Ibrahim Int. J. Res. Chem. Environ. Vol.

1 Issue 1 July 2011(179-185)

International Journal of Research in Chemistry and Environment

Vol. 1 Issue 1 July 2011(179-185)
ISSN 2248-9649

Research Paper

Comparative Analysis of the Thermodynamics and Adsorption Isotherms for the

Adsorption of Some Metal Ions from aqueous solution using Sawdust Material
Ibrahim Muhammad B.
Department of Pure and Industrial Chemistry, Bayero University, NIGERIA

Available online at: www.ijrce.org

(Received 18th June 2011, Accepted 7th July 2011)

Abstract: The experimental results of the thermodynamic and adsorption isotherms of best fit for the
adsorption of Cr(VI), Ni(II), Fe(II) and Cd(II) from aqueous solution onto Sawdust were studied.
Adsorption experiments were carried out using batch process with a fixed (8g) weight of adsorbent and
variable adsorbate concentrations. Changes in concentration of