Canadian Metallurgical Quarterly

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2+
UPTAKE OF Cd FROM AQUEOUS SOLUTIONS
USING PROTONATED DRY ALGINATE BEADS

J.P. IBÁÑEZ & Y. UMETSU

2+
To cite this article: J.P. IBÁÑEZ & Y. UMETSU (2008) UPTAKE OF Cd FROM AQUEOUS
SOLUTIONS USING PROTONATED DRY ALGINATE BEADS, Canadian Metallurgical Quarterly,
47:1, 45-50, DOI: 10.1179/cmq.2008.47.1.45

To link to this article: http://dx.doi.org/10.1179/cmq.2008.47.1.45

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 45

Canadian Metallurgical Quarterly, Vol 47, No 1 pp 45-50, 2008

© Canadian Institute of Mining, Metallurgy and Petroleum
Published by Canadian Institute of Mining, Metallurgy and Petroleum
Printed in Canada. All rights reserved

UPTAKE OF Cd2+ FROM AQUEOUS SOLUTIONS USING

PROTONATED DRY ALGINATE BEADS
J.P. IBÁÑEZ1 and Y. UMETSU2
1
Department of Metallurgical Engineering, Arturo Prat University, Av. Arturo Prat 2120,
P.O. Box 121, Iquique, Chile
jpibanez@unap.cl
2
Institute of Multidisciplinary Research for Advanced Materials, Tohoku University,
Katahira 2-1-1, Aoba-ku, Sendai 980-8577, Japan

(Received in revised form November, 2007)

Downloaded by [University of California, San Diego] at 10:54 08 April 2016

Abstract — The use of protonated dry alginate beads for the uptake of cadmium ions from aqueous
solutions was studied at 25 ºC. The uptake of Cd2+ produced a release of protons, for which a molar ratio
d[H+]/d[Cd2+] of 2.0 was established. This ion exchange was the mechanism of cadmium uptake which
followed a pseudo-second order kinetic model.
The uptake was strongly dependent on the solution pH up to a value of 4.5 after which it remained
constant. The maximum Cd-uptake was computed in 285.7 mg per gram of alginate beads (dry wt.) at
pH 4.5 by the Langmuir adsorption model. A residual concentration of around 0.09 mg/L of Cd2+ which
allowed safety discharge of some types of effluents having this heavy metal ion, was reached with a
solution initially having 25 mg/L of Cd2+.
EPMA-EDX of Cd-loaded beads showed a uniform distribution of the metal ions throughout the
structure of the alginate bead, regardless the solution pH.

Résumé — On a étudié l’utilisation de billes à protons d’alginate sec pour la capture d’ions cadmium à
partir de solutions aqueuses à 25°C. La capture de Cd2+ produisait un dégagement de protons, pour
lesquels on a établi un rapport molaire d[H+/]/d[Cd2+] de 2.0. Cet échange d’ion constituait le mécanisme
de capture du cadmium, lequel suivait un modèle cinétique de pseudo second ordre.
La capture était fortement dépendante du pH de la solution jusqu’à une valeur de 4.5, au-delà duquel
elle restait constante. On a calculé la capture maximale de Cd à 285.7 mg par gramme de billes d’alginate
(poids sec) au pH de 4.5 au moyen du modèle d’adsorption de Langmuir. Une concentration résiduelle
d’environ 0.09 mg/L de Cd2+, qui permettait la décharge sécuritaire de certains types d’effluents contenant
cet ion métal lourd, était atteinte avec une solution ayant initialement 25 mg/L de Cd2+.
L’analyse d’EPMA-EDX de billes chargées de Cd a montré une distribution uniforme des ions de
métal dans toute la structure de la bille d’alginate, peu importe le pH de la solution.

