 200 ppm and 2000 ppm additive concentrations.

For each test, the solution was fed into the Teledyne-Isco pump and injected into the steam generator in

order to produce steam. The steam generator and the line heaters were set to the desired temperature

and the ISCO pump was operated on a constant pressure setting. The operator chooses to flow the

steam either through the chip or the bypass using a pair of 3-way valves. Initially, the steam is circulated

through the bypass line in order to establish stable temperature and pressure conditions for 20 minutes.

The pressure builds up behind the back-pressure regulator (BPR) membrane until it reaches the desired

pressure and then steam flow proceeds out of the BPR and into a steam collection vessel. The piston in

the pump compresses and expands in order to achieve the set constant pressure. Thermocouples are

located at various points on the stainless steel tubing and pressure gages are in place at the inlet and

outlet of the micromodel.

3.2.1 SAGD Micromodel Recovery

Three injection tests were done with steam, steam + 200 ppm additive and steam + 2000 ppm additive

at 155˚C and 344 kPa for duration of 160 minutes. The resulting recovery profile and evolution of the

steam chamber are shown in Figure 10A, 10B and 10C respectively. When steam is injected into the

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micromodel, a steam chamber develops which is larger at the top of the model and narrower at the

base towards the outlet. The high temperature steam heats up the adjacent interface and a steady flow

of bitumen down to the outlet port is observed. Steam has the lowest recovery followed by the 200 ppm

then 2000 ppm additive test with the highest recovery.

Figure 10A – Time-lapse progression of Steam (0ppm additive) injection test

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Figure 10B – Time-lapse images of steam + 200pppm additive injection test

Figure 10C - Time-lapse images of steam + 2000pppm additive injection test

The general shape of the chamber can be explained by considering that a specific volume of bitumen

which drains from the top of the micromodel will fill the lower section of the model on its way to the

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outlet. Moreover, the outlet is a single point and this leads to an increase in the slope of the interface at

lower model height. The conditions within the micromodel broadly match with the conditions observed

at the edge of the steam chamber in the SAGD process.

The advancing steam forms a distinct front during the early phase of injection with steam behind and

bitumen ahead of the interface. However, the steady development of a ‘drainage layer’ with residual

bitumen at the interface occurs in all cases. The drainage layer appears to be most pronounced with the

steam injection case and is also larger in the 2000 ppm run that the 200ppm. The layer is thicker at the

top of the model than at the base for the additive tests but not for the steam test. The exact nature of

bitumen drainage and fluid flow within this layer is discussed in section 3.2.2.

Figure 11 shows the recovery curves plotted against time for each test. The recovery is calculated from

the runtime images of the chip since the produced volumes are too small to collect. The high resolution

Nikon camera is able to capture the pore-scale advance of the steam front and thus allows accurate

measurement of the recovery. Bitumen production is expressed as a percentage of the total pore

volume. The shape of the recovery curve is similar for all the runs with a high initial rate of production

followed by a steady decay. The steam injection temperature and pressure were maintained constant

throughout the test. The steam case has the lowest recovery with 25.6% final recovery while the 200

ppm additive shows a slight improvement at 33.2% of total pore volume produced at 160 minutes of

runtime. The 2000 ppm additive test shows the greatest improvement in total recovery at 68.8% of the

micromodel volume produced after 160 minutes of steam injection.

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Figure 11 – Bitumen Recovery vs. Time

Figure 12 - Final Recovery vs. additive concentration in ppm

Figure 12 shows the final recovery for each test plotted against the additive concentration. The

relationship between bitumen recovery and the parts-per-million concentration of the additive appears

to be linear within the context of this micromodel, but more tests must be conducted to ascertain the

trend.

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The rate of advance of the steam front in the last 2 hours of the test was computed from the chip

images. The front for the steam case progressed 1.667 mm in the last 114 minutes of the run,

corresponding to a rate of 2.104 cm/day. For the 200ppm additive test, the front advanced 6.553 mm in

the last 107 minutes and this corresponds to 8.819 cm/day. The 2000 ppm additive test exhibits a

15.2332 mm advance in the last 124 min, corresponding to 17.69 cm/day. The ‘front’ was measured all

the way to the intact bitumen region and encompasses the drainage layer of residual bitumen.

3.2.2 Physical Morphology of Steam-Bitumen Interface

One of the primary objectives of this study is to analyze the morphology of bitumen drainage and steam

front advance at the pore scale. This section discusses the main findings pertaining to bitumen mobility

at the interface.

Figure 13 shows a composite image of the interface amalgamated from the pore-scale video. The

Dinolite USB camera was used to monitor the steam-bitumen interface The USB camera is placed as

close as possible to the micromodel in order to capture a maximum of detail. To view a larger area, as is

the case in figure 13, it is necessary to sweep the camera over the area and then create a composite.

Due to the variable nature of the interface, both over the micromodel height and with respect to time,

any comparison in the interface morphology between different tests must occur at a fixed height and

run time. Figure 13 compares the drainage layer between the pure steam, 200 ppm and 2000 ppm

additive tests at approximately 100min of runtime at a height of approximately half of the micromodel.

The camera was maintained at an equal distance from the chip in all tests, therefore the scale shown at

the top applies to all image within figure 13.

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Figure 13 – Steam chamber interface for steam (0 ppm), 200ppm, 2000ppm additive

(A – In-situ bitumen, B – Leading Edge, C – Lagging Edge, D – Steam Chamber)

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All of the runs conducted show a relatively distinct 4 step model of steam front morphology:

o (A) In-Situ Bitumen: The bitumen adjacent to the interface is heated due to the latent

heat of condensing steam. There is temperature decay within the in-situ bitumen region

(and a corresponding viscosity increase away from the interface).

o (B) Leading Edge: Steam from the chamber reaches the reservoir bitumen and

condenses into water, forming a flowing ‘stream’ at the leading edge. Steam in vapor

form is not observed directly adjacent to the bitumen except at the very top of the

model. The flow of bitumen within the leading edge is limited at the top of the chamber

but a greater flow is observed with decreasing height. The condensate flows past the

heated bitumen at the leading edge and snaps off droplets from the bitumen, resulting

in a multitude of small fast-moving bitumen droplets. The leading edge seems to act as a

narrow ‘highway’ for rapid bitumen recovery. Water fingers originating from the leading

edge develop into the in-situ bitumen region.

o (C) Lagging Edge: The continuous losses of small bitumen droplets from the leading

edge tend to accumulate into larger droplets and eventually form a lagging edge of slow

draining bitumen behind the leading edge, over time. Bitumen droplets are forced out

of the high flow condensate stream due drainage through the porous media. The lagging

edge drains more slowly since it does not experience as much shear forces from the

condensate flow. The lagging edge boundary adjacent to the steam chamber is subject

to regular invasion by small steam bubbles, which subsequently become encapsulated in

bitumen and do not progress further. The lagging edge itself can be separated into a

rear section (in front of the steam chamber) where significant steam invasion is

observed and a front section (behind leading edge) with higher bitumen saturation and

no steam pockets.

o (D) Steam Chamber: The majority of the clear volume in the pores is occupied by steam

vapors. The steam chamber interfaces with the lagging edge and vapor steam droplets

sometimes enter into the lagging edge and become encapsulated with bitumen.

