J Radioanal Nucl Chem (2017) 311:1459–1464

DOI 10.1007/s10967-016-4989-9

Removal of cesium and strontium using natural attapulgite:

evaluation of adsorption isotherm and thermodynamic data
A. Kilincarslan Kaygun1 • M. Eral2 • S. Akyil Erenturk3

Received: 24 June 2016 / Published online: 17 August 2016

Ó Akadémiai Kiadó, Budapest, Hungary 2016

Abstract Natural attapulgite was used for removal of and 29 years, respectively [1, 2]. Both radionuclides are
cesium and strontium ions from aqueous media by using a considered as the most hazardous radioactive fission
batch technique. It was found that cesium and strontium products because of their high radiotoxicities [3].
exhibits a physical adsorption mechanism onto the natural Furthermore, radioactive cesium as an excellent gamma
attapulgite with a good adsorption efficiency. The adsorp- source used for some applications such as surgical instru-
tion thermodynamic parameters of cesium and strontium ment disinfection, radiotherapy and food sterilization [4].
referred to an exothermic nature for strontium ion and an Radioactive strontium, very strong pure b-emitter, chemi-
endothermic nature for cesium ion and spontaneity of the cally resembles calcium and strongly deposits within the
adsorption process. Dubinin–Radushkevich isotherm living organisms, mainly in the bones as a source of long
model were the best fitted the adsorption equilibrium data term radiation [1, 3].
of cesium and strontium ions. Ea values showed that the Therefore, the removal of cesium and strontium in even
interaction among cesium and strontium ions and the trace amount from aqueous media should be considered for
adsorbent are a physical adsorption. protection of eco-system [5, 6]. Adsorption process is one
of the most important separation processes for hazardous
Keywords Adsorption  Cesium  Strontium  Aqueous elements and prevents to use of the toxic and carcinogenic
media  Adsorption isotherms  Thermodynamic solvents during separation process [4, 5, 7, 8].
In the past decade, clay minerals have been investigated
as an adsorbent to removal of water pollutants from
Introduction aqueous media [9, 10]. In recent years, natural and man-
made clay minerals become attractive materials again for
With the rapid development of nuclear energy, fission water purification and radioactive waste management.
products especially 137Cs, 90Sr, and 239Pu are generated Attapulgite is a widely used mineral clay composed of
from nuclear weapon testing and nuclear reactor technol- hydrated magnesium aluminium silicate mineral and has
ogy, and enter the eco-system as a serious environmental large specific surface area. Magnesium ions as an
issue. 137Cs and 90Sr have a long half-life (t1/2) of about 30 exchangeable cation in attapulgite can easily exchange
with heavy metal ions and radionuclides [11–13].
The goal of this work was to investigate the adsorption
& S. Akyil Erenturk behaviour of cesium and strontium onto natural attapulgite
[email protected]
to understand the interaction between cesium/strontium
1
Cekmece Nuclear Research and Training Center, and attapulgite to develop a treatment system for waste
Yarimburgaz Mah, 34303 Kucukcekmece, Istanbul, Turkey disposal areas. Therefore, adsorption data of cesium and
2
Institute of Nuclear Sciences, Ege University, strontium were fitted to adsorption isotherm models. The
35100 Bornova, Izmir, Turkey thermodynamic parameters such as free energy (DG°),
3
Energy Institute, Istanbul Technical University, enthalpy of adsorption (DH°) and entropy (DS°) were cal-
34469 Maslak, Istanbul, Turkey culated separately for cesium and strontium.

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1460 J Radioanal Nucl Chem (2017) 311:1459–1464

