Separation and Purification Technology 65 (2009) 282–289

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Separation and Purification Technology

journal homepage: www.elsevier.com/locate/seppur

Preparation, characterization and performance of nanofiltration membranes

for the treatment of electroplating industry effluent
Alka G. Boricha, Z.V.P. Murthy ∗
Department of Chemical Engineering, S.V. National Institute of Technology, Surat 395007, Gujarat, India

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

Article history: Two new nanofiltration (NF) membranes were prepared by coating (cast and spray) of strong chelating
Received 13 August 2008 agent diethylene triamine pentaacetic acid (DTPA), using polyether sulfone (PES) ultrafiltration (UF) mem-
Received in revised form 25 October 2008 brane as substrate and their performance were studied to treat actual electroplating industry wastewater.
Accepted 27 October 2008
The resulting membranes, observed to be nanofiltration membranes, were characterized with the help
of scanning electron microscopy (SEM) and swelling behavior. The structure of sprayed membranes was
Keywords:
observed to be more porous than that of cast membranes and hence, the sprayed membranes gave higher
Nanofiltration
permeation rate than that of cast membranes. Effects of pressure, feed flow rate, feed pH, and concen-
Cast coating
Spray coating
tration of DTPA on the rejection of zinc and iron were investigated. The rejection was higher for cast
Electroplating wastewater membrane when compared to spray membrane. The maximum observed rejection for cast and spray
Rejection membranes was found to be 94% and 89% for zinc and 93% and 88% for iron, respectively. The rejec-
tion of SS and TDS was over 99.4%. From the experimental results it was evident that as pressure, and
feed flow increased, the observed rejection of both the metal ions increased. Also, it was observed that
the feed pH had great effect on permeate flux but marginal influence on observed rejection for both
ions.
© 2008 Elsevier B.V. All rights reserved.

1. Introduction ume of retentate that needs to be handled, (3) selective removal of

One of the critical pollution problems arising from the elec-
troplating industry is the generation of a large amount of rinse
water for electroplated parts. The used rinse water consists of many
heavy metals and chemicals that can be detrimental to the health of
organic bodies when exposed in the environment. At the same time,
however, the rinse water has a great possibility for reuse if the heavy
metals are effectively removed. Due to the increasing environ-
mental awareness and tighter legislations, wastewater containing
heavy metals can no longer be discharged into rivers or sea in most
countries. Hence, the removal or recovery of heavy metals from
industrial wastewater such as that from electroplating industries
is highly desired. Conventionally, the processes and technologies
involved in the removal of heavy metals from industrial wastew-
ater are many; like precipitation, ion exchange, complexation,
adsorption, evaporation, membrane technology and electrochem-
ical processes. Among all membrane separation technology has
many advantages like (1) low energy requirements, (2) small vol-
∗ Corresponding author. Tel.: +91 261 2201641/2223371–2223374;
fax: +91 261 2227334/2201641.
E-mail addresses: zvpm2000@yahoo.com, zvpm@ched.svnit.ac.in
(Z.V.P. Murthy).
pollutants with complexing agents by membrane surface modifi-
cation, etc.
Nanofiltration (NF) has found applications in a wide range of
fields. With separation characteristics between ultrafiltration (UF)
and reverse osmosis (RO), NF is used when low molecular weight
(MW) solutes have to be separated from a solvent. Compared
to UF, NF membranes have a smaller pore size, so that smaller
organic molecules can be retained (MW > 200). Compared to RO
a lower retention is found for monovalent ions. NF is used for the
production of drinking water (water softening, removal of microp-
ollutants) as well as for the treatment of waste and process waters
[1].
Diethylene triamine pentaacetic acid (DTPA) is one of the
most well-known chelating agent and is an organic compound
consisting of a diethylenetriamine backbone modified with five car-
boxymethyl groups (deprotonated). DTPA is used as its conjugate
base, often undefined, which has a high affinity for metal cations.
Studies have established that the most common chelating agents
ethylene diamine tetraacetic acid (EDTA) and DTPA can effectively
remove various metal ions from wastewater [2–6]. Researchers
have also found that DTPA is capable of producing stable complexes
with various metal ions [7,8]. However, to our knowledge, there is
no literature available on composite membranes using DTPA coat-
ing as the active layer material.