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The lagging edge seems to be considerably wider in the pure steam injection case compared to the

additive runs; this can be attributed to the absence of alkaline additive in the condensed water since

there would be no additive-induced reduction in interfacial tension. This may be due to the significantly

greater bitumen recovery for 2000 ppm, since the lagging edge is created from the accumulation of

draining bitumen falling out of the condensate stream, it follows that the greater bitumen recovery from

the 2000 ppm run gives rise to a larger lagging edge when compared to the 200 ppm test, despite the

IFT-reducing effect of the additive.

Figure 14 – Bitumen recovery through droplet generation at the interface (Time-lapse: 2 sec)

The flow of condensed water at the leading edge of the steam chamber appears to exert shear forces on

the adjacent bitumen. Figure 14 shows droplets are created when the falling water forces the bitumen

against the posts until snap-off occurs and a bitumen drop is generated. The size and frequency of the

bitumen droplets is dependent on the bitumen viscosity, steam temperature and pressure in addition to

the morphology of the pore network. The droplet generation occurs at short time-scales (time-lapse of 2

seconds for figure 14). The relevance to field-scale SAGD projects is that the rate of bitumen production

from an area may be linked to the degree of condensed water flow within that area.

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Figure 15 – Finger Displacement of bitumen (Time-lapse: 1 min)

A common mechanism of bitumen displacement at the interface is through the appearance and

expansion of water fingers ahead of the interface, demonstrated in Figure 15. Condensed water that

flows down along the leading edge of the interface may be funneled into fingers which then steadily

expand due to the high pressure in the steam chamber and due to continued water condensation and

flow at the interface. The finger displacement morphology is relatively narrow and directional and the

fingers always develop in the direction of gravity (downwards). The finger displacement occurs in the

mid-section of the interface and not as much at the top of the model since there is little condensed

water flow at the top.

Figure 16 – Non-directional Gravity Drainage at the top of steam chamber (Time-lapse: 5min)

Figure 16 shows the typical bitumen displacement at the very top of the steam chamber. The area

highlighted red shows that the heated bitumen seems to drain under the effect of gravity with no role

from the flow of condensed water (as opposed to recovery in the middle section of the interface where

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condensed water has a greater impact). The gravity drainage at the top proceeds steadily in all

directions and differs from the finger displacement mechanism of the previous figure because there is

much less directionality.

Figure 17 – Emulsion generation under limited bitumen drainage rate at outlet port

Figure 17 shows the generation of emulsions at the outlet of the chip. This phenomenon was observed

during the steam run at the time of initial steam injection. The rate of bitumen drainage is limited by the

physical size of the outlet port (1mm diameter circle) as well as the high viscosity of the bitumen. The

water is squeezed through the bitumen and breaks up into numerous small droplets. The significance of

this finding is that the character of the emulsions produced from the SAGD process is not solely

determined within the reservoir. The pressure, temperature and geometry that the SAGD produced fluid

are exposed to during its movement to the surface play an important role in the final properties of the

emulsion.

Figure 18A documents the tendency for steam bubbles to enter into the lagging edge and become

encapsulated in bitumen. The figure shows still frames from pore-scale video taken at the steam

chamber and lagging edge interface (between layers C and D from figure 13). This kind of steam invasion

into the lagging edge was a common and frequent occurrence and two separate instances of steam

invasion and encapsulation are shown at the top and bottom frames.

As Figure 19A shows, trapped steam bubbles that are completely surrounded by bitumen shrink due to

heat loss over time leading to water condensation A specific instance of trapped steam condensation is

shown over a time lapse of 2 minutes. The formation and subsequent condensation of a second steam

bubble is also highlighted in yellow.

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Within moments of the full condensation of the steam bubble in Figure 19, the bitumen droplet

(highlighted in red) was then able to drain downwards, this shows that steam invasion and

encapsulation by bitumen at the rear boundary of the lagging edge is detrimental to bitumen drainage

because it ‘inflates’ the apparent size of the bitumen droplets. Moreover, the dynamics of gravity

drainage for a bitumen drop that contains within it a large bubble of steam will differ markedly from the

drainage of bitumen-only droplets. It is expected that the steam buoyancy would act in opposition to

the force of gravity and slow down the drainage of steam-invaded bitumen.

Since isolated steam will condense into water due to heat loss over time, the persistent presence of

steam bubbles at the boundary between the steam chamber and lagging edge would require consistent

invasion of steam in order to balance the steady loss. As mentioned in the description of figure 18, it

was indeed observed that steam invasion into the lagging edge was a common and frequent occurrence.

Therefore, one of the important findings of this work is that the development of a lagging edge at the

interface, with a high level of residual bitumen, acts as a physical barrier to the advance of steam.

Figure 18A – Steam vapor bubble invasion & trapping into lagging edge,

(two distinct examples top & bottom row)

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Figure18B - Maximum extent of steam invasion into lagging edge (steam test) amounts to ~3mm

The maximum extent of the steam vapor invasion into the rear boundary of the lagging edge is

highlighted in figure 18B. The steam injection test is shown since the large lagging edge allows clear

observation of this phenomenon. The degree of steam penetration into the lagging edge is dependent

on the rate of steam invasion and the thickness of the lagging edge.

Figure 19A – Trapped Steam bubble condensation (Time-lapse: 2min)

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Figure19B - Size of condensing trapped steam droplet vs. Time

Figure 19B shows a plot of the rate of condensation of the steam bubble as observed in the earlier figure

19A. The condensation rate of multiple steam bubbles must be plotted against the distance of the

bubble from the steam interface and the thickness of the encapsulating bitumen in order to understand

the dynamics of steam condensation in the lagging edge.

