Desalination 358 (2015) 27–32

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Desalination
journal homepage: www.elsevier.com/locate/desal

Treatment of produced water streams in SAGD processes using tubular

ceramic membranes
Adel Guirgis a,b,⁎, Rafael Gay-de-Montella b, Rami Faiz c
a
Sunshine OilSands Ltd., 903-8 Avenue SW, Calgary, Alberta T2P 0P7, Canada
b
Department of Civil Engineering, University of Calgary, Alberta T2N 1N4, Canada
c
Department of Chemical Engineering and Chemical Technology, Imperial College London, SW7 2AZ, UK

H I G H L I G H T S

• We tested boiler feed water from a Steam-Assisted Gravity Drainage facility that produces oil sands in Alberta Canada.
• The testing was a proof of concept.
• The main criteria were the removal of water soluble organics, mainly naphthenic acids (NAs).
• The NAs were completely removed using the tubular ceramic membranes.
• Selection of the pore size of the ceramic membrane was concluded.

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

Article history: The presence of fine solids and dissolved organics in produced water from Steam-Assisted Gravity Drainage
Received 25 May 2014 (SAGD) process can potentially block pressure vessels and cause fouling and corrosion in steam boilers. Ceramic
Received in revised form 1 December 2014 membranes in tubular configurations with pore sizes of 20 kDa, 50 nm and 100 nm were investigated for the re-
Accepted 9 December 2014
moval of solids and dissolved organics from boiler feed water (BFW). The original BFW sample contained 125,
Available online xxxx
1300 and 20 mg/L of oil and grease (O&G), naphthenic acids (NAs) and total suspended solids (TSS), respectively.
Keywords:
It was found that lowering the pH of the BFW to 4 prior to membrane treatment increased the permeate flux and
Ceramic membranes also eliminated operating drawbacks such as foam formation. Among all the investigated membranes, the Al2O3
Ultrafiltration membrane with 100 nm pore size showed the best performance in terms of flux and removal efficiencies as no
Naphthenic acids detection of total suspended solids was observed in the permeate streams while achieving a high removal effi-
Suspended solids ciency of 80% and 95% for O&G and NA, respectively.
Produced water © 2014 Elsevier B.V. All rights reserved.

1. Introduction The PW re-use has to conceptually accomplish many aspects of the

The two primary in-situ steam injection technologies currently used
in enhanced oil recovery methods are SAGD and cyclic steam stimula-
tion (CSS) [1]. The steam and associated water used in these technolo-
gies are classified as produced water (PW) which becomes inevitably
contaminated with hydrocarbons, water-soluble fractions, suspended
solids and insoluble organics. These contaminants and impurities can
affect the process equipment such as plugging of production vessels
and heat exchangers and causing damage to steam boilers. In Canada,
approximately 179 million m3 of fresh water was used in 2009 for oil
sands-related activities [2]. This in return reflects the need for sustain-
able solutions to utilize PW instead of constantly supplying fresh water.
⁎ Corresponding author at: Sunshine OilSands Ltd., 903-8 Avenue SW, Calgary, Alberta
T2P 0P7, Canada.
E-mail address: aguirgis@sunshineoilsands.com (A. Guirgis).
operating constrains such as de-oiling of water streams and removal
of many soluble organics and suspended solids. A typical water treat-
ment train in SAGD processes is shown in Fig. 1. The process starts
with a knock-out drum to remove undissolved solids and gases, follow-
ed by Induced Gas Flotation (IGF) units and oil filters to remove residual
oils, and finally softening of the water to meet the boiler feed water
(BFW) specifications. The PW stream is further processed through an
ion-exchange unit to replace ions that are responsible for hardness,
alkalinity and mineralization. Despite this extensive treatment, oil drop-
lets were still regularly reported in downstream effluents, particularly
fine droplets less than 25 μm in size. Current reports have also shown
that solids of (b40 μm) were found in BFW samples collected down-
stream of IGF units in SAGD plants in north-eastern Alberta, Canada
[2]. Additionally, among the many organics found in BFW, Naphthenic
Acids (NAs) comprise a group of long-chain carboxylic acids that can
cause many issues. They are very corrosive and cause pitting in boiler
tubes, which necessitates their removal prior to recycling the water

http://dx.doi.org/10.1016/j.desal.2014.12.007
0011-9164/© 2014 Elsevier B.V. All rights reserved.
28 A. Guirgis et al. / Desalination 358 (2015) 27–32

Table 1
Properties of the ceramic membrane modules.