1383-5866/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.seppur.2008.10.047
 A.G. Boricha, Z.V.P. Murthy / Separation and Purification Technology 65 (2009) 282–289 283

Table 1
Composition of the raw electroplating wastewater.

Particulars Concentration (mg/L)

Appearance Green-yellow liquid

pH 0.94
C.O.D. 42,940
B.O.D. 15,313
Chloride 6212
Sulphate 2250
S.S. 23,400
T.D.S. 52,000
Oil & grease 28
Iron (Fe) 618
Zinc (Zn) 584
Copper (Cu) 0.97
Chromium (Cr) 0.71
Nickel (Ni) 0.64
Lead (Pb) 0.46
Phenolic compound 2.7

The bold values indicates that we have considered these parameters during the UF
pretreatment (see Table 4).

Hence, an attempt was made to evaluate the performance of
newly prepared composite membrane with DTPA layer coating
as the active membrane layer. Resulting membranes (NF mem-
branes) were characterized with the help of scanning electron
microscopy (SEM) and swelling behavior, and used to treat elec-
troplating industry wastewater. Permeate fluxes and rejection, of
various constituents of wastewater, were measured with result-
ing composite NF membranes at different operating conditions, i.e.,
pressure, feed flow rate, DTPA concentration, and pH of the feed.
2. Materials and methods
2.1. Materials
The wastewater used in this work was from an actual elec-
troplating plant from nearby industrial area. Except for the NF
concentration experiments, the same batch of wastewater was used
in the experiments and the composition of this batch can be seen
in Table 1. It can be seen from Table 1 that the electroplating
wastewater has a higher Zn and Fe content than other heavy metals.
Therefore, the removal of Zn and Fe from electroplating wastewater
through NF membranes was investigated in this work. In the exper-
iments, flat sheet polyethersulfone (PES) UF membrane (30KD)
(M/S. Permionics, Vadodara, India) as a substrate membrane, DTPA
powder (MW = 393.35 g mol−1 , Finer Chemicals, India), hydrochlo-
ric acid (Merck, India) and sodium hydroxide (Thomas Baker, India)
were used. In all experiments and for washing purpose, ultra-pure
water (pH 5.9 ± 0.2 and conductivity 1.0 (␮S/cm)) was used (MilliQ,
Millipore, India). Microprocessor-based pH system (model 1012E,
Swastik, India) and TDS meter (model 1601E, Swastik, India) were
used to find pH and TDS of the solutions, respectively.
2.2. Preparation of coated membrane
The high flux PES UF membrane (see Table 2) was used as a sub-
strate membrane for coating of DTPA. Before cast or spray coating
Table 2
Characteristics of PA and PES UF membranes used in the experiments.
PA UF membrane PES UF membrane
Configuration Spiral wound Flat sheet
Membrane material Polyamide Polyethersulfone
pH 2–11 2–11
Thermal stability 90 ◦ C 90 ◦ C
Pure water flux (L/(m2 h)) at 25 ◦ C 145 35
Effective membrane area 1 m2 150 cm2
Fig. 1. The illustration picture of the setup for spray membrane preparation.
of the casting solution (DTPA) as the active layer, the PES UF mem-
brane was immersed in water overnight, rinsed with deionized
water thoroughly, and surface was dried with filter papers. Aqueous
DTPA solutions of 10 mM and 50 mM were prepared by dissolving a
certain amount of DTPA in 0.1 M NaOH solution and filtered with a
sandfilter [9]. After 24 h, the degassed DTPA solutions were ready to
coat onto the PES UF membrane. Coating on membrane was done
by two different methods. In the first method, two different con-
centration DTPA solutions (10 mM and 50 mM) were coated on PES
UF membrane with the help of doctor blade with approximately
equal thickness, followed by natural solvent evaporation, and then
cured in an oven at 50 ◦ C for 1 h. In the second method, spray coated
membrane was made by using an apparatus shown in Fig. 1. The
equipment included a feed tank, pump and spraying nozzle. DTPA
solution was pumped through a pump from a feed tank to spraying
nozzle. Spraying nozzle kept at 40–50◦ angles and located at 10 cm
above the membrane [10]. Spraying nozzle radius was 1 mm and
DTPA solution was sprayed out at a flow rate of 0.25 mL/min. The
solution of coating material was sprayed on the surface of substrate
membrane and this process was captured by a high-speed camera
(1000 FPS, X-PR1, AOS Technology, Switzerland), which shows that
a film formed on the surface after the solvent evaporation. Fig. 2(a)
and (b) shows the photographs at the time of spraying and after
spraying. From both Fig. 2(a) and (b), it can be clearly visualized that
DTPA was coated on membrane by using spray technique. Different
concentration DTPA solutions (10 mM and 50 mM) were sprayed on
the PES UF membranes by using same sprayed condition followed
by natural solvent evaporation and after that curing in an oven at
50 ◦ C for 1 h. The nomenclature of all the coated membranes was
given in Table 3. All the coated membranes were stored in polyethy-
lene sample bags till their characterization and subsequent use for
experimentation.
2.3. Characterization of coated composite membranes
2.3.1. SEM
The top surface and cross-sectional views of the substrate and
coated membranes, hereafter referred as NF membranes, were ana-
lyzed using scanning electron microscopy. The membranes were
cut into pieces of various sizes and mopped with filter paper. These
pieces were immersed in liquid nitrogen for 20–30 s and frozen. The
frozen bits of the membranes were broken and kept in a desiccator
till SEM studies.
284 A.G. Boricha, Z.V.P. Murthy / Separation and Purification Technology 65 (2009) 282–289