3.2.3 Thermal Morphology of Steam-Bitumen Interface

The development of the thermal profile was captured using the RAZ IR NANO infrared camera. The

camera is able to measure temperatures up to 250°C. The camera was placed as close as possible to the

glass chip while still ensuring the visibility of the whole chip. The resolution of the thermal sensor is

160x120 pixels with a measured temperature associated to each pixel. In our experiments, one pixel was

found to correspond with 1.075 mm of distance across the chip.

Figure 20 shows a time-lapse of the steam chamber development as observed by the infrared camera

over the 160 minute duration of the tests. As indicated on the scale, the deep red areas are at 110°C or

more and the black areas have a temperature lower than 80°C. An important observation concerning

the thermal profile is that the thermal chamber always seems to have a relatively sharp and distinct

forward edge throughout the test (as opposed to the emergence of a thick drainage layer in the physical

chamber).

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Figure 20 - Time-lapse thermal images over the 160 minute duration of the tests

Figure 21 shows a composite image with the thermal profile and physical profile of the steam chamber

superimposed. The thermal profile shows temperatures between 130°C (in red) and 75°C (in faded blue)

with a bright yellow band at temperatures from 100°C to 115°C.

In the highlighted area of detail of 4 cm in length, the temperature was plotted along the distance of the

central horizontal axis in order to allow comparison between the temperature profile and corresponding

changes in the physical chamber morphology. The temperature data point closest to 100°C is shown in

red.

The 10min and 85 min temperature profiles should not be directly compared to one another within

Figure 21 since the scales on the temperature axis are not matched. The 10 min and 85 min temperature

profiles can be compared with each other in Figure 22.

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Figure 21 – Thermal & Physical Steam Chamber Comparison:

lagging edge acts as barrier to steam chamber expansion (temperature axes are not scale-matched)

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Figure 22 – Temperature profile at the interface

Figure 21 shows that, at 10 minutes of runtime, the bitumen drainage interface coincides with the

condensation of the steam at the 98.5°C. During the early stages of the run, the physical interface

consists of a sharp front and the steam directly contacts the bitumen. In contrast, the 100.3°C point at

85 minutes corresponds with the rear boundary of the lagging edge.

Figure 22 shows that at 10 minutes, the temperature beings to decay closer to the interface but shows a

more significant drop across the interface; whereas at 85 minutes, the temperature drop begins slightly

further from the interface and the decay is more gradual. The early chamber at 10 minutes of runtime

appears to be closer to the established understanding of SAGD and to Butler’s theory (discussed in 2.2.3)

which assumes a sharp interface.

Therefore, two distinct thermal regimes are observed in the test. Upon the injection of the steam, a

chamber develops with ‘direct contact’ between the steam and the bitumen giving rise to a high rate of

recovery. However, with the continued drainage of bitumen and the development of a lagging edge, a

transition soon occurs to a second thermal regime that is defined/characterized by obstruction to steam

advance due to residual bitumen, a ‘thermal gap’ between the edge of the physical and thermal steam

chamber, leading to a tapering of the rate of bitumen recovery. It is important to note that the bitumen

recovery does not decay to zero in the late stages of the test. Recovery continues, albeit at a much

slower pace. The rate of interface advancement calculated over the last two hours of the test is equal to

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2.104 cm/day (steam), 8.819 cm/day (200 ppm) and 17.69 cm/day (2000 ppm) and this corresponds

broadly to the rate of interface advance in field-scale SAGD projects of 2 to 27 cm/day [52].

For the 85 min profile, it is observed that there is a greater distance between the forward boundary of

the leading edge and the thermal chamber at the top of the model than at the bottom. As mentioned in

section 3.2.1, the large apparent thickness of the drainage region at the top of the micromodel is

explained by considering that a specific volume of bitumen which drains from the top will fill the lower

section of the model on its way to the outlet and thus any bitumen drained from the very top of the

model is not itself replenished by incoming flow from above.

Figure 23 further reinforces the argument that residual bitumen from the lagging edge prevents steam

chamber development as it shows minimal advance of the rear boundary of the lagging edge while the

leading edge has advanced to a greater extent.

Figure 23 – Comparison of the rate of advance of leading & lagging edge of steam chamber

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3.2.4 Pore-Scale Fluorescence Imaging of Steam-Bitumen Interface

After the completion of each run, the micromodel was immediately taken to the fluorescence

microscope for imaging. The fluorescence microscopy is useful in undertanding micro-scale behaviors

such as wetting since it provide a higher magnification observation of the system. It should be noted

that stopping the steam flow to the model resulted in depressurization and condensation of the steam

chamber. The interface was disturbed as a result and the imaged sample may differ significantly from its

runtime conditions of high temperature and pressure.

Figure 24 shows a composite image of fluorescent (top) and brightfield (bottom) microscope images for

each run. The large images were stichted from smaller individual images. The bitumen appears green

under the fluorescent light and appears black in the brightfield images. Despite the disruption of the

interface (due to drawdown of the pressure), the four stages of interface morphology are still broadly

distinguishable (as indentified by the blue-box labels below each image). The main observations from

this figure is that the emulsions at the interface are mostly found between the steam chamber and

lagging edge boundary. Also, the leading edge has a higher bitumen saturation in the steam case

compared to the additives and in the 200 ppm case compared to the 2000ppm.

Figure 25 shows the morphology at the interface within the reservoir bitumen region just ahead of the

leading edge. While the reservoir bitumen region appears to be a continuous mass from macro-scale

optical observation, a magnified pore-scale view reveals that it comprises a collection of small bitumen

droplets (especially for the for the 2000 ppm case). Droplet accumulation at the interface is more

common at lower heights within the model and this indicates that the bitumen droplets are most likely

to have been generated upstream (as shown in figure 14) and became trapped within the porous

medium on their way to the outlet. The fact that adjacent drops of bitumen did not agglomerate shows

the effectiveness of the additive at reducing IFT. The size of these droplets steadily increases (due to

increased tendency towards agglomeration) with lower additive concentration.

Figure 26 also shows are in the reservoir bitumen ahead of the steam chamber for the steam case. Very

small droplets of water (highlighted in yellow in the figure) are seen to invade a few millimeters into the

bitumen. These droplets suggest that the bitumen in that region is heated and sufficiently mobile to

slowly drain under gravity as well as in response to the pressure gradient in the chamber within the

model (a similar pressure gradient should also exist in the field-scale SAGD chamber).

