Al-Nahrain University, College of Engineering Journal (NUCEJ) Vol.91 No.2, 6192 pp.

186 - 193

Eggshell Powder as An Adsorbent for Removal of Cu (II) and

Cd (II) from Aqueous Solution: Equilibrium, Kinetic and
Thermodynamic Studies
Ziad Tark Abd Ali Mohammed A. Ibrahim Huda M. Madhloom
Environmental Engineering Department Civil Engineering Department Civil Engineering Department
Coll. of Engineering/University of Baghdad College of Engineering College of Engineering/Al-
E-mail: z.teach2000@yahoo.com Al-Nahrain University Mustansiriyah University

Abstract materials capable of removing toxic heavy metals

The adsorption of Cu (II) and Cd (II) ions onto from contaminated water [3].The sorption
eggshell was investigated. The effects of contact process, which includes metal immobilization in
time, initial pH of solution, adsorbent dosage, contaminated water, has gained attention in the
initial metal concentration, agitation speed, and past few decades because it offers advantages
temperature were studied in batch experiments. such as high efficiency and low operating cost,
The maximum adsorption capacities for Cu(II) and because it is eco-friendly when compared to
and Cd(II) were 8.4 and 7.01 mg/g, respectively. conve ntional treatment methods[4]. Adsorbents
Thermodynamic parameters such as Gibbs free such as activated carbons prepared from some
energy change, Enthalpy change and Entropy agricultural by-products, some cellulosic wastes
change have been calculated. These and their carbonization products, bituminous coal
thermodynamic parameters indicated that the and commercial activated carbons were used[5].
adsorption process was thermodynamically Due to the high cost of the activation process,
spontaneous under natural conditions and the there is a need to adopt cheaper and readily
adsorption was endothermic in nature. available materials which can be used
Experimental data were also tested in terms of economically on a large scale [6]. Domestic egg
adsorption kinetics, the results illustrated that the consumption is high and continues to increase
adsorption process was following pseudo second- with the rapid increase of population, waste
order kinetics. In addition Fourier transfer eggshells contain high contents of calcium
infrared spectroscopy (FTIR) analysis suggests carbonate (85–95%); therefore, their recycling or
that Cu (II) and Cd (II) interact with metal oxides reuse has the potential to reduce environmental
and -OH functional group present in eggshell pollution while acting as a cost effective material
powder. for the immobilization of heavy metals in
Keywords: Eggshell, Copper ions, Cadmium wastewater and soil [7]. Therefore, this study was
ions, Adsorption, Kinetic. conducted to evaluate the effectiveness of waste
eggshells on the removal of heavy metals Cu (II)
1. Introduction and Cd (II) from aqueous solutions.
The presence of inorganic pollutants such as
heavy metals in aquatic systems is of considerable 2. Experimental Work and Methods
concern because of their non-biodegradability, 2.1. Preparation of Adsorbent
mobility and toxicity. Heavy metals can Chicken eggshells were used as the adsorbent
accumulate in the human body over time, causing in this study. The chicken eggshells were
serious health effects Accordingly, the removal of collected from kitchen waste and washed by
heavy metals from wastewater has received a deionized water for several times to remove the
great deal of attention in recent years [1]. Several dirt particles. The eggshells were then air-dried
conventional physical and chemical wastewater and incubated in hot air oven at 40 ºC for 35
treatment technologies including coagulation, minutes (protein component in eggshell can
filtration, evaporation recovery, precipitation, denature at high temperature; > 40 ºC) [8].
oxidation/reduction, electrochemical treatment, Eggshells were ground to a powder in a grinder,
ion exchange and reverse osmosis have been used and sieved to obtain between 60-100 mesh mesh
to remove heavy metals from aqueous systems. to obtain (0.25-0.104 mm) size particles. The
However, these methods are economically eggshell powder comprises of 94 % calcium
unfavorable or technically complicated, and are carbonate, with small amounts of magnesium
only used in special cases of wastewater treatment carbonate, calcium phosphate and other organic
[2]. Moreover, most of these processes are only matter including protein [9].
effective when there are high levels of metals in
aqueous solution There has recently been
increased interest in the development of new

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2.2. Preparation of Simulated 2.5. PH Variation

