ORIGINAL ARTICLE

Cu(II) adsorption from aqueous solution using red mud activated
by chemical and thermal treatment

Fabiano T. da Conceição1
• Beatriz C. Pichinelli2 • Mariana S. G. Silva2

•

Rodrigo Braga Moruzzi1 • Amauri Antonio Menegário3
• Maria Lucia Pereira Antunes4

Received: 24 February 2015 / Accepted: 20 August 2015 / Published online: 22 February 2016

� Springer-Verlag Berlin Heidelberg 2016

Abstract Brazil is the third-largest producer of alu-

minium, with the red mud generated during the extraction of

aluminium from bauxite through the Bayer process. The red

mud has been studied for use as an adsorbent for removing of

elements/compounds from wastewater and/or contaminated

soil. However, there are several compounds and treatments

that were not tested yet. In this study, the Cu(II) adsorption

potential for natural red mud (NRN) and red mud activated

by thermal treatment at 400 �C (TRM) and chemical treat-

ment with hydrochloric acid (HCl) at 0.05 mol L-1 (CRM1)

and calcium nitrate [Ca(NO3)2] 0.1 mol L-1 (CRM2) was

evaluated using adsorption isotherms obtained by the

Langmuir and Freundlich models. The NRM and TRM

presented Cu(II) adsorptions of ca. 100 % in aqueous solu-

tion with lower concentrations of the metal (0.5 and

1.0 mmol 25 mL-1). The Langmuir isotherm was more

appropriate to describe the phenomenon of Cu(II) removal

using NRM, TRM, CRM1 and CRM2, with the thermally

activated red mud presenting the highest adsorption capacity

at 2.08 mmol g-1 for Cu(II). Thus, these results indicate that

TRM has the potential for use in applications that treat

effluents and/or contaminated soil from industrial activity.

Keywords Aluminium production � Red mud � Cu(II)
adsorption � Isotherms models

Introduction

Pollution changes the physical, chemical and biological

characteristics of many hydrospheric, atmospheric, bio-

spheric and pedospheric components by interfering with

their quality and preventing their use for human activities.

Depending on the industry, metals can be released in the

environment as emissions, effluents or solid waste. Although

certain metals are biogenetic and essential for living organ-

isms, the majority are accumulative poisons when they are

ingested at higher concentrations than the recommended

values because they undergo biomagnification and have the

potential to cause mutagenic, teratogenic and carcinogenic

effects or even death (Aguiar et al. 2002; Von Sperling

2005); therefore, removing metals are very essential.

The main anthropogenic sources of the metal copper are

mining and casting, burning coal as an energy source and

incinerating waste. Depending on the particle size, com-

pounds that contain copper undergo dry disposal or are

carried by rainwater. The major routes of exposure are

inhalation, food and water ingestion, dermal contact and

oral administration. The ingestion of copper salts causes

vomiting, lethargy, acute haemolytic anaemia, kidney and

liver damage, and even death (Cetesb 2012).

Several methods have been used for the removal of

metals from industrial effluents and contaminated soils,

including precipitation, membrane filtration, ion exchange,

electrolysis and adsorption by activated carbon (Nadaroglu

et al. 2010). However, the economic and technical criteria

are not always achieved. Hence, low-cost methods for

environmental remediation and industrial effluent

& Fabiano T. da Conceição

ftomazini@rc.unesp.br

1 Instituto de Geociências e Ciências Exatas (IGCE), UNESP,

Universidade Estadual Paulista, Avenida 24-A, No. 1515,

Bela Vista, Rio Claro, São Paulo CEP 13506-900, Brazil

2 Faculdade de Engenharia de Bauru (FEB), UNESP,

Universidade Estadual Paulista, Bauru, Brazil

3 Centro de Estudos Ambientais (CEA), UNESP, Universidade

Estadual Paulista, Rio Claro, Brazil

4 UNESP, Universidade Estadual Paulista, Campus

Experimental de Sorocaba, Sorocaba, Brazil

123

Environ Earth Sci (2016) 75:362

DOI 10.1007/s12665-015-4929-y

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treatment that do not change the characteristics of the

environment must be developed.