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Figure 24 – Fluorescent (bitumen = green) & Brightfield (bitumen = black) post-run microscope images

Figure 25 – Small water droplets are observed in the bitumen ahead of the leading edge

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Figure 26 – Bitumen droplets drainage ahead of the interface

3.2.5 Key Findings on the Nature of Pore-Scale Steam Front Dynamics

The experimental results of the steam additive tests are described in detail in the previous subsections

of 3.2. The key findings of this micromodel study on the dynamics of the SAGD chamber interface are

outlined below.

New insights physical & thermal pore-scale morphology of SAGD Interface:

The four-stage morphology at the steam chamber edge is identified and described. The

interface can be segmented into:

o (A) reservoir bitumen ahead of the front

o (B) leading edge

o (C) lagging edge of the condensed water front defined by low drainage rates and high

bitumen saturation

o (D) steam chamber behind the lagging edge is mostly filled with steam

The leading edge forms when steam at the interface condenses into water and is defined by

high drainage rates and low bitumen saturation.

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o High flow rates at the leading edge are only apparent from 2 cm below the top of the

model onwards, since there is less volume of condensed water flow at the top of the

micromodel

o Bitumen displacement at the top of the leading edge proceeds through slow, non-

directional gravity drainage

o Bitumen displacement closer to the center of the leading edge is more heavily affected

by condensate flow. Two distinct mechanisms are observed at the boundary between

the leading edge and the reservoir bitumen:

Droplet generation (when condensed water pushed bitumen against the posts)

Water finger initiation and growth (when the draining condensate is funneled by

the porous media into a finger and leads to finger growth)

The lagging edge develops, over time, behind the leading edge and is defined by low drainage

rates and high bitumen saturation.

o The lagging edge forms as a result of bitumen droplets being forced out of the high flow

condensate stream due to the pore network

o Bitumen within this layer drains slowly due to the absence of the condensate flow

o Vapor bubbles from the expanding steam chamber invade into the back of the lagging

edge and become trapped due to encapsulation by bitumen.

Trapped steam bubbles tend to condense over time and the persistent

existence of trapped steam at the back of the lagging edge is due to continued

steam invasion

Trapped steam contributes towards the slow drainage due to steam buoyancy

There exists two distinct thermal regimes of steam chamber temperature during the test:

o Direct-contact regime: sharper temperature drop over interface

o Thermal gap regime: due to lagging edge hindrance/obstruction of steam flow

Effect of alkaline additive on recovery dynamics

The inclusion of alkaline additives into the steam improves bitumen recovery from 25.6%

(steam-only) to 33.2% (200 ppm aqueous solution) and 68.8% (2000 ppm aqueous solution).

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Recovery is defined as percentage of total volume of the micromodel produced (with 100%

initial bitumen saturation)

Interface velocity over the last two hours of the tests is found to be equivalent to 2.104 cm/day

(steam), 8.819 cm/day (200 ppm) and 17.69 cm/day (2000 ppm) and this corresponds broadly to

the rate of interface advance in field-scale SAGD projects of 2 to 27 cm/day [52]

The specific effects of the alkaline additive are observed as follows:

o Lower interfacial tension (IFT) on bitumen surfaces due to the surfactant effect of the

additive is observable in terms of:

Increase oil-in-water emulsions at the reservoir bitumen interface

Bitumen saturation in the leading edge is reduced from the steam case to the

200 ppm case and further reduced with 2000 ppm additive. The width of the

leading edge also generally increase with additive content

200 ppm additive test a thinner drainage layer than the steam test

The reduction in the lagging edge thickness that stems from the additive-induced lower IFT is

crucial in helping steam chamber growth because the lagging edge was found to impede steam

advancement.

As mentioned in section 2.2.3 existing SAGD models make assumptions regarding the nature of the

steam chamber interface and the pore-scale observations from the micromodel tests can be used to

evaluate the validity these assumptions. The original derivation of the Butler equation for bitumen

production from SAGD made the assumption that the interface consists of a single boundary with

the steam chamber on one side and the in-situ bitumen on the other. The micromodel tests

revealed that the interface actually consists of two distinct layers with a lagging edge and a leading

edge. A new model can be developed based the new interface morphology that accounts for the

distinct physics of each layer, as shown in figure 27.

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Figure 27 – Physical model allows evaluation of validity of interface assumptions

For instance, the new model can evaluate the behavior of the leading edge by considering:

Leading edge thickness (based on steam flow pattern, condensation rate, model height, steam

temperature & pressure, pressure drop from inlet to outlet)

Size and frequency of droplet generation (based on shear effect of condensate, pore network

geometry, viscosity ratio of heated bitumen & condensate, IFT)

Entrapment of draining bitumen droplets within the pore network (based on droplet generation

dynamics, pore network geometry)

Effect of convective heat transfer from drainage of heated bitumen

Effect of convective heat transfer from lateral flow of condensate (based on an adapted version

of the Lauwerier Equation, which is used to understand heat transfer from the flow of a heated

fluid laterally alongside a porous media)

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The new model could account for the negative effect of trapped steam on bitumen drainage in the

lagging edge by considering:

Lagging edge thickness (based on bitumen droplet generation rate, pore geometry, rate of

accumulation of bitumen droplets behind leading edge, gravity drainage)

Frequency of steam bubble invasion (based on chamber steam flow velocity field)

Extent of steam invasion into lagging edge (based on invasion & condensation rate)

Effects of trapped steam vapor on bitumen gravity drainage (based on density differences, IFT)

3.3 Bitumen Displacement from Gasification of Reservoir Liquid

The start-up phase of the SAGD process involves injecting steam into the reservoir to establish initial

communication between the injection and production wells. A large amount of steam is injected into

the reservoir with no production during the start-up phase and there is an interest in reducing the time

and energy requirements for this step. Within the context of reducing SAGD start-up time, a test was

conducted to investigate the morphology of bitumen displacement resulting from the gasification of a

liquid pocket in a bitumen-filled micromodel. An additive was also added to the water in this case to

produce a 10wt% solution of the additive in water. The exact nature of the additive for this section

cannot be disclosed and it is not related to the alkaline steam additive employed in section 3.2.

Figure 28 shows the initial condition of the micromodel, which is 85% saturated with bitumen and the

remaining 15% of the volume being occupied by the aqueous additive solution. The liquid exists as a

single large pocket and is not dispersed in the porous media. The two ports adjacent to the liquid

chamber are closed to prevent the leakage of generated gas while the ports on the bitumen side are left

open in order to allow bitumen displacement. The model is heated on a hot plate to a temperature of

120°C and gasification of the liquid pocket is allowed to occur.

The overall result of the experiment was that the gas was continually generated from the liquid pocket

for a span of 45 minutes and was able to displace bitumen and reduce the bitumen saturation of the

pore volume from 85% to 50%, as shown in Figure 28.

