Journal of Saudi Chemical Society (2015) xxx, xxx–xxx

King Saud University

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ORIGINAL ARTICLE

Calcium hydroxide as low cost adsorbent for the

effective removal of indigo carmine dye in water
Thimmasandra Narayan Ramesh *, Devarahosahally Veeranna Kirana,
Ashwathaiah Ashwini, T.R. Manasa

Department of Studies and Research in Chemistry and Prof. C. N. R. Rao Centre for Advanced Materials,
Tumkur University, Tumkur 572 103, India

Received 14 December 2014; revised 28 February 2015; accepted 2 March 2015

KEYWORDS Abstract Adsorption of indigo carmine dye onto calcium hydroxide was investigated in this work.
Adsorption; The variation in the pH, adsorbent dose, dye concentration, duration and the temperature was eval-
Indigo carmine; uated. Adsorption of indigo carmine dye onto calcium hydroxide was effective at pH 12 (50 min)
Calcium hydroxide; and follows Langmuir-type isotherm behaviour. The adsorption process follows pseudo-second
Isotherms; order rate kinetics. Enthalpy, entropy, free energy and the activation energy parameters have been
Kinetics; reported.
Dye ª 2015 The Authors. Production and hosting by Elsevier B.V. on behalf of King Saud University. This is
an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction photovoltaics, leather processing and tanning industries utilize

Several million tons of different types of synthetic dyes are
manufactured every year across the world [1,2]. The character-
istic features of the synthetic dyes can be altered by substitut-
ing a suitable functional group to the dye [3]. Dyes have been
classified into azo dyes, phthalocyanine dyes, VAT dyes (which
bind the substrate in basic medium), cationic dyes and anionic
dyes (which attain the charge in aqueous medium), insoluble
dispersive dyes, reactive dyes, indigoid dyes etc. Textile, paper
and pulp, food processing and technology, dye sensitized
* Corresponding author. Tel.: +91 0816 2260220.
E-mail address: adityaramesh77@yahoo.com (T.N. Ramesh).
Peer review under responsibility of King Saud University.
Production and hosting by Elsevier
large quantities of synthetic organic dyes as colourants [4–8].
During the synthesis and application of dyes, large quantities
of untreated dyes are discharged into the environment.
Indigo carmine is one of the most common dyes used in textile,
medical and pharmaceutical applications [9,10]. Discharge of
indigo carmine into the environment is hazardous and causes
skin related diseases, affects the cornea and exhibits cytotoxi-
city [11–13]. It has been found that a majority of the dyes can-
not be practically treated effectively prior to their release into
the environment. Traditional methods to treat the water were
found to be ineffective due to the complex nature of the dyes
and their reactivity [14]. Several methods and techniques have
been developed for the treatment of dye effluents. Chemical,
biological and physical methods have been developed [15–
18]. The chemical methods involve precipitation, oxidation,
chemisorption, and photocatalysis [11,12,19,20].
Even though the efficiency of the chemical methods is high,
scalability is a major hurdle. Biological methods involve