Currently, the most frequently used technique for metal

removal in the remediation of contaminated soils or treat-

ment of industrial effluents is adsorption because it is more

efficient and easy to use and has a greater variety of pos-

sible low-cost adsorbents. Different industrial wastes are

used as adsorbents for the removal of metals from con-

taminated soils or industrial effluents, and red mud, which

is a by-product of the processing of bauxite, is highlighted

(Nadaroglu et al. 2010).

Red mud is generated in large quantities from the

extraction of aluminium from bauxite through the Bayer

process, and it is disposed in locations referred to as

‘‘disposal lagoons’’. The amount of red mud generated by

such activities is up to twice the amount of alumina pro-

duced. Hence, its disposal requires an extensive area,

which contributes to the increased of cost of the aluminium

production process. Red mud is not classified as hazardous

waste (EPA 2014), but it may cause the contamination of

water springs, produce caustic rains, and harm plants and

animals in the region around the disposal lagoon.

To reuse this industrial waste, red mud in its natural

form or chemically or thermally treated can be used as a

low-cost metal adsorbent. Studies have evaluated the

adsorption of copper by natural red mud (Nadaroglu et al.

2010) and red mud chemically treated with hydrochloric

acid (Apak et al. 1998a; Agrawal et al. 2004) or calcium

sulphate (Lopez et al. 1998). However, no studies have

been produced in Brazil using natural red mud or with

different thermal or chemical activations for the adsorption

of Cu(II) from aqueous solutions.

Thus, the purpose of this study was to evaluate the

Cu(II) adsorption potential for red mud activated with

different treatments from aqueous solution and the results

were modelling by means of Langmuir and Freundlich

isotherms. The natural red mud (NRM) was activated by

thermal treatment at 400 �C (TRM) and by chemical

treatment with hydrochloric acid (HCl) at 0.05 mol L-1

(CRM1) and calcium nitrate [Ca(NO3)2] 0.1 mol L-1

(CRM2), and then characterised by different techniques,

such as pH, electrical conductivity, ion exchange capacity,

specific surface area and mineralogical composition.

Experimental method

Sampling and activation

The red mud samples were collected from an aluminium

production company located in the city of Alumı́nio, near

Sorocaba City in the countryside of São Paulo State, Brazil.

To initiate the activations, all of the NRM samples were

crushed in a porcelain crucible and passed through a

150 lm.

For the thermal treatment, the samples were placed in

porcelain crucibles and heated in a muffle oven at 400 �C
(TRM), where they remained for a period of 2 h. For the

activation with HCl, the NRM samples were mixed with

0.05 mol L-1 HCl (CRM1) at a ratio of 1:25 (g of red mud

per mL of HCl). The beakers with the mixture were agi-

tated for 2 h, and they were then left to rest for the

decantation of activated mud. Then, the supernatant was

removed and distilled water was added to the remaining red

mud; this process was repeated once more to wash the mud.

The remaining mud was dried throughout the night in the

oven at a temperature of 60 �C. Another chemical treat-

ment for NRM was performed with 0.1 mol L-1 Ca(NO3)2
(CRM2), and the same activation procedures described

above for HCl 0.05 mol L-1 were followed.

Characterisation of natural red mud and red mud

with different activations

For the grain-size analysis of the NRM samples, the pro-

cedures described by Klute (1986) were followed. The pH

values and electrical conductivity were determined at a

ratio of 1 g of red mud to 25 mL of distilled and deionised

water. A YSI 556 MultiProbe System (Yellow Springs,

OH, USA) was calibrated to characterise highly pure

standards at pH 4.00 (4.00 ± 0.01 at 25± 0.2 �C) and 7.00

(7.00 ± 0.01 at 25 ± 0.2 �C) and with a standard KCl

solution (1.0 mmol L-1) of known conductivity for 147 lS
cm-1 at 25 �C. The ion exchange capacity (IEC; mmol(?)

kg-1) was obtained with Eq. 1 (Claessen 1997):

IEC ¼ 8� MEDTA � Vbð Þ � MEDTA � Vamð Þ½ � � 106; ð1Þ

where MEDTA = the molar concentration of EDTA (mol

L-1); Vb = the EDTA volume used for the titration of the

blank (L); Vam = the EDTA used for the titration of the

sample (L).

