Bioresource Technology 159 (2014) 460–464

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Bioresource Technology
journal homepage: www.elsevier.com/locate/biortech

Short Communication

Activated biochar derived from cactus fibres – Preparation,

characterization and application on Cu(II) removal from
aqueous solutions
Loukia Hadjittofi, Melpomeni Prodromou, Ioannis Pashalidis ⇑
Department of Chemistry, University of Cyprus, P.O. Box 20537, Cy-1678 Nicosia, Cyprus

h i g h l i g h t s

 Lamellar structures constitute the activated biochar cactus fibres.

 Activated biochar presents extraordinary adsorption capacity for Cu(II) ions.
 pH-depended formation of inner- or outer-sphere Cu(II) surface complexes.
 Formation of inner-sphere Cu(II)-carboxylate surface complexes at near neutral pH.

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

Article history: The adsorption efficiency of activated biochar prepared from cactus fibres regarding the removal of Cu(II)
Received 16 January 2014 from aqueous solutions has been investigated as a function of various physicochemical parameters (e.g.
Received in revised form 11 March 2014 pH, initial metal concentration, ionic strength, temperature and contact time). Activation of the biochar
Accepted 16 March 2014
took place using nitric acid oxidation and characterisation was performed by SEM analysis, FTIR spectros-
Available online 25 March 2014
copy, N2 adsorption and acid–base titrations. The results show that laminar structures constitute the
material and carboxylic moieties are the predominant binding sites. The experimental data were ana-
Keywords:
lyzed by the Langmuir, Freundlich and Dubinin–Radushkevich adsorption models and the monolayer
Biomass by-product
Activated carbon
adsorption capacity was found to be 3.5 mol kg1. The effect of ionic strength and temperature on the
Metal ions adsorption efficiency indicates that at low pH outer-sphere and at near neutral pH inner-sphere
Adsorption complexes are the predominant surface species and the kinetic data obtained were fitted very well by
Waters the Lagergren rate expression.
Ó 2014 Elsevier Ltd. All rights reserved.

1. Introduction range of different materials, including low-cost and highly avail-

Wastewaters produced by industrial activities have usual com-
plex compositions and contain increased amounts of toxic metal
ions. Toxic metal ions in wastewaters are of major environmental
concern and contaminated waters, which may cause environmen-
tal and health problems, need to be treated prior to their disposal
into environment. Removal of toxic metal ions from large volumes
of wastewaters require a cost effective remediation technology.
Conventional technologies relying on mineral adsorbents or chem-
ical flocculating agents are relatively expensive. Adsorption and
ion exchange are among the most studied wastewater treatment
technologies, which have been effectively applied using a wide
⇑ Corresponding author. Tel.: +357 22 892785.
E-mail address: pspasch@ucy.ac.cy (I. Pashalidis).
able biomass by-products (Hernandez-Ramirez and Holmes, 2008).
Activated carbons and biochars are very good adsorbents for the
removal of heavy metal ions and the treatment-purification of
waters, because of their large surface area and the high affinity
of their surface active groups for polyvalent metal ions and other
pollutants (Sulaymon et al., 2012). Therefore, activated carbons
are used in a number of possible technological and analytical appli-
cations. Removal of heavy metal cations from water is influenced
by various factors, such as solution concentration and pH, contact
time, carbon dosage, and sorbent surface modification procedure.
Although the mechanism of metal ion adsorption has been exten-
sively studied is not yet adequately understood (Ioannidou and
Zabaniotou, 2007) and hence investigations on the interaction of
metal ions with the carbon surface active groups are of particular
interest and fundamental for the development of wastewater
treatment technologies based on sorption/desorption processes.