http://dx.doi.org/10.1016/j.jscs.2015.03.001
1319-6103 ª 2015 The Authors. Production and hosting by Elsevier B.V. on behalf of King Saud University.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Please cite this article in press as: T.N. Ramesh et al., Calcium hydroxide as low cost adsorbent for the effective removal of indigo carmine dye in water, Journal of
Saudi Chemical Society (2015), http://dx.doi.org/10.1016/j.jscs.2015.03.001
2 T.N. Ramesh et al.
microorganisms, fungi and enzymes for the degradation and
decolourization of dyes [21]. Bulk methods have also been
employed for the removal of indigo carmine dye in waste water
[22]. Electrocoagulation, electroflocculation, electrochemical
precipitation routes have also been employed but they are
energy intensive [23–25]. When compared to the above meth-
ods, physical methods of treatment of dyes were found to be
economically and technologically simple and easy to handle.
Adsorption is one such method in which synthetic dyes will
adsorb onto the solid substrate during the treatment of dyes.
Metal oxides, agrowaste, chitosan, cross-linked polymers, zeo-
lite, coal fly ash, alumina, calcium oxide, cynodon dactylon
have been used as adsorbents for the removal of indigo car-
mine dye [13,26–28]. Agrowaste is one of the cheap materials
which is abundantly available that can be used to treat indigo
carmine dye but its adsorption efficiency is poor [29]. It is
desirable for any adsorbent to be cheaper, easy to handle,
environmentally benign, possess high greater affinity for the
dyes, highly efficient and regenerative. There is no universal
adsorbent, which can be used for the effective removal of dif-
ferent types of dyes. Recently we had reported the removal of
indigo carmine using magnesium oxide as an adsorbent and
the efficiency is more than 90% [30]. This promotes us to
explore new adsorbent i.e. calcium hydroxide for the removal
of indigo carmine dye. In this work, we used calcium hydrox-
ide as a low cost adsorbent to examine its effectiveness on the
adsorption of indigo carmine dye by varying different parame-
ters such as pH, dose, concentration, temperature and anal-
ysed the nature of adsorption process.
2. Experimental section
Calcium hydroxide and indigo carmine dye were purchased
from SD-Fine Chemicals, India and used without purification.
2.1. Preparation of indigo carmine dye solution
Indigo carmine dye stock solution was prepared by dissolving
50 mg of indigo carmine dye in 1000 mL of distilled water. A
series of dye concentrations in the range of 1.0721 · 105 M
to 1.0721 · 104 M or 0.50 mg to 5.0 mg/100 mL were further
prepared by transferring 10 mL, 20 mL, 30 mL, 40 mL, 50 mL
and 100 mL of the dye solution into a standard flask followed
by dilution to 100 mL using distilled water. The pH of the
indigo carmine dye solution was adjusted using either 1 M
HCl or 1 M NaOH (pH = 3, pH = 6, pH = 9, pH = 12) to
test the effect of pH on the adsorption of dye on calcium
hydroxide.
2.2. Adsorption measurements
Kinetic experiments for the adsorption of indigo carmine dye
solution on calcium hydroxide was carried out by adding
0.1 g of calcium hydroxide in 100 mL of indigo carmine solu-
tion of known concentration (5 mg/100 mL) at room tempera-
ture (25–28 C).
The effect of temperature on the adsorption of indigo car-
mine dye solutions (at different pH, dosage 0.1 g) was mea-
sured. The effect of temperature as a function of time (10,
20, 30, 40, 50 min) on the dye removal was also examined at
a predetermined equilibrium conditions i.e. pH = 12, dose of
Please cite this article in press as: T.N. Ramesh et al., Calcium hydroxide as low cost adsorbent for the effective removal of indigo carmine dye in water, Journal of
Saudi Chemical Society (2015), http://dx.doi.org/10.1016/j.jscs.2015.03.001
calcium hydroxide 0.1 g. The duration at which equilibrium
state is attained was estimated to determine the effectiveness.
The maximum absorption was observed at 600 nm and the
entire adsorption measurements were performed at 600 nm.
Batch experiments were performed by varying the adsorption
conditions. Concentrations of the dye solutions after adsorp-