INTRODUCTION associated with an uptake of metal ions from low

The capacity of certain materials such as chitosan,
zeolites, clays, flash and biological entities (such as
algae, bacteria, fungi and yeast) to uptake heavy metal
ions from dilute aqueous solutions has been proven [1-
6]. Immobilization of those entities in solidified
polymers such as alginate creates sorbent materials with
the right size, mechanical strength, rigidity and porosity
[2].
The predominant role of the alginate present in
algae on the uptake of heavy metals has been
demonstrated [7-13]. However, there are relatively few
studies on the sorbent properties of this biopolymer
concentration aqueous solutions [11-15]. Even after
the formation of alginate beads with calcium or barium
ions, the particular structure of this biopolymer leaves
free carboxylic groups which react with metal ions as
reported in our previous papers [12,13].
Cadmium represents a great potential hazard to
humans and the environment. A disease known as “Itai-
Itai” in Japan is specifically associated with cadmium
poisoning resulting in multiple fractures arising from
osteomalacia [16]. The industrial uses of cadmium are
widespread and increasing in electroplating, paint
pigments, plastics, electronic circuits and silver and
nickel cadmium batteries. The legal discharge limit of

CANADIAN METALLURGICAL QUARTERLY, VOL 47, NO 1

 46 J.P. IBÁÑEZ and Y. UMETSU

cadmium may contain a concentration range of 0.01 to RESULTS AND DISCUSSIONS

1.0 mg/L [17] depending on the country, processing
and waste water treatment methods.
This paper reports on the use of protonated dry
alginate beads (PDAB) as a potential sorbent material
for the uptake of cadmium and the mechanism involved
in this process.
EXPERIMENTAL
All chemicals were of analytical reagent grade and were
used without further purification. Stock and test solutions
of cadmium were prepared from Cd(NO3)2*4H2O. Sodium
alginate with a viscosity range of 0.10-0.15 Ns/m2 for 1
w/v% was used. Aqueous solutions were prepared with
doubly distilled water. Chemical analyses of the stock and
sample solutions were made by using an inductively
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Figure 1 shows typical experimental results as a
function of time. The equilibrium condition was
reached in less than 300 minutes of contact time; 300
rpm were sufficient for a mass transfer independent
uptake process. Plot A shows the mmoles of NaOH
used to keep the pH constant, i.e., it corresponds to the
amount of protons liberated during the Cd-uptake. Plot
B shows the analytical concentration of cadmium and
calcium in the working solution and Plot C shows the
uptake of cadmium.
The uptake of Cd 2+ was coupled to a release of
protons from the PDAB (Figure 1a). There is a rapid
first step of release that is extended for less than 90
minutes and then a slow release of protons. This

coupled plasma atomic emission spectrometer (ICP-AES).

Examination of the beads’ surface by scanning electron a
microscope (SEM) was made after coating them with a
thin layer of gold. To analyze the cross-section of Cd-
loaded beads coated with a thin layer of graphite, an
electron probe X-ray microanalyzer in the mode of energy
dispersive X-ray spectroscopy (EPMA-EDX) was used.
Calcium and barium protonated dry alginate beads
were produced according to the protocol described in our
previous work [12]. Both Ca- and Ba-PDAB showed the b
same physical and chemical properties in aqueous
solutions [12]. Briefly, PDAB have a corrugated surface
with a mean diameter of 1.0 ± 0.1 mm. PDAB are stable
up to pH values of 6, after which Ca or Ba is released and
the PDAB lose rigidity. The loss of weight during drying
was about 95% which indicates a high porosity in the
solidified beads.
The uptake experiments were conducted as described
in our previous work [13]. Briefly, 400 mL of the Cd-
bearing solution with a desired concentration (from 25 to
500 mg/L) was contacted with 80 mg of PDAB for a fixed
time at 25.0±0.1 °C. The pH of the Cd solution was kept
constant by adding sodium hydroxide solution. Samples
of 1 mL, for chemical analysis, were withdrawn at c
selected time intervals. The samples were diluted to 10
mL with doubly distilled water and then filtered through a
cellulose acetate membrane filter. The concentrations of
remaining cadmium and released calcium (or barium) in
the filtrates were analyzed by ICP-AES. The beads were
collected at the end of the experiments, washed several
times with doubly distilled water, air dried and stored for
SEM observation and EPMA-EDX analysis. Most of the
experiments were carried out singly. Experimental
reproducibility was evaluated with experiments in
duplicate and triplicate which showed variations lower
than 2.5%. For these experiments, the average values are Fig. 1. Typical experimental results as a function of time. a)
given. Consumption of NaOH, b) Concentration of Cd and Ca in solution
and c) Cd uptake. Conditions: [Cd] initial = 43 mg/L, pH = 4.5 &
PDAB = 80 mg.