Experimental where V is initial volume (mL), Vi is final volume of the

suspension. Swelling capacity of the attapulgite was found
Materials and methods as 11 %.
Adsorption–desorption experiments to calculate the
All the reagents used in this work were of analytical specific surface area (BET) was carried out using a nitro-
reagent grade and were obtained from chemical commer- gen gas sorption system at 10-4 Pa and 150 °C with
cial suppliers. Quantachrome Instruments Autosorb 1-Ultrapycnometer
Natural attapulgite obtained from Amcol Mineral and 1000 equipments. Specific surface area of the natural
Mining Company was used as an adsorbent for adsorption attapulgite sample was estimated as 198 m2 g-1 using
experiments. Natural attapulgite was grinded and placed in multipoint BET methods. Density of the samples was
a drying oven at 105 °C for 4 h. The mineral composition determined as 2.55 g cm-3 by using Archimedes principle.
of dried attapulgite sample was analysed by X-ray fluo- The adsorption of cesium and strontium on natural
rescence technique (XRF) (Panalytical Axios Advanced attapulgite were implemented by a batch technique.
Model WDXRF) and shown in Table 1. Cesium nitrate and strontium nitrate (Merck) was used for
Cation exchange capacity (CEC) was determined using adsorption experiments. Solutions of cesium and strontium
methylene blue method which is much faster and is still were prepared by dissolving known quantities of cesium
widely used method than others. Attapulgite suspension nitrate and strontium nitrate in distilled water. For pH
was prepared in ratio 6 % solid/liquid. 3 ml of attapulgite adjustment of cesium and strontium solutions, the buffers
suspension was placed in a beaker and 10 mL of distilled of pH 4 and 8 were used for the calibration of pH meter.
water, 0.5 mL of 5 N H2SO4 and 15 mL of 3 % H2O2 was Solutions of HNO3 and Na2CO3–NaHCO3 were added for
added and stirred for 10 min on magnetic stirrer. 0.01 M of pH adjustment.
methylene blue was added with titration method and the 0.1 g of the attapulgite was equilibrated with 25 mL of
mixture was stirred. Cation exchange capacity (CEC) was the cesium and strontium solutions of known concentration
calculated using the equation below: in a flask at ambient temperature in a thermostated shaker
 
NV water bath for a known period of time. After equilibration,
CEC ¼  100 ð1Þ
m solid and solution phases were separated by filtration using
Whatman No. 42 filter paper. The cesium and strontium
where N is normality of methylene blue, V is methylene
concentrations in solution were determined by ICP-OES
blue volume dissipated in titration (mL), m is amount of
(Perkin Elmer). The results are the average of at least
dried attapulgite (g). Cation exchange capacity (CEC) of
duplicate independent measurements. Adsorption effi-
the attapulgite was 7.032 meq per 100 g.
ciency (%) were calculated using mass balance equation as
Swelling capacity of the attapulgite in water was
follows:
determined using a rapid and simple method. 6 g of natural  
attapulgite was placed in a graduated cylinder and read the Ci  Cf
Adsorption yield (%Þ ¼  100 ð3Þ
volume. 90 mL of the distilled water was added to the Ci
graduated cylinder and wait for 24 h. Last volume was where Ci is the concentration of the initial cesium or
recorded. Swelling capacity of the attapulgite was calcu- strontium solution (mg mL-1), Cf is the concentration of
lated using the equation in below: the cesium or strontium solution in equilibrium
Vi  V (mg mL-1).
% Swelling capacity ¼  100 ð2Þ
V

Table 1 Mineral composition

Metal oxides Chemical Metal oxides Chemical
of natural attapulgite
composition (%) composition (%)

SiO2 75.90 Cr2O3 0.021

MgO 2.231 MnO 0.045
Al2O3 12.24 Fe2O3 3.990
Na2O 0.440 ZrO2 0.018
P2O5 0.042 BaO 0.055
SO3 0.361 Cl 0.024
CaO 1.960 K2O 2.014
TiO2 0.566 Total 99.909

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J Radioanal Nucl Chem (2017) 311:1459–1464 1461

All experiments were carried out in duplicate. Uncer-

tainties connected with results were different. Total
uncertainties in all experimental parameters changed
between 5 to 10 %. Total uncertainties never exceeded
10 % for each replicate.

Adsorption isotherms

Various adsorption isotherm models namely Langmuir,

Freundlich and Dubinin–Radushkevich (D–R) were used to
describe the interaction between concentration of cesium Fig. 1 Effect of initial concentration on cesium and strontium
and strontium in solution and attapulgite at ambient tem- adsorption
perature. Linear regression was used to determine the best-
fitting isotherm amongst the adsorption isotherm models by cesium and strontium ions onto the natural attapulgite
judging the correlation coefficients. decreased. The adsorbent and ions attained equilibrium at
50 lg mL-1 as 77 % for cesium and at 40 lg mL-1 for
Thermodynamic parameters strontium.
On the basis of these results, effect of pH on the cesium
Thermodynamic parameters comprised Gibbs energy and strontium adsorption capacities was studied in the
change (DG°), enthalpy change (DH°) and Entropy change range from pH 2 to 10. Figure 2 shows the influence of pH
(DS°) were estimated to exhibit types and mechanisms on the cesium and strontium adsorption onto the atta-
adsorption process. Thermodynamic parameters on the pulgite. With the increase of pH, the cesium and strontium
sorption of cesium and strontium ions onto natural atta- adsorption efficiencies increased until pH 4. After pH 4,
pulgite were calculated in different temperature from 293 adsorption efficiencies of both ions remained steady as
to 333 K. about 78 % for cesium ions and as about 67 % for stron-
tium ions. When the pH was higher than 8, the adsorption
Kinetic models efficiencies of cesium and strontium ions decreased with an
increasing the pH. The results reveals that the adsorbent
Based on the effect of the contact time on cesium and can be used to remove of both ions from waste solution in a
strontium adsorption, different kinetic models including the wide range of pH from 4 to 8 with a quite high efficiency.
pseudo first-order, the pseudo second-order and Elovich The effect of contact time on the adsorption of cesium
models were used to fit the adsorption data for accurately and strontium ions onto natural attapulgite was investigated
describing the adsorption process. Kinetic experiments at to understand the kinetic modelling of both ions for using
preset time intervals (from 5 to 360 min) were carried out to design of a low cost wastewater treatment system. The
at ambient temperature. variation of adsorption efficiencies for both ions with
contact time was given in Fig. 3. The adsorption efficiency
of cesium and strontium ions onto natural attapulgite
Results and discussion slightly increased with an increasing the contact time and
reached an equilibrium within 15 min. for cesium ions and
Effect of parameters on Cs and Sr ions sorption 30 min. for strontium ions.
onto attapulgite