http://dx.doi.org/10.1016/j.biortech.2014.03.073
0960-8524/Ó 2014 Elsevier Ltd. All rights reserved.
 L. Hadjittofi et al. / Bioresource Technology 159 (2014) 460–464
On the other hand, relatively high production costs make the
use of activated carbon impractical for the treatment of large quan-
tities of wastewater by domestic use and industry. Hence, finding
cheap alternative sources and enhancing the efficiency of the exist-
ing materials could make activated carbon attractive agents for a
large-scale treatment of wastewaters (Hernandez-Ramirez and
Holmes, 2008). Biomass by-products could be viable sources be-
cause they are abundant in nature or are produced in large quan-
tities as by-products or wastes from agricultural or industrial
activities (Hossain et al., 2012). Although most organic materials
are suitable for conversion into activated carbon, lignocellulosic
materials with high hardness and density are far better precursors
(Hernandez-Ramirez and Holmes, 2008; Issabayeva et al., 2010).
On the other hand, the efficiency of the materials can be enhanced
by oxidizing the surface of the carbon in order to increase the num-
ber of surface active sites, mainly given by oxygenated active
groups such as carboxylic and phenolic moieties (Dias et al.,
2007; Ioannidou and Zabaniotou, 2007).
The present study deals with the adsorption of bivalent copper
(Cu(II)) by activated carbon/biochar prepared from a biomass by-
product (Opuntia ficus indica cactus fibres). The fibrous structure
of the precursor material, which is a biomass by-product is ex-
pected to result in relatively low-cost product (activated biochar)
with increased separation efficiency because of its large external
surface available for adsorption (Prodromou and Pashalidis,
2013). Cu(II) has been used in this study as analogue for bivalent
toxic metal ions (e.g. Cd(II) and Pb(II)). The main goal of the study
is besides characterisation of the material, the investigation of var-
ious parameters (e.g. pH, Cu(II) concentration, ionic strength, tem-
perature and contact time) affecting the biosorption performance
and the determination of thermodynamic parameters (e.g. Kd,
DGo, DHo and DSo), which are of fundamental importance for the
development of water treatment technologies related to toxic me-
tal removal.
2. Methods
All experiments were performed under normal atmospheric
conditions in aqueous solutions. The preparation of the metal ion
solutions was carried out using a standard solution (Sigma–Al-
drich) and the Cu(II) concentration in solution was determined
by potentiometry using an Cu2+ ion-selective electrode, which
was calibrated prior and after each experiment (Rachou et al.,
2007). pH measurements were performed by a commercial glass
electrode, which was calibrated using a series of buffer solutions
(pH 2, 4, 7 and 10). The adsorbent used in this study was activated
biochar prepared from O. ficus indica cactus fibres, which were sep-
arated from dried cladodes.
2.1. Preparation and characterization of activated biochar
O. ficus cladodes were collected from plants used as effective
living fence in a suburb of Larnaca, Cyprus. The cladodes, which
had been broken off the plants, were extensively sun-dried and
partially disintegrated. The cladodes were carefully hand-peeled
and thoroughly washed by distilled water and the wooden residu-
als (e.g. primary and secondary fibres) were dehydrated at 70 °C
(Prodromou and Pashalidis, 2013). The dried fibres were thermally
treated gradually for 30 min at 200 °C and for 1 h at 600 °C to ob-
tain the carbonized product (biochar). Activation took place by sus-
pending the carbonized product in concentrated nitric acid (12 M
HNO3) for 24 h at room temperature and 3 h at 80 °C (reflux under
continuous stirring). The product has been washed several times
with distilled water and the neutralized material was dried in