tion were monitored using colorimeter (CL-63 model).
2.3. Adsorption isotherms
Batch adsorption isotherm studies were conducted to deter-
mine the different adsorption isotherm models. The adequacy
of the different models will be evaluated to determine the
adsorption process. For adsorption isotherms, indigo carmine
solutions of different concentrations ranging from 0.5 to
5 mg/L (1.0721 · 105 M to 1.0721 · 104 M) were examined
by adding different quantities of calcium hydroxide (0.025 g,
0.05 g, 0.075 g, 0.1 g).
Calcium hydroxide sample was characterized using a
Bruker D-8 Advanced X-ray powder diffractometer with Cu
Ka = 1.5418 Å, scan rate 2 min1 (steps: 0.02); scan range
of 10–55.
The crystallinity of the sample was examined by comparing
the data with the international centre for diffraction data.
Elico CL-63 colorimeter was used for the measurements. The
filters used for the measurements is kmax = 600 nm up to pH
12 (blue colour). At pH 13, the solution of indigo carmine
dye will exhibit yellow colour.
3. Results and discussion
The structure of indigo carmine dye (C16H8N2Na2O8S2) is
shown in Fig. 1. The reflections in the powder X-ray diffrac-
tion pattern of calcium hydroxide was indexed to hexagonal
system with the space group P-3m1 (see Supplementary
Fig. 1). The average crystallite size of calcium hydroxide was
calculated using Scherrer formula and is in the range of 30–
50 nm [31]. The relativity involving the removal of indigo car-
mine as a function of pH, dye concentration, temperature and
time with the adsorbents was considered to validate the rate of
dye removal.
3.1. Effect of pH
The effect of initial pH of dye solution on the percentage of
removal of alizarin red was investigated by maintaining the
solution pHs at 3, 6, 9 and 12 and the data are shown in
Fig. 2. It has been observed that adsorption of indigo carmine
on calcium hydroxide is maximum at pH 12.
Figure 1 Structure of indigo carmine dye.
Calcium hydroxide as adsorbent for dye removal
Figure 2 Effect of pH variation as a function of adsorption.
3.2. Adsorbent dose
Fig. 3 shows the effect of adsorption of indigo carmine dye as a
function of an increase in the dosage of calcium hydroxide.
The equilibrium adsorption capacity (qe – mol/g) was calcu-
lated and the adsorption was maximum when 0.1 g of calcium
hydroxide was used at pH 12, 0.1 g of calcium hydroxide was
used for all future studies.
3.3. Dye concentration
0.5–5 mg/100 mL of dye concentrations was varied as a func-
tion of time at pH 12 (298 K). The equilibrium adsorption
(qe – mol/g) has been estimated and the results are shown in
Fig. 4. The effect of temperature on the adsorption capacity
of indigo carmine dye at different concentrations has also been
shown (see Fig. 4). The adsorption is found to increase linearly
with the increase in temperature.
Figure 3 Variation of adsorbent dosage.
Please cite this article in press as: T.N. Ramesh et al., Calcium hydroxide as low cost adsorbent for the effective removal of indigo carmine dye in water, Journal of
Saudi Chemical Society (2015), http://dx.doi.org/10.1016/j.jscs.2015.03.001
3
Figure 4 Effect of concentration as a function of % of
adsorption.
3.4. Effect of duration
Adsorption of indigo carmine on calcium hydroxide at differ-
ent contact times was examined by adding 0.025 g, 0.05 g,
0.075 g and 0.1 g of adsorbent to indigo carmine dye solution
(5 mg/100 mL). Adsorption at different temperatures such as
298 K, 313 K, 323 K and 333 K was measured for 50 min
duration. Fig. 5 shows the effect of duration or contact time
on the adsorption of indigo carmine on calcium hydroxide.
3.5. Effect of temperature
Fig. 6 shows the effect of temperature such as 298 K, 313 K,
323 K and 333 K on the adsorption process. It was found that
at 333 K, the adsorption is maximum (pH = 12). Adsorption
also increases with the increase in temperature indicating that
the reaction is endothermic in nature. The equilibrium adsorp-
tion capacity (qe – mol/g) with equilibrium concentration of
Figure 5 Effect of duration on the adsorption of indigo carmine
dye on calcium hydroxide.
4 T.N. Ramesh et al.