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Figure 28 – Gasification of liquid volume over a span of 45 minutes leads to 35% bitumen displacement

Figure 29 – Pore-scale view of gas expansion (left) and liquid finger region (right)

Gasification of the aqueous solution leads to a pressure gradient that drives flow towards the open ports

on the opposite side. During the initial stages of the test, evenly spaced fingers of gas emerged from the

interface with the bitumen. However, within 12 minutes from the start of the test, the expansion of the

gas fingers stopped and instead a multitude of liquid fingers emerged and expanded towards the outlet

ports. Some of these liquid fingers initiated from the edge of the gas fingers.

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As is shown in Figure 29, gas fingers are more effective at displacing the bitumen than the liquid fingers.

The amount of residual oil within the gas-cleared area is much lower than the residual oil left being in

the liquid-cleared area. It is also interesting to note that liquid droplets exist at the interface between

the gas and the bitumen, indicating there is no direct contact between the bitumen and the gas.

Figure 30 shows the pore-scale fluorescence images obtained after the test. The high recovery area

stemming from the expansion of the gas fingers is shown at the top, a mixed-wet condition is observed

and a large distribution of bitumen emulsion sizes is shown. The lower recovery area from the liquid

fingers is at the bottom of the figure, an oil-wet condition is observed along with a continuous oil phase.

The main finding of this experiment is that there is an initial period of rapid gas expansion at the

interface that later gives way to liquid finger expansion. Gas expansion is desirable since the gas-cleared

regions have low residual oil while the liquid-cleared regions leave behind a larger amount of residual

bitumen. Further tests are needed with different concentrations to determine the effect of the additive

on the gas generation and bitumen displacement dynamics.

Figure 30 – Fluorescence microscope images of bitumen displacement in gas & liquid region

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3.4 Emulsion Analysis & Semi-Automated Video Segmentation

Automated image analysis is a useful tool that can be used to extract various types of numerical data

from different sets of images. Theories previously examined in a qualitative manner through the use of

images can now be studied quantitatively using charts, graphs and tables. A large amount of the data

produced from the pore-scale experimental apparatus is in the form of images and video. When

extracting information from images, it is desirable to minimize human error and bias. For instance, the

manual counting and measurement of an emulsion may yield different data based on the definition or

biases of the individual who counts the emulsion; alternatively, the same individual manually counting

an emulsions multiple times may find slightly different distributions each time due to human error. In

order to ensure the accuracy and reliability of the data, an emulsion analysis procedure was developed.

A brief review of these efforts will be presented in this section.

A semi-automated method was developed to obtain the particle size distribution from an emulsion

image. Our method is tailored towards emulsions with circular droplets of two different

substances/colors but can also be applied to multi-component emulsions with more than two different

types of particles provided they each have a unique coloration that allows differentiation.

The overall process of obtaining the particle size distribution involves 4 steps:

(I) Improve image quality & contrast to allow easier analysis

(II) Threshold image to separate particles/features from the background and to create a

particle mask

(III) Separate the particle mask into 2 categories for the different components of the

emulsion (a separate mask for the light and dark particles)

(IV) Process the image masks to generate a particle size distribution bar chart for the light

and dark particles

While image analysis is simple in principle, numerous image segmentation errors and artifacts must be

corrected in practice to obtain reliable data. The tool that is used to conduct image analysis in this

procedure is the analysis software Fiji (a variant of ImageJ) which is available for download for a variety

of operating environments.

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Figure 31 – (Top) Original image of emulsion (Bottom) Semi-automated analysis identifies emulsions

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Figure 31 shows test fluid obtained from a SAGD facility, the exact nature of the fluid cannot be

disclosed due to confidentiality. The original image at the top displays a multi-component emulsion with

large yellow droplets and smaller brown droplets. An emulsion of this complexity would be difficult to

manually characterize to a satisfactory level of accuracy. The semi-automated emulsion analysis

procedure was applied to obtain the annotated image at the bottom of the figure, with a separate color

scheme for the yellow and brown emulsions. Figure 32 shows the plot of the emulsion size distribution

extracted from the image. A full explanation of the procedure is provided in Appendix B.

Figure 32 – Semi-automated analysis is used to accurately and quickly obtain particle size distribution.

The light/dark blue distribution is the particle sizes for the corresponding emulsions from figure 31

A semi-automated analysis method was also developed for segmentation of the interface from pore

scale videos. Figure 33 shows a still image from a video being processed with this method. The basic

process begins with extracting an image sequence from the video file and combining the images into a

single TIFF image stack.

Each image in the stack is then converted to a binary black and white version with care being taken that

the binarized image is representative of the bitumen location in the original. The binary images are then

collapsed into a single gray-scale image using the Z-project function which assigns a gray-scale value

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from 0 to 255 to each pixel based the average for that pixel throughout the stacked images. The

resulting gray-scale image is then threshold to identify the stable and mobile regions of bitumen.

Figure 33 – Automated image segmentation of the SAGD interface

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4.0 Conclusion & Future Directions

The high temperature-pressure pore-scale microfluidics apparatus developed in this work was used to

investigate the pore-scale physical and thermal morphology of the steam chamber advance in the SAGD

process. It was identified that four distinct regions exist at the interface: in-situ bitumen, leading edge of

condensate flow with low bitumen saturations, a lagging edge of high bitumen saturation and low

drainage rate and the steam chamber. Novel dynamics concerning the advancement of the steam front

were documented, including the tendency of the lagging edge to act as a barrier to steam advance. The

significant impact of alkaline additive on recovery was found and the importance of the additive-induced

decrease in IFT was observed in terms of reducing the thickness of the lagging edge.

A wide range of future directions are possible with respect to the micromodel. One path is to develop a

detailed simulation model of the micromodel and to conduct experimental tests in tandem with the

simulation to inform the theoretical framework of the SAGD process. For instance, separate models

could be created, each based on a different set of assumptions and the experimental data from the set-

up would help us evaluate the validity of the assumptions. Moreover, numerous questions, such as the

role of shear forces in the leading edge, can best be answered by comparing simulation and

experimental data.

Alternatively, another direction to pursue would be to introduce heterogeneity in the model. The oil

sands reservoirs are known to be highly heterogeneous and the effect of shale barriers or fractured

reservoirs on bitumen recovery in the context of SAGD are yet to be understood. Another approach

would be to inject other substances, such as solvents for VAPEX or solvent-assisted SAGD. Injecting light

hydrocarbons into the micromodel can be achieved with minimal changes in the experimental set-up.