To understand the cesium and strontium adsorption beha-

viours, the effectual parameters were investigated under
varying conditions in initial activity concentration of
cesium and strontium, pH of the adsorptive solution, con-
tact time and temperature.
The effect of initial concentration from 5 to 60 lg mL-1
on cesium and strontium adsorption was investigated at
30 °C. Figure 1 shows the effect of initial concentration of
cesium and strontium ions on the adsorbent. As shown in
Fig. 1, when the initial activity concentration was Fig. 2 Effect of pH on the cesium and strontium adsorption
increased in range from 5 to 60 lg mL-1, adsorption of capacities

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1462 J Radioanal Nucl Chem (2017) 311:1459–1464

Activation energy was calculated using Arrhenius

equation that expressed by the following equation [18, 19]:
Ea
ln k1 ¼ ln A  ð6Þ
RT
where k1 is the rate constant for the reaction, A is a pro-
portionality constant that varies from one reaction to
another, Ea is the activation energy for the reaction, R is the
ideal gas constant (8.314 J mol-1 K-1) and T is the tem-
perature in kelvin.
Fig. 3 Variation of adsorption efficiency of cesium and strontium The positive value of enthalpy indicates that the inter-
ions with contact time action between cesium and adsorbent is an endothermic
reaction which consumes energy. On the other hand, the
In order to determine thermodynamic parameters of adsorbent and strontium interaction gave a negative
cesium and strontium adsorption behaviours, influence of enthalpy value which indicates an exothermic nature.
temperature on the adsorption of both ions on the adsorbent Enthalpy value shows the type of solid/ion interaction. If
was studied at different temperatures (from 293 to 333 K) the enthalpy value is lower than 40 kJ mol-1, the type of
under optimized conditions. As shown in Fig. 4, the adsorption is physical process [13, 20, 21]. The enthalpy
adsorption efficiency for cesium ions slightly decreased values for cesium and strontium were found as lower than
from 80 to 76 % with rise of temperature from 293 to 40 kJ mol-1. Entropy values for cesium and strontium
333 K. On the other hand, the adsorption efficiency for were obtained as positive which indicates increasing ran-
strontium ions was obtained regularly stable as 68 %. domness at the solid/liquid interface. The negative values
of Gibbs free energy suggest spontaneous nature of the
Thermodynamic parameters adsorption and required energy to carry out the reaction
[22, 23]. Gibbs free energy values for cesium and strontium
To evaluate the spontaneity and the heat change of the has a spontaneous and physisorption nature of the
cesium and strontium adsorption processes, thermody- adsorption reaction.
namic parameters (DH°, DS° and DG°) were estimated the The activation energy plays a key role to get information
equations in below [14–17]: on whether interaction between solid and ions is physical
DS DH  or chemical. If the magnitude of the activation energy has
ln Kd ¼  ð4Þ
R RT 4–40 kJ mol-1, the adsorption is a chemisorption process.
DG ¼ DH   TDS ð5Þ When the activation energy is lower than 4 kJ mol-1, the
interaction between solid and ions accepts as adsorption
where Kd is the thermodynamic stability constant, DS° is [24]. The value of activation energies were calculated
standard entropy (J mol-1 K-1), DH° is standard enthalpy using Eq. 6 to be 4.39 and -1.81 kJ mol-1 for cesium and
(kJ mol-1), T is the absolute temperature (K) and R is the strontium, respectively. These values indicate that the
gas constant (8.314 J mol-1 K-1). Table 2 shows ther- reaction between strontium and the adsorbent leads by
modynamic parameters for cesium and strontium adsorp- physical adsorption mechanism. Although activation
tion onto natural attapulgite. energy value is in lower limit for cesium adsorption,
physical adsorption mechanism could be accepted for
cesium adsorption.