Fig. 2. Photographs (a) at the time of DTPA spray and (b) after DTPA spray.

2.3.2. Degree of swelling
The swelling properties of the membrane samples were studied
by immersing the dried DTPA coated membranes, cut into constant
small squares, in water and actual electroplating wastewater at dif-
ferent periods of time at room temperature. At predetermined time
intervals, the pieces of membranes were taken out from the water
and the actual electroplating wastewater, and gently wiped with
filter papers to remove the surface solution, weighed and returned
to the same container until equilibrium. The swelling ratios (SR) of
these samples were calculated by the following relation:
Ws − Wd
swelling ratio (%) = × 100
Wd
where, Wd is the weight of the dry membrane and Ws is the weight
of the membrane swollen in the solution.
2.4. Permeation experiments
Since the original wastewater contains many suspended solids
and very low pH, pretreatment of the wastewater was necessary
to prevent the membranes from fouling, plugging, and to reduce
concentration polarization which will cause flux decline, decreased
rejection or even membrane failure. The pretreatment adopted in
this study included filtration, precipitation, pH adjustment and
than UF. One micron pore size filter cloth was used to remove the
suspended solids from the wastewater, which removed almost all
the suspended solids. Then pH of the wastewater was brought to 2.5
by adding 0.1 M NaOH solution. During the pH increment process
to the real wastewater, the colloidal particles were aggregated and
settled down, which were filtered out and the light greenish super-
natant was used in the next step of pretreatment. This supernatant
solution was passed through the spiral wound PES UF membrane
module for removal of some of SS and TDS. All the characteristics of
permeate from the spiral wound polyamide (PA) UF membrane was
given in Table 4. The important parameters are measured according
to the standard methods [11]. The permeate solution from the UF
(1) experiments was used as the feed solution to the NF experiments.
The experiments were performed on a Perma® pilot scale mem-
brane system (Permionics, India) using rectangular DTPA cast (DC)
and DTPA sprayed (DS) composite NF membranes having effective
membrane area of 150 cm2 (length 15 cm and width 10 cm). The
experimental set-up was shown in Fig. 3. The membrane-housing
cell was made of stainless steel with two halves fastened together
with high tensile bolts. The top half of cell contained the flow dis-
tribution chamber and the bottom half was used as the membrane
support system. Experiments were performed with cast and spray
coated composite NF membranes. Before conducting the actual
experiments for the rejection of zinc and iron from electroplat-
ing wastewater, the composite NF membranes were subjected to
stabilization at 10 atm, which is the maximum pressure used in
the experiments, for 2 h to avoid possible membrane compaction

