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J. Anal. Appl.

Pyrolysis 87 (2010) 188–193

Contents lists available at ScienceDirect

Journal of Analytical and Applied Pyrolysis


journal homepage: www.elsevier.com/locate/jaap

Adsorption of copper from aqueous solution by activated carbons obtained


by pyrolysis of cassava peel
J.C. Moreno-Piraján a,*, L. Giraldo b
a
Departamento de Quı´mica, Facultad de Ciencias, Universidad de Los Andes, Grupo de Investigación en Sólidos Porosos y Calorimetrı´a, Bogotá, Colombia
b
Departamento de Quı´mica, Universidad Nacional de Colombia, Bogotá, Colombia

A R T I C L E I N F O A B S T R A C T

Article history: Activated carbons (ACs) were prepared by pyrolysis of cassava peel in presence of chloride zinc (chemical
Received 29 October 2009 activities). Cassava peel from Colombian cassava cultives were impregnated with aqueous solutions of
Accepted 14 December 2009 ZnCl2 following a variant of the incipient wetness method. Different concentrations were used to
Available online 22 December 2009
produce impregnation ratios of 40, 70, 110 and 160 wt.%. Activation was carried out under argon flow by
heating to 823 K with 1 h soaking time. The porous texture of the obtained ACs was characterized by
Keywords: physical adsorptions of N2 at 77 K and CO2 at 273 K. The impregnation ration had a strong influence on
Cassava peel
the pore structure of these ACs, which could be easily controlled by simply varying the proportion of
Adsorption
ZnCl2 used in the activation. Thus, low impregnation ratio led to essentially microporous ACs. At
Surface area
Activated carbon intermediate impregnation ratios, ACs with wider pore size distribution (from micropores to mesopores)
Langmuir were obtained. Finally, high impregnation ratios yielded essentially mesoporous carbons with high
Prausnitz–Radlke surface area and pore volume. The four best-fit three-parameter isotherms Sips, Toth, Radke–Prausnitz
and Vieth–Sladek suggests that the sorption capacity of activated carbon of cassava peel to uptake
copper ions to be 55 mg/g.
ß 2009 Elsevier B.V. All rights reserved.

1. Introduction Cassava is one of the primary foods in our country and usually
used for traditional food, cake, etc. The cassava production in
Activated carbons are materials having complex porous Colombia is very huge and only small amounts are utilized by
structures with associated energetic as well chemical inhomoge- traditional food industries, and the rest are used as the raw
neities. Their structural heterogeneity is a result of existence of material for cassava starch industries. Cassava starch making
micropores, mesopores and macropores of different sizes and operation produces a large amount of solid wastes (cassava peel),
shapes. Activated carbon is one of the most important adsorbents and direct discharge of this solid wastes will cause the
from an industrial view point. The main application of this environmental problems. Here we report on the porous texture
adsorbent is for separation and purification of gaseous and liquid characteristics of ACs prepared by ZnCl2 activation of cassava peel,
phase mixtures [1–7]. i.e. the shells covering cassava. These constitute a by-product from
There are two processes for preparation of activated carbon: cassava processing following harvest with few practical applica-
chemical activation and physical activation. Chemical activation is tions and whose uncontrolled spill (e.g. in rivers) causes some
known as a single step method of preparation of activated carbon environmental concern. In fact, applications of cassava peel are
in the presence of chemical agents. Physical activation involves limited to use as fuel or as feedstock to obtain food for animal. We
carbonization of a carbonaceous materials followed by activation will show that carbon adsorbents with high surface areas and pore
of the resulting char in the presence of activating agents such as volumes can be obtained from this material, and that development
CO2 or steam. The chemical activation usually takes place at a of the porous structure can be modulated by changing the relative
temperature lower than that used in physical activation, therefore proportions of feedstock and ZnCl2.
it can improve the pore development in the carbon structure
because of the effect of chemicals. The carbon yields of chemical
activation are higher than physical one [6,8]. Cassava is one of the 2. Experimental
most important foods in Colombia, an agricultural country.
2.1. Reagents

* Corresponding author. Tel.: +57 13394949; fax: +57 13324366. All chemicals were of reagents grade, purchased Merck and
E-mail address: jumoreno@uniandes.edu.co (J.C. Moreno-Piraján). cassava peel were obtained from cultives Colombian.

0165-2370/$ – see front matter ß 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.jaap.2009.12.004
J.C. Moreno-Piraján, L. Giraldo / J. Anal. Appl. Pyrolysis 87 (2010) 188–193 189

Fig. 1. Furnace vertical to obtain activated carbon from cassava peel.

