Energy Nexus 7 (2022) 100141

Contents lists available at ScienceDirect

Energy Nexus
journal homepage: www.elsevier.com/locate/nexus

Feasibility of thin film nanocomposite membranes for clean energy using

pressure retarded osmosis and reverse electrodialysis
Arvin Shadravan a,∗, Mahmood Amani b, Anish Jantrania c
a
Department of Industrial and Systems Engineering, Texas A&M University, College Station, TX 77843, USA
b
Department of Petroleum Engineering, Texas A&M University at Qatar, 23874 Doha, Qatar
c
Department of Biological and Agricultural Engineering, Texas A&M University, College Station, TX 77843, USA

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

Keywords: Power generation from renewable energy sources is becoming increasingly significant as global energy consump-
Thin film nanocomposite membranes tion increases. The non-renewable energy sources we use now are on the verge of extinction. Reverse electro-
Separation processes dialysis and pressure retarded osmosis are two methods of harvesting renewable energy using salinity gradients.
Pressure retarded osmosis
There are non-polluting sources of energy that can be found at the interface of two solutions with varying salinity
Reverse electrodialysis
gradients. Reverse electrodialysis makes use of ion-selective membranes while uses salt rejecting membranes. It is
Industry 4.0 and Power generation
necessary to employ membranes. Unlike pressure retarded osmosis membranes, ion-exchange membranes involve
controlled mixing. The ion flux is employed by ion-exchange membranes in reverse electrodialysis to extract en-
ergy. Pressure retarded osmosis is an emerging membrane process uses for harvesting energy and desalination
applications. Salinity gradient energy is a zero-emission and sustainable technology that can be practically ap-
plied worldwide. By employing a semipermeable membrane to control the mixing process, the osmotic pressure
gradient energy can be generated in terms of electrical power via pressure retarded osmosis without causing
adverse environmental impacts. In this study, the thin film nanocomposite membrane was fabricated by forming
a polyamide thin film on the polysulfone substrate through the interfacial polymerization process.

1. Introduction 1. Literature review

The most efficient advantage in energy production through salinity The two major methods to have energy generation through salinity
gradient is that it can be continuous, non-stop and provide constant gradient contains PRO and RED. According to the function of reverse
energy production. There are various kinds of methods that are available osmosis (RO) and electrodialysis (ED), PRO process and RED process
for energy generation through salinity gradients which contains reverse functions vice versa. Through PRO, molecules of water will spread from
electrodialysis (RED) and pressure retarded osmosis (PRO) [1–3]. a low salinity towards the pressurized and high salinity solution through
If two solutions with various sorts of molecular structure connect a membrane. The concentrated solution will go across a hydro-turbine
with each other, they will mix instantly and produce energy. In addi- to produce power which is shown in the Fig. 1 [7].
tion, if two solutions with different concentrations of chloride face each In the process of RED, ion exchange membranes will separate the two
other it can produce energy by the pressure which called osmotic power. kinds of solutions with high salinity and low salinity. The different con-
Therefore, the concentration of salt is prone to produce energy. Osmotic centration of these two solutions will be the reason to spread counter-
pressure has been widely used for harvesting energy among renewable ions through these membranes [8–13]. Ion exchange membrane which
energies. In the following, free Gibbs energy of mixing is one of the ways consists of anion and cation will separate so much channel pairs with
to produce energy [4–6]. high salinity and low salinity during RED. This process can be observed
in the Fig. 2 [7].
∆G mix = Frictional Losses + Unutilized energy + Extractable Work The comparison between PRO and RED is stated in the following
(1) sentences: the major improvement for PRO is about increasing the water
permeabilities and simultaneously decreasing the salt permeability for
membranes while in RED the conduction will be increased and there is
no need for decreasing perm selectivity (decreasing the thickness of the

∗
Corresponding author.
E-mail address: [email protected] (A. Shadravan).