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Appendix A

PEEK Manifold CAD Drawings

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The drawings for the top clamp (above) and base clamp (below) of the PEEK manifold are shown. The

glass chip fits between the clamps with the inlet/outlet holes aligned with the ports. All dimensions are

in millimeters.

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Appendix B

Glass Fabrication Standard Operating Procedure

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The following standard operating procedure was developed for glass etching:

Book all required equipment on the cleanroom system, enable upon entry into cleanroom

Check photomask under microscope (sharp focus = side touching glass).

The side on which the pattern is printed must be touching the glass to ensure proper exposure.

Exposure

Conduct 50s cycles 3 times with the empty exposure box (to 'warm up' the light)

Place glass into exposure box with photoresist facing up, align photomask

Close cover, create vacuum to ensure optimum photomask contact

Close box, set time (45s typical, varies with different photoresist), expose

Mix developer

Find vessel (that can accommodate the chip) and clean with DI water

Mix: 1 AZ400K : 6 DI water (20ml : 120ml)

Stir well

Place exposed glass into developer

Agitate for 1min30s

Rinse in DI water until developer removed

Examine under microscope

Repeat in 30s increments until proper developing

Exposure Box

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Wash glass in DI water, air dry (to remove developer)

Examine under microscope to ensure correct pattern exposure & development

Hard Bake

Turn on hot plate and set to 130°C

Place developed glass on hot plate at 130°C for 30min, this will harden photoresist

After the hard bake step, all cleanroom steps take place in etching room (white-lit)

Prepare Dechromer

Work in the wetbench that you booked (left or right side)

Find glass vessel and clean with DI water

Fill with dechromer enough to submerge chip (approx. 4mm high)

Optical Microscope

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Place glass into dechromer (chrome exposed due to UV exposure is removed)

Wash with DI water until dechromer removed

Prepare HF solution

(Note: HF is a highly dangerous substance; you MUST be trained by the lab

manager to safely handle HF or Piranha prior to glass etching)

Find and clean thick-walled polymer vessel with DI water (No glass vessel)

Mix: 1 HF : 3 HNO3 : 5 DI water

Always Add Acid to Water *

(For 1400ml HF: 156ml HF, 467ml HNO3, 778ml H20)

Sufficient HF solution is needed to submerge a vertically standing chip completely

Clean with DI water the tools used to prepare HF

Etching:

A wafer-holder is typically used to handle glass slides (large ones in particular)

Place glass in HF vessel for glass etching, time in HF determines etch depth

BoroFloat33 glass etches at approximately 1μm/min

Remove glass from HF and dip gently into water every 15 minutes

Wetbench in Cleanroom

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When etching period is complete, rinse with DI water, inspect under microscope

Use Teflon utensils, do not use metal

Etching Depth Measurement:

Optical profilometer is in CMS (MC405), equipment must be booked prior to use

Use optical profilometer to obtain the actual etching depth for each chip

Drill holes in cover glass

Wrap glass to be drilled in Aluminum, take to MC413

Drill holes in glass (align holes correctly using hole alignment mask)

While drilling, use DI water on the glass as coolant to prevent drill-bit damage

Wipe the drill to prevent rusting due to water

Return to cleanroom with drilled glass

If needed, use dicer in Pratt cleanroom to cut glass to required dimensions

Prepare Pirhana solution

(Note: Piranha is a highly dangerous substance; you MUST be trained by the

lab manager to safely handle HF or Piranha prior to glass etching)

Find glass vessel and wash with DI water

Mix: 1 H2O2 : 3 H2SO4 (or 1:2)

Always add Peroxide to Sulfuric Acid

(For 1400ml Piranha: 467ml H2O2, 933ml H2SO4)

Wait 1 min for reaction to begin

Clean with DI water tools used to prepare Pirhana

Drill Press

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Final Dechroming

Place etched glass in Piranha (photoresist will be removed) until glass is metallic

Rinse in DI water

Place etched glass into dechromer until complete removal of remaining chrome

Rinse in DI water

Place etched glass into Piranha (removes all dirt and residual dechromer)

Rinse in DI water

Once the glass has been cleaned in Piranha, caution must be exercised to prevent any deposition of

dirt/dust which may cause issues with glass thermal bonding. From now on:

Wear face mask, do not breathe on the glass chip

Do not set down the glass chip on the table or on a wipe. Only place it on Aluminum foil.

Dispose of Dechromer, HF and Piranha (in the appropriate waste bottles)

Piranha must be de-gassed overnight before disposal

Sonicate to clean glass (on the day of bonding)

Set up sonication station (Get 2 beakers that can fit glass, place in sonicator)

Fill beakers and sonicator with DI water

Sonicate glass for 10 min, replace water in beakers

Rinse glass under running water for 1 minute

Repeat three times

Hold cover and base glass under running water for 15 minutes

Water-bond or Dry-bond glass

Ensure the correct orientation of glass pieces (etched side inwards)

Dry glass completely then bring both sides together (Dry bond, recommended)

Bring both sides together under running water (Water bond)

Inspect glass under microscope:

If any particulate contaminants are observed: Carefully separate the two pieces of glass and repeat the water/dry bonding step

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If there are no particulate contaminants between the glass sides: Wrap chip in aluminum foil, proceed to next step for thermal fusion bonding, Be sure to turn off microscope lamp to prevent burn-out

Glass thermal fusion bonding

Carefully transport glass to the furnace lab

Wipe clean the inside of the furnace from dust, use IPA and DI water

Wipe clean all weights to be used & alumina plates with IPA and DI water

Place the alumina, glass and weights within the furnace (as shown in the figure)

Set furnace stages of 400°C/3hr, 645°C/6hr, 50°C/5minutes at ramp rates 2°C/hr.

Bond overnight, check glass on the next day to ensure proper bonding

If incomplete bonding occurred, bond again at 400°C/2hr, 645°C/2hr, 50°C/5minutes

*SAFETY NOTE: Always Add Acid to Water

If water was added to acid in a beaker, then the initial point where the water first enters the acid would

form a highly concentrated mixture of acid and large amounts of heat may be produced, leading to

hazard of splashing or explosion. If acid is added to the water in a beaker then the initial point where the

acid first enters the water would form a very dilute mixture of acid and the risk is minimized. Pour the

acid slowly into the water.

SAFETY NOTE: Training is required before you can work with hydrofluoric acid (HF) or piranha. Please

consult the lab manager.