temperature on the adsorption equilibrium constant (Ka) have

been calculated. The parameter-KR (dimensional separation
factor) provides information about the adsorption of dye solu-
tion onto adsorbate and its favourability. When (i) KR = 1,
the process of adsorption is linear; (ii) KR > 1, process of
adsorption is unfavourable; (iii) KR = 0, process of adsorption
is irreversible; (iv) 0 < KR < 1, process of adsorption is
favourable. The effect of temperature on the correlation coeffi-
cient (r/R2) and the dimensional separation factor (KR) has
been estimated.

3.6. Different types of adsorption isotherms-data analyses

We have evaluated different models to understand the nature

Figure 6 Effect of temperature on the adsorption of indigo
carmine on calcium hydroxide.
the dye solution (Ce – mg/100 L) has been examined with
change in the concentrations of indigo carmine dye solutions
after equilibrating with calcium hydroxide.
The adsorption of indigo carmine dye adsorption on cal-
cium hydroxide at 298 K, 313 K, 323 K and 333 K was calcu-
lated and for 333 K is shown in Table 1 (maintained at
pH = 12; adsorbent dose: 0.1 g).
Correlation coefficient (r or R2) for the adsorption of indigo
carmine dye on calcium hydroxide was calculated at different
temperatures [28]. To get an insight into the process of adsorp-
tion, thermodynamic and kinetic factors have been evaluated.
The nature of adsorbent and their interaction with the adsor-
bate, rate of adsorption, chemical kinetics, rate of the reaction
etc., were determined. The Pearson correlation coefficient
(r/R2) values approach unity at higher temperatures indicating
that the adsorption is more favourable at higher temperatures.
The rate constant can be calculated using the equation:
2:303 Co
k¼ log
t Ct
where,
Co = initial concentration of the dye solution (mg/L),
Ce = equilibrium concentration of the dye solution (mg/L),
t = time in minutes, and,
k = rate constant (min1).
The kinetic constant (K min1) for the adsorption of indigo
carmine dye on calcium hydroxide and the effect of
of adsorption of dye onto the adsorbent [28,32]. Langmuir
isotherm, Freudlich isotherm, Temkin isotherm, Harkin–Jura
isotherm, Halsey isotherm and Redlich–Peterson isotherms
models were used to analyse the adsorption data of indigo
carmine dye on calcium hydroxide. The details of the different
isotherm models are as follows:
3.6.1. Langmuir isotherm
Langmuir adsorption isotherm can be estimated by plotting a
graph of Ce/qe vs Ce (mg/100 mL). If the points are joined with
a straight line then slope provides information about 1/Qo and
intercept on 1/Qob. From the data, we can predict that the
adsorption of indigo carmine onto calcium hydroxide is of
monolayer type [33].
3.6.2. Freundlich isotherm
Freundlich isotherm model is generally used for multilayer
adsorption between the interaction between adsorbate and
adsorbent [33–35]. A plot of log qe vs log Ce should be a
straight line with a slope 1/n and intercept on log kA, if the
adsorption follows Freundlich isotherm. Constant ‘n’ is a
dimensional quantity providing information about the inten-
sity of adsorption (see Supplementary information Fig. S-2).
(i) If the values of ‘n’ are in the range 0.1 < n < 0.5, it indi-
cates that good adsorption is possible, (ii) If 0.5 < n < 1 mod-
erate adsorption takes place, while n > 1 indicates it to be of
weak adsorption [36].
3.6.3. Temkin isotherm
The plot of lnCe vs qe, should be a straight line with a slope
1/kT and intercept on bT
kT
. The data indicate that it is not linear
fit, thus Temkin isotherm cannot be applied for the adsorption
of indigo carmine onto calcium hydroxide.

Table 1 Parameters calculated for the Indigo carmine dye on calcium hydroxide at 333 K (pH = 12): (duration: 50 min) used for
isothermal analyses.
C0 Ce qe (mol/g) Ce/qe 1/qe 1/Ce log Ce log qe lnCe lnqe qe/Ce log Ce/qe %
(mg/100 mL) (mg/100 mL) adsorption
0.50 0.15 0.343 0.456 2.91 6.38 1.301(6) 0.345(1) 3.030(3) 0.794(2) 9.3519 0.9710 90.33
1.00 0. 21 0.782 0.277 1.277 4.59 1.061(9) 0.039(3) 2.445(3) 0.090(6) 10.534 1.022(7) 91.33
1.50 0.29 1.205 0.243 0.829 3.40 0.980(8) 0.144(7) 2.258(5) 0.333 13.3540 1.126(0) 93.03
2.00 0.36 1.631 0.225 0.612 2.71 0.933(3) 0.274(9) 2.149 0.633 16.152(6) 1.208(3) 95.17
2.50 0.38 2.11 0.179 0.471 2.628 0.814(3) 0.376(2) 2.105(3) 0.866(3) 19.525(4) 1.290(7) 96.32
5.00 0.65 4.34 0.151 0.230 1.516(3) 0.871(2) 0.687(1) 2.006(1) 1.582(1) 36.174(7) 1.559 97.31