https://doi.org/10.1016/j.nexus.2022.100141
Received 14 May 2022; Received in revised form 28 August 2022; Accepted 5 September 2022
Available online 6 September 2022
2772-4271/© 2022 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/)
A. Shadravan, M. Amani and A. Jantrania Energy Nexus 7 (2022) 100141

as a very clean technology which is because of no by-product forma-

Nomenclature tion and no CO2 emission. The essential requirements in the membrane
for PRO process are: i) high water flux, ii) moderate tolerance to pH
Symbols change and chlorine attack, iii) high mechanical strength and stability
PRO Pressure Retarded Osmosis and iv) low internal concentration polarization effect [39–41]. The feed
RED Reverse Electrodialysis solutions in PRO processes are typically freshwater, wastewater efflu-
TFN Thin Film Nanocomposite ent, and brackish water, while the draw solutions are usually seawater,
Fo Forward Osmosis RO brine concentrate, etc. Thin film nanocomposite (TFN) membranes
FESEM Field Emission Scanning Electron Microscope are widely used in recent years for the desalination applications. It is
AFM Atomic Force Microscopy mainly due to the achievement of high flux without compromising the
Jw Water Flux (L.m2 .h) salt rejection. Hydrophilicity is the main required property in attaining
JS Reverse Solute Flux (g/m2 h1 ) the higher water flux [42]. The conventional TFC RO membranes are
UF Ultra-Filtration dense skin layer, which aids in high salt retention and lower flux. Con-
TMC 1,3,5-benzenetricarbonyl trichloride versely, PRO membrane should be of thin skin for the achievement of
MPD 1,3-phenylenediamine high flux. PRO based on the mechanism of osmotic pressure gradient.
PSF Polysulfone Thus, the design of TFN membrane is the prerequisite for achieving the
ΔG mix Gibbs free energy of mixing (kWh/m3 ) high-power density [43–46]. Hence, TFN was fabricated in this study
AL-DS Active Layer Facing Draw Solution by forming a polyamide thin film on the polysulfone (PSF) substrate
AL-FS Active Layer Facing Feed Solution through the interfacial polymerization (IP) process. Prior to the forma-
ICP Internal Concentration Polarization tion of thin film, the substrate was embedded with zeolite which acts
A Water permeability coefficient (L/m2 .h.bar) as the hydrophilic fillers [47]. The resultant TFNs was then subjected to
TFC Thin Film Composite different physical characteristics such as field emission scanning elec-
Δ𝜋 Osmotic Pressure difference tron microscope (FESEM), atomic force spectroscopy (AFM) and con-
tact angle analyses. Finally, the performance of the membrane in terms
of osmotic power generation was assessed in PRO testing. The power
membrane) and the channel height is enormously decreased [14–19]. density of PRO membranes is highly dependent on osmotic pressure
To generate power from salinity gradients, PRO is in better condition and water flux. The mechanical stability at high hydraulic pressures is,
according to the power density calculations [20–23]. therefore, one concern for PRO membranes. 3D zeolites are microporous
The result of comparison between PRO and RED with each other is crystalline aluminosilicates with well-defined nanoscale pore structures
that in RED there is more power density production for the low salinity in their regular frameworks. The hydrophilicity and permeability of 3D
gradients such as facing river water and sea water through a membrane zeolites facilitate the permeability/selectivity and fouling resistance of
[24–26]. Forward osmosis (FO) membranes make PRO more trustwor- ultrafiltration and reverse osmosis membranes [48]. 3D Nanomaterials
thy method and higher potentiality. The mixing of water and sea water have advantage as higher surface area, water absorption capacity and
has the power density about 2.3 W/m2 while in RED the power density assembly on the polyamide layer. Thus, the current study is dedicated to
is 1.3 W/m2 [27–29]. investigation of the TFN membrane incorporated with zeolite for PRO
In another study, reverse osmosis membrane incorporated with application. The foremost approach, unlike other studies, which have
Graphene Oxide (GO) was embedded into the active layer of the mem- dealt with commercial TFC membrane for the power generation. Zeo-
brane. A gradient nanocomposite membrane has been demonstrated lite is a 3D nanomaterial which is highly hydrophilic as well as the salt
through simulation-guided design. The simulation results suggested that rejection properties. It is mainly due to the cage-like structure of the ze-
the protective layer should be > 100 nm thick with <130 nm pores at a olite. Hence, in this study, the zeolite is incorporated in TFN polyamide
porosity of 72% [30–32]. (PA) layer to improve the membrane surface properties for PRO appli-
Developing osmotic processes which are driven by membrane may cations [49–51].
supply sustainable solutions for the needs globally of either clean wa- 3D printing which is also called Additive Manufacturing (AM), is one
ter or the clean energy. Osmotic processes use the difference of osmotic of the fundamental elements of Industry 4.0 where three-dimensional
pressure solutions through a semipermeable membrane for drawing wa- (3D) objects are efficiently manufactured through layer-by-layer addi-
ter from a diluted feed solution to a draw solution which is more concen- tion [52–56]. Polymers are the main materials used in 3D printing, even
trated [33–35]. This kind of energy can have the harvesting potential though a minority of ceramic and metal particles are utilized in some
to generate power by utilizing PRO. It was predicted that all the poten- high-end machines [57–61]. Materials with good printability are vital
tial energy sources can harvest almost 2000 TWh every year of power for 3D printing, and are associated with material properties, fabricating
generation that can be more than 10% for the existing demand of en- means, and the complexity of the final printed structure. In fact, the mul-
ergy in the world [36–38]. Furthermore, PRO is somehow considered

