Ecotoxicology and Environmental Safety ()

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Ecotoxicology and Environmental Safety

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

Effective removal of humic acid using xanthan gum incorporated

polyethersulfone membranes
R. Sathish Kumar a, G. Arthanareeswaran a,n, Diby Paul b, Ji Hyang Kweon b
a
b

Membrane Research Laboratory, Department of Chemical Engineering, National Institute of Technology, Tiruchirappalli 620015, India
Department of Environmental Engineering, Konkuk University, Seoul 143-701, South Korea

art ic l e i nf o

a b s t r a c t

Article history:
Received 9 January 2015
Received in revised form
19 March 2015
Accepted 21 March 2015

In this study, xanthan gum (XA) was used as a hydrophilic biopolymer additive for the modication of
polyethersulfone (PES) membrane to removal of humic acid (HA). The membranes are prepared using
phase inversion technique and the concentration of XA was varied from 0.5 to 1.5 wt%. The prepared
membranes are characterized as a function of hydrophilicity, equilibrium water content (EWC), porosity
studies and functional group analysis. Membrane surface and cross-sectional morphology was studied
using scanning electron microscope. The lower contact angle value 64.2 was exhibited, when 1.5 wt% of
XA incorporated in PES membrane and this ensures that increase of hydrophilicity in pristine PES
membrane. Further, higher water permeability (PWP) of 68.9
9 m/s kPa was observed for 1.5 wt% of XA/
PES membrane. The effect of pH on HA removal was studied for neat PES and XA/PES membranes. The
rejection performance of XA incorporated in PES membranes were compared with commercial available
PES membrane.
& 2015 Elsevier Inc. All rights reserved.

Keywords:
Xanthan gum
Hydrophilicity
Flux recovery ratio
Removal of humic acid

1. Introduction
Surface water is being intensively polluted by various industrial
activities, modern agricultural practices, and a natural accumulation of dead leaves, sh and bird faeces, and anthropogenic activities. Moreover, dead leaves degradation and in situ anaerobic
digestion of algal or microbial biomass generate humic substances
in the surface water streams. Humic acid (HA) is an organic matter.
Presence of HA in surface water, can cause the following adverse
effects. There are, (a) Impart unpleasant the odour, (b) Changes the
colour, (c) Absorbs the metals and (d) Increase the microbial population (Kilduff et al., 1996; Chen et al., 2003; Thurman, 1985).
Hence, HA has to be properly treated to provide the portable water
to the Public. It is difcult to treat by the conventional water
treatment methods. Because, during the conventional water
treatment process like coagulation and clarication, it may react
with coagulants, forms by-products and hinders the treatment
process. Moreover, during the disinfection process, phenolic hydroxyl groups of HA reacts with chlorine and forms trihalomethanes (THMs) as disinfection by-product (Krasner et al., 2006;
Zularisam et al., 2006).
Membrane treatment are widely recognized alternative water
treatment process to conventional treatment methods for removal
n

Corresponding author. Tel.: 91 431 2503118; fax: 91 431 2500133.

E-mail address: arthanaree10@yahoo.com (G. Arthanareeswaran).

the pollutants and meet the stringent environmental regulations

(Katsoudou et al., 2005; Susanto and Ulbricht, 2008; Shao et al.,
2011; You et al., 2013). The selection of suitable membrane materials for removal the pollutants with desired properties is important task. Polyethersulfone (PES) is widely used membrane
materials because it has good mechanical strength, high thermal
stability, better chemical resistance and lm-forming property.
However, the major bottleneck of usage of PES is hydrophobic
property. Hydrophobic surfaces are more prone to fouling (Wang
et al., 2011; Wang et al., 2006; Rahimpour et al., 2010; Rahimpour,
et al., 2012). Fouling hinders productivity, affects permeation of
ions, transport of pollutants and also the lifetime of the membrane. Hydrophobic polymeric membranes have been modied by
using additives to enhance permeability and increase their hydrophilicity to prevent the fouling. The work reported the inuence of hydrophilic polymeric additives such as Polyethylene glycol (PEG) (Xu et al., 1999b), Polyvinylpyrrolidone (PVP) (Xu et al.,
1999a; Marchese et al., 2003) and poly sulfoxide amide (Rahimpour et al., 2009) that increase the hydrophilic property of the
modied membrane. Hydrophilic biopolymers are also a potential
material for modication of hydrophobic polymers. There had also
been reports on novel membranes synthesised by blending cellulose acetate (CA) with hydrophilic biopolymer carboxymethyl
cellulose acetate (CMC) which shows enhanced hydrophilic characteristics and higher pure water ux (PWF) (Han et al., 2013).
Lakra et al. (2013) reported Chitosan blend membranes such as
PES and PES/CA with improved ux and without compromising

http://dx.doi.org/10.1016/j.ecoenv.2015.03.036
0147-6513/& 2015 Elsevier Inc. All rights reserved.