Wastewater The pH value of the solution is an important
Stock solutions (1000 mg/L) of single Cu(II) controlling parameter in the adsorption process,
and Cd(II) were prepared by dissolving an and the initial pH value of the solution has more
appropriate weight of pure salt Cu(N03)2 and influence than the final pH, which influences both
Cd(N03)2 (manufactured by BDH, England) in the the adsorbent surface metal binding sites and the
desired volume of de-ionized water. The stock metal chemistry in water [11]. The effect of pH
solution was successively diluted with de-ionized on the single adsorption of Cu(II) an Cd(II) using
water to obtain the desired test concentration of eggshells was carried out within the range that
metal ions. Concentration of Cu(II) and Cd(II) would not be influenced by the metal precipitated
were measured using atomic adsorption [9]. It was reported that the suitable pH range for
spectrophotometer (AAS) (Shimadzu, Japan). the adsorption of Cu(II) and Cd(II) was (3 - 7).
This experiment was conducted at 20 °C to study
2.3. Batch Experiments the effect of initial pH value of solution on the
Series of batch adsorption tests were adsorption of Cu(II) and Cd(II) by contacting 0.25
conducted to determine the effects of contact g of the adsorbent (eggshells) with 50 mL of 50
time, initial pH, initial concentration of pollutants, mg/L contaminant solution in a volumetric flasks.
adsorbent dosage, and operating temperature on
adsorption performance of eggshells used as 2.6. Adsorbent Dosage
adsorbent materials. Therefore, various adsorbent The solution of metal ion of 50 mL with
dosages of 0.05, 0.1, 0.25, 0.3, 0.4, 0.5, 1, and 2 g concentration of 50 mg/L was added to various
were introduced into 250 mL flasks with 50 mL amount of the several adsorbents (0.05-2 g) in 250
solution containing 50 mg/L of single Cu(II) and mL volumetric flasks and agitated for 90 minute
Cd(II). The flasks were then placed in an orbital on a shaker, then the solution was filtered and
shaker (Edmund Buhler SM25, German) and analyzed.
agitated up to a total contact time of 180 min at a 2.7. Initial Metal Concentration
fixed agitation speed of 250 rpm. Samples were The initial metal concentration provides an
taken at predetermined time intervals (10, 15, 20, important driving force to overcome all mass
30, 35, 40, 50, 60, 80, 90, 120 and 180 minute) transfer resistance of metal between the aqueous
and then separated by filtration (filter paper type: and solid phases [12]. The initial concentrations
Whatman 542, England). Contaminants of Cu (II) and Cd (II) were ranged from 50 to 100
concentration in the samples were analyzed by mg/L.
atomic absorption spectrophotometer (AAS)
(Shimadzu, Japan). 2.8. Agitation Speed
Batch tests were carried out in a pH range of 3–7 The effect of agitation of the sorbent/sorbate
to determine the effect of initial pH on adsorption system for Cu (II) and Cd (II) adsorption was
because the precipitation of Cu(II) and Cd(II) is at monitored at (0, 50, 100, 150, 200 and 250 rpm).
pH greater than 9.7 [10]. The pH of the aqueous
solution was adjusted by adding 0.1 M HNO3 or
2.9. Temperature Variation
The batch adsorption process was studied at
0.1 M NaOH as required. Effects of various
different temperatures of 20, 30, 40, and 50 °C in
operating temperatures ranging from 20 to 50 ºC
order to investigate the effect of temperature on
were also investigated in the batch studies.
the adsorption process using eggshells. This was
Temperature adjustments were conducted in the
achieved by contacting 0.25 g of adsorbents with
same orbital shaker. The efficiency of adsorption
50 mL of 50 mg/L single contaminant solution at
(%) was calculated as follows:
pH 6 for 90 minute with agitation speed of 250
R = [(Co-Ce)/Co] × 100 … (1) rpm by using shaker incubator. The results were
used to investigate the thermodynamics of the
Where Co and Ce are the initial and the adsorption process.
equilibrium contaminant concentrations
respectively. R is the removal efficiency (%). 3. Kinetic Equations
2.4. Contact Time The kinetics of Cu(II) and Cd(II) adsorption on
Batch adsorption tests were carried out at eggshells were analyzed using pseudo-first-order
different contact time intervals (0 - 180 minute) at [13] and Pseudo-second-order models [14], The
initial contaminants concentration of 50 mg/L. pseudo-first order kinetic rate equation is:
This was done by contacting 0.25g of adsorbent (dqt /dt)=k1 (qe-qt) … (2)
with 50 mL of single contaminant solution at the
pH 4. Where k1 is the rate constant of pseudo first order
adsorption (min-1), qe is the amount of
contaminant sorbed at equilibrium (mg/g) and qt
the amount of contaminant sorbed at time t