Fig. 1. Schematic of pressure retarded osmosis

process for generating the electricity [7].

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A. Shadravan, M. Amani and A. Jantrania Energy Nexus 7 (2022) 100141

Fig. 2. Schematic of reverse electrodialysis

function through ion exchange membrane [7].

tifunctional applications of the 3D printed structures based on graphene Firstly, dried PSF substrate was mounted on a frame, 2 wt% of aqueous
or graphitic fillers and zeolite-based membranes open up the countless monomer solution of MPD was poured onto a membrane for 1 minute
possibilities of current research [62–65]. In addition, the concept of the to form the amine layer over the substrate. Then, the excess MPD solu-
system of systems leverages interconnected systems to address the needs tion was drained and removed using the rubber roller. Subsequently, 0.1
of efficient farming, energy distribution, and water conservation [66– wt% of TMC solution in n-hexane solution was poured onto the amine-
70]. catalyzed PSF membrane. It was allowed to react for 50 sec to form a
thin polyamide layer over the commercial PSF membrane. Immediately,
2. Experimental the thin film was allowed to get bound in substrate by keep in an oven
at a temperature of 60˚C for 5 min. Finally, the reaction was terminated
During the period of osmosis process, permeate water rapidly diluted by storing the membranes in distilled water. For TFN membranes, the
draw solution, when the feed solution is being concentrated. The pres- molecular sieves were dispersed using ultrasonicator in organic TMC/n-
sure which is hydrostatic is entitled to osmotic pressure such as water hexane solution. The above mentioned were also followed for the prepa-
transportation passing through the membrane while it is functionalized ration of TFN membranes. The molecular sieves were loaded in three
to draw solution. At any step while ∆P can be between zero to Δπ (Os- different fractions from 0.05 to 0.3 and labeled as Zt TFN 0.05, Zt TFN
motic pressure), water can flow into the saline water because Δπ is still 0.1, Zt TFN 0.3.
larger than the pressure which is ∆P. This process is entitled to PRO
[71–72]. 2.3. Characterization of membranes
In order to calculate the water flux through PRO process we need to
calculate Jw which is the sign of water flux and is shown by the following 2.3.1. Morphology analysis of membranes
Eq. (2) [73]: Top surface of TFC and TFN membranes were analyzed using mor-
phology analysis methods using field emission scanning electron mi-
J𝑤 = A𝑤 (Δπ − Δ𝑃 ) (2) croscope (FESEM, Zeiss Crossbeam 340) and atomic force microscopy
(AFM, SII Nano Technology SPA 300HV using dynamic force contact
In this equation Aw is membrane permeability coefficient
(L/m2 h.bar) and ∆P is differential feed pressure (bar) and Δπ is mode (DFM)). Dried membranes were sputtered with gold particles and
viewed in FESEM under high vacuum condition.
the osmotic pressure (bar).
2.3.2. Contact angle analysis of membranes
2.1. PRO membranes The contact angle of membrane is used to determine the surface
wettability of membranes by sessile drop method. Goniometer was uti-
The general equation to estimate the PRO membrane water flux is lized to determine the hydrophilic property of membranes by placing
Eq. (3). Salt permeates across the membrane in the opposite direction of the dropping of water on the surface of membranes.
the water flux, from the more concentrated draw solution into the feed
solution. The reverse solute flux, Js , is described by [73]: 2.4. Performance evaluation
( )
J𝑠 = B C𝐷,𝑚 , m − C𝐹 ,𝑚 (3)
The membrane performance was studied by three different
Where B is the salt permeability coefficient of the membrane, the membrane-based desalination methods such as Reverse Osmosis (RO),
active layer, and CD,m and CF,m are the solute concentrations in the so- Forward Osmosis (FO) and Pressure Retarded Osmosis (PRO).
lution at the active layer interface on the draw and feed sides.
2.4.1. Water flux analysis of membranes
2.2. Materials and methods Dead end filtration (HP4750, Stirred Cell, for operation up to
1000 psi, Sterlitech) was used to study the water permeability of the
The chemicals and materials utilized in this research are as follows: membranes. In dead end filtration, nitrogen cylinder used to maintain
A commercial UF PS membrane support (PS35, Nanostone Flat Sheet the transmembrane pressure. The membrane was initially compacted at
Membrane) was purchased from Sterlitech Corporation. N-Hexane was a pressure of 1600 kPa for 45 min. The water flux (Jw ) of the membrane
obtained from Fisher Scientific. TMC, MPD, Zeolite (Molecular Sieves, was measured using the following Eq. (4):
3 Å), Sodium Chloride were purchased from Sigma Aldrich. Prior to 𝑄
𝐽𝑊 = (4)
TFC membrane preparation, commercial polysulfone membrane was 𝐴
soaked in RO water for an overnight. Interfacial polymerization tech- where, Q is the permeate rate (LMH) and A is the effective cross-
nique was adopted for the fabrication of polyamide layer membrane fab- sectional area of the membrane (m2 ). Membrane permeability was mea-
rication. The schematic of interfacial polymerization is shown in Fig. 3 sured from the slope of the plot between pure water flux and pressure.