Membrane modules 100 nm/19 50 nm/19 50 nm/7 20 kDa/7

Material Al2O3 Al2O3 Al2O3 ZrO2

Pore size (nm) 100 50 50 2
Number of channels 19 19 7 7
Membrane length (m) 1.178 1.178 1.178 1.178
Membrane area (m2) 0.200 0.158 0.158 0.158

acceptable separation efficiencies, the use of other membrane shapes

Fig. 1. Block flow diagram for water treatment process in SAGD processes. High tempera-
ture separators (HTS), skim tanks, induced gas flotation (IGF), filters, warm lime softening
(WLS), ion exchangers (IONX) and steam generators (SG).
[3]. Currently over 90% of the produced water in SAGD processes is
recycled back to boilers as BFW. The presence of contaminants in BFW
has limited the use of boilers and demanded the frequent replacement
of these units.
The use of membranes has been the focal point of many researchers
and industrial institutions as a new means for waste water treatments.
This is demonstrated by the numerous publications in reverse osmosis
(RO) [4,5], ultrafiltration (UF) [6,7] and microfiltration (MF) [8] mem-
brane technologies. Although polymeric membranes have shown a
great certainty of success in these applications, they still suffer from sta-
bility issues such as fouling and their questionable ability to operate for
extended periods [7]. On the other hand, the use of ceramic membranes
offers great advantages such as high thermal and chemical resistance
while providing long term stability [9]. Recent publications in the liter-
ature also demonstrate the preferential use of ceramic membranes than
convention polymeric counterparts to treat oily water [10,11]. Neverthe-
less, Chen et al. [12] was one of the early authors to carry out a pilot plant
analysis to remove oil and grease (O&G) and total suspended solids (TSS)
from BFW using alumina ceramic membranes. Reasonable removal rates
were achieved while reporting detection limits of O&G and TSS less than 5
and 1 ppm, respectively [12].
Deriszadeh et al. [3,13,14] also reported on the improved ultrafiltra-
tion process of BFW with cationic micelles and were able to remove NAs
by filtration using a series of 13 kDa polyacrylonitrile (PAN) polymeric
membranes followed by TiO2 ceramic membranes of 15 and 50 kDa.
However, the study was carried out using synthetic NA solutions,
which does not fulfill industrial requirements and specifications of
BFW, which usually supplied at high temperatures and could be highly
corrosive due to the presence of concentrated organics. Peng et al. [15]
discussed the successful removal of NAs from actual BFW samples and
reported a 95% removal rate with a flux of 15 L/m2 h. However, their
bench-scale system was carried out using flat sheet membranes which
explains the low flux. In order to achieve high permeation rates with
such as hollow fiber, monolith, or honeycomb configurations is proposed
instead. Beni [21] tested different ceramic membranes with synthetic pro-
duced water with 100% oil removal rates with ultrafiltration. This paper is
unique in that it tested BFW from an operating SAGD plant.
The purpose of this study is to investigate different ceramic
membrane modules with monolith configurations for the treatment
of BFW samples from actual SAGD plants to simultaneously remove
oil and grease, suspended solids and dissolved organics of NAs. The mem-
brane performances and removal rates of all contaminants are analyzed
and discussed in details.
2. Experimental
2.1. Materials
2.1.1. Ceramic membrane modules
The ceramic membrane with different monolith configurations and
properties were supplied by SJE-Rhombus, USA and can be assembled
into membrane modules as shown in Fig. 2. Alumina (Al2O3) and zir-
conium oxide (ZrO2) were the primary constituents of the ceramic mem-
branes used in this study due to their high chemical and thermal stability.
Four specific types of tubular monolith configurations were tested in the
experimental analysis, (a) 100 nm-19 channels (b) 50 nm-19 channels
(c) 50 nm-7 channels (d) 20 kDa-7 channels. The complete properties
and specifications of the ceramic membrane modules are summarized
in details in Table 1.
2.1.2. Description of the BFW sample
The original BFW sample was provided from a SAGD plant in Alberta,
Canada. The properties of the BFW sample were dark black, non-viscous
and loaded with solids and colloidal emulsions. The feed BFW used in
the experimental runs had an initial pH of 10. Initially, using these sam-
ples resulted in rapid foaming due to the presence of additives such as
surfactants (naphthenic acids and suspended solids) that were coated
by oil and grease and formed a stable colloidal emulsion in the BFW.
And thus, hydrochloric acid (HCl) was added to the samples prior to
testing to lower the pH. Several runs were carried out at different pHs,
including 7, 5.5 and 4. The process performance at a pH of 4.0 was deter-
mined to be the most stable with no operating drawbacks, and thus was
chosen as optimum conditions for the analysis considered in this work.

