Journal of Industrial and Engineering Chemistry 24 (2015) 107112

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Journal of Industrial and Engineering Chemistry

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

Removal of nickel ions from industrial wastewater using immobilized

sericite beads
Choong Jeon *, Ju-Hyun Cha
Department of Biochemical Engineering, Gangneung-Wonju National University, Jukhen-gil 7, Gangneung-si, Gangwon-do 210-702, South Korea

A R T I C L E I N F O

Article history:
Received 16 July 2014
Received in revised form 11 August 2014
Accepted 14 September 2014
Available online 20 September 2014
Keywords:
Sericite
Nickel ion
Immobilization
Column operation
Adsorption

A B S T R A C T

To efciently remove nickel ions from actual industrial wastewater which is coexisted with high sodium
concentration, powdered sericite was immobilized as a bead form by entrapment method using sodium
alginate. The beads with surface area of 7.1 m2/g were not untangled to 45 8C and pH 11.0 in
wastewater and have excellent mechanical strength and swelling characteristics. It was also conrmed
that natural sericite beads did not appear the characteristic peak for nickel ions, nickel-adsorbed beads
clearly shows the peak of nickel ions as about 4.00 wt% by means of SEMEDX analysis. The effect of
sodium ions on nickel removal was negligible and the maximum adsorption capacity using Langmuir
equation was 10.743 mg/g at pH 7.5 of wastewater in batch. The nickel ions can be removed from actual
wastewater over 95% up to 90 (1.0 mL/min) and 140 bed volumes (0.5 mL/min), respectively and 7 bed
volumes of 20 mM of HNO3 solution was required to get 96% of nickel desorption in continuous process
using packed-bed column. Also, breakthrough point of nickel ions could be still maintained as 130 up to
the 2nd cycle by reused immobilized sericite beads.
2014 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights
reserved.

Introduction
Metals are generally playing important roles in most industries.
Especially, nickel is widely used in electroplating, batteries
manufacturing, mining, metal nishing, porcelain enameling and
paint formulations [1,2]. Recently, the concern for nickel recovery
from the industrial wastewater has been recently increased in
terms of resources recycling. On the other hand, when nickel exists
as high concentration of Ni2+ in aqueous solution it may cause
severe damage to lungs, kidneys, gastrointestinal distress (nausea,
vomiting and diarrhea), pulmonary brosis, renal edema and skin
dermatitis [3]. From the literature survey, the concentration of
nickel ions in wastewaters varies from a low value of 0.5 mg/L to a
high value of 1000 mg/L while the maximum permissible
discharge level of nickel ions with industrial efuents into inland
water is 3 mg/L [4,5].
Therefore, many techniques have been tried to develop efcient
process including both removal and recovery for nickels from
industrial wastewater before being released. Among them,
adsorption has recently attracted considerable interest because
cheaper and abundantly available materials like sawdust, rice husk

* Corresponding author. Tel.: +82 33 640 2405; fax: +82 33 641 2410.
E-mail address: metaljeon@gwnu.ac.kr (C. Jeon).

and crab shells are being used for the removal and recovery of
valuable metals in wastewaters [6,7]. It is also well known that
adsorption has many advantages of high efciency, adsorbatespecicity, applicability at very low concentrations, suitability for
using batch and continuous processes, ease of operation, little
sludge generation, and possibility of regeneration and reuse, as
compared with other methods [8].
Among cost effective adsorbents, the possibility as a novel
adsorbent of sericite which is generally recognized as white ne
powders of muscovite in form, with nano-sized layer structure,
interlayer spacing of (0 0 2) plane is 10 A has been studied to
recover valuable metals or remove toxic metals [9]. We also
showed that sericite could efciently recover nickel ions in
industrial wastewater as a novel adsorbent in batch [10].
However, the use of powdered sericite is not acceptable to apply
to the up and/or down ow packed-bed column operation because
of cracking of powdered sericite and pressure drop occurred during
operation [11]. Therefore, it needs for powdered sericite to be
immobilized in a bead form to have good mechanical strength and
preserve adsorptive properties similar to those of commercial
activated carbon or ion exchange resins. Many immobilization
methods for adsorbent were developed and immobilized adsorbents were successfully applied to water and wastewater
treatment system [12]. Among immobilization methods, entrapment method which has some merits such as easy and low cost

http://dx.doi.org/10.1016/j.jiec.2014.09.016
1226-086X/ 2014 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights reserved.