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A. Shadravan, M. Amani and A. Jantrania Energy Nexus 7 (2022) 100141

Fig. 3. Schematic of interfacial polymerization of PA-TFC

membrane. (a) PS35 commercial membrane and TFC utensils,
(b) MPD treatment by roller, (c) treatment of membrane by
TMC and (d) immersion of TFC membrane in RO water.

Fig. 4. FO-PRO cross flow cell experimental

setup.

2.4.2. RO Filtration studies of membranes feed solutions or AL-FS) and PRO mode (active layer facing the draw
After compaction of membranes, the membrane was assessed using solution or AL-DS).
the filtration of 2000 mg/L of sodium chloride solution in dead-end fil- Initially, RO water was filled in both feed and the draw solution tank.
tration set up at a pressure of 1500 kPa for 1 h. The concentration of per- Prior to experiments, RO water was circulated in FO mode for 15 min.
meate (Cp ) and feed (Cf ) was measured using conductivity measurement Next, 2 M NaCl solution replaced in draw solution tank and placed in
(Conductivity meter 4520, Jenway). The salt rejection of membrane was digital weighing balance. The experiments were started after the flux
estimated by the Eq. (5): stabilization and carried out for 90 min. The samples were analyzed at
( ) the time interval of 30 min. Again, water was replaced in draw solution
𝐶𝑝
Per centage of r ejection (R%) = 1 − × 100 (5) and feed tank also was circulated for 15 min. Then, the membrane ori-
𝐶𝑟
entation towards PRO was conducted as per the above-mentioned pro-
cedure. For PRO, the pressure was maintained at the level of 5000 kPa
2.4.3. FO and pro filtration studies of membranes and the draw pump was replaced with the high-power pump speed. The
Fig. 4 shows the lab-scale FO and PRO cross-flow cell test setup. The general water transport across the membrane is expressed in Eq. (6).
feed and draw solution of RO and PRO experiments are as RO water The water flux and solute flux of the membrane was estimated using
and 2 M NaCl solution respectively. The feed and draw solution were the followings Equation:
pumped through the membrane using peristaltic pump at the speed of
300 rpm. Digital weighing balance was used to monitor the draw solu- Δ𝑉𝑓 𝑒𝑒𝑑 Δ𝑚 ∕𝜌𝑓 𝑒𝑒𝑑
𝐽𝑣 = = (6)
tion tank. Feed was continuously monitored using conductivity meter. 𝐴𝑚 × Δ𝑡 𝐴𝑚 × Δ𝑡
In FO modes, the active PA is facing towards the feed solution and
draw solution is circulated over the bottom layer. Feed and draw solu- Where ΔV is the volume of feed solution, and Δ𝑚 ∕𝜌𝑓 𝑒𝑒𝑑 is the differ-
tion were interchanged in PRO mode. All the membranes were tested in ence in mass of feed solution. 𝜌𝑓 𝑒𝑒𝑑 is the density of feed solution; Am
two different operational modes i.e., FO mode (active layer facing the is effective membrane area and the effective membrane area is 42 cm2