Please cite this article as: Sathish Kumar, R., et al., Effective removal of humic acid using xanthan gum incorporated polyethersulfone
membranes. Ecotoxicol. Environ. Saf. (2015), http://dx.doi.org/10.1016/j.ecoenv.2015.03.036i

R. Sathish Kumar et al. / Ecotoxicology and Environmental Safety ()

the rejection efciency.

The increase in HA rejection rates was observed when 1.25 wt%
ZnO added in PES membrane (Ahmad et al., 2014). Further, HA ux
was also enhanced by incorporation ZnO in PES polymer matrix.
The accumulation of humic elements on hydrophobic PES surfaces
favoured and reduce the ux due to the prevalent hydrophobic
property of these compounds (Peeva et al., 2011). In our previous
work (Lukka et al., 2014), removal of HA was studied using zirconia
(ZrO2) embedded PES membranes. Hydrophilicity enhancement
was reported due to addition of zirconia nanopartciels in PES
membranes. The modication of PES membranes with hydrophilic
biopolymer for removal humic acid is limited.
Xanthan gum (XA) is hydrophilic biopolymer and is produced
by aerobic fermentation of sugar by a gram-negative bacterium
Xanthomonas campestris (Fink, 2013; Altay and Gunasekaran, 2013;
Jaipal et al., 2013). It has received a great deal of attention as
stabilizing agent in food industries and slow drug release applications in pharmaceutical industries due to its non-toxic, biocompatible property, biodegradable property, excellent mechanical property, better thermal stability and pseudoplastic rheological property (Psomas et al., 2007; Jiangyang et al., 2008; Bhattacharya et al., 2013). In the present study, interaction between XA
and PES is studied by various membrane characterization techniques like FTIR, contact angle and scanning electron microscope
(SEM). The pure water ux and removal of humic acid are extensively studied using low-pressure cross ow UF module. In
addition, separation performance of as prepared membranes at
different feed pH are carefully investigated and compared with
commercially available PES membrane.

2. Materials and methods

Table 1
Compositions of PES and PES/XA membranes
Membrane type

M-I
M-II
M-III
M-IV

Composition of dope solution in solvent DMAc (82.5 wt%)

PES (wt%)

XA (wt%)

100
99.5
98.5
97.5

0.5
1.0
1.5

Scientic Nicolet i5S FTIR analyser (Thermo Nicolet Corporation,

USA). To further understand the relationship between surface
morphology and biopolymer loading, cross section and top surface
layer images are taken using SEM (TESCAN VEGA 3 SEM, USA). The
hydrophilicity of the neat and modied PES membranes, contact
analysis is performed by the sessile drop method using goniometer (Model 250-F1 Rame Hart Instruments, Succasunna, NJ).
2.4. Equilibrium water content (EWC) and porosity studies
EWC is an indirect method to analysis the hydrophilicity or
hydrophobicity of the membrane. The membrane samples are
soaked in DD water for 24 h at room temperature. Weight of the
soaked membrane is measured (W1) using an electronic weighing
balance immediately after mopping with tissue paper. These wet
samples are placed in a vacuum oven for 24 h at 60 C and then
dry weights of membranes (W2) are determined. The percentage
water content was calculated as follows. (Chakrabarty et al., 2008)
and values are tabulated in Table 2.