Please cite this article in press as: T.N. Ramesh et al., Calcium hydroxide as low cost adsorbent for the effective removal of indigo carmine dye in water, Journal of
Saudi Chemical Society (2015), http://dx.doi.org/10.1016/j.jscs.2015.03.001
Calcium hydroxide as adsorbent for dye removal 5

3.6.4. Harkin–Jura isotherm
The plot of lnCe vs 1/qe, should be a straight line for a mono-
layer adsorption. The data fit better indicating that the mono-
layer adsorption of indigo carmine onto calcium hydroxide is
favoured.
3.6.5. Halsey isotherm
The plot of lnCe vs lnqe, should be a straight line with a slope
‘n’ and intercept lnK. Importance is that this model fits well for
the multilayer adsorption method. The data are non-linear in
nature ruling out the possible occurrence of multi-layer
adsorption.
3.6.6. Redlich–Peterson isotherm
The importance of Redlich–Peterson isotherm is that it com-
bines Langmuir and Freundlich isotherms. The plot of lnCe
 log Ce/qe, should be a straight line with a slope
vs
KR þ log Cqee (see Supplementary information Fig. S-4).
The various fitting parameters and their values used in the
graph and equations to derive information for different types
of isotherms are estimated and the values are given in Table 2.
The correlation coefficients for different isotherm models
and the equations were used to calculate the R/r value.
Based on the correlation coefficient (R2) value, different
types of adsorption isotherm fits are arranged in the following
order: Halsey isotherm, < (0.3022), < Harkin–Jura Isotherm
(0.3249), < Temkin isotherm (0.7411) < Redlich–Peterson
isotherm (0.8430) < Freundlich isotherm (0.9326) < Langmuir
isotherm (0.9724). R2 value of Harkin–Jura isotherm and
Halsey isotherm is low indicating that adsorption follows
monolayer adsorption.
3.6.7. Kinetics of adsorption process
Different types of kinetic models were investigated to evaluate
the adsorption of indigo carmine dye onto calcium hydroxide.
The pseudo-first order and pseudo-second order rate equations
were most commonly used to verify the experimental data
[37,38]. The negatively charged indigo carmine dye will interact
with calcium hydroxide (which is also a basic oxide).
‘qe’ value (mol/g) does not agree with the calculated ‘qe’ (mol/g)
plot, indicating that the pseudo-first order model does not fit
well with the adsorption of indigo carmine onto calcium
hydroxide. Also the r = 0.9364 indicates that it is not
pseudo-first order reaction.
Pseudo-first order equation has been effectively applied for
explaining the rate of the adsorption of methylene blue and
other dyes on low cost adsorbents.
3.6.7.2. Pseudo-second-order rate equation. If the adsorption
involves chemical interaction/bonding due to charge transfer
process between the adsorbent and adsorbate then pseudo-sec-
ond order rate equation should be considered [39]. The graph
fits well with a straight line, indicating that the adsorption pro-
cess is a pseudo-second order process (see Fig. 7). The value of
r/R2 was calculated using the equation:
P P P
n t log qtt  t qtt
r ¼ sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
h P P i P 2  P h i2
n t2  ðtÞ2 n qt  q
t
t t
The calculated r or R2 value is 0.9999 indicating that
adsorption follows pseudo-second order. The experimental
(4.8655) and calculated qe values (mol/g) (4.8850) are closer
indicating that the adsorption could be of pseudo-second order
in nature.
3.6.8. Thermodynamic parameters
The free energy change-DG (kJ mol1), enthalpy-DH
(kJ mol1) and entropy-DS (kJ mol1 K1) for the adsorption
process of indigo carmine onto calcium hydroxide was esti-
mated using equilibrium constant Ka values (Table 3).
The negative free energy values indicate that adsorption
process occurs spontaneously and the free energy values
increase at higher temperatures indicating that the adsorption
of indigo carmine onto calcium hydroxide is endothermic. The
adsorption process is more favourable at higher temperatures.
The estimated activation energy (Ea) for the adsorption of
indigo carmine dye on calcium hydroxide was found to be
71.5936 kJ mol1.