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A. Shadravan, M. Amani and A. Jantrania Energy Nexus 7 (2022) 100141

Fig. 5. FESEM surface morphology of (a) TFC,

(b) 0.05 Zt 3ÅTFN (c) 0.1 Zt 3ÅTFN and (d) 0.3
Zt 3ÅTFN.

and Δt is the measuring time interval.

( )
Δ Ct Vt
Js = (7)
Am × Δt

Where Ct and Vt are the salt concentration (g/L) and the volume of
the feed solution (L) at the end of the tests, respectively. The experiments
were conducted in both FO and PRO modes. Power density (W/m3 ) was
calculated by following equation:

W = Jw ΔP = A(Δπ − ΔP)ΔP (8)

4. Results

4.1. Characterization of the fabricated membranes

Fig. 5 shows the surface morphology of TFC, and zeolite incorporated Fig. 6. Water flux in AL-FS and AL-DS mode for TFC and zeolite incorporated
TFN membranes captured using FESEM. From Fig. 5 (a), TFC membrane TFN membranes.
shows the dense pores but the pore structures of TFN membranes are dif-
ferent. A defect-free polyamide separation layer with surface crumbles
was formed on the substrates after the interfacial polymerization of the 4.2. Effect of zeolite on the FO and pro performance of tfn membrane
polyamide layer with polysulfone. The zeolite is clearly distributed on
the surface of TFN membranes which is shown in Fig. 5 (b) to (d). It The FO water flux is presented for both AL-DS and AL-FS (Fig. 6)
indicates the zeolites’ existence on the surface of the polyamide layer. orientations by using 2 M NaCl as draw solution and deionized (DI) wa-
This is due to the attachment of zeolite through the hydrogen bonding ter as feed solution. Figs. 6 and 7 show the corresponding water and
between the surface hydroxyl (-O-) group of zeolites and the carbonyl solute flux in FO mode for AL-FS and AL-DS of TFC and zeolite incor-
group of the polyamide layer. During the interfacial polymerization pro- porated TFN membranes. Without zeolite loading, the TFC membrane
cess, the steric hindrance of the zeolite in aqueous solution decreased had an FO water flux of 3.8 L/m2 h in AL-DS for the DI water as FS.
the diffusion of polyamide layer and thereby retarded the formation of It is observed that the water flux increased progressively in the TFN
the PA layer. Moreover, the surface crumples were reduced in zeolite membranes. It is due to the increase of hydrophilicity and reduction
incorporated TFN membranes. This can be ascribed to steric hinderance of membrane thickness. The reduction in membrane thickness refers
effect of zeolite nanoparticles flakes and the delayed interfacial poly- to modification of polyamide layer formation during interfacial poly-
merization arising from the excess aqueous monomer’s concentration. merization while with the addition of inorganic zeolite. Higher water
Thereby, it tends to increase the interaction between the nanoparticles flux of 5.6 L/m2 h observed in AL-DS modes on 0.1 wt% zeolite loaded
and the active layer of the TFN matrix. TFN membranes. As can be seen in Fig. 6 (d), the zeolite particles were

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A. Shadravan, M. Amani and A. Jantrania Energy Nexus 7 (2022) 100141

creases in the salinity gradient in terms of power density. Furthermore,

contemporary RED membranes are severely constrained to impractically
low efficiency due to the Donnan exclusion effect, which confers selec-
tivity to ion exchange membranes, being overwhelmed at high solution
concentrations. Due to these considerations, small salinity gradients are
suitable for the application of RED energy production. PRO is one of the
most promising applications for power generation and membranes are
the heart of this method. To improve this process, there are a variety
of nanoparticles that are somehow promising to be incorporated with
composite membranes. In addition, the recent results have shown that
they are more promising to use in the PRO process in comparison with
the control TFC membrane.