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(mg/g). Integrating equation (2) for the boundary to diffusion of the metal ions into the inner part of
conditions t = 0 to t=t and qt=0 to qt= qe and the eggshells.
rearranging yields the linear time-dependent
4.2. Effect of pH on Adsorption
function.
The pH of solution was examined at different
Log (qe-qt) = Log qe-(kt /2.303) … (3) pH values, covering a range of 3-7. The
maximum adsorption was obtained at pH 6 for
The intercept of the straight-line plots of log both contaminants. Removal of Cu (II) and Cd
(qe-qt) against t equal log qe , However, if the (II) by eggshells was pH dependent as shown in
intercept does not equal qe, then the reaction is not Figure (2).
likely to be first-order, irrespective of the
magnitude of the correlation coefficient. The
Co=50 m g/L, t=90 m in, dose=0.25 g/50 m L,
pseudo- second- order kinetic rate equation is: agitation speed=200 rpm
100

(dqt/dt)=k2 (qe-qt)2 … (4) 80

Removal %
60
Where k2 is the rate constant of pseudo second 40
order adsorption (mg.mg-1.min-1).Taking into 20
Cu
Cd
account, the boundary conditions t=0 to t=t and
0
qt=0 to qt=qe .The integrated form of Equation (4) 2 3 4 5 6 7
can be rearranged to obtain Equation (5): pH

Figure 2: Effect of pH on the removal

(t/ qt)= (1/k2 qe2) + (t/qe) … (5) percent
The plot of (t/qt) and t of Equation (5) gives a At pH < 3.0, H+ ions compete with Cu (II) and
linear relationship, qe and k2 can be determined Cd (II) ions for the surface of the adsorbent which
from the slope and intercept of the plot, would hinder metal ions from reaching the
respectively. binding sites of the sorbet caused by the repulsive
forces. At pH > 7, the Cu (II) and Cd (II) will
4. Result and Discussion precipitate due to hydroxide anions forming
copper and cadmium hydroxide precipitate. For
4.1. Effect of Contact Time this reason the maximum pH value was to be 6.
The effect of contact time on the removal At pH = 6 the highest removal efficiency was
percent of Cu(II) and Cd(II) from the solution is observed 84% and 70% for Cu (II) and Cd (II),
shown in Figure (1). respectively.
Co=50 m g/L, dose=0.25 g/50 m L, PH=4,
100 agitation speed=200 rpm 4.3. Effect of Eggshells Dosage
The adsorption of ions was observed to
80
increase as the amount of adsorbent increased
Removal %

60
gradually from 0.05 to 2 g, as shown in Figure(3).
40
Cu
20 Cd Co=50 m g/L, t=90 m in, pH=6, agitation speed=200 rpm
0 100
0 20 40 60 80 100 120 140 160 180
Tim e (m in) 80
Removal %

60
Figure 1: The effect of contact time on the 40
removal percent. 20 Cu
Cd
0
It was observed that the removal of Cu(II) and 0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6 1.8 2
Cd(II) by the eggshells increased with increase in Eggshell dosage (g/50 m L)

contact time. The adsorption of Cu(II) was rapid

Figure 3: Effect of eggshells dosage on the
for the first 80 minute as a result of available
binding sites on the eggshells, while the removal percent
adsorption of Cd (II) was less than Cu(II). The
adsorption reached equilibrium within 90 minute The maximum removal was obtained at the
where the removal percent reached 61% and 53% adsorbent dose of 0.4 and 0.5 g for Cu (II) and Cd
for Cu(II) and Cd(II), respectively. The period of (II), respectively. Where further increase in the
90 minute was therefore used for the adsorption quantity of the adsorbent more than (0.4 and 0.5)g
of Cu (II) and Cd (II) by eggshells. The initial fast had no more effect on the adsorption rate for Cu
removal occurs due to surface adsorption on the (II) and Cd (II), respectively. Therefore, 0.4 and
adsorbent. The subsequent slow phase occurs due 0.5 g of the adsorbent was sufficient to adsorb