The NRM samples and red mud with different activa-

tions were characterised according to their specific surface

area using nitrogen adsorption curves. The samples were

degasified at 200 �C overnight before analysis. To obtain

the nitrogen adsorption isotherms, a Micromeritics ASAP

Tristar 3000 analyser (Norcross, GA, USA) was operated at

-196 �C. The specific surface areas and grain sizes were

calculated with the mathematical model by Brunauer,

Emmett and Teller (Brunauer et al. 1938). The miner-

alogical analyses were performed by X-ray diffraction in a

Siemens D5000 diffractometer (Erlangen, Germany) with

Cu radiation (WL = 1.542 Å) and a Ni filter. The

goniometer speed was defined as 3� min-1 with an expo-

sure time of 1 s for every 0.05�. An additional method was

used for the mineralogical visualisation and identification

362 Page 2 of 7 Environ Earth Sci (2016) 75:362

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that included scanning electron microscopy coupled with

energy dispersive spectroscopy (SEM–EDS) using an SEM

Field Emission Gun (JSM 6330F, JEOL, Boston, MA,

USA). This technique identified the mineral phases that

occurred at percentages of less than 5 %, which is a lim-

iting factor for X-ray diffraction.

Adsorption studies

The test samples were prepared according to the proce-

dures of Santona et al. (2006). Eight solutions containing

different concentrations of hydrated copper(II) nitrate

(Cu(NO3)2�3H2O) were prepared: 0.5, 1.0, 1.5, 2.0, 2.5,

3.0, 3.5 and 4.0 mmol 25 mL-1. One gram of NRM was

added to each of the solutions, and the same procedures

were performed for the TRM, CRM1 and CRM2. All of the

adsorption tests were performed under conditions of con-

trolled pH during all experiment time, varying from 5.0 to

5.5. The Cu(II) concentrations were quantified by induc-

tively coupled plasma optical emission spectrometry (ICP-

OES) at the Centre for Environmental Studies (Centro de

Estudos Ambientais, CEA) of the State University of São

Paulo (Universidade Estadual Paulista, UNESP) at Rio

Claro. The amount of Cu(II) retained by the adsorbent qe
(mmol g-1) was calculated by the mass balance ratio

presented in Eq. 2. The adsorption percentage (%A) of

Cu(II) was obtained with Eq. 3. All of the Cu(II) analyses

used for the adsorption tests were performed in triplicate

and the average values are reported.

qe ¼
Co � Ceð Þ � V

m
; ð2Þ

%A ¼ ðCo � CeÞ
Co

� 100; ð3Þ

where C0 and Ce = the initial and equilibrium concentra-

tion of Cu(II), respectively (mmol 25 mL-1); V = the

volume of the solution (25 mL); m = the adsorbent mass

(1 g).

Results and discussion

Characterisation of natural red mud and red mud

with different activations

The results obtained for the grain-size fractions of NRM

display variations in the grain size of 49, 42 and 9 % for

clay, silt and sand, respectively. According to the Guide for

the Texture Classes and Guide for Grouping of Texture

Classes (Manual Técnico de Pedologia 2007), the red mud

samples belong to the ‘‘silty clay’’ class. The results

obtained for the parameters pH, electrical conductivity,

IEC and specific surface area characterised for the NRM,

TRM, CRM1 and CRM2 are presented in Table 1.

The NRM presents an alkaline pH (10.3) and high

electrical conductivity (3700 lS cm-1). After the activa-

tions with 0.05 mol L-1 HCl and 0.1 mol L-1 Ca(NO3)2,

the pH and electrical conductivity values were reduced to

8.7 and 7.9 and 247 and 137 lS cm-1, respectively. The

thermal treatment increased the pH values from 10.3 to

10.9 and decreased the electrical conductivity to 1600 lS
cm-1. Regarding the IEC, the highest result was obtained

for CRM1 (112 mmol(?) kg
-1). The CRM2 presented the

second highest IEC (110 mmol(?) kg
-1), followed by the

NRM (109 mmol(?) kg
-1) and TRM (101 mmol(?) kg

-1).

The observed values approached the values obtained by

Santona et al. (2006), which were 106.5 and 120.6 mmol(?)

kg-1 for the NRM and 98.2 mmol(?) kg
-1 for mud treated

with HCl.