the oven at 100 °C. The dried activated biochar was ground for a
461
few minutes in a coffee grinder, the ground product was sieved
and the particle fraction between 200 and 500 lm was selected
for the adsorption experiments.
The material was characterized by Scanning Electron Micros-
copy (SEM, Vega TS5136LS-Tescan) prior and after carbonization
or nitric acid activation, specific surface area measurements based
on the Brunauer–Emmett–Teller-theory (BET measurements) by
means of N2-adsorption (ASAP 2000, micromeritics) and Fourier
Transform Infra Red Spectroscopic measurements (FTIR spectrom-
eter 8900, Shimadzu) by means of translucent KBr disks including
finely ground biomass at a 10:1 mass ratio, prior and after Cu(II)
adsorption. In addition, acid–base titrations were performed to
study the acid–base behavior and determine the proton exchange
capacity of the activated biochar. Suspensions of 0.05 activated
biochar in 20 ml distilled water, were titrated with a pH meter
(Hanna Instruments) equipped with a glass electrode by adding
small aliquots of 0.1 M NaOH or 0.1 M HClO4 until the desired
pH was reached. Similar acid–base titrations were also performed
with distilled water samples and samples containing 0.05 non-acti-
vated biochar suspended in 20 ml distilled water.
2.2. Adsorption measurements
The adsorption studies were performed by conducting batch-
equilibrium experiments in 20 ml PE screw-cap vials. Specifically,
test solutions (15 ml) containing the metal ion of known composi-
tion and concentration were mixed with a given mass of the acti-
vated biochar (0.01 g) and the mixture was shaken in a
thermostated orbital shaker (at 100 rpm) for 24 h to assure that
equilibrium had been reached. The effect of various parameters
(pH, Cu(II) concentration, ionic strength, temperature and contact
time) on the Cu(II) adsorption by the activated biochar has been
investigated by performing different classes of experiments. These
experiments were performed using suspensions of 0.01 g biochar
in 15 ml of the respective solution. Generally, the Cu(II) concentra-
tion ([Cu(II)]o = 5  104 M) in the suspension and the temperature
(T = 23 °C) were kept constant and the experiments were per-
formed at pH 3 and 6.5. However, the effect of the various param-
eters was investigated by varying the specific parameter while the
other experimental parameters were kept constant. Specifically,
the effect of pH was studied in the pH range between 1.5 and
6.5, and the effect of the ionic strength (I) was investigated using
different solutions of NaClO4 (0.001, 0.01, 0.1, 0.5, 0.7 and 1 M)
as background electrolyte. For studying the effect of initial Cu(II)
concentration, the latter was varied between 1  105 M and
9  103 M and the effect of temperature was studied between
10 and 70 °C. Finally, for the kinetic studies certain amount of
the activated biochar (0.01 g) was mixed with 15 ml of Cu(II) solu-
tions (([Cu(II)]o 5  104 M, T = 23 °C) at pH 3 and 6.5 and the me-
tal concentration was determined by potentiometry at regular time
steps.
2.3. Statistical analysis
All experiments were performed in triplicate and the data are
presented as mean ± standard deviation. The uncertainty of
the values was generally below 10% and is basically attributed to
the error associated with analytical method used (e.g. potentiome-
try by ion selective electrodes). The analytical error was deter-
mined by the method calibration performed daily using seven
reference solutions of various analyte concentrations. Differences
between the means of two groups were analyzed by Student’s t
test at 95% confidence level. Generally, data analysis and plotting
of diagram was performed using Kaleidagraph, a graphing and data
analysis software.
462 L. Hadjittofi et al. / Bioresource Technology 159 (2014) 460–464