EWC(%) =

w1w2
100
w1

(1)

2.1. Materials
Polyethersulfone (PES) (Veradale 3000p) is procured from
Solvay Chemicals India Ltd, Mumbai, India. Dimethyl acetamide
(DMAc) is obtained from Alfa Aesar, U.S.A. Sodium Lauryl Sulphate
(SLS) is purchased from Avantor Performance Materials, U.S.A.
Xanthum gum and humic acid are supplied by Loba Chemie Pvt.
Ltd., Mumbai, India. The commercial PES membrane at 30 kDa was
purchase from Orelis Environnement SAS, France. All reagents
were analytical reagent grade without further purication. Double
distilled (DD) water is used throughout the study.
2.2. Preparation of biopolymer blend PES membranes
Base polymer as PES and solvent as DMAc were chosen for the
preparation of membrane using phase inversion method. Base
polymer PES was dried in hot air oven at a temperature of 80 C
before use. Initially casting dope solution was prepared by dissolving PES in a solvent DMAc using magnetic stirrer at a temperature of 60 C. And then homogeneous mixture is cast on glass
plates using casting knife with a thickness of 250 m. Then, cast
membranes are allowed to evaporate in air for 30 s and then glass
plates was immersed in a non-solvent water bath containing
2 wt% SLS at 10 C for 3 h. The resultant membrane was stored in
container containing water for 24 h. In order to improve the
membrane performance, XA was used as an additive. Similarly, the
above procedure was followed for preparation of XA incorporated
membranes and its composition are provided in Table 1.
2.3. Membrane characterizations
Chemical structure of neat and modied PES membranes are
studied at 4 cm
1 resolution using ATR mode of Thermo Fisher

Porosity of membranes are calculated by the formula (Raguime

et al., 2007) given below and depicted in Table 2.

Porosity% =

w1 w2
100
w xVT

(2)

Where

VT =

w1 w2
w2
+
w
Mo

(3)

where VT is the membrane volume (m3) in the wet state and w is

the density of water (1 g/cm3), Mo is the density of the membrane
in the dry state.
2.5. Pure water permeability
Commercial PES membrane and PES/XA membranes were precompressed with DD water at 200 KPa for 1 h. After that, water
ux measurements are conducted at 200 KPa pressure by using
cross ow module (Model: PLEIADE Rayows, Orelis Environnement SAS, France). Pure water ux (PWF) of the membranes was
calculated using the following expression:

Jw =

Q
TA

(4)

2

1

where Jw is the pure water ux (L m h ); Q is the amount of

permeate collected (L); T is the sampling PO time (h); and A is the
membrane area (m2).
Pure water permeability (PWP) is the slope plotted between
pure water ux and transmembrane pressure (P).

PWP=

Jw
P

(5)

Please cite this article as: Sathish Kumar, R., et al., Effective removal of humic acid using xanthan gum incorporated polyethersulfone
membranes. Ecotoxicol. Environ. Saf. (2015), http://dx.doi.org/10.1016/j.ecoenv.2015.03.036i

R. Sathish Kumar et al. / Ecotoxicology and Environmental Safety ()

Table 2
Membrane characteristics
Membrane type

Contact angle ()

Purewater permeabilityx10
9 m/s KPa

Equilibrium water content (EWC) (%)

Porosity (%)

M-I
M-II
M-III
M-IV

72.1 71.4
68.3 72.1
66.8 71.7
64.2 71.2

4.83
25.0
62.5
68.9

48.40
56.44
58.18
61.46

42.1
55.8
57.9
60.8

spectra of modied membranes shown that extra vibrational frequencies at 2945 cm
1 owing to existence of CH bond.

2.6. Rejection studies

Rejection performance of PES/XA membranes was studied by
using HA solution (10 mg L
1). pH of HA feed solution was altered
by adding 1 M HCl or 1 M NaOH, and rejection experiments were
conducted at different pH. The removal HA solution was studied
through cross ow UF module using PES/XA membranes at 2 KPa.
The concentration of HA in the feed and permeate was analysed
by UV spectrophotometer (Hitachi-2000) at 254 nm and rejection
of HA was calculated as follows:

Cp
Rejection% = 1
Cf

100

(6)

where Cf is the initial concentration of feed and Cp is the permeate

concentration.
Further, performance of PES/XA membranes were compared
with commercial PES membrane.

3.2. Surface morphology studies

The SEM images of the surface and the cross-section of the neat
PES membrane and the modied membranes are shown in Fig. 2.
SEM results revealed that neat PES membrane had asymmetric
structures, consisting of top dense layers and nger-like structures
with the macro voids in the bottom layer (Rahimpour and Madaeni, 2007). Fig. 2 demonstrated signicant changes in sub-layer
morphology owing to the addition of XA. When XA concentration
increased from leads to typical changes in asymmetric structure to
microcellular structure could be observed in the cross section
morphology of the membrane and surface morphology shows
more pores on surface of the membrane owing to hydrophilic
nature of XA. The similar results were obtained for PES membrane
with PEG as polymeric additive (Arthanareeswaran et al., 2010).