2.2. Treatment and preparation of sample adsorption data were analyzed by the Dubinin–Radushkevich–
Kaganer (DRK) equation.
Prior to the use, the cassava peel was repeatedly washed with
distilled water in order to remove dust and other inorganic 2.4. Study of pH and determination of isotherms of
impurities, then oven-dried for 24 h at 393 K to reduce the adsorption from aqueous solution
moisture content. Peel from Colombian cassava was impregnated
with aqueous solutions of chloride zinc following a variant of the Batch adsorption experiments were carried out in a series of
incipient wetness method; similar cases have been described in stoppered reagent bottles. 100 mL of CuSO4 solution with
the literature [9,10]. This consists of adding dropwise (while predetermined initial concentration of 10, 20, 30, 40, 50–
stirring the solid, to facilitate homogeneous absorption of liquid) 100 mg/L was put inside the 30 mL stoppered reagent bottles,
the amount of aqueous solution (2.0 mL g1 cassava peel) which contained 0.5 g using the activated carbon of mayor area
necessary to produce swelling until incipient wetness. Different (CP160). Prior to that, the pH solution was adjusted to the desired
concentrations of ZnCl2 in aqueous solution were used to vary the values by adding HNO3 or NaOH. The reagent bottles with
content of impregnation agent, which will be expressed as activated carbon–CuSO4 mixture were shaken using an orbital
impregnation ratio (Xp, wt.%), defined as (gram ZnCl2 per g cassava incubator shaker, which operated at 100 rpm and 298 K (1 K) for
peel)  100. Impregnation ratios of 40, 70, 110 and 160 wt.% were 8 h to attain the equilibrium condition. Blank solutions were treated
used. After impregnation, the samples were dried for 8 h at 383 K similarly without the adsorbent, and the recorded concentrations at
in air. Pyrolysis treatments (activations) were carried out in a the end of each operation were taken as the initial. The final
vertical tubular reactor made of quartz in furnace CarboliteTM, concentrations of the solution were then determined from a
Fig. 1, using in all cases 25 g of impregnated and dried material. calibration curve. The solutions were continuously agitated for at
All treatments were done at a constant heating rate of least 8 days, which is the maximum contact time to reach equilibrium
10 K min1 and with an argon (99.999% pure) flow of with this sorbent and particle size (according to previous studies with
30 STP cm3 min1, which was kept during heating and cooling. many other metals). Blank samples were also processed in the
An activation temperature of 823 K and a soaking time of 4 h were absence of sorbent to check for sorption on the experimental
used. After cooling the solid pyrolysis residue to room temperature equipment (flasks, filtration units, etc.) and the absence of
it was washed with milli-Q distilled water until lowering the precipitation phenomena. Samples were finally collected and filtered
conductivity of the washing liquids to <5 mS cm1 (measured with using 1.2 mm pore size filter membranes. Metal content in the filtrate
a pH/conductivity meter HP, model MARK 602). The resulting ACs was measured using atomic emission spectrometry (AES) (Perkin
were dried at 383 K for 24 h in a vacuum furnace. The activated Elmer AAnalyst 300, US). The mass balance equation was used to
carbon were labeled here as: CP40, CP70, CP110 and CP160, calculate the amount of copper at equilibrium. Therefore, the sorption
according to their impregnation ratios with ZnCl2. capacity q (mg Cu g1) was obtained from:
VðC o  C eq Þ
2.3. Pore structure characterization q¼
m

The porous texture of ACs was characterized by physical where V is the volume of the solution (l), m is the amount of sorbent
adsorption of nitrogen at 77 K (using an automatic volumetric (g), Co and Ceq are the initial and equilibrium concentration in the
adsorption apparatus, AUTOSORB 3B from Quantachrome instru- solution (Cu, mg L1).
ments) and carbon dioxide at 273 K (using a automatic volumetric
adsorption apparatus, AUTOSORB 3B from Quantachrome instru- 3. Results and disscusion
ments). In either case the samples were degassed overnight at
573 K before every adsorption measurement. Gases used had 3.1. Physical properties of activated carbons obtained
minimum purities of 99.999% (N2) and 99.98% (CO2). N2 adsorption
data were analyzed by means of the BET and Dubinin–Radushke- Fig. 2 shows adsorption–desorption isotherms of N2 at 77 K on
vich (DR) equations, the aS method (using Spheron-6 carbon black ACs from cassava peels impregnated with different amounts of
as reference material) and the density functional theory (DFT). CO2 ZnCl2. The isotherms are type Ia for the AC with Xp = 40 wt.%
190 J.C. Moreno-Piraján, L. Giraldo / J. Anal. Appl. Pyrolysis 87 (2010) 188–193

Fig. 2. N2 adsorption–desorption isotherms at 77 K on ACs prepared at different Fig. 3. PSDs obtained by applying the DFT theory to N2 adsorption data at 77 K.
impregnation ratios. Empty symbols, adsorption; full symbols, desorption.