Fig. 2. Different monolith ceramic membranes and modules considered in this work.
 A. Guirgis et al. / Desalination 358 (2015) 27–32
Fig. 3. Experimental setup for the BFW treatment.
2.2. Experimental setup
The ceramic tubular membrane (CTM) system consisted of a feed
drum attached to the inlet of a horizontal stainless steel housing con-
taining the monolith ceramic membrane as shown in Fig. 3. The outlet
of the stainless steel housing was connected to another drum for collec-
tion of the rejected water stream (known as retentate). Pressure gauges,
flow meters and sample valves corresponding to the feed, permeate and
retentate streams were also attached at the inlet and outlet of this sys-
tem as shown in Fig. 3. Initial experiment runs with deionized water
were carried out to determine the membrane performance under opti-
mum conditions. Afterwards, treatment of BFW samples was tested at
different trans-membrane pressures using the membrane modules
mentioned above. Each process run consisted of a single pass through
the ceramic membrane while measuring the inlet and effluent pressures
and flow rates. The BFW was pre-heated to 45 °C using a heating belt to
simulate realistic field operating conditions. At the end of the process
test run, the membrane was subjected to a rigorous cleanup process,
followed by duplicate baseline experiment and test runs. An online ac-
quisition system was connected to the experimental setup to measure
the effluent flow rates and pressures. A conductivity and pH meter
were used for each run to measure the feed, permeate and retentate
properties.
2.2.1. Analytical analysis
Analytical testing was carried out using Fourier Transform Infrared
Spectroscopy–Attenuated Total Reflectance (FTIR–ATR) analysis to
determine the initial content of the NAs, O&G [19,20] and TSS in the
BFW samples prior and after treatments. The removal efficiency was
Fig. 4. Influence of feed pH on the performance of 100 nm/19 membrane module.
29
determined considering the area under the absorbance spectra in the
range between 3058 and 2800 cm−1. The absorbance of the C\H
bond and the stretching of the aliphatic groups in CH2 and CH3 was de-
termined to be at 2930 cm−1 and 2969 cm−1, respectively.
The performance of the ceramic membrane modules with different
pore sizes of 20 kDa, 50 nm and 100 nm was evaluated by comparing
the permeate flux at various trans-membrane pressures (TMPs) and
calculating the percent removals of the contaminants in the BFW.
2.2.2. Particle size distribution
Particle size analysis of the TSS in the feed, permeate and
retentate streams was carried out using a Malvern particle size ana-
lyzer, Mastersizer 3000, Canada.
3. Results and discussions
3.1. pH adjustments
As mentioned earlier, the original BFW sample had an initial pH of
10. However, carrying out experiments with this sample resulted in
massive foam formations and reduced the performance of the ceramic
membranes significantly, as the majority of the feed exited the mem-
brane as a retentate without producing any permeate flux. The reason
for this rapid foam formation was due to the existence of many addi-
tives in the original BFW sample such as surfactants (including NAs),
suspended solids and other stable colloidal emulsions in the BFW.
These chemicals are usually present in the BFW collected from SAGD
plants, and thus the pH of the BFW must be lowered before treatment
Fig. 5. Performance of the ceramic membrane modules as a function of trans-membrane
pressure.
30 A. Guirgis et al. / Desalination 358 (2015) 27–32

Table 2
Performance of ceramic membrane modules.