108

C. Jeon, J.-H. Cha / Journal of Industrial and Engineering Chemistry 24 (2015) 107112

operation has been generally applied to make immobilized

adsorbent and agar, polyacrylamide, sodium alginate and kcarrageenan have been used as chemicals for entrapment [13]. Wu
et al. reported that alginates can be extensively applied to the
biomedicine and biotechnology to immobilize or encapsulate
enzymes and living cells because of excellent gel forming
properties [14].
The aim of this work is to evaluate adsorption behavior of
immobilized sericite bead using entrapment method with sodium
alginate for nickel ions discharged from actual industrial
wastewater in batch and column studies. The basic data obtained
from this study could be helpful for the understanding of the
adsorption process and will provide possibility for application of
actual wastewater containing nickel ions treatment system which
is operated by continuous process.
Materials and methods
Sericite used in this study was kindly obtained from the SG
mining industry located in the city of Gangneung in Korea.
Pretreatment methods and chemical composition for sericite were
already described in our previous study [15].
Actual industrial wastewater was provided from the Toricom
company, which is located in the city of Chun-An in Korea and
nickel ions were coexisted with sodium ions. Each concentration of
nickel and sodium ions was measured as about 100 and 133.3 mg/
L, respectively. All of the chemicals used in this study were of
analytical grade (Sigma Aldrich, USA) and deionized water was
used to prepare all of solutions.
To immobilize sericite, some amount of sericite, 1 g of sodium
alginate and 50 mL of distilled water were mixed under stirring to
get a uniform mixture at 60 8C for 2 h. The mixture was added
dropwise to a 4% of CaCl2 solution with stirring to get bead form.
The beads were separated from the CaCl2 solution after aging
process for 24 h and then washed with deionized water several
times. After drying at room temperature for 24 h, the beads were
used to evaluate adsorption behavior for nickel removal in batch
and continuous process. Experimental methods for physical
properties and swelling characteristics of the immobilized sericite
beads were followed as presented in the work [16].
To investigate the effect of sericite content in beads on removal
efciency of nickel ions, various beads with different mixing ratio
between sodium alginate and sericite in beads were made and each
0.1 g of the dried beads was dispersed in 100 mL wastewater. The
isothermal adsorption experiments were also carried out at the
desired initial nickel concentration, nal pH and temperature. All
the batch type adsorption experiments were performed by shaking
incubator (JEIO TECH, SI-600R, Korea) and the equilibrium pH of
wastewater was adjusted as 7.5 with dilute NaOH and HCl
solutions. Adsorption time was set to 24 h which is an enough time
to get an equilibrium state. When the desired pH for wastewater
with nickel ions was maintained constantly the solution was
centrifuged at 4000 rpm for 30 min to remove suspending sericite
beads by centrifuge (Gyrozen, Gyro 1236 MG, Korea) and then
concentration of nickel ion in supernatant was analyzed by ICP
(Inductively Coupled Plasma spectroscopy, Perkin-Elmer, UK). The
removal efciency (R) and amount of nickel ions adsorbed onto the
immobilized sericite bead (Q) were calculated by following Eqs. (1)
and (2), respectively:
R %

Ci  C f
Ci

Q mg=g

Ci  V i  C f  V
m

(1)

(2)