(typical of microporous materials where micropore filling may continuously with increasing impregnation ratio as does the
take place by primary filling at very low p/p0) [10] with a small mesopore volume, Vmp (DFT, N2) (volume of pores with widths
development of mesopores, and type Ib when Xp = 70 wt.% (typical between 2 and 50 nm). The ultramicropore volume, Vumicrop. (DFT,
of microporous materials where micropore filling may take place N2) (volume corresponding to pores of width <0.7 nm) follows the
by co-operative filling in wider micropores over a range of higher opposite trend.
p/p0 than in type Ia) [10]. The AC prepared by impregnation at Let us examine now the variation of the micropore volume as a
Xp = 110 wt.% gives a type Ib isotherm, but in this case a plateau is function of Xp. Parameters such as Vmicrop. (DRK, CO2) and Vmicrop.
not clearly reached, indicating widening of pores; this isotherm (DFT, N2) (the latter being calculated as the volume of pores of
exhibits a type H4 hysteresis loop, characteristic of slit-shaped width <2 nm) go through a maximum at Xp = 70 wt.%. The
pores. Finally, the AC prepared by impregnation with 160 wt.% alternative parameter Vmicrop. (DR, N2) increases with increasing
chloride zinc yields a type IIb isotherm but with an important Xp over the entire range of impregnation ratios studied, albeit the
adsorption at low p/p0, indicative of simultaneous presence of increase is small above Xp = 70 wt.%. Vmicrop. (DRK, CO2) is always
micro- and mesopores. Similar evolutions from type I to type II smaller than Vmicrop. (DFT, N2) and Vmicrop. (DR, N2), this being
isotherms with increasing amount, but with phosphoric acid have attributable to the presence of wide micropores that are not filled
been reported by other authors [1–3]. with CO2 at the low relative pressures (<0.03) attained at 273 K; it
Table 1 reports textural parameters deduced from N2 and CO2 is well-known that, under these conditions, CO2 only measures
adsorption isotherms. The BET (SBET) and micropore [Smicrop. (DR, narrow microporosity [11]. The differences between Vmicrop. (DFT,
N2)] surface areas increase with increasing Xp, sharply from N2) and Vmicrop. (DR, N2) are ascribable to the artifactual minimum
Xp = 100–160 wt.% and less markedly above the latter impregna- around 1 nm that arises systematically in DFT calculations. This
tion ratio (40–70 wt.%). The micropore surface areas deduced from minimum, introduced by modelling assumptions [12,13], certainly
CO2 isotherms [Smicrop. (DRK, CO2)] go through a maximum at contributes to underestimate the micropore volume as calculated
160 wt.%. The external surface area [Sext (aS, N2)] increases with by this method.
increasing Xp, slightly at low impregnation ratios and more steeply Fig. 3 shows pore size distributions (PSDs) calculated by means
above 110 wt.% ZnCl2, as could be expected from the shape of the of the DFT method from N2 adsorption data. Values below 1 nm can
isotherms. be noticed in all cases. The width of the distribution increases with
The total pore volume, Vp (N2) (calculated from N2 adsorption increasing Xp. The AC prepared at Xp = 40 wt.% exhibits a maximum
data as volume of liquid N2 at a relative pressure of 0.975) increases at 0.50 nm, which becomes displaced towards larger pore sizes

Table 1
Textural parameters deduced from N2 adsorption at 77 K and CO2 adsorption at 273 K on ACs prepared at different impregnation ratios (Xp).

Xp (wt.%) N2 CO2

SBET Sext Vp DFT-method DR-method DRK-method

Vumicrop. Vmicrop. Vmp. Smicrop. Vmicrop. Smicrop. Vmicrop.

40 834 7 0.33 0.12 0.24 0.03 876 0.30 650 0.23


70 945 12 0.57 0.10 0.32 0.22 965 0.47 660 0.31
110 1276 17 0.91 0.09 0.33 0.45 1289 0.48 698 0.25
160 1567 143 1.18 0.06 0.25 0.87 1560 0.62 723 0.24

Surface areas in m2 g1 and pore volumes in cm3 g1.