Table 3
Nomenclature of different coated membranes. Table 4
Results after PA UF membrane pretreatment.
DTPA concentration Coating method Membrane

10 mM Cast DC10 Particulars Raw electroplating wastewater After UF pretreatment

50 mM Cast DC50 pH 0.94 2.5
10 mM Spray DS10 Zinc (ppm) 584 500
50 mM Spray DS50 Iron (ppm) 618 526
D = DTPA, C = Cast, S = sprayed, and 10 and 50 = DTPA concentration of DTPA in coat- SS (ppm) 23,400 926
ing. TDS (ppm) 52,000 20,345
 A.G. Boricha, Z.V.P. Murthy / Separation and Purification Technology 65 (2009) 282–289
Fig. 3. Parma® pilot scale membrane system.
during the experimentation. Experiments were performed for 2 h,
for each set of rejection data in batch circular mode. The perme-
ate samples were collected from high pressure to low pressure for
a particular feed concentration and feed flow rate. Both permeate
and concentrates were returned to the feed vessel in order to keep
a constant concentration. Samples of permeate were collected in
mL at a given time interval, to measure the observed salt rejection
(Ro ) and permeate volume flux (JV ). Here, Ro = [1 − (CA3 /CA1 )], where
CA1 is the feed solute concentration and CA3 is the permeate solute
concentration. The experiments were carried out for different feed
flow rates (4 L/min, 8 L/min, 12 L/min and 16 L/min), applied pres-
sures (2 atm, 4 atm, 6 atm, 8 atm and 10 atm) and feed pH (2, 4, 6 and
8) corresponding Ro and Jv were measured. The zinc and iron metal
concentrations are measured by UV–vis Spectrophotometer (SL-
159, M/S. ELICO Limited, India) following standard methods [11].
After each set of experiments for a given experimentation condi-
tion, the set-up was rinsed with distilled water for 30 min at 2 atm
to clean the system. This procedure was followed by measurement
of pure water permeability (PWP) with distilled water to ensure
that the initial membrane PWP is restored.
3. Results and discussion
3.1. Membrane characterization
3.1.1. SEM
Fig. 4(a)–(j) shows the SEM images of surface and cross-sectional
view of substrate membrane and composite NF membrane. Fig. 4(a)
and (b) shows the top surface and cross-sectional view of PES UF
membrane, which show that the PES UF membrane had a smooth
surface and had a finger-like pore structure. Fig. 4(c)–(j) represents
the surface and cross-sectional views of DC and DS membranes
prepared via solution cast and spray methods. Compared to sub-
strate membrane, it can be clearly seen from Fig. 4(c)–(j) that coated
membrane had a dense selective layer on the top surface of mem-
brane. The top surface of the DS membranes was rougher than
that of DC membranes. Coating layer was denser in DC membranes
when compared with DS membranes and this may be due to the fact
that the DC membranes has equal thickness coating via casing but
285
in DS membranes case it was not so, may be because of non-uniform
spray coating on the whole surface of the membranes. Fig. 4(g)–(j)
shows the cross-sectional views of the DC and DS membranes from
which, it was clearly seen that a selective layer of DTPA was formed
on all the membranes. Fig. 4(g)–(j) indicates that DS membranes
are more porous than DC membranes. The reasons for more porous
structure in DS membranes may be that during spray coating pro-
cess some bubbles collapse and left a loosely packed structure and
the others remain as empty holes on the membranes. On the other
hand, the DC membranes tend to trap fewer amounts of air bubbles
when it was coated on the membrane surface.
3.1.2. Degree of swelling
Sorption experiments were carried out with water and actual
electroplating wastewater at room temperature by using all the
four coated composite NF membranes. Fig. 5 shows the plot of
percentage swelling of the membrane and temperature. Initially,
for all the membranes, the rate of water uptake sharply increased
and then begins to level off. The equilibrium swellings for all the
membranes were achieved after 60 min. In this study, the DS mem-
branes showed maximum swelling ratios of 107 and 95; and DC
membranes showed 72 and 63 for water. For actual electroplating
wastewater DS membranes showed the maximum swelling ratio of
69 and 62 and for DC membrane 60 and 56. These results support
the observations made from the SEM figures and rejection data for
various solutes, as explained later.
3.2. PWP
Before the solute rejection experiments, the PWP of all the
membrane using distilled water was measured at 25 ± 1 ◦ C. A plot
of PWP versus applied pressure (figures not shown) will give a
slope LP , known as the PWP coefficient of the membrane. The
LP values for all the composite NF membranes used were given
in Table 5, which were in the range of nanofiltration membranes
[12–14], hence the new membranes were called NF membranes.
The LP was considered to be a reference to evaluate cleaning pro-
cedure, concentration polarization and fouling of the membrane.
These values indicate that the permeate fluxes were in the order of
286 A.G. Boricha, Z.V.P. Murthy / Separation and Purification Technology 65 (2009) 282–289