The CRM1 presented a larger specific surface area (79 m2

g-1), and the NRM presented the smallest value of this

parameter (31 m2 g-1). The results obtained for the TRM

and CRM2 were 56 and 40 m2 g-1, respectively. Hence, the

activations caused an increase in specific surface area rela-

tive to natural mud. The pore diameter for the NRM, CRM1

and CRM2 was between 3 and 4 nm and classified as

mesopores. The TRM presented diameters varying from 1 to

4 nm and was classified as micro to mesopores. Natural red

mud and red mud with different treatments were composed

of particles of different sizes and shapes (Fig. 1), with par-

ticles ranging from lower than 1 lmup to higher than 10 lm
of diameter. In addition, the different activations did not

change the mineral morphology.

Figure 2 illustrates the XRD patterns obtained for the

NRM and with different activations. The NRM presented

the following mineralogy: muscovite (KAl2Si3AlO10(-

OH)2), goethite (FeOOH), calcite (CaCO3), sodalite (Na8-
Al6Si6O24Cl2), gibbsite (Al(OH)3), quartz (SiO2) and rutile

(TiO2). CRM1 and CRM2 contained the same minerals as

NRM, whereas the peaks corresponding to goethite and

gibbsite were not observed for the TRM, however, the peak

for hematite (Fe2O3) was verified. According to Antunes

et al. (2012), thermal treatment is responsible for changing

of goethite to hematite at 234 �C (FeO(OH) ? Fe2O3) and

Table 1 Characterization of NRM, TRM, CRM1 and CRM2

Parameter NRM TRM CRM1 CRM2

pH 10.3 10.9 8.7 7.9

Electrical conductivity (lS cm-1) 3700 1600 247 137

IEC (mmol(?) kg
-1) 109 101 112 110

Specific surface area (m2 g-1) 31 56 79 40

Pore diameter (nm) 3–4 1–4 3–4 3–4

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gibbsite to alumina at 272 �C (Al(OH)3 ? Al(OH)(S) ? -

H2O ? Al2O3 ? H2O). The increment of alumina in the

red mud, which has a specific surface area higher than the

original aluminium hydroxide, promotes the increase in the

specific surface area of TRM.

Percentage of Cu(II) adsorption

The percentages of Cu(II) adsorption obtained for NRM

and with different activations are presented in Fig. 3a, and

the ratio C0 versus qe is presented in Fig. 3b. The total

amount of Cu(II) in the aqueous solutions was high enough

to satisfy the cationic exchange capacity of NRM and all of

its activations. The removal of Cu(II) by all of the red muds

was higher than their respective IEC. In addition, there was

no precipitation of Cu(II) during the adsorption experi-

ments due to pH of solution, which varying from 5.0 to 5.5.

The analysis of Cu(II) removal demonstrated a different

percentage of removal for each red mud according to the

following increasing order: TRM, NRM, CRM2 and CRM1.

The relative standard deviation for all samples was lower

than 4 %.TheNRMpresentedCu(II) adsorption percentages

varying from 44.8 to 99.8 % as a function of the initial

concentration (C0). The TRMwas thematerial that presented

the highest percentage of Cu(II) adsorption, with values

between 54.2 and 99.9 %. Additionally, the NRM and TRM

present values approaching 100 % Cu(II) removal for lower

concentrations (0.5–1.0 mmol 25 mL-1). After chemical

activation, the CRM1 and CRM2 presented values of Cu(II)

removal varying from 39.4 to 79.4 % and 45.8 to 93.9 %,

respectively, which represented the lowest percentages for

the removal of this metal.

Sodalite is a calcium and sodium tectosilicate of open

porous structure and can be considered a material with

Fig. 1 SEM-EDS of NRM

Fig. 2 XRD patterns of NRM, TRM, CRM1 and CRM2. Sdl sodalite, Gds gibbsite, Gt goethite, Kln kaolinite, Hem hematite, Qtz quartz, Cal

calcite

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zeolite-type properties. This crystalline phase was found in

all red mud samples examined in this study. This mineral

appears to be the main phase related to the adsorption

capacity of red mud because all of the mud samples pre-

sented high adsorption capacity for this metal. Because the

equilibrium pH of the aqueous solutions used in the

experiments was lower than the point of zero charge, with

value ca. 9.0 to red mud as reported by Antunes et al.

(2012), a positive charge density was observed in its lattice,

which does not favours the adsorption of metals on sodalite

surface.