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 NUCEJ Vol.91 No.2, 2016 Ali et al., pp.186 - 193

maximum quantity of ions and also the percent which promotes effective transfer of contaminants
removal of Cu (II) was more than that of Cd (II). to the eggshells sites.
Also the removal efficiency is associated with the
Co=50 m g/L, pH=6, t=90 m in
adsorbent dose due to the availability of more 100
adsorbing sites at higher doses.
80

4.4. Effect of Initial Metal

Removal %
60

Concentration 40
The effect of initial Cu (II) and Cd (II)
20 Cu, eggshell dosage=0.4 g/50 mL
concentration on the adsorption of these Cd, eggshell dosage=0.5 g/50 mL
contaminants onto eggshells is shown in Figure 4. 0
0 50 100 150 200 250
It could be seen that the removal percent of Cu Agitation speed (rpm )
(II) decreased from 98% to 76% with the increase
in initial concentration from 50 to 100 mg/L, Figure 5: Effect of agitation speed on the
while this value decreased from 95% to 69% with removal percent.
the same range of increase in the value of initial
concentration for Cd (II). This means that the 4.6. Effect of temperature
amount of these contaminants sorbed per unit The extent of Cu (II) and Cd (II) adsorption on
mass of adsorbent decreased with the increase in the eggshells at various temperatures is shown in
initial concentration. This plateau represents Figures (6) and (7).
saturation of the active sites available on the
eggshells samples for interaction with Co=50 m g/L, dose=0.25g/50m L, pH=6,
contaminants, indicating that less favorable sites 100
agitation speed=250 rpm

became involved in the process with increasing

80
concentration [15].
Removal %

60

T=20 C
40
T=30 C

20 T=40 C
T=50 C
0
0 10 20 30 40 50 60 70 80 90
Tim e (m in)

Figure 6: Effect of temperature on the

removal percent of Cu (II).
Co=50 m g/L, dose=0.25g/50m L, pH=6,
agitation speed=250 rpm
Figure 4: Effect of initial metal 100

concentration on the removal percent. 80

Removal %

60
4.5. Effect of agitation speed T=20 C
40
The effect of agitation speed on the removal T=30 C
T=40 C
percent of Cu (II) and Cd (II) was studied by 20
T=50 C
varying the speed of agitation from 0 to 250 rpm 0
0 10 20 30 40 50 60 70 80 90
and keeping other parameters equal to the best
Tim e (m in)
obtained from the previous steps. Figure 5 shows
that about 7.5% and 5% of the Cu (II) and Cd (II), Figure 7: Effect of temperature on the
respectively, were removed before shaking and removal percent of Cd (II).
the uptake increases with the increase in shaking
rate. However, there was an increase in As observed from the figures, temperature
contaminants uptake when agitation speed was rises resultes in an increase in the removal a
increased from zero to 250 rpm at which about percentage of the metals ions. The enhancement
100% of Cu (II) and Cd (II) were removed. These of the adsorption capacity when temperature is
results can be associated to the fact that the increased is due to increased mobility and
increase in the agitation speed improves the diffusion of the ionic species. The adsorption
diffusion of contaminant towards the surface of experiment could be regarded as a heterogeneous
the reactive media (eggshells). Thus, proper and reversible process at equilibrium. The
contact is developed between contaminants in the apparent equilibrium constant for the process is
solution and the binding sites on the eggshells, shown to be:
Kc = (Co - Ce)/Ce … (6)

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The Gibbs free energy of the adsorption process

[16] is: Cu(II)
0
-1
ΔG° = - RT In Kc … (7)

Gibbs free energy

-2
-3 y = -0.1222x + 31.738

(KJ/mol)
o
where ΔG is the standard Gibbs free energy -4 R2 = 0.9242

change for the adsorption process (J mol-1); R the -5

-6
universal gas constant (8.314 J mol-1K-1), while T -7
-8
is the temperature (K). The effect of temperature -9
on the adsorption of Cu (II) and Cd (II) by 283 293 303 313 323 333
Tem perature (K)
eggshell is listed in Table (1).