J.C. Moreno-Piraján, L. Giraldo / J. Anal. Appl. Pyrolysis 87 (2010) 188–193 191

(0.80 nm) at higher Xp values. For all samples this is the maximum. Table 2
Isotherms and the parameters involved in the different equilibrium sorption
An increase in the pore volume and a displacement towards higher
isotherms.
pore sizes can be clearly noticed as the impregnation ratio
increases. Finally, the mesopore volume also increases with Isotherm Expression Parameters
increasing Xp; for instance, mesopores only represent 21% of the Freundlich [15] qe ¼ K F Ce
1=nF
K F, nF
total pore volume of the AC prepared at an Xp = 40 wt.%, whereas qm K L C e
Langmuir [16] qe ¼ 1þK L C e KL, qm
they amount to 56% for the sample prepared at Xp = 160 wt.%.
AC e
From the above results one can deduce that the ACs obtained at Redlich–Peterson [17] qc ¼ 1þB Ce
g A, B, g
low impregnation ratios are essentially microporous. As the Toth [18] qe ¼ qm C e ðbT þ Ce T Þ
n 1=nT
bT, nT, qm
amount of ZnCl2 increases, pores with a wide range of sizes are K RP qm C e
Radke–Prausnitz [19] qe ¼ ð1þK RP C e ÞmRP
KRP, qm, mRP
developed so that at high Xp the ACs become predominantly
K q C
FS m e
mesoporous. Similar effects of the amount but with using Fritz–Schluender [20] qe ¼ 1þq Cm
KFS, qm, mFS
m e

phosphoric acid on porosity development have been reported qm ðK S C e ÞmS


Sips [21] qe ¼ 1þðK S C e ÞmS
KS, qm, mS
for other lignocellulosic precursors [1,2,4,5]. It is generally m bC e
Vieth and Sladek [22] qe ¼ K VS C e þ q1þ bC e  q KVS, qm, b
accepted that the porosity is generated with phosphoric acid
remaining intercalated in the internal structure of lignocellulosic
materials. As the amount of ZnCl2 used increases, the volume filled
by it and various polyphosphates will increase, resulting in larger and pH 10) there is a decrease in the adsorption capacity. This is
pore volume and pore size. due to the occurrence of copper precipitation. At pH 6 there are
three species present in solution as suggested by Elliot and Huang
3.2. Effect of initial pH and isotherm from aqueous solution [4], Cu2+ in very small quantities and Cu(OH)+ and Cu(OH)2 in large
quantities. Three species are adsorbed at the surface of adsorbent
The acidity of solution pH is one of the most important by ion exchange mechanism with the functional groups present in
parameters controlling the uptake of heavy metals from waste- adsorbent or by hydrogen bonding.
water and aqueous solutions. The uptake and percentage removal
of copper from the aqueous solution are strongly affected by the pH 3.3. Adsorption isotherm of copper from aqueous solution
of the solution as illustrated in Fig. 4. The uptake of copper
increases from 0.20 to 1.43 mg/g when the pH increases from pH 1 The capacity of the adsorption isotherm is fundamental, and
to pH 5. Copper sorption is noted to increase significantly at pH 3 plays an important role in the determination of the maximum
with 0.40 and 1.43 mg/g adsorption capacity at pH 5 respectively. capacity of adsorption. It also provides a panorama of the course
After that the capacity of adsorption decreases slightly in pH range taken by the system under study in a concise form, indicating how
of 6–10. The minimum adsorption observed at low pH (pH 1) may efficiently a carbon will adsorb and allows an estimate of the
be due to the fact that the higher concentration and higher economic viability of the carbons commercial applications for the
mobility of H+ ions present favored the preferential adsorption of specified solute. In order to adapt for the considered system, an
hydrogen ions compared to Cu(II) ions. It would be plausible to adequate model that can reproduce the experimental results
suggest that at lower pH value, the surface of the adsorbent is obtained, equations of Langmuir, Freundlich, Redlich–Peterson,
surrounded by hydronium ions (H+), thereby preventing the metal Toth, Vieth–Sladek, Fritz–Schluender, Radke–Prausnitz and Tem-
ions from approaching the binding sites of the sorbent. This means kin have been considered. Thus, the non-linearized forms of the
that at higher H+ concentration, the biosorbent surface becomes different isotherm models were shown in Table 2. Fig. 5 shows the
more positively charged such that the attraction between biomass adsorption of ions copper adjusted of Lagmuir model.
and metal cations is reduced. Experiments were performed at controlled pH using sodium
In contrast, as the pH increases, more negatively charged hydroxide and sulfuric. The pH of the solutions was regularly
surface becomes available thus facilitating greater copper removal. checked and the pH was controlled when the variation was 0.1.
It is commonly agreed that the sorption of metal cations increases
with increasing pH as the metal ionic species become less stable in
the solution. However, at higher pH values (pH 6, pH 7, pH 8, pH 9

Fig. 5. Adsorption of copper. Model Langmuir. Conditions: pH: 5.0, temperature:


Fig. 4. Effect of pH on adsorption capacity of copper ions on activated carbon CP160. 298 K.
192 J.C. Moreno-Piraján, L. Giraldo / J. Anal. Appl. Pyrolysis 87 (2010) 188–193

Table 3 Table 4
Isotherm parameters for copper ions onto activated carbon CP160 Sorption capacities of several adsorbents for the uptake of ions copper from its
from cassava peel obtained by non-linear method at 298 K. aqueous solutions.