CANADIAN METALLURGICAL QUARTERLY, VOL 47, NO 1

 UPTAKE OF Cd2+ FROM AQUEOUS SOLUTIONS USING PROTONATED DRY ALGINATE BEADS
behaviour is in agreement with that observed for the
Cd 2+ concentration in solution showed in Figure 1b;
this figure shows no Ca in solution. Therefore, the
uptake may be associated with an ion exchange
between protons of the PDAB and cadmium ions.
Figure 1c shows that most of the Cd-uptake takes place
within 90 minutes; the removal reaches a value of
around 80%.
Figure 2 summarizes the main experimental results
as a function of solution pH after 300 minutes of
contacting time at 25 ºC. Figure 2a shows mmoles of
NaOH consumed for the neutralization of protons. Data
for pH values lower than 3.5 were not included because
of the inaccurate reading obtained when small amounts
of protons were released into solutions of low pH.
Figure 2b shows residual concentration of cadmium and
released Ca from the alginate beads. Figure 2c presents
the uptake of cadmium; it also includes the Cd uptake
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when Ba-PDAB was used which will be analyzed in the
next section. Figure 2b indicates a continuous decrease
of the residual concentration of cadmium as the solution
a not detectably affected during removal of Cd 2+; this,
b
c not affected by the metal used in preparation of the
Fig. 2. Summary of the main experimental results as a function of
pH. a) consumption of NaOH, b) Ca and Cd ions in solution and c)
uptake of Cd by using Ca-PDAB and Ba-PDAB. Conditions:
[Cd] initial = 43 mg/L, t = 300 min, T = 25 ºC and PDAB = 80 mg.
47
pH increases starting at about pH 2.0. This figure also
shows that the cross-linking calcium ion was not
released from the alginate beads during cadmium
removal. Figure 2c shows a continuous increase of the
Cd uptake by increasing pH; a rise in uptake from 0 to
about 190 mg/g (dry wt) by increasing pH from 2.0 to
4.0 was observed. The uptake slightly increased by
about 5% when the pH was further increased to 4.5 and
stayed unchanged at higher pH values. Therefore, the
uptake is considered to be constant over a pH range
above 4.5. No uptake was observed at a pH lower than
2.0.
This effect of pH on the uptake has been explained
by the presence of the weak alginic acid as main
component of the alginate beads. This means that there
is a low amount of active sites with a low pH, i.e., low
removal of Cd and high amount at higher pH values
(higher Cd-uptake) which agree with the experimental
data. An apparent dissociation constant of 10 -4 for
alginic acid has been reported [7] which could be shifted
to a value of 10 -4.5 [13]. These values agree with the pH
at which the maximum uptake of Cd 2+ is reached by the
alginate (Figure 2c).
Both the size and shape of the alginate beads were
coupled with the fact that no Ca was released during the
Cd-uptake, strongly suggests the chemical and
structural stability of the PDAB in the pH range studied.
Based on Figures 1b and 2b, exchange of structural
calcium of the alginate beads with cadmium ions was
not present during the uptake process.
Since an uptake of Cd was not observed at low pH
values, the mechanism associated with the formation of
the alginate beads probably differs from the mechanism
of the Cd-uptake. To support this, alginate was cross-
linked with barium instead of calcium. Both types of
PDAB have similar morphology and behaviour in
aqueous solutions [11,12]. Figure 2c showed the Cd-
uptake by Ba- and Ca-PDAB as a function of solution
pH after 300 minutes of contact time. Ba was not
released from the beads during Cd-uptake; identical
behaviour was observed for Ca-PDAB. The uptake was
alginate beads. Alginate beads are considered to keep
their structure by coordination of the Ca or Ba ions with
oxygen atoms of the alginic acid chains, while the
uptake is due to the carboxylic functional groups
remaining free in the structure of the bead [11,12].
There are different mechanisms involved in the
production of alginate and in the removal of Cd 2+.