500g Weight

3 x 100g Weights Alumina

SlideGlass ChipAlumina Slide

Weight stack arrangement for Furnace bonding

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TIMING FOR GLASS CHIP FABRICATION

The glass chips are usually fabricated in batches because making single chips is not practical. The

batches are usually for 3 chips at a time (the hot plate in the pratt cleanrrom accommodates 3 chips for

10x10cm chips). Often, 2 people work together to fabricate glass chips (it is recommended to work in

pairs when dealing with HF, piranha).

Below are the typical times and costs associated with glass chip fabrication.

Day 1:

Steps: Exposure, developing, hard baking, dechroming, hole-drilling on cover glass

Day 2:

Steps: Prepare HF solution, etch glass, optical profilometer measurement, dispose HF

Day 3:

Steps: Prepare piranha, piranha cleaning of glass, sonication, dry-bonding, furnace bonding cycles

Day 4,5,6:

Steps: Typically 3-4 furnace bonding cycles are required for chip bonding. The bonding takes 12+ hours

and the cycle runs overnight. The bonding time (at 650C) or the weights can be increased to minimize

bonding cycles but the risk of channel collapse in the glass is also increase in this case. Personnel time

requirements are minimal during the bonding phase (takes 30 minutes to set-up each furnace cycle).

Furnace bonding is typically done a single chip at a time, but multiple chips can be stacked to reduce the

time requirements.

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COSTS FOR GLASS CHIP FABRICATION

This section assumes 3 chips are made in one batch. Equipment costs are listed and multiplied by typical

time requirements. Personnel costs are not directly listed but a template is provided. This section

assumes fabrication proceeds without significant mishap or delays.

Material costs:

Glass slides (Pre-coated, pre-cut. 2.25mm thick, BF33) $1200/20 slides $60

Photomask (one-time cost, printed by CAD/Art Services) $150

Equipment costs:

(Rates shown are for U of T users for the TNFC Pratt cleanroom except where indicated)

UV exposure box 27 $/hr 3hr (Day 1) $81

Hot plate 27 $/hr 2hr (Day 1) $54

Wetbench 42 $/hr 5.6.6hr (Day 1/2/3) $714

Optical Profilometer 30 $/hr (CMS) 2hr (Day 2) $60

Drill press free (lab equipment)

Furnace free (lab equipment)

Personnel costs:

2 x $/hr x 8 hr/day x 3 days = ___

Total costs = $1119 + Personnel costs

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Appendix C

Semi-Automated Emulsion Analysis Standard Operating Procedure

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Introduction & Overall Method

Automated image analysis is a useful tool that can be used to extract various types numerical data from

different sets of images. Theories previously examined in a qualitative manner through the use of

images can now be studied quantitatively using charts, graphs and tables. One metric of particular

interest is particle size distribution (PSD) which is useful in a variety of circumstances, including the

analysis of petroleum emulsion. Particle size distribution is difficult to obtain manually, especially in the

presence of a large number of particles, emulsion components and sizes.

An automated method was developed to obtain the particle size distribution from a given image. This

method is tailored towards emulsions with circular droplets of two different substances/colors but can

also be applied to multi-component emulsions with more than two different types of particles provided

they each have a unique coloration that allows differentiation. The image analyzed in this procedure is

shown below, the emulsion consists of 3 components (yellow background, yellow droplets, brown

droplets).

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The overall process of obtaining the particle size distribution involves 4 steps:

(I) Improve image quality & contrast to allow easier analysis

(II) Threshold image to separate particles/features from the background and to

create a particle mask

(III) Separate the particle mask into 2 categories for the different components of

the emulsion (a separate mask for the light and dark particles)

(IV) Process the image masks to generate a PSD bar chart for the light and

dark particles

While image analysis is simple in principle, numerous image segmentation errors and artifacts must be

corrected in practice to obtain reliable data. The tool that is used to conduct image analysis in this

procedure is the analysis software Fiji (a variant of ImageJ) which is available for download for a variety

of operating environments at: http://fiji.sc/Downloads.

Image Analysis Procedure

The procedure for obtaining the particle size distribution is described below. For clarity and readability,

each overall task has been listed as a separate section with its own subsections and numbering of steps.

1.0 Obtain a mask of all particles

(1) Download and install the Fiji software. Open the program.

(2) Open the image that you will analyze into the program. You can either go to File>Open or click and

drag the image into the Fiji task bar.

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1.1 Enhance Local Contrast to allow better contrast between features and background:

(1) Go to Process> Enhance Local Contrast (CLAHE); while optimal parameter may vary for different

images, the parameters shown here work well for this image.

(2) Another way to improve contrast of the image is to go to Process>Enhance Contrast

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1.2 Threshold enhanced image to get the precursor to the particle mask:

Go to Image>Adjust>Color Threshold, a menu will pop up allowing manual control. Depending on the

image, it may be impossible to obtain all particles with a single threshold setting because settings that

capture the small droplets may leave out the larger ones and vice-versa. The solution is to obtain

multiple masks at various threshold levels then combine all the images. In this case, 10 distinct masks

were obtained using both of the enhanced images from 1.1. Each image is saved in TIFF format (as other

formats may lead to data/quality loss). Two examples are shown below:

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1.3 Analyze particles to obtain a particle masks from each of the precursor images:

Go to Analyze>Analyze Particles, use the settings provided below for all precursor images. The size is

expressed in pixels but can be changed to microns if the scale was previously set. The upper limit on the

particle size will eliminate the large black background spots from the precursor image but will keep the

particles in place. Some of the images obtained from this step are shown below:

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1.4 Add together all previously generated masks to obtain the mask for all particles

The numerous masks obtained in the previous step must be combined into a single mask. There are

various means to sum all of the images. Each of the pixels in the image have a value associated with it,

when the image is 8-bit black and white, the values range from 0 to 255, where typically white

corresponds to a pixel value of 255 and black to 0 (although this can be inversed through Edit>Invert or

Image>Color>Edit LUT).

One way to sum two images is to:

(1) Convert images to 8-bit grayscale (white = 255, black = 0) (Image>Type 8-bit);

manipulate polarity so that we get the particles in white and black background

(2) Add one image to the other (Process>Image Calculator) such that a pixel that is part

of the background (black with value =0) will not change anything in the combined image but a pixel

that is part of the particles (white with value = 255) will be added into the combined image

(3) Repeat the image addition with all of the masks previously obtained to get the mask of

all particles

The final step is to 'clean up' the mask by applying the de-speckle function 5 times consecutively

(Process>Noise>Despeckle) and analyzing particles to exclude those fragments smaller than 40 pixels in

terms of area. It should be kept in mind that the specific numbers that work best may vary for other

images.