However, sodalite possesses b-cages (with aperture

diameter of 0.22 gm) made up of six-membered rings in its

frameworks, which are negatively charged due to substi-

tution of Si4? by Al3? (Mon et al. 2005). Therefore, Cu(II)

can be exchanged with cations presents in the b-cages,
which are responsible for balancing the charge of the

structural framework of sodalite. Thus, due to NRM, TRM,

CRM1 and CRM2 used in this study contains large

amounts of sodalite, they present a high capacity for

removing Cu(II).

The chemical treatment with hydrochloric acid dissolves

a portion of the sodalite, approximately 9 % according to

Santona et al. (2006), and almost all of the muscovite found

in NRM, which can be observed in Fig. 2. Although there

is an increase in the specific surface area for CRM1, this

adsorbent presents the lowest percentage of Cu(II)

removal, which reinforce the idea that sodalite is an

important mineral for the adsorption process of Cu(II) by

NRM and at different activations.

However, there are other minerals in addition to sodalite

that contribute to the adsorption process. When NRM is

thermally activated at 400 �C, there is an increase in its

specific surface area (from 31 to 51 m2 g-1), decrease in

the pores diameters and transformation of goethite and

gibbsite into hematite and alumina, respectively. The

presence of Al and Fe oxides allows the adsorption of

Cu(II) due to positively charged surfaces through the for-

mation of specific inner-sphere bonds (Santona et al. 2006).

Therefore, TRM was the adsorbent that presented the

greatest percentage of Cu(II) removal for all of the con-

centrations used in the experiments.

Cu(II) adsorption isotherms

Adsorption isotherms are obtained by mathematical equa-

tions used to describe adsorption. These isotherms repre-

sent the amount of an adsorbed element relative to the

remaining concentration in the equilibrium solution. The

most frequently used models to describe adsorptions are

those proposed by Freundlich and Langmuir.

The model by Freundlich (Eq. 4) considers the non-

uniformity of real surfaces and describes the ionic

adsorption within certain limits of concentration; however,

this model presents difficulties for higher values, and its

main disadvantage is that it is not based on physical models

(Di Bernardo and Dantas 2005; Valladares et al. 1998).

qe ¼ KF � C
1
n
e; ð4Þ

where KF = the adsorption capacity (mmol g-1) (L

mmol-1)1/n; 1/n = the adsorption intensity.

The Langmuir model (Eq. 5) is based on adsorption

occurring at uniform sites with a monolayer cover and

ionic affinity regardless of the amount of adsorbed mate-

rial. Its main disadvantage is the use of its linear form

where the maximum adsorption is not properly estimated

(Di Bernardo and Dantas 2005; Valladares et al. 1998).

qe ¼
qm � KL � Ceð Þ
1þ KL � Ceð Þ ; ð5Þ

where qm = the maximum adsorption capacity

(mmol g-1); KL = the adsorption equilibrium constant.

Isotherms of Cu(II) adsorption created with the observed

values and values obtained by the Langmuir and Fre-

undlich models for NRM and at different activations are

found in Fig. 4. The results of these adjustments are pre-

sented in Table 2. The experimental data provided a good

fit for both models, which can be observed in Fig. 4 and

Fig. 3 The percentages of

Cu(II) adsorption (a) and the

ratio C0 versus qe (b) for NRM,

TRM, CRM1 and CRM2

Environ Earth Sci (2016) 75:362 Page 5 of 7 362

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Table 2, and the relatedness coefficients presented values

that were high and similar.

The highest value for maximum Cu(II) adsorption

capacity was obtained for the TRM (2.08 mmol g-1), fol-

lowed by CRM2 (2.01 mmol g-1), CRM1

(1.84 mmol g-1) and NRM (1.76 mmol g-1). The highest

value associated with TRM can be attributed to presence of

sodalite and transformation of goethite and gibbsite into

hematite and alumina, respectively, increase in specific

surface area and decrease in pore diameter. The parameters

obtained by the Freundlich model complemented the

results obtained by the Langmuir model. The highest KF

value [in (mmol g-1) (L mmol-1)1/n] was obtained for the

TRM (1.85), thus confirming its highest adsorption

capacity, being this fact associated with presence of

hematite in TRM. The lowest KF value was 1.05, which

was obtained for the CRM1. For the NRM and CRM2, the

KF values were 1.60 and 1.50, respectively.