The uptake of cadmium ions occurred along with a
release of protons as shown with the NaOH
consumption plotted in Figures 1 and 2. An ion
exchange involving protons could be responsible for the
cadmium uptake from the solution according to the
reaction
2{COO-H} + Cd 2+ = {COO} 2 − Cd + 2H + (1)
CANADIAN METALLURGICAL QUARTERLY, VOL 47, NO 1
 48 J.P. IBÁÑEZ and Y. UMETSU
The molar ratio between the neutralized protons
(consumption of NaOH) and Cd 2+ removed from
solution should have a value of 2.0. Figure 3 shows
that ratio as a function of pH. This figure clearly shows
that the molar ratio d[H + ]/d[Cd 2+ ] has a value of 2.0
which indicates that Reaction 1 is responsible for the
Cd uptake.
It has been reported [18] that most of the sorbent
process follows a kinetic behaviour described by a
pseudo-second order model. The model is represented by
dqt
= k ( qe – qt )
2 (2)
dt
where k is the pseudo-second order constant of reaction
in g/mg/min, q e is the uptake at equilibrium in mg/g, q t
is the uptake at time t and t is time in minutes.
By integrating Equation 2 for qt = 0 at t = 0 and q t at
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time t, linearizing the integrated expression and
evaluating the experimental data shown in Figure 1c
produced Figure 4 which represents t/qt as a function of t.
This figure shows a good correlation (R 2 = 0.998)
between the experimental data at pH 4.5 and this
kinetic model. It is possible to represent the Cd-uptake
by an ion exchange process with a kinetic behaviour
given by a pseudo-second order model. From the slope
Fig. 3. Molar ratio d[H + ]/d[Cd 2+ ] as a function of the pH.
Conditions: [Cd] initial = 43 mg/L, t = 300 min and PDAB = 80 mg.
Cd uptake, mg/g (dry wt.)
Fig. 4. Linearization of the pseudo-second order kinetic model, t/q
vs t for Cd-uptake at 25 ºC. Correlation coefficient, R 2 = 0.998.
CANADIAN METALLURGICAL QUARTERLY, VOL 47, NO 1
of the straight line plotted, the q e was calculated to be
227.3 mg/g and the kinetic constant, k, was found to be
9.72x10 -5 g/mg/min.
The saturation of alginate beads with cadmium
ions was studied by extending the concentration of
Cd 2+ from 25 to 500 mg/L. The results are given in
Figure 5 which presents Cd-uptake as a function of
equilibrium (or terminal) concentration for pH levels
of 3.5 and 4.5. SEM observation of the beads’ surfaces
after experimentation at the highest concentration of
Cd 2+ and at a pH of 4.5 showed clean corrugated
surfaces without precipitation. This agrees with the
thermodynamics of the system Cd 2+ -CO 2 -H 2 O at 25 ºC
reported Baes and Mesmer [19] which, for the experi-
mental conditions used, suggest the occurrence of
CaCO 3 at pH higher than 5.5. Figure 5 shows the
complete saturation of the PDAB with Cd 2+ when the
equilibrium concentration was around 50 mg/L at pH
4.5 and around 25 mg/L at pH 3.5. The maximum
uptakes were found to be about 280 and 170 mg of Cd
per gram (dry wt) of PDAB at pH 4.5 and 3.5, respec-
tively. It should be noted that when PDAB were
challenged with an initial concentration of Cd 2+ of 25
mg/L at pH 4.5, a residual concentration of 0.09 mg/L
was reached (with an uptake of 114 mg/g) which
allowed discharge of some types of effluents such as
those from the accumulator industry [17].
The experimental data were fitted with the
adsorption isotherms of Langmuir and Freundlich,
whose parameters are shown in Table I. This table
shows that data are fitted better to Langmuir than the
Freundlich model. The maximum uptakes given by the
Langmuir model (285.7 and 169.7 mg/g at pH 4.5 and
3.5, respectively) are in perfect agreement with the
values observed in Figure 5.
As reported in previous works [11-13], the drying
of the beads during production resulted in PDAB
having high porosity with channels and open pores
throughout the structure. Hence, the Cd 2+ could
Fig. 5. Uptake of cadmium as function of equilibrium concentration
of cadmium. Conditions: pH = 4.5, T = 25 ºC, t = 300 min and PDAB
= 80 mg.
 UPTAKE OF Cd2+ FROM AQUEOUS SOLUTIONS USING PROTONATED DRY ALGINATE BEADS 49