Fig. 4. SEM image of (a) top surface of PES UF membrane, (b) cross-sectional view of PES UF membrane, (c) top surface of DC10, (d) top surface of DC50, (e) top surface of
DS10, (f) top surface of DS50, (g) cross-sectional view of DC10, (h) cross-sectional view of DC50, (i) cross-sectional view of DS10 and (j) cross-sectional view of DC50.
 A.G. Boricha, Z.V.P. Murthy / Separation and Purification Technology 65 (2009) 282–289
Fig. 5. Swelling behavior of prepared composite NF membrane.
Table 5
LP values for all composite NF membranes.
2 tive transport becomes important and retention will, therefore, also
Membrane LP value, (L/(m h atm))
DS10 12.97
DS50 12.32
DC10 10.85
DC50 10.11
DS10 > DS50 > DC10 > DC50, which suggest that the DS membranes
were more porous than DC membranes. These results support
the SEM observations that higher porosity and rough surface give
higher flux [15].
3.3. Effect of applied pressure
Experiments were carried out to study the effect of applied
pressure, ranging between 2 atm and 10 atm, at pH 2.5. The effect
of applied pressure on zinc and iron rejection from electroplat-
ing wastewater was reported in Fig. 6. It shows that the rejection
increases with increase in applied pressure for all the membranes,
because ion transport due to convection becomes significant com-
pared to diffusion. A high diffusive transport of salts through the
membrane compared to convective transport may be the reason
Fig. 6. Influence of applied pressure on percentage rejection of zinc and iron at
16 LPM feed flow rate by using different NF membranes.
287
Fig. 7. Effect of applied pressure on permeate volume flux at 16 LPM feed flow rate
by using different NF membranes.
for low retention at low pressure. With increasing pressure, convec-
increases [13,16]. Fig. 6 indicates that for both the ions, the rejection
efficiency was in the order of DC50 > DC10 > DS50 > DS10. This trend
may be due to the fact that in DC membrane the coating layer is
denser compared to the DS membrane. When DTPA comes in con-
tact with metal ions present in wastewater they form larger size
chelate with metal ions and the molecular weight of this chelates
exceed the molecular weight cut-off of the membrane, hence the
rejection of metal ions increases [17]. As DTPA concentration was
increased from 10 mM to 50 mM in coating of membrane, rejection
of Zn and Fe by nanofiltration increased (see Fig. 6). This may be
due to the formation of more larger-sized Zn–DTPA and Fe–DTPA
chelates [24]. Fig. 6 also indicates that for all the membranes Zn
rejection was more compared to Fe rejection. This may be due to
the fact that the size of Zn2+ is larger than that of Fe2+ .
Fig. 7 shows the effect of applied pressure on the per-
meate volume flux. Permeate volume flux is in the order of
DS10 > DS50 > DC10 > DC50 [18]. This is in line with the observa-
tions made in Section 3.1.2. As the DTPA concentration increased,
the permeate flux decreases due to the increase of concentration
difference across the membrane and subsequent increase in the
osmotic pressure which opposes permeate flux. This is also possible
that if DTPA concentration increased on the surface of membrane
then the membrane pores may also be blocked up to certain extent
in both the cases (DS and DS membrane) and because of that the
permeate volume flux decreased. Another reason may be that more