where Ci and Cf are the nickel ion concentration in the wastewater

before and after adsorption (mg/L), Vi and Vf are the wastewater
volumes before and after adsorption (L), and m is the dry weight of
the immobilized sericite bead used in the experiment (g).
Scanning electron microscopy (SEM) and energy dispersive Xray spectroscopy (EDX) were also used to characterize immobilized sericite beads for before and after adsorption of nickel ions.
SEM images of the beads were taken on a Hitachi model S-4100
(Japan) instrument and EDX spectra were obtained from an Oxford
INCA instrument.
Continuous adsorption experiments using borosilicate glass
column with 1.0 cm of diameter and 10 cm of height was
performed at room temperature. 1.5 g of immobilized sericite
beads was stored in a column and the wastewater was constantly
conducted across the column by Acuow Series II high-pressure
liquid chromatograph (USA). Inuent concentration of nickel ions
was set as 20 mg/L and inuent pH was maintained as 7.5 in
wastewater. For sequential desorption and regeneration experiments, 20 mM of HNO3 solution was used. Flow direction was upow, as is the case in most column operations and rate was
controlled as 0.5 (retention time: 2.4 min) and 1.0 mL/min
(retention time: 1.2 min). Efuent samples were automatically
collected by Spectra/Chrom CF-1 fraction collectors. The inuent
and efuent concentration of nickel ions was also measured by ICP.
Results and discussion
The physical and swelling characteristics of sericite beads
The optimal manufacture mixing ratio for immobilization of
sericite was the 3:7 (sodium alginate:sericite) in 50 mL of distilled
water and the beads were used to remove nickel ions in actual
wastewater for batch and sequential adsorption (data not shown).
The diameter of bead was about 2.0 mm and surface area was
measured as the 7.1 m2/g. The bead was not untangled to 45 8C
and pH 11.0 in wastewater especially, the bead did not crack
under the condition of 120 h and 700 rpm in batch operation, as
described in my earlier work [16]. Khoo et al. [17] used milder
condition of 70 h and 500 rpm than that of this study to investigate
cracking of the fungal bead the mechanical strength. For references, the fracture strength for calcium-alginate cylinders with
3.8 mm of diameter and 15 mm long was found to the 2.25 N from
the literature survey [18]. Swelling characteristics of immobilized
sericite beads were investigated by swelling ratio and distention
index and the values slightly increased up to 15 h and they did not
change any more [16]. These results support the applicability of
immobilized sericite beads as a novel adsorbent to the actual
wastewater treatment using batch and continuous process.
Adsorption characteristics of immobilized sericite bead for nickel ion in
batch operation
As mentioned above, nickel ions coexist with sodium ions with
133.3 mg/L of concentration in the wastewater. It is well known
that the sodium ions cause ionic strength effect to metal ions,
therefore, adsorption capacity of metal ions decreased [19]. Therefore, the effect of sodium ions on the removal efciency of nickel
ions was investigated and the result was shown in Fig. 1. It shows
that the removal efciency of nickel ions for immobilized sericite
beads between actual wastewater used in this study and articial
wastewater was almost same. It means the ionic strength only had
a slight effect on the decrease of removal efciency for nickel ion.
From the result, adsorption mechanism between immobilized
sericite beads and nickel ions is thought to be forming of inner
sphere complexes by covalent and ionic binding which are well
known that ionic strength effect is negligible [20].

C. Jeon, J.-H. Cha / Journal of Industrial and Engineering Chemistry 24 (2015) 107112

Removal efficiency of nickel ions

(%)

70
60
50
40
30
20
10
0

Artificial wastewater

Actual wastewater

Fig. 1. Effect of ionic strength on removal efciency of nickel ion (immobilized

sericite bead concentration: 10 g/L, initial concentration of nickel ions: 100 mg/L,
nal pH of nickel solution: 7.5, working volume: 100 mL).

109

The SEM images of immobilized sericite beads for before and

after adsorption of nickel ions were applied to investigate the
surface condition and Fig. 2 shows electron dense part (more
bright) which is thought to be nickel adsorption was appeared at
the (b), as compared with the (a). However, it was very difcult to
differentiate whether adsorption of nickel ion is happened with
SEM images only. Therefore, EDX spectrum was applied to clarify
whether the electron dense part on the surface of immobilized
sericite beads is composed up of nickel ions. While the EDX
spectrum (a) for natural sericite beads did not appear the
characteristic peak for nickel ions, nickel-adsorbed beads clearly
shows the peak of nickel ions as about 4.00 wt%, as shown in
Fig. 2(b).
The effect of various mixing ratio between sodium alginate and
sericite in beads on removal efciency of nickel ions in actual
wastewater was tested. The removal efciency of nickel ions
increased as the contents of sericite increased and the highest
value was about 60% at the 3:7 (sodium alginate:sericite) of mixing
ratio, as shown in Fig. 3. The value was lower than that of powdered
sericite with 90% of removal efciency. It can be explained as the
reducing of function groups such as silanol and aluminol which
play important role in adsorption of nickel ions due to the use of

Fig. 2. SEM images and EDX spectra of immobilized sericite beads.

C. Jeon, J.-H. Cha / Journal of Industrial and Engineering Chemistry 24 (2015) 107112

110

1.1

90
1.0

80

Log(qe) (mg/g-dry mass)

Removal efficiency of nickel ions

(%)

100

70
60
50
40
30
20

0.9

0.8

0.7

Experimental data
Regression using Freundlich model

0.6

10
0.5

Powder

10:0

9:1

7:3

5:5

3:7

0.8

1:9

1.0

Contents ratio (Sodium alginate : Sericite)

1.2

1.4

1.6

1.8

2.0

Log(Ce) (mg/L)

Fig. 3. Removal efciency of nickel ions according to the contents of sericite in

immobilized bead (initial concentration of nickel ions: 100 mg/L, immobilized bead
concentration: 10 g/L, nal pH of nickel solution: 7.5).