3. Results and discussion

3.1. Characterisation of activated biochar

According to the SEM images, cactus fibres are composed of

highly oriented series of lamellar structures giving the material a
strong and tough structure, and providing microchannels and ex-
tended surface for rapid fluid exchange. In nature and technology
lamella-similar structures are found extensively because lamellar
structures provide material strength with less weight and in-
creased surface area, and permits a much higher amount of sub-
stances adsorbed by the surface active sites (Dabbs and Aksay,
2012). Comparison of the SEM images corresponding to the non-
carbonized and biochar cactus fibres shows that carbonization
and chemical modification does not affect significantly the texture
of the fibres. In addition, surface analysis of non-carbonized and
carbonized cactus fibres indicates that there is no internal meso-
porous surface (BET surface <5 m3 g1). This is in agreement with Fig. 1. Titration curves derived from the acid–base titration of suspensions made
literature data, which ascribe the internal surface of biochars up of 0.05 g of activated biochar (AC) and non-activated biochar (C) in distilled
mainly to micropores (d < 2 nm). This microporosity of biochars 20 ml water or 20 ml distilled water (H2O), and titrated with 0.1 M NaOH or 0.1 M
HClO4.
is significant for gas adsorption, but of minor importance for metal
ion adsorption from aqueous systems (Issabayeva et al., 2010).
FTIR spectra obtained for the carbonized and the activated bio- the equivalence point (pH > 9) indicate the presence of additional
char cactus fibres clearly indicate that HNO3 activation results acid–base reacting groups such as carboxylic, lactonic and phenolic
basically in the formation of carboxylic moieties on the carbonized groups. Nevertheless, the main acidic group on the activated
fibre surface. In contrast to the spectra of the carbonized cactus fi- biochar surface are the carboxylic moieties, which act also as
bres, which show two distinct peaks at 1574 and 1429 cm1 and strong binding sites for metal ions even in the acidic pH area
are characteristic for carbonized cellulosic materials, the IR spectra (Moreno-Barbosa et al., 2013).
of the activated material show absorption bands at 3430, 1713 and
1242 cm1, which are attributed to –OH stretching vibrations, car-
3.2. Adsorption studies
bonyl stretching vibrations and carboxylic acid bending vibration,
respectively. In addition, the spectrum of the deprotonated form
According to the FTIR spectra of the activated biochar derived
of the activated material shows bands at 1588 and 1428 cm1,
from cactus fibres, which show a red shift of the bands correspond-
which correspond to the asymmetric and symmetric vibrations of
ing to stretching modes of the carboxylic moieties upon Cu(II)
the deprotonated carboxylic moieties (Chen et al., 2011) and prove
adsorption, the binding of the Cu(II) cations on activated biochar/
the formation of carboxylic acids upon activation.
carbon occurs through binding by the carboxylic moieties present
To estimate the proton exchange capacity associated with the
on the activated carbon surface. Hence, the solution pH is one of
acidic surface groups of the activated biochar the incremental titra-
the most important parameters affecting adsorption on surfaces,
tion curves were measured. Fig. 1 shows the acid–base titration
because pH may govern both the chemical behavior of a metal
curves corresponding to aqueous suspensions of carbonized cactus
ion in solution and the surface charge of an adsorbent. Generally,
fibres (C) and activated biochar derived from the carbonized cactus
the relative adsorption increases with increasing pH and reaches
fibres (AC). Fig. 1 includes also the acid–base titration of distilled
a maximum value (100%) at pH P 6. For pH values below 6 the
water. The titration curve of the carbonized cactus fibres is similar
relative adsorption decreases with pH and its value becomes al-
to the titration curve of distilled water indicating that the carbon-
most zero for pH < 1.5. Because at pH < 6 Cu(II) is exclusively pres-
ized cactus fibres react neutral and do not posses any acidic or
ent in the form of positively charged aqueous species (Baes and
alkaline reacting groups. However, the titration curve of the acti-
Mesmer, 1976), the adsorption of the metal ion is solely governed
vated biochar is significantly different, indicating the presence of
by cation exchange reactions and hence the proton concentration
acidic groups on the surface of the activated material. Specifically
in solution. The corresponding cation-exchange reaction between
the acidic pH (pH 3) of the corresponding suspension corrobo-
protons and Cu(II) cations on the cactus fibres surface, is
rates the presence of acidic groups and particularly carboxylic moi-
formulated by Eq. (1).
eties on the activated biochar surface (Moreno-Barbosa et al.,
2013). As the pH is raised the suspension exhibits considerable R-COOH þ Cu2þ ! R-COO-Cuþ þ Hþ ð1Þ
buffer capacity in the pH range between 4.2 and 7.0 (Fig. 1), which
reflects the deprotonation of carboxylic groups (4.5 < pKa < 7.5). In Above pH 6 hydrolysis of the Cu(II) ions becomes significant leading
addition the shape of the buffer zone (4.5 < pH < 7), which is char- most probably to the formation of the neutral surface complex R-
acteristic for polyelectrolytes, prove the predominance of the car- COO-CuOH (Eq. (2)). Neutral surface complexes are generally more
boxylic acid moieties on the activated biochar surface (Worthen stable than their corresponding charged compounds.
and Lapitsky, 2011).
R-COOH þ CuOHþ ! R-COO-CuOHþ þ Hþ ð2Þ
For the estimation of the proton exchange capacity the inflec-