Membrane TMP bar Flux (L/m2 h) O&G in feed (ppm) O&G in permeate (ppm) % Removal NA in feed (mg/L) NA in permeate (mg/L) % Removal (NA)
module (O&G)

100 nm/19 0.99 271 125 24.8 80% 1300 22 98%

50 nm/19 1.40 94 125 25.5 79% 1300 70 95%
50 nm/7 1.28 131 125 28.9 77% 1300 34 97%
20 kDa/7 1.41 84 125 25 80% 1300 18 99%

to minimize foam formation and increase the performance. In fact, it
was confirmed that the permeate flux with the membrane module of
100 nm pore size and 19 channels increased with lowering the pH of
the solution. Fig. 4 depicts the flux of the 100 nm/19 membrane module
as a function of trans-membrane pressure for BFW samples with differ-
ent pHs. It can be noticed that passing deionized water (pH of 7) through
the membrane resulted in a linear relationship with operating pressure
while demonstrating a low breakthrough pressure of 0.3 bar. On the
other hand, treatments of the BFW samples with different pHs showed
higher breakthrough pressures at approximately 1 bar and suggested that
the permeate flux increased with lowering the pH of the solution. For in-
stance, the observed permeate fluxes were 100, 170 and 300 L/m2 h when
the pHs of the samples were 7, 5, and 4, respectively, while operating at a
trans-membrane pressure of 1.2 bar. And thus, a pH of 4 was chosen as
optimum conditions for the remaining experimental analysis with the
other membrane modules.
3.2. Membrane performances
The permeation fluxes through all four ceramic membrane modules
considered in this work are demonstrated in Fig. 5 as a function of trans-
membrane pressure while operating a pH of 4. It can be shown that the
permeate flux increased with increasing the trans-membrane pressure
for the 100 nm/19, 50 nm/7 and 50 nm/19 membranes. However, the
flux through the membrane module with the smallest pore size of 20
kDa/7 showed a decrease in flux with further increase in the operating
trans-membrane pressure. This can be explained by complete pore
blockage occurring at the ceramic membrane surface caused by the
high concentration of solids and particles in the feed. These results are
in line with other studies in the literature as shown by Bacchin et al.
[16]. The critical permeate flux of the 20 kDa/7 membrane module
was determined where the performance starts to decrease with further
increase in the trans-membrane pressure. This value was determined to
be 140 L/m2 h as shown in Fig. 5.
Moreover, it can be noticed that the highest flux was obtained
through the 100 nm/19 module. This can be attributed to the larger
pore size of the membrane, i.e. 100 nm compared with 50 nm and
2 nm, and thus higher flux was also achieved. On the other hand, filtra-
tion through the 50 nm/7 and 50 nm/19 membrane modules showed
the operating trans-membrane pressure. It was anticipated that the per-
formance of 50 nm/7 module should outperform the 50 nm/19 due to
higher fluid velocity through lower channels in the module. However,
since the performances of both modules were identical as shown in
Fig. 5, it can be concluded that the membrane flux depends solely on
the pore size and not the operating velocity of the solution. This was
also demonstrated by the high performance of the 100 nm/19 module.
3.3. Oil and grease removal efficiency
The initial O&G concentration in the BFW sample was measured to
be 125 mg/L. It should be noted that the presence of high O&G and
lighter hydrocarbons content in BFW created a stable colloidal emul-
sion. However, after lowering the pH of the BFW to 4 coagulation of
the colloidal emulsion occurred and resulted in the small oil droplets co-
agulating to form larger droplets. These newly formed larger oil droplets
were easily trapped in the small membrane pores. The same phenome-
non was observed by Salahi et al. [17] who used a 20 kDa tubular ultra-
filtration PAN membranes to treat oily wastewater from a refinery
stream. It was demonstrated that the optimum conditions for cross
flow velocity configurations would be operating at a higher tempera-
ture with a lower pH and moderate trans-membrane pressures [17].
This observation was also supported by the study of Chen et al. [12]
with ceramic crossflow microfiltration and confirmed that chemical
pre-treatment of the feed resulted in flotation of the oil-wet solids and
helped separating the solids from the PW. In this work, all four of the ce-
ramic membrane modules were able to treat more than 80% of the initial
O&G concentration of 125 mg/L. Table 2 shows the percentage removals
of O&G by different membrane modules at several operating conditions.
3.4. Naphthenic acid removal
The initial NA concentration in the feed stream was determined to
be 1300 mg/L. This concentration is considered quite high since it was
obtained under plant upset conditions. However, a normal BFW sample
usually contains a NA concentration of approximately 250 mg/L. The re-
moval efficiency of NA using the membrane modules is summarized
20

similar and moderate fluxes that improved gradually with increasing

15

100nm RETENTATE
50nm RETENTATE
% Volume

20kDa RETENTATE
10

0
1 10 100
Particle Size (um)