Fig. 5. Isothermal adsorption for nickel ions of immobilized sericite bead using
Freundlich model (nal pH of nickel solution: 7.5, working volume: 100 mL).

sodium alginate for immobilization of sericite [21]. Also, transfer

resistance may happen because of the characteristics of entrapment method which can be achieved by mixing an adsorbent with
a polyionic polymer material and then crosslinking the polymer
with multivalent cations in an ion exchange reaction to form a
lattice structure when nickel ions were moved to the bead [13]. The
immobilized beads composed of sodium alginate only could
remove 15% of nickel ions and the result shows the possibility for
applicability of sodium alginate to remove nickel ions.
The adsorption isotherms of immobilized sericite beads for
nickel ions are shown in Figs. 4 and 5. There are several isotherm
models, which can be used to describe the equilibrium nature of
adsorption. However, adsorption mechanisms in aqueous solution
and/or wastewater are very complicated that no simple theory can
adequately represent all experimental data [14]. In this work, the
most widely used Langmuir and Freundlich equations were tested
against experimental data at nal pH 7.5 and 25 8C of wastewater.
Langmuir (3) and Freundlich equations (4) are generally expressed
as follows:

Log qe Log K f

1
1
11=qm K L

qe qm
Ce

(3)

(4)

In the above equations, qm (mg/g) is the maximum adsorption

capacity and KL (L/mg) represents the adsorption intensity or
Langmuir coefcient. Also, kf is the Freundlich equation constant
related to the adsorption capacity and 1/n is an empirical
parameter respect to the adsorption intensity which varies with
the heterogeneity of material [22]. The Langmuir and Freundlich
isotherm constants determined from the tting of experimental
data are summarized in Table 1. Each qm and KL parameters of
immobilized sericite bead for nickel ions was 10.743 mg/g and
0.083 L/mg, respectively. Also, the estimated values of 1/n and Kf
for nickel ions were 0.347 and 2.154, respectively. It was also found
that the Langmuir model with higher correlation coefcient
(0.984) ts experimental data better than the Freundlich model
(0.974). To compare the validity of the isotherm equations more
denitely, normalized standard deviation (%) was calculated as
follows:
"
Standard deviation % 100 

2
X qexp
 qcal =qexp
e
e

#0:5

(5)

N1

where superscripts exp and cal indicate the experimental and

calculated values with the tted parameters and N is the number of
measurements. From the result, each SD (%) for Langmuir and
Freundlich isotherm equation was 1.41 and 1.98, respectively.

12

Adsorption and regeneration characteristics of immobilized sericite

bead for nickel ion in continuous process using packed bed column

10

qe (mg/g-dry mass)

 
1
Log C e
n

Experimental data
Curve fitting using Langmuir model
4

20

40

60

80

Ce (mg/L)
Fig. 4. Isothermal adsorption curve for nickel ions of immobilized sericite bead
using Langmuir model (nal pH of nickel solution: 7.5, working volume: 100 mL).

Fig. 6 shows the breakthrough curve for nickel ions using

packed bed column with immobilized sericite bead. The breakthrough point is generally dened as 5% of the feed concentration
[23]. As shown in the gure, breakthrough point was appeared
around 90 (1.0 mL/min) and 140 bed volumes (0.5 mL/min). In this
study, 1 bed volume equates to the 1.2 mL. From the result, it was
Table 1
Langmuir and Freundlich isotherm constants of immobilized sericite beads for
nickel ions.
Langmuir isotherm model

Freundlich isotherm model

qm (mg/g)

KL (L/mg)

r2

SD (%)

1/n

Kf (L/g)

r2

SD (%)

10.743

0.083

0.984

1.41

0.347

2.154

0.974

1.98

C. Jeon, J.-H. Cha / Journal of Industrial and Engineering Chemistry 24 (2015) 107112
1500

1.1
1.0

Concentration of nickel ions (mg/L)

1350

0.9

Flow rate : 0.5 mL/min

Flow rate : 1.0 mL/min
Breakthrough point

0.8

Ce/Co

0.7
0.6
0.5
0.4
0.3
0.2

1200
1050
900
750
600
450
300
150

0.1

0.0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200

Bed volumes

found that nickels can be continuously removed from actual

wastewater over 95% up to 90 and 140 bed volumes for each ow
rate. The effect of ow rate on bed volumes can be explained as
different contact time between adsorbent and owing metal
solution. The breakthrough curves are analyzed by the Thomas
equation expressed as follows [9]:
Ce
1

C o 1 EXP K T qo m  C o V=Q

Fig. 8. Development of desorption of nickel ions using 20 mM of HNO3 solution

(amount of pre-loading with nickel ions: 3100 mg/L, one bed volume: 1.2 mL, ow
rate: 0.5 mL/min).
Table 2
Breakthrough throughputs from sequential adsorption
and desorption cycle (ow rate: 0.5 mL/min, initial
concentration of nickel ions: 20 mg/L, breakthrough
point: 0.05 mg/L, one bed volume: 1.2 mL, inuent pH
of nickel solution: 7.5).