tion point at pH 9.3, which corresponds to the equivalence point In order to evaluate the maximum adsorption capacity (qmax),
of carboxylic acids, has been considered as equivalence point. adsorption experiments with varying Cu(II) concentrations have
Based on this assumption, the evaluation of the titration data re- been performed at pH 3 and pH 6.5. The adsorption data have been
sulted in an amount of dissociable protons per unit mass of acti- fitted by three different isotherm models (e.g. Langmuir, Freund-
vated material, which is 3.0 ± 0.5 meq g1 (Worthen and Lapitsky, lich and Dubinin–Radushkevich) and the corresponding parame-
2011). The differences between the titration curves even above ters and goodness of fits of the three models are summarized in
 L. Hadjittofi et al. / Bioresource Technology 159 (2014) 460–464
Table 1
Fitting parameters and goodness of fits for three different isotherm models (e.g. Langmuir, Freundlich and Dubinin–Radushkevich) applied to the experimental adsorption data.
The corresponding experiments were performed with suspensions of 0.01 g activated biochar in 15 ml distilled water ([Cu(II)]tot = 1  1059  103 mol l1, T = 23 ± 2 °C and
24 h of reaction time).
Isotherm model
Langmuir Freundlich
qmax (mol kg1) KL R2 Kf
pH 3
0.31 ± 0.01 1250 ± 100 0.999 2.7 ± 0.6
pH 6.5
3.5 ± 0.3 (1.4 ± 0.3)  105 0.986 967 ± 900
Table 1. The best fits of the data correspond to the Langmuir
isotherm model and the average adsorption energy value obtained
from the Dubinin–Radushkevich isotherm model is above the
critical value E > 8 kJ mol1, indicating chemisorption of Cu(II) on
the activated biochar prepared from cactus fibres and being in
agreement with the FTIR spectroscopic data.
The qmax data (Table 1) indicate that the activated biochar
derived from cactus fibres possesses extraordinary adsorption
capacity for Cu(II). The qmax value 3.5 mol kg1 is almost an order
of magnitude higher compared to adsorption capacities of
activated biochars obtained from other biomass by-products
(Hernandez-Ramirez and Holmes, 2008; Trakal et al., 2014). This
enormous higher adsorption capacity of the activated biochar de-
rived from cactus fibres can be attributed to the laminar structure
of the cactus fibres and the corresponding increased external
surface.
The existence of two different adsorption mechanisms at neu-
tral (pH 6.5) and acidic pH (pH 3) is supported by the thermody-
namic parameters evaluated from the corresponding data
(Prodromou and Pashalidis, 2013). In contrast to adsorption at
pH 6.5, which declines with temperature (exothermic process)
the adsorption at pH 3 is favoured with temperature (endothermic
process). The values of the thermodynamic parameters
indicate clearly that the adsorption at pH 6.5 presents higher
(DHo = 23 ± 5 kJ mol1; DSo = 161 ± 53 J K1 mol1) and the
adsorption at pH 3 lower (DHo = 3 ± 2 kJ mol1; DSo = 36 ± 35
J K1 mol1) chemical affinity for Cu(II). Nevertheless, the values
of the thermodynamic parameters evaluated are close to corre-
sponding values reported in literature for similar systems (Li
et al., 2013) and higher than those related to systems which in-
clude adsorption on activated carbon/biochar prepared by other
starting materials (Demirbas et al., 2009).
The effect of ionic strength on the relative adsorption of Cu(II)
gives further insight into the mechanisms of Cu(II) binding by acti-
vated biochar fibres. According to the experimental data the rela-
tive adsorption in the acidic pH region (pH 3) is strongly affected
by increasing salinity and the relative adsorption decreases to
30% at I = 1.0 M, indicating that Cu(II) binding on the activated bio-
char surface is strongly governed by electrostatic interactions. On
the other hand, the relative adsorption in the near neutral pH re-
gion (pH 6.5) is not affected by increasing salinity and indicates
specific interactions and the formation of inner-sphere complexes
between Cu(II) and the carboxylic groups of the activated biochar
surface (Prodromou and Pashalidis, 2013).
The reaction kinetics support also the existence of two different
pH-dependent reaction mechanisms. In contrast to the adsorption
reaction at pH 6.5, which is very fast and could not be followed by
the analytical method applied (e.g. potentiometry), the adsorption
process at pH 3 is significantly slower. The kinetic data correspond-
ing to the adsorption process at pH 3 are well fitted by the first or-
der rate expression (R2 = 0.988) and the corresponding values for
the reaction rate constant (kads) and the qe (mmol g1) are
0.022 ± 0.001 and 0.080, respectively (Ho, 2004). The kads for the
463
Dubinin–Radushkevich
n R2 qmax (mol kg1) E (kJ mol1) R2
3.2 ± 0.9 0.977 1.0 8.8 0.962
1.8 ± 0.3 0.956 1.4 8.5 0.993
adsorption of Cu(II) on the activated biochar is similar to corre-
sponding values reported in literature for similar adsorption sys-
tems (Demirbas et al., 2009; Chen et al., 2011).
4. Conclusions
Activated biochar produced from O. ficus indica cactus fibres
were used to adsorb Cu(II) ions from aqueous solutions. The mate-
rial presents relatively very high capacity and chemical affinity for
Cu(II) ions even at low pH, which is attributed to the laminar struc-
tures and the carboxylic moieties present on the surface, respec-
tively. The effect of physicochemical parameters (e.g. pH, ionic
strength, temperature) indicates the formation of outer-sphere
and inner-sphere complexes at near-neutral and acidic pH, respec-
tively. The material could be a very attractive candidate for the re-
moval of toxic metal from waters and wastewaters.
Acknowledgement
The authors would like to thank Mr. Petros Theodorou for the
supply of the cactus cladodes.
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