Table 1: Gibbs free energy values obtained Figure 8: The Gibbs free energy plot for the
from the adsorption of Cu (II) and adsorption of Cu(II) using eggshell.
Cd (II) using eggshell
Cd(II)
Temperature ΔGo (KJ mol-1K-1 ) 0
(K) -0.5
-1
Cu (II) Cd (II)

Gibbs free energy

-1.5 y = -0.0514x + 12.996

(KJ/mol)
-2 R2 = 0.9902
293 -4.03 -2.06 -2.5
303 -5.02 -2.63 -3
-3.5
313 -7.16 -3.00 -4
323 -7.39 -3.65 -4.5
-5
283 293 303 313 323 333

The free energy change (ΔGo) obtained for the Tem perature (K)
adsorption of Cu (II) and Cd (II) at 293 K, initial
concentration of 50 mg/L, and pH = 6 is (-4.03
Figure 9: The Gibbs free energy plot for the
and -2.06)kJ mol-1 for Cu (II) and Cd (II) ,
respectively. The negative value of (ΔGo) adsorption of Cd(II) using eggshell.
obtained for the adsorption of Cu (II) and Cd (II)
onto eggshells shows spontaneity of the 4.7 Kinetic study
adsorption process at that temperature. However, It is clear from Figures (10, 11, 12 and 13)
the result in Table (1) shows that the free energy and Table (2) that the reactions for Cu (II) and Cd
values for the two contaminants decreases with (II) are not likely to be first order because of the
increasing temperature. This implies that the value of qe (experimental) does not equal to the
spontaneity of the adsorption process increases value of qe (theoretical), irrespective of the
with increasing the temperature. Consequently, magnitude of the correlation coefficient, while the
the adsorption of the Cu (II) and Cd (II) using values of qe (experimental) and qe (theoretical) are
eggshells as adsorbent is endothermic hence the very close with higher value of correlation
process is better carried out at kindly high coefficient in case of second - order, therefore the
temperature. From thermodynamics: adsorption processes followed well pseudo
second- order kinetics for the two contaminants.
ΔGo = ΔH -TΔS … (8)
Or Pseudo first order, Cu(II)
ΔGo = - ΔS (T) + ΔH … (9) 1

A plot of temperature against ΔGo gives a 0.8

y = -0.0221x + 1.0895
straight line with slope ΔSo and an intercept of 0.6
R2 = 0.9678
Log(qe-qt)

0.4
ΔH. In (Figures 8 and 9) the slopes are (0.1222 0.2
and 0.0514) kJ/mol for Cu (II) and Cd (II), 0
respectively. Therefore, the values of the entropy -0.2
are (0.1222 and 0.0514) kJ/mol and enthalpy are -0.4
(31.738 and 12.996) kJ/mol for Cu (II) and Cd 0 10 20 30 40 50 60 70
Tim e (m in)
(II), respectively.
Figure 10: Pseudo-first order for Cu (II).

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Pseudo second order, Cu(II) Pseudo second order, Cd(II)

10
12
9 11
8 10
7 9
8
6 7
t/qe

t/qe
6
4 5 y = 0.1376x + 2.4378
y = 0.1163x + 1.8689 4
3
R2 = 0.9838 3 R2 = 0.9789
2 2
1 1
0 0
0 10 20 30 40 50 60 70 0 10 20 30 40 50 60 70
Tim e (m in) Tim e (m in)

Figure11:Pseudo-second order for Cu (II). Figure 13: Pseudo-second order for Cd

Pseudo first order, Cd(II)
(II).
1
0.8
y = -0.0225x + 1.0451
0.6
R2 = 0.9474
Log(qe-qt)

0.4
0.2
0
-0.2
-0.4
-0.6
0 10 20 30 40 50 60 70
Tim e (m in)

Figure 12: Pseudo-first order for Cd (II).