6. Conclusion

In this study, improving the performance of TFN membranes through

PRO process is mostly rely on the nanomaterials using in the substrate or
Fig. 7. Reverse solute flux in AL-FS and AL-DS mode for TFC and zeolite incor- active layer (polyamide layer). It has been observed that using nanoma-
porated TFN membranes. terials in TFN membranes has led into having higher water flux and con-
sequently to have a higher power density compared to the control TFC
membrane. Working under different testing conditions will result in hav-
agglomerated on the surface. Thus, 0.3 wt%, flux declined due to an ing various performance ranges which are between the 1.7 – 38.0 W/m2 .
uneven arrangement of zeolite in polyamide layer formation. In addition, achieving better performance through the PRO process re-
The incorporation of zeolite nanoparticles increased the FO water lies on the parameters such as different concentrations in the draw and
flux initially for a zeolite loading up to 0.3 wt%, and further increase feed solution and operation pressure. The application of zeolite incor-
zeolite loading resulted in water flux reduction. This trend matched well porated TFN for power generation through PRO is still a new field to be
with the one for the RO water permeability of the TFN membranes. In- explored. Despite of some promising findings obtained from this work,
deed, the membrane with the highest FO water flux (TFN 0.1) also had there is always room for improvement. Therefore, some suggestions are
the highest water permeability. The same trend was also observed for recommended as the future directions of this research. In order to fur-
the AL-FS orientation, where once again the membrane TFN 0.1 showed ther improve the membrane flux and power density of the PRO system,
the optimal water flux. With a 2 M NaCl DS and DI water NaCl FS, TFN the desired membrane should be of very thin selective layer and sub-
0.1 had FO water fluxes of 5.6 L/m2 h in AL-DS and 4.0 L/m2 h in AL-FS. strate layer. Triethylamine and diamine-based monomers act as catalyst
These values were nearly 50% higher than the respective values of the in PA layer formation under interfacial polymerization. Thereby, high
TFC membrane, suggesting that the incorporation of zeolite nanopar- power density can be achieved in PRO techniques. The thickness and
ticles can serve as an alternative approach to enhance FO water flux the structure of substrate also plays critical role in determining the flux
performance. and power density. Hence it is recommended to fabricate thin substrate
Nevertheless, a clear trend can still be observed that optimal increase to facilitate the transport of water. Another approach is to improve the
in zeolite loading increased the solute flux, with the highest solute flux porosity of the substrate through the addition of hydrophilic additive or
obtained for 0.1 Zeolite 3 Å incorporated TFN membrane. The results prepare the substrate using technique such as electrospinning.
indicated that optimized loading of zeolite is important to ensure the
good performance of the membranes as excessive zeolite (e.g., from 0.1
Declaration of Competing Interest
to 0.3 wt.% in this study) may significantly increase the solute flux with-
out the benefit of gaining additional water flux (Figs. 6 and 7).
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
5. Discussion
the work reported in this paper.
During the usage of flat sheet RO membrane, the big problem is not
enough membrane flux which will occur due to the concentration po- Acknowledgement
larization. This will come up with the other problem that is prone to
occur which is decreasing osmotic pressure [63–66]. To be clear, con- This work is supported by National Institute of Food and Agricul-
centration polarization has two kinds: External and internal. Every one ture (NIFA) [grant no. 2016-67032-24993/CRIS no. 1009030] from
of them will happen at the one side of the membrane [67–69]. Internal the United States Department of Agriculture (USDA). Special thanks to
Concentration Polarization (ICP) happens on the feed side, but External Dr. Mahmood Amani at Texas A&M University at Qatar and Dr. Anish
Concentration Polarization happens on the side which contains draw so- Jantrania at Texas A&M University at College Station, TX, USA.
lution. To decrease the influence of Internal Concentration Polarization
through PRO, draw solution should contact active layer. Although the References
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