The results obtained for the qm (mmol g-1) of Cu(II) for

NRM and at different activations were higher than those

found in other studies for natural red mud (and

0.08 mmol g-1—Nadaroglu et al. 2010), red mud treated

with HCl. i.e. 1.05 mmol g-1 (Apak et al. 1998a) and

0.04 mmol g-1 (Agrawal et al. 2004) and aggregated pre-

pared using red mud and CaSO4 (1.02 mmol g-1—Apak

et al. 1998b). Furthermore, the observed qm values for all

activations were higher than the value obtained for red mud

activated with calcium sulphate (0.31 mmol g-1) (López

et al. 1998).

The qm values presented in this study are even higher

than those found for other adsorbents, such as coal mining

waste (0.004 mmol g-1—Geremias et al. 2012), clay

(0.007–0.032 mmol g-1—Aragão et al. 2013), bentonite

(0.039 mmol g-1—Tito et al. 2008; 0.50 mmol g-1—

Anna et al. 2015), moriche palm activated charcoal

(0.007 mmol g-1—Pinto et al. 2012), chitosan capsules

(0.098 mmol g-1—Valentini et al. 2000), water treatment

residues (0.089 mmol g-1—Castaldi et al. 2015), cotton

boll (0.18 mmol g-1—Ozsoy and Kumbur 2006), xan-

thate-modified magnetic chitosan (0.54 mmol g-1—Zhua

et al. 2012), porous geopolymeric spheres

(0.82 mmol g-1—Ge et al. 2015) and expanded perlite

(0.14 mmol g-1—Saria et al. 2007).

Fig. 4 Adsorption isotherms of

Cu(II) by NRM, TRM, CRM1

and CRM2 using the Langmuir

and Freundlich adsorption

models

Table 2 Parameters of adsorption using Langmuir and Freundlich

models for the NRM, TRM, CRM1 and CRM2

NRM TRM CRM1 CRM2

Langmuir parameters

qm (mmol g-1) 1.76 2.08 1.84 2.01

KL 17.20 13.09 3.83 1.69

R2 0.97 0.97 0.92 0.95

Freundlich parameters

KF [(mmol g-1) (L mmol-1)-1/n] 1.60 1.85 1.05 1.50

1/n 0.15 0.16 0.43 0.32

R2 0.95 0.95 0.95 0.96

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Conclusion

In this study, the characterisation of red mud and adsorp-

tion of Cu(II) by the NRM and at different chemical (HCl

0.05 mol L-1—CRM1; and Ca(NO3)2 0.1 mol L-1—

CRM2) and thermal (400 �C) activations (TRM) were

evaluated. The heat treatment of red mud at 400 �C
increases the specific surface area due to chancing of

goethite to hematite and gibbsite to alumina and decreases

the pores particles. The highest percent removal of Cu(II)

was observed by the NRM and TRM at pH values ranging

from 5.0 to 5.5. The removal of Cu(II) in aqueous solution

obeys the Langmuir model, with maximum adsorption

capacity related to TRM (2.08 mmol g-1). The qm values

presented in this study are even higher than those found for

natural or activated red mud and other adsorbents. Thus,

this study suggests that the natural red mud or red mud with

different treatments, especially the TRM, have the potential

for use in the treatment of effluents and/or contaminated

soil from industrial activity.

Acknowledgments The authors acknowledge the Fundação de

Amparo à Pesquisa do Estado de São Paulo (FAPESP, Process No.

2009/02374-0), Conselho Nacional de Desenvolvimento Cientı́fico e

Tecnológico (CNPq, Process No. 480555/2009-5) and Companhia

Brasileira de Alumı́nio (CBA).

Compliance with ethical standards

Conflict of interest The authors declare that they have no conflict

of interest.

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	Cu(II) adsorption from aqueous solution using red mud activated by chemical and thermal treatment
	Abstract
	Introduction
	Experimental method
	Sampling and activation
	Characterisation of natural red mud and red mud with different activations
	Adsorption studies

	Results and discussion
	Characterisation of natural red mud and red mud with different activations
	Percentage of Cu(II) adsorption
	Cu(II) adsorption isotherms

	Conclusion
	Acknowledgments
	References