Table I – Parameters of the Langmuir and Freundlich adsorption models and regression coefficients
pH Langmuir Freundlich
q max b R 2
k n R2
4.5 285.7 0.307 1.00 189.8 0.0708 0.952
3.5 169.5 0.299 1.00 121.5 0.0578 0.966
q max : Langmuir maximum uptake
b: Langmuir isotherm parameter
k, n: Freundlich isotherm constants

Table II – Uptake of cadmium by several kinds of sorbents

Sorbent material Uptake pH Reference
mg/g
IX resins 29 - 63 4.9 [8]
Anaerobic sludge 80 7.3 [20]
Ascophyllum nodosum 18 - 172 4.9 [8]
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Saccharomyces c. 23 - 71 4.5 [21]

Clay minerals 11 - 137 n.a. 1 [22]
Chitosan vedas 250 n.a. [22]
Exopolysaccharide 125 5.0 [23]
PDAB 170-286 3.5-4.5 this work
Sargassum fluitants 214-292 4.0-6.0 [24]
Data for batch experiments, working temp.: 20-30 °C, initial conc. of Cd: 10-700 mg/L, sorbent concentration:
0.2-4.0 g/L.
1
Not available

interact with functional groups on the external surface
of the beads and the surface of the channels and pores.
Figures 6a, 6b and 6c show EPMA-EDX micrographs
of the cross section of beads after Cd-uptake at pH
levels of 2.5, 4.5 and 5.5, respectively. The distribution
pattern of cadmium was measured along the white line
crossing the bead. The relative intensity of the peaks in
the micrographs indicates the amount of Cd taken up
by PDAB: at pH 2.5 there is low intensity because the
uptake was only about 17 mg/g; however, for pH of 4.5
and 5.5, there were the same high intensities for
uptakes of about 200 mg/g (Figure 2c). These
micrographs show a uniform distribution of cadmium
ions throughout the cross section of the beads at
different values of pH. This indicates that functional
groups are homogeneously distributed in the alginate

Fig. 6. EPMA-EDX micrographs of the cross-section of beads loaded with Cd at pH values of 2.5 (A), 4.5 (B) & 5.5 (C). The Cd distri-
bution pattern was measured along the white line crossing the beads

CANADIAN METALLURGICAL QUARTERLY, VOL 47, NO 1

 50 J.P. IBÁÑEZ and Y. UMETSU
structure and that cadmium ions are capable of
penetrating into the beads and reacting with functional
groups. Therefore, the protonated dry alginate beads
can be considered as porous ion exchangers having
high permeability.
Table II summarizes the uptake of cadmium,
reported in the technical literature, by several sorbent
materials and by PDAB. This table shows that Cd
uptake is significantly affected by the sorbent used.
Due to the high Cd uptake shown by protonated
alginate beads, they have an interesting potential for
use in removal of this toxic heavy metal from aqueous
solutions.
CONCLUSIONS
The uptake of cadmium was studied at 25 ºC using
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protonated and dry alginate beads. The uptake of
cadmium ions significantly increases with a rise in pH
of the Cd-bearing solution up to 4.5; above this point
to pH 5.5, Cd-uptake becomes constant. The maximum
uptake of cadmium at pH 4.5 was computed to be 285.7
mg/g (dry wt) according to the Langmuir model.
The uptake of cadmium was found to be an ion
exchange process represented by Reaction 1, experi-
mental data showed a molar ratio proton released from
the beads to cadmium ions removed from solution of
2.0. This ion exchange process followed a pseudo-
second order kinetic model, for which a rate constant
of 9.72x10 -5 g/min/mg was found. The residual concen-
tration of Cd in solution after contact with PDAB was
below the standards for discharge of several types of
industrial effluents.
ACKNOWLEDGMENT
J.P. Ibáñez thanks the Ministry of Education, Science
and Culture of Japan for the financial support provided
through the Monbusho Scholarship Program.
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