chelating groups on the membrane result in increased concentra-
tion polarization which results in less permeate flux. At 10 atm
applied pressure the highest rejection observed was 94% and 93%
for zinc and iron for DC50, respectively, which were in line with the
published literature [19]. NF had effectively separated the SS from
961 mg/L to 125 mg/L and TDS concentration from 20,345 mg/L to
304 mg/L at 10 atm pressure and 16 L/min (LPM) feed flow rate for
DC50.
3.4. Influence of feed flow rate
Fig. 8 shows the rejection percentages of zinc and iron salts at
different feed flow rates (4–16 LPM) at 10 atm applied pressure. It
can be seen from Fig. 8 that the increase in feed flow rate leads to
an increase in the retention. Similar results were found in literature
for the zinc ions [18]. At constant applied pressure and concentra-
tion, the mass transfer coefficient increases with increase in feed
flow rates which in turn reduces the concentration polarization and
288 A.G. Boricha, Z.V.P. Murthy / Separation and Purification Technology 65 (2009) 282–289
Fig. 8. Effect of feed flow rate on percentage rejection of zinc and iron at 10 atm
pressure by using different NF membranes.
increase the rejection [20]. For all the membranes it can be seen
that as feed flow rate increases then rejection of zinc and iron also
increases.
3.5. Influence of feed pH
Fig. 9(a) and (b) shows the influence of pH on percentage rejec-
tion and permeate flux. The wastewater pH was adjusted by the
addition of NaOH and/or HCl, depending on the requirement. At
constant applied pressure of 10 atm and 16 LPM, Fig. 9(a) shows that
pH had significant effect on permeate flux, but in case of percent-
age rejection of Zn and Fe, pH shows marginal difference, as shown
in Fig. 9(b). Such type of behavior has been observed in the litera-
ture with NF [21,22]. Fig. 9(a) and (b) shows that as pH of the feed
solution was increased the permeate volume flux was decreased.
Fig. 9. Influence of feed solution pH on (a) permeate volume flux for DS10 and (b)
percentage rejection for DC50.
This may be due to the fact that at higher pH the active skin layer of
the membrane might have hydrolyzed to some extent, due to the
difference of hydration of ionized groups present in the membrane
[23].
4. Conclusions
In the present work an attempt had been made to prepare new
composite membranes by casing (normal coating and spray coat-
ing) with diethylene triamine pentaacetic acid (DTPA) on PES UF
substrate membrane, which showed NF membrane properties. The
newly prepared membranes were characterized by SEM and their
swelling behavior. Then the membranes were used to test their
performance in treating actual plating industry wastewater. It was
observed that these NF membranes were capable of separating
heavy metal ions more than 93% and nearly 100% separation in
case of suspended solids and total dissolved solids. For both types
of coatings, it was observed that the rejection of both the solutes
increased with increase in applied pressure and feed flow rate. pH
had a great influence on permeate flux compared to percentage
rejection.
Acknowledgement
The second author (ZVPM) acknowledges the financial support
from the Ministry of Human Resources Development, New Delhi,
under the TAPTEC Research Grant.
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