3. Results and discussion

3.3. Equilibrium water content (EWC) and porosity studies

3.1. FTIR analysis

The relationship between water content, porosity of the

membranes and the humic compounds plays an important role.
EWC of the membrane relates hydrophilicity of the membrane
(Chakrabarty et al., 2008). The water content of neat PES and PES/
XA membranes are shown in Table 2. As it is described in Table 1,
the water content of neat membranes (M1) is lower than that of
the membrane prepared in the presence of XA as hydrophilic additive. EWC values increased from 56.44 to 61.46 for PES/XA
membranes. Increasing the concentration of XA in dope solution
increases the EWC of membrane signicantly. It is also supported
by the contact angle results and permeability studies of the
membranes.
The porosity of the membranes listed in Table 2. The porosity
results show that in the increasing trend. Concentration of XA
increased in dope solution increases the porosity from 40.1% to
60.8%. The rapid increase in porosity could also be attributed to
hydrophilic moieties of the XA. The fractions of humic compounds
caused severe fouling during UF process with lower porosity of
neat PES membrane, while humic compounds not serve any
fouling in higher porosity of PES/XA membranes (Yu et al., 2008).
When compare the porosity results of the neat PES membranes,
the small molecules retained on the membrane. However, in case
of PES/XA membranes the small molecules penetrated into the
membrane inner surface, which could transport thorough internal
pores and also to the formation of more large and less fouling layer

The chemical stability of as prepared membranes and the

chemical constitutions on the surface of the prepared membranes
are investigated by attenuated total reection Fourier transform
infrared spectroscopy (ATR-FITR), and the resulted spectra were
shown in Fig. 1. Spectra of XA/PES membranes show the presence
of an extra vibrational band at 15501650 cm
1 and which
corresponds to the carboxylic functional group (Fig. 1). It is observed that the coordination interaction of OH
group of the
biopolymer with H group of PES that is conrmed by increasing
the stretching frequency at 31003450 cm
1. Compared with neat
PES membranes (M1), there may be spectral difference in the
range of 16501750 cm
1 that represents C O and it becomes
more intense due to the addition of hydrophilic biopolymers. FTIR

3.4. Hydrophilicity and permeability of the membranes

Fig. 1. FTIR spectra of membranes.

Contact angle and PWP values are depicted in Table 2. The

results revealed that the hydrophilicity of the membranes enhanced signicantly by the addition of biopolymers such as XA
due to the higher afnity of XA with water molecules. It can be
observed that the neat PES membrane has high contact angle of
72.1 71.4 owing to its hydrophobic nature. The deposition of
humic substances on hydrophobic surfaces caused more fouling,

Please cite this article as: Sathish Kumar, R., et al., Effective removal of humic acid using xanthan gum incorporated polyethersulfone
membranes. Ecotoxicol. Environ. Saf. (2015), http://dx.doi.org/10.1016/j.ecoenv.2015.03.036i

R. Sathish Kumar et al. / Ecotoxicology and Environmental Safety ()

Fig. 2. SEM images (a) Surface morphology of Membrane (M1), (b) Surface morphology of Membrane (M3), (c) SEM Surface morphology of Membrane (M4) (d) cross section
of Membrane (M1) (e) cross section of Membrane (M3) (f) cross section of Membrane (M4).

Please cite this article as: Sathish Kumar, R., et al., Effective removal of humic acid using xanthan gum incorporated polyethersulfone
membranes. Ecotoxicol. Environ. Saf. (2015), http://dx.doi.org/10.1016/j.ecoenv.2015.03.036i

R. Sathish Kumar et al. / Ecotoxicology and Environmental Safety ()

Fig. 3. Pure water permeability of the membrane.