Adsorption isotherm

To study the adsorption isotherms of cesium and strontium

ions onto attapulgite, different sorption isotherm models,
namely Langmuir, Freundlich and D–R which were
described in detailed in our previous studies [25–27], were
examined for the experimental sorption equilibrium data.
To provide sufficient physicochemical information about
mechanism properties and to describe sorption capacities
Fig. 4 Influence of temperature on the adsorption of cesium and of attapulgite for cesium and strontium ions, the adsorption
strontium on the attapulgite data was fitted the sorption isotherm models.

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J Radioanal Nucl Chem (2017) 311:1459–1464 1463

Table 2 Thermodynamic
DH° (kJ mol-1) DS° (J mol-1 K-1) DG° (kJ mol-1)
parameters for adsorption of
cesium and strontium ions 293 K 303 K 313 K 323 K 333 K
onto the adsorbent
Cs? 4.39 41.98 -16.69 -17.11 -17.53 -17.95 -18.37
Sr2? -1.81 57.98 -18.79 -19.37 -19.95 -20.53 -21.11

Table 3 Values of Langmuir, Freundlich and D–R constants indicates that ion exchange process is dominant. If the
Ion Qm (mg g-1) kL (mg L-1) R2
process is chemical adsorption, E should be in the range
16–40 kJ mol-1 [14, 28]. For this study, E values were
Langmuir Cs? 9.091 0.723 0.9677 found as 0.83 kJ mol-1 for cesium ions and 1.19 kJ mol-1
2?
Sr 8.110 0.236 0.9640 for strontium ions. The results show that the adsorption
kF (mg g )-1
nF R2 process is a physical adsorption for both ions.

Freundlich Cs? 2.159 2.22 0.9890

2?
Sr 1.936 2.38 0.8637 Conclusions
-1 2
Xm (mg) b (kJ mol ) R
This research study has demonstrated the adsorption
D–R Cs? 7.6865 0.7244 0.9949 mechanism of cesium and strontium ions onto the natural
Sr2? 7.9818 0.3543 0.9967 attapulgite as a function of effectual parameters such as
Qm and kL Langmuir’s constants related to the capacity and energy of
initial concentration, pH, contact time and temperature.
the adsorption, kF the adsorption capacity of adsorbent, nF a dimen- Based on the experimental results of this study, it is
sionless constant related to adsorption intensity, Xm the maximum observed that the natural attapulgite which is an economic
sorption capacity, b the activity coefficient related to mean sorption and environmental benefits, has a potentially good adsor-
energy
bent capacity to remove the cesium and strontium ions
from aqueous solution.
The results show that adsorption mechanisms of cesium
Table 3 shows the regression coefficients and the con-
and strontium onto the adsorbent is highly dependent on
stant values for all isotherm models. Regression coeffi-
pH and initial concentration of solution. The results reveals
cients indicated that the Freundlich (R2 = 0.99) and D–R
that the attapulgite can be used to remove of cesium and
(R2 = 0.99) isotherm models well fitted the cesium
strontium ions from waste solution in a wide range of pH
adsorption data and only D–R (R2 [ 0.99) isotherm model
from 4 to 8 with a quite high efficiency in a short time.
well fitted the strontium adsorption data onto the atta-
Removal of cesium and strontium were slightly affected by
pulgite at ambient temperature.
increasing temperature. This result reveals that physical
Freundlich isotherm models describe multiple layer
adsorption leads the adsorption mechanism of both ions.
molecular adsorption process on surface of attapulgite. The
Various isotherm models were properly applied to
factor ‘‘1/n’’ indicates that adsorption is favourable for the
experimental data of both ions. Freundlich isotherm model
ions. If values of 1/n smaller than 0.5, it shows that
was well fitted for only cesium adsorption data, while D–R
adsorbate is easily adsorbed; if values of 1/n larger than 2,
isotherm model was well utilized for cesium and strontium
it indicates that the adsorbate is hardly adsorbed
adsorption data. It can be considered that adsorption
[14, 24, 28]. For cesium adsorption onto the adsorbent, the
mechanism leads multilayer coverage on the adsorbent
1/n value was determined as 0.45. This result indicates that
surface and in micro pores of the adsorbent.
the adsorption process was favourable for cesium ions.
Adsorption enthalpy changes indicated an exothermic
Adsorption capacity was found as 2.16 and 1.94 lg g-1 at
process for strontium and an endothermic process for
ambient temperature for the removal of cesium and stron-
cesium. Adsorption process for both ions was increasing
tium ions, respectively.
randomness at the solid/liquid interface.
The regression coefficients were well fitted the D–R
isotherm models (R2 [ 0.99) for both ions with a good
adsorption capacity given by Xm values. Mean sorption
energy (E) value reveals that the adsorption process is
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