Fig. 6. Particle size distribution of the suspended solids in the feed sample. Fig. 7. Particle size distribution of the suspended solids in the retentate stream.
 A. Guirgis et al. / Desalination 358 (2015) 27–32
25
20
20kDa PERMEATE
50nm PERMEATE
15
% Volume
10
5 Finally, it can be concluded that the ceramic membrane modules
0 solid content in the feed. Fig. 9 shows the images of the BFW samples
1 10
Particle Size (um)
Fig. 8. Particle size distribution of the suspended solids in the permeate stream.
and shown in Table 2. It can be noticed that a significant amount of NA
removal was observed for all four membranes (N95% removal). This
excellent removal efficiency of NAs by the ceramic membranes can be
explained by the electrostatic charge model [18]. The change in the pH
of the feed can influence the membrane's performance by affecting
the membrane surface charge. The point of zero charge for alumina
and zirconia was approximately 8 and 6.4, respectively [18]. However,
when the pH of the feed water was reduced to 4 both of the surfaces
were positively charged and adsorbed NAs, resulting in the efficient re-
moval of NAs from BFW.
3.5. Solid removal
Particle size analysis of the solids in the feed, permeate and retentate
streams was carried out using a particle size analyzer. The original BFW
sample obtained a bell-shaped pore size distribution with a maximum
particle size of 250 μm as shown in Fig. 6. It was also evident that the
majority of the particle size in the BFW sample lied within the range
of 10 μm. The particle size distribution of the retentate and permeate
streams through the tested membrane modules are shown in Figs. 7
and 8, respectively. The analysis of the 50 nm/7 membrane module
was excluded due to the similarity in the experimental behavior with
the 50 nm/19 module as demonstrated earlier in Fig. 5. Since the 20
kDa/7 membrane module showed the worst performance among
others, the presence of large size particles is expected to be found in
Fig. 9. Images of the BFW before and after treatment with the ceramic membranes. Left (original sample without acid treatment), Right (lowering pH to 4).
31
both the retentate and permeate streams. This was confirmed in Fig. 7
with the largest particle size distribution in the retentate stream was de-
tected for the 20 kDa/7 membrane module. The 20 kDa/7 membrane also
showed the presence of large particle size in the range of 50–100 μm in
the permeate stream as shown in Fig. 8. On the other hand, the 100 nm/
19 module showed the best performance as no particles of any size was
detected in the permeate stream (Fig. 8). It should also be noted that
the majority of the particle size detected in the retentate streams of all
membrane modules were in the range of 1 μm which also confirms that
applicability of the ceramic membranes in treating the BFW samples re-
garding of their performances.
were very successful in treating the BFW samples and were able to
remove N95% of NAs, N80% of O&G and the majority of suspended
100 before and after treatment with ceramic membrane modules. The im-
ages on the left side were carried out without acid treatments, whereas
the images on the right were a result of lowering the pH of the BFW to 4
prior to membrane treatments.
4. Conclusions
Treatment of BFW samples was carried out using Al2O3 and ZrO2
ceramic membrane modules with different properties and monolith
configurations. These modules consisted of 100 nm, 50 nm, and
20 kDa pore sizes. It was confirmed that treatment of the BFW by ultra-
filtration mechanisms alone cannot remove all dissolved ions and or-
ganics in the feed. However, pretreatment of the feed by acid injection
improved the permeate flux and eliminated operating drawbacks such
as foam formation. Among all the investigated ceramic membrane mod-
ules, the membrane with 100 nm and 19 channels showed the best
performance in terms of permeate flux and contaminant removal. On
the other hand, pore clogging and blockage were observed for the
membrane with the smallest pore size of 20 kDa, whereas the
50 nm membrane showed moderate performances while allowing
the passage of very fine particles in the permeate streams. The
100 nm macroporous ceramic membrane was determined to be the
best choice in this application due to the absence of any suspended solids
in the permeate streams.
Acknowledgements
The authors would like to thank Mike Metalek from SJE-Rombus
and Louis Mabarre from Mabarex for coordinating the supply of the
32 A. Guirgis et al. / Desalination 358 (2015) 27–32
membranes and the experimental apparatus. Vita Martez from SAIT
is gratefully acknowledged for completing the experiment work.
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