3.6.7.1. Pseudo-first order. Value of k1 was calculated by plot-

ting a graph of log (qe  qt) versus ‘t’ (min) to evaluate the data
for pseudo-first order rate equation. The intercept of the
straight line should be equal to log (qt) [39]. The experimental

Table 2 Summary of the data analysed for different types of

isotherms.
Isotherm Parameters
Langmuir b (L/mol) 5.720(8)
Qo (mg/g) 0.9500
R2 0.972(4)
Harkin–Jura A 0.512(8)
B 1.89
R2 0.324(9)
Halsey isotherm N 0.184(2)
K 2.331(8)
R2 0.302(2)
Figure 7 Pseudo second order kinetics fit.

Please cite this article in press as: T.N. Ramesh et al., Calcium hydroxide as low cost adsorbent for the effective removal of indigo carmine dye in water, Journal of
Saudi Chemical Society (2015), http://dx.doi.org/10.1016/j.jscs.2015.03.001
6 T.N. Ramesh et al.
Table 3 Thermodynamic parameters for adsorption of Amido black 10B.
Adsorbent Temperature (K)
Alizarin red 298
313
323
333
Figure 8 Schematic representation of mechanism of interaction
of indigo carmine and calcium hydroxide.
Several factors affect the adsorption of dye onto the
adsorbent. The nature of functional groups (hydrophobic/
hydrophilic) present on the surface of the adsorbent i.e. cal-
cium hydroxide, hydrogen bonding and electrostatic attrac-
tions, Indigo carmine acts as redox as well as pH indicator.
At pH > 12, Indigo carmine dye exhibits intra-molecular
hydrogen bonding network between the C‚O and NAH
within the molecule. The hydrogen bonds weaken the NAH
bond in the sulphonated indigo carmine dye which results in
the strong binding of the NAH group to OH groups of cal-
cium hydroxide thus resulting in the colour change. The results
also demonstrate that monolayer chemical adsorption occurs.
The increase in the adsorption with the increase in the pH is
due to the electrostatic force of attractions between the func-
tional groups of the indigo carmine dye and calcium hydroxide
and the mechanism is schematically shown in Fig. 8.
4. Conclusions
Different types of adsorption isotherm models for the
adsorption of indigo carmine dye on calcium hydroxide were
examined to understand the nature of interaction between
the adsorbent and adsorbate. The thermodynamic parame-
ters such as free energy, entropy, enthalpy and activation
energy (Ea = 71.59 · 103 kJ mol1) estimated during the
adsorption of indigo carmine dye on calcium hydroxide.
The optimum conditions for the effective removal of indigo
carmine dye solution using calcium hydroxide as an adsor-
bent are:
Please cite this article in press as: T.N. Ramesh et al., Calcium hydroxide as low cost adsorbent for the effective removal of indigo carmine dye in water, Journal of
Saudi Chemical Society (2015), http://dx.doi.org/10.1016/j.jscs.2015.03.001
DG (kJ mol1) DH (kJ mol1) DS (kJ mol1 K1)
1.96 1.35 0.246
7.38
8.128
9.481
(i) 0.1 g of calcium hydroxide,
(ii) Effective pH for dye removal is 12,
(iii) Maximum alizarin red S dye concentration used was
5.0 mg/100 mL,
(iv) Temperature: 333 K and,
(v) Contact time is 50 min.
The results demonstrate that the process of adsorption is
endothermic, spontaneous (at higher temperatures).
Monolayer adsorption occurs during the adsorption of indigo
carmine onto calcium hydroxide and follows pseudo-second
order kinetics. Therefore calcium hydroxide can be used as
an effective low cost adsorbent for the removal of indigo car-
mine dye.
Acknowledgements
Authors gratefully thank Tumkur University for facilities and
Vision Group of Science and Technology (VGGST-SPiCE
program 2011-12) for financial support.
Appendix A. Supplementary data
Supplementary data associated with this article can be found,
in the online version, at http://dx.doi.org/10.1016/j.jscs.2015.
03.001.
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