The final particle mask acquired for this image is shown below:

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1.5 Overlay 'all particles mask' onto the original image to verify if mask is adequate

Before proceeding further, the mask obtained in the previous section must be placed as an overlay on

top of the original image to ensure that it is adequate. If it is found that too many spots are missing from

the mask, then the steps of section 1.0 would be repeated to add more particles to the mask.

The overlay is applied by opening the original image and the mask (ensure the particles are white (255)

and background is black (0) in the mask), selecting the original image and going to Image>Overlay>Add

Image (select to add the mask, make sure to check 'zero is transparent'). The overlay image shown

below demonstrates that the mask produced in this example is adequate for particle size distribution

analysis.

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2.0 Separate Light vs. Dark Particles

2.1 Create separate masks for light and dark particles

Enhance contrast of the original image (Process>Enhance Contrast) by 80% (not equalized) to obtain the

image below:

Use the image calculator (Process>Image Calculator) to calculate:

[Enhanced(80%, not equalized)] XOR [All Particles mask (ensure particles are white)]

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In the above image, we can see that the coloring of the brown particles is light blue while the coloring of

the yellow particles is dark blue. This occurs because the XOR operation between image 1 and 2 is

applied to every pixel. The 80% contrasted image has pixels of red color in all the spots where brown

droplets are present and yellow pixels in all the sports where yellow droplets are present.

2.2 Artifact removal from the light particle mask

In the previous image, it may be noticed that a frequent pattern of error occurs of a ring of light blue

color surrounding the large dark blue particles, examples of this type of artifact are shown below.

The light blue color should only appear where the brown droplets occur and the presence of these ring

artifacts would give rise to a significant error during the size distribution analysis. These rings occur due

to the fact that in the original image, brown rings are present around the large yellow droplets.

In order to correct this artifact, it is necessary to first extract the light particles mask and dark particles

mask from the XOR image:

(1) Go to Image>Adjust>Color Threshold, adjust the threshold to obtain only the light blue and dark

blue particles respectively. It can be seen that the ring artifact is present in the light blue mask that

represents the yellow droplets from the original image.

(2) Dilate the mask for the yellow droplets three time consecutively. (Process>Binary>Dilate)

(3) Convert the masks for both yellow and brown droplets to 8-bit black and white.

(4) Use the image calculator (Process>Image Calculator) to subtract as follows:

[Original brown particle mask] - [Dilated yellow particle mask]

(5) De-speckle the resulting image 3 times to obtain the final mask for the brown particles

(Process>Noise>Despeckle).

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Following the above steps, the separate particle masks are obtained for the yellow and brown droplets

as shown below (may need Image>Color>Edit LUT to define colors).

.

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2.3 Overlay light & dark particle masks onto original to verify if mask is adequate

The next step is to overlay the light and dark particles masks onto the original image in order to verify

that the image segmentation is adequate. Use Image>Overlay>Add Image. The final result is shown

below, it is observed that the masks are adequate.

2.4 Create data tables to provide the numbers for the particle size distribution charts

(1) Go to Analyze>Set Measurements, check area &

centroid (x,y position) & perimeter.

(2) Open the mask image for the light particles, go to

Analyze>Analyze Particles, enter the desired values for

particle sizes & circularity, choose to show outlines,

labeled outlines as well as a table of results will appear.

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3.0 Process Final Data File

(1) Transfer the data from the Fiji measurements window to an Excel file.

(2) If an image scale was not previously set in Fiji, all values will be in units of pixels and it will be

required to convert the units to microns on excel.

(3) Use the measured area of the particle to calculate the diameter of the particle. The diameter is used

as the measure of 'particle size'.

(4) Prepare the histogram and charts from the data as shown below:

Particle Size Light Particle Frequency Dark Particle Frequency

0 ˃ x ≥ 1.5 12 35

1.5 ˃ x ≥ 3 28 82

3 ˃ x ≥ 4.5 47 314

4.5 ˃ x ≥ 6 35 205

6 ˃ x ≥ 7.5 22 130

7.5 ˃ x ≥ 9 16 72

9 ˃ x ≥ 10.5 12 52

10.5 ˃ x ≥ 12 11 24

12 ˃ x ≥ 13.5 9 40

13.5 ˃ x ≥ 15 4 20

15 ˃ x ≥ 16.5 7 16

16.5 ˃ x ≥ 18 7 10

18 ˃ x ≥ 19.5 12 16

19.5 ˃ x ≥ 21 5 12

21 ˃ x ≥ 22.5 2 6

22.5 ˃ x ≥ 24 5 4

24 ˃ x ≥ 25.5 1 3

25.5 ˃ x ≥ 27 8 1

27 ˃ x ≥ 28.5 2 1

28.5 ˃ x ≥ 30 1 1

30 ˃ x ≥ 31.5 1 0

31.5 ˃ x ≥ 33 2 2

33 ˃ x ≥ 34.5 0 0

34.5 ˃ x ≥ 36 0 0

36 ˃ x ≥ 37.5 0 0

37.5 ˃ x ≥ 39 1 0

39 ˃ x ≥ 40.5 0 0

40.5 ˃ x ≥ 42 1 0

42 ˃ x ≥ 43.5 1 0

43.5 ˃ x ≥ 45 0 0

More 0 1

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Concluding Remarks

This procedure demonstrates a versatile method for the extraction of numerical data from images.

Explanation and guidance is provided to allow the plotting of the particle size distribution histogram

from the original image. While a three-phase emulsion (yellow background, yellow droplets, brown

droplets) was analyzed, it is possible to readily apply the method for more complex multi-component

emulsions.

Some of the plug-ins and functions built into Fiji are a result of academic research in image analysis and

proper referencing must be provided in published works using those functions. Tutorials on the various

Fiji plug-ins along with information on the authors of those plug-ins are provided at

http://fiji.sc/Category:Tutorials. A detailed guide about the basics of Fiji can be found at

http://rsbweb.nih.gov/ij/docs/guide/146.html.

As indicated throughout the text, the specific numbers that appear in this procedure are optimal for the

sample image used and different numbers may be needed for other images. Fiji has a built-in macro tool

(Plugins>Macros) that allows the creation of custom macros. Ultimately, the ability to automate the

image analysis depends on the similarity between the set of images analyzed. If all of the images that

are analyzed are sufficiently similar to one another in their general form and content, it would be

possible to run the exact same process to obtain reliable particle size distributions for every image.

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