Fig. 4. Rejection performance of the prepared membrane.

this may due to the prevalent hydrophobicity of these compounds

(Korbutowicz, 2008). Moreover a hydrophilic surface yielded less
fouling behaviour during ultraltration of humic acid solution. As
shown in Table 2, the contact angle of neat membrane gradually
decreased with increasing the content of XA, the contact angles of
modied PES membranes reach a lowest value of 64.2 71.2 at
2.5% of XA. It is interesting to note that the hydrophilicity is enhanced for PES/XA blend membranes.
The effect of an introduction of biopolymers in the dope solution on the hydrophilicity of modied membranes are also investigated by measuring pure water permeability (PWP). It is demonstrated that an increasing of PWP with increasing concentration of XA. From the Fig. 3, PWP of modied PES/ XA
membranes increased from 25.0 to 68.9  10
9 m/s kPa. Lower
contact angle (Table 2), formation of the large macro void (Fig. 2f)
are contributed to enhanced pure water permeability of the PES/
XA modied membrane. These results are evident that XA is a
good hydrophilic modier, and it may be alternative for reported
polymeric additives. Lakra et al. had also reported the surface
hydrophilicity of novel PES membrane blended with biopolymers
and the result is similar to our experimental results.
3.5. Rejection performance of the membrane
If humic acid persists in surface water, it may change the colour,
and may cause a bitter taste or odour. Moreover, HA may absorb
the metals present in the water that may increase the concentration of metals in water. It will lead to water pollution (Kamunde
and MacPhail, 2011). Hence, HA has to be removed to provide safe
water to environment.
In this study, UF membranes are synthesized for a low pressure
ultraltration process for HA removal. In addition, the ltration

performance of PES/XA membranes, pristine PES and commercial

PES membrane is extensively studied using HA as feed solution
and the inuence of the pH on HA removal is also investigated. HA
Rejection % of membranes is calculated using the Eq. 4 and shown
in Fig. 4. Rejection % HA for modied membranes varied from 80 to
88, 84 to 89, 86 to 94, 88 to 97 for pH 3, 5, 7 and 9 respectively.
These results have shown that effect pH on the rejection is increases with an increase in pH for both modied and unmodied
PES membranes. This demonstrates that rejection characteristics
of HA may depend on the hydrophilic nature of the membrane.
The HA rejection % is order of PES 30 kDa 4 M4 4 M3 4M24M1.
This can be attributed to the fact that the humic acid aggregates
are larger on commercial PES membrane (PES 30 kDa)and may
retain humic acid molecules on the membrane surface with relatively high rejection. For all the pH, the modied PES membranes
(M4) displayed is higher than neat PES, which is also shown in
Fig. 4. Rejection of humic acid in neat PES membrane was low
since the large size fraction of humic acids had been removed. The
effect of an addition of biopolymer in the casting solution, rejection of humic acid was increased and higher rejection was obtained for all XA incorporated PES membranes due their higher
hydrophilicity. Furthermore, higher rejection may be partly attributed to more porosity on the membrane but it is mainly due to
less resistance, lose structure and transport of species that could
be permit by the membrane. Moreover, these results supported
that low-pressure ultraltration system is affordable method for
HA removal. Ultraltration system may be the better option for
conventional treatment system to obey stringent environmental
regulations and provide safe water to public.

4. Conclusion
The inuence of XA in PES is extensively studied. Contact angle
measurement and PWP studies shown that hydrophilicity of
modied PES membranes is enhanced signicantly owing to an
incorporation of hydrophilic groups of biopolymers. FTIR revealed
the presence of OH group, COO
group in the XA incorporated
membranes that are due to the successful modication of XA on
the PES membrane. This study also conrmed that the presence of
XA on modied membranes. The SEM, and performance of modied membranes prepared with different concentrations of XA in
the casting solution showed that the increasing concentration of
XA differs the morphology, enhance the permeability of the
membranes. The ltration experiments conrmed that the modied PES membranes exhibit similar characteristics like commercial PES 30 kDa membrane. The above results indicate that XA
addition have enhanced PES membrane performance thus results
in effective and better removal of HA.

Acknowledgement
The authors are extremely thankful to Department of Science
and Technology, Government of India, for providing nancial assistance by sanctioning Indo- Korea project (DST Reference no:
INT/Korea/P-20/2013).

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membranes. Ecotoxicol. Environ. Saf. (2015), http://dx.doi.org/10.1016/j.ecoenv.2015.03.036i

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Please cite this article as: Sathish Kumar, R., et al., Effective removal of humic acid using xanthan gum incorporated polyethersulfone
membranes. Ecotoxicol. Environ. Saf. (2015), http://dx.doi.org/10.1016/j.ecoenv.2015.03.036i