(6)

where Ce is the nickel concentration in the efuent (mg/L), Co is

the nickel concentration in the feed (mg/L), KT is the Thomas rate
constant (L/min-mg), qo is the maximum amount of nickel ions
can be adsorbed (mg/g), m is the mass of the adsorbent loaded (g),
V is the throughput volume (L) and Q is the ow rate (L/min). The
non-linear regression of the breakthrough data using Thomas
equation was shown in Fig. 7 and the tting constants KT and qo
for the removal of nickel ions by immobilized sericite beads are
found to be respectively 9.75  104 L/min-mg and 5.254 mg/g
for 0.5 mL/min and 2.45  104 L/min-mg and 3.507 mg/g
for 1.0 mL/min. The calculated nickel adsorption capacity
(5.254 mg/g) at 0.5 mL/min was smaller than that of batch test

1.2

1.0

Bed volumes

Fig. 6. Effect of ow rate on breakthrough curve of nickel ions using immobilized

sericite bead (one bed volume: 1.2 mL, inuent concentration: 20 ppm,
immobilized sericite bead: 1.5 g, inuent pH of nickel solution: 7.5,
breakthrough point: 0.05).

Experimental data (Flow rate : 0.0005L/min)

Experimental data (Flow rate : 0.001L/min)
Calculated result (Flow rate : 0.0005L/min)
Calculated result (Flow rate : 0.001L/min)

0.8

Ce/Co

111

0.6

0.4

Cycle number

Bed volumes

1
2
3
4

137
130
95
55

(10.743 mg/g). It can be explained as insufcient contact time for

the adsorption between nickel ions and immobilized sericite
beads under dynamic conditions, as compared with batch
conditions [9].
Fig. 8 shows the development for desorption of nickel ions using
20 mM of HNO3 solution, whose efciency had been chosen in
batch experiments as the optimum concentration, in our previous
work [10]. Nickels bound onto the sericite beads was easily
desorbed and quantitatively recovered in just a few bed volumes.
7 bed volumes of desorbing agent was required to get 96% of
desorption efciency and the 1430 mg/L of maximum nickel
concentration was obtained in just 2 bed volumes.
It is necessary to evaluate regeneration ability of adsorbent in
sequential adsorption process because of its cost-effectiveness.
Table 2 shows the regeneration result of immobilized sericite
beads for nickel ions using packed-bed column and 130 bed
volumes could be still maintained up to the 2nd cycle by reused
immobilized sericite beads. However, the value sharply decreased
after the 2nd cycle. It may be due to the incomplete desorption and
structural damage of adsorbent. From the result, it was found that
immobilized sericite beads have the regeneration ability for nickel
ions, to some extent in continuous process.
Conclusions

0.2

0.0
0.00

0.05

0.10

0.15

0.20

0.25

Throughput Volume (L)

Fig. 7. Breakthrough curve of nickel ions on immobilized sericite beads tted for
Thomas model (Co: 20.0 mg/L, m: 1.5 g).

Powdered sericite was successfully immobilized by entrapment

method using the 3:7 (sodium alginate:sericite) of optimal mixing
ratio in beads. The beads have excellent mechanical strength and
swelling characteristics to apply to the packed-bed column in
continuous process. The surface condition and the existence of
nickel ions onto the immobilized sericite beads were conrmed by
the SEM and EDX instrument analyses. Each maximum adsorption

112

C. Jeon, J.-H. Cha / Journal of Industrial and Engineering Chemistry 24 (2015) 107112

capacity and Langmuir coefcient was 10.743 mg/g and 0.083 L/

mg at nal pH 7.5 of wastewater in batch type and the Langmuir
model with higher correlation coefcient (0.984) ts experimental
data better than the Freundlich model (0.974). The breakthrough
point was appeared around 90 (1.0 mL/min) and 140 bed volumes
(0.5 mL/min) and 96% of nickel desorption was obtained within
7 bed volumes of 20 mM of HNO3 solution. Therefore, it could be
concluded that the immobilized sericite beads which have
excellent mechanical strength and good regeneration ability can
be sufciently used to the recover nickel ions in batch and
continuous process and the technique could sufciently replace
conventional treatment process such as solvent extraction and ion
exchange resin.
Acknowledgement
The authors gratefully acknowledge the Korea Institute of
Energy Technology Evaluation and Planning for the nancial
support toward this study.
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