Langmuir Freundlich Sorbent Sorption capacity Reference

qm (mg/g) = 56.17016779 KF = 7.476458 Bark pine pulp 45.2 [23]


KL = 0.061459875 1/nF = 0.436197 Manganese nodule power 40.0 mg/g [24]
r2 = 0.989458796 r2 = 0.949785 Tourmaline 30.0 mg/g [25]
Bamboo 15.0 mg/g [26]
Redlich–Peterson Toth isotherm
Humic acids from Fluka AG and Aldrich 51.47 mg/g [27]
A = 1.985288877 m (mg/g) = 52.96222 Activated charcoal 10.20 mg/g [28]
B = 0.0678388877 bT = 17.24579 Zeolite 5.0 mg/g [29]
g=1 nT = 1 Fungal mycelium pellets of Aspergillus niger 4.5 mg/g [30]
r2 = 0.989824598 r2 = 0.978278 Alumina 15.0 mg/g [31]
Clay 18.0 mg/g [32]
Radke–Prasunitz Fritz–Schluender Activated carbon of cassava peel 52 mg/g This study
qm (mg/g) = 54.96344751 qm (mg/g) = 71.00181
KRP = 0.072145873 KFS = 8.548796
mRP = 1 mFS = 0.72458
r2 = 0.978123 r2 = 0.965785 4. Conclusion
Sips Vieth–Sladek
In summary, pyrolysis of cassava peel impregnated with
qm (mg/g) = 53.54032617 qm (mg/g) = 52.96357
KS = 0.086478964 KVS = 0 chloride zinc produces materials with a well-developed pore
mS = 1 b = 0.075486 structure and high adsorption capacities, making possible to attain
r2 = 0.997698745 r2 = 0.978315 surface areas as high as 1567 m2 g1 and pore volumes as large as
1.18 cm3 g1. The impregnation ratio has a strong influence on the
pore structure of these ACs, which can be easily controlled by
simply varying the proportion of chloride zinc used in the
We have followed the same treatment for our adsorption data from activation. Thus, low impregnation ratios lead to microporous
aqueous solution suggested in [14]. For non-linear method, a trial and ACs with almost no mesopores. At intermediate impregnation
error procedure, which is applicable to computer operation is ratios, ACs with wide PSDs (from micropores to mesopores) are
developed using solver add-in, Microsoft spreadsheet, Microsoft obtained. At high impregnation ratios one obtains essentially
Excel [14–22] shows the calculated isotherm parameters and their mesoporous carbons with a high pore volume. Finally, the four
corresponding coefficient of determination, r2, values were shown in best-fit three-parameter isotherms Sips, Toth, Radke–Prausnitz
Table 3. From this table, it was observed that the higher r2 values for and Vieth–Sladek suggest that the sorption capacity of activated
the three-parameter Sips, Redlich–Peterson and the two-parameter carbon of cassava peel to uptake copper ions to be 55 mg/g.
Langmuir isotherms suggests the applicability of these models to
represent the equilibrium sorption of copper ions by activated carbon Acknowledgements
of cassava peel particles. In addition to Sips, Langmuir and Redlich–
Peterson isotherm the equilibrium copper ions uptake by activated The authors would like to thank the Departments of Chemistry
carbon of cassava peel particles was reasonably well represented by of the Universidad Nacional de Colombia and of the Universidad de
Toth, Radke–Prausnitz and Vieth–Sladek isotherms with r2 values of Los Andes (Colombia) and the Master Agreement established
0.978. The value of Sips isotherm constant mS and the Redlich– between these two institutions. Special gratitude to the Fondo
Peterson isotherm constant g equal to unity suggests that the Especial de Investigaciones de la Facultad de Ciencias de la
isotherm is approaching the Langmuir isotherm and not Freundlich Universidad de Los Andes (Colombia) for its partial financing of
isotherm. The lower r2 values for Freundlich and Fritz–Schluender these research.
isotherm shows it is not appropriate to use these models to represent
the uptake of copper ions by activated carbon of cassava at References
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