Table 2: Constants of pseudo-first and second order
Adsorbent qe(mg/g),Exp. pseudo-first-order pseudo-second- order

K1, (min)-1 0.0508 K2 ,(mg.g-1min-1) 0.0072

Cu (II) 8.40
qe, (mg/g) 12.28 qe, (mg/g) 8.59
R2 0.9678 R2 0.9838
-1 K2 ,(mg.g-1min-1) 0.0077
K1, (min) 0.0518 qe, (mg/g) 11.09
qe, (mg/g) 7.2600
Cd (II) 7.01 R2 0.9474
R2 0.9789

4.8 FTIR analysis of eggshells

The Fourier transfer infrared spectroscopy (a)
(FTIR) analysis has been considered as a kind of
direct mean for identifying the characteristic
functional groups on the surface of the eggshell,
which are responsible for adsorption of metal ions
[17]. The FTIR spectrum of eggshell powder was
recorded to obtain the information regarding the Bold curve=Before Cu(II) loaded
Normal Curve= After Cu(II) loaded
stretching and bending vibrations of these
functional groups. The FTIR spectra of eggshell
powder before and after Cu (II) and Cd (II)
adsorption are shown in Fig.14. The FTIR
spectral analysis of eggshell powder shows (b)
distinct peak at 713.66, 875.68, 1419.61, 2515.18,
2912.5 and 3410.15 (1/cm). The peak observed at
3410.15 (1/cm) may be assigned to the presence
of alcohol hydroxyl group (-OH) stretching. This
result suggests that Cu (II) and Cd (II) interact
with metal oxides and -OH functional group
present in the eggshell powder. Bold curve=Before Cd(II) loaded
Normal Curve= After Cd(II) loaded

Figure 14: FTIR spectrum of eggshell

powder before and after loaded of (a) Cu (II),
and (b) Cd (II).

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5. Conclusion [8 ]Rohaizar N. A., Hadi N. A., Sien W. C.,

The potential use of eggshells as an adsorbent (2013). "Removal of Cu(II) from water by
for Cu (II) and Cd (II) was studied. It was found adsorption on chicken eggshell.",
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maximum adsorption capacities for Cu (II) and [9] Animesh A., (2013). "Removal of Cu and Pb
Cd (II) were 8.4 mg/g and 7.01mg/g, respectively. from aqueous solution by using eggshell as an
The percentage removal was strongly dependent adsorbent.", International Journal of Research
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‫مسحوق قشر البيض كمادة ممتزة ألزالة أيونات النحاس والكادميوم من المحلول‬
‫المائي‪ :‬دراسة الموازنة‪ ،‬الحركية والديناميكية الحرارية‬

‫هدى مهدي مظلوم‬ ‫محمد عبدالخالق ابراهيم‬ ‫زياد طارق عبد علي‬
‫قسم الهندسة المدنٌة‬ ‫قسم الهندسة المدنٌة‬ ‫قسم الهندسة البٌئٌة‬
‫كلٌة الهندسة‪/‬الجامعة المستنصرٌة‬ ‫كلٌة الهندسة‪/‬جامعة النهرٌن‬ ‫كلٌة الهندسة‪/‬جامعة بغداد‬

‫الخالصة‪:‬‬
‫تم التحقق فً هذا البحث من استخدام قشور البٌض كمادة ممتزة المتزاز اٌونات النحاس والكادمٌوم‪ .‬وتم دراسة تاثٌر‬
‫عدة عوامل منها زمن التوازن‪ ,‬الدالة الحامضٌه االبتدائٌه للمحلول‪ ,‬كمٌة الماده الممتزه‪ ,‬التركٌز االبتدائى‪ ,‬سرعة‬
‫الرج‪ ,‬باالضافه الى درجه الحراره‪ .‬وكان الحد االعلى لسعة االمتزاز )‪ (8.4mg/g‬و)‪ (7.01mg/g‬الٌونات‬
‫النحاس والكادمٌوم على التوالً‪ .‬كذلك تم حساب بعض العوامل الثرمودٌنامٌكٌة مثل ‪Gibbs free energy‬‬
‫‪ Entropy, Enthalpy‬وقد اشارت هذه العوامل بان عملٌة االمتزاز هً عملٌه ثرمودٌنامٌكٌا تلقائٌة وماصه‬
‫للحرارة ‪ .‬النتائج العملٌه اشارت اٌضا بان عملٌه االدزوربشن تتبع ل " ‪" pseudo second- order kinetics‬‬
‫‪ .‬واخٌرا تم اجراء فحص ‪ FTIR‬الذي اشار بوجود تداخل بٌن اٌونات النحاس والكادمٌوم مع اكاسٌد المعادن‬
‫والمجموعه الفعالة (‪ )-OH‬الموجوده فً قشور البٌض‪.‬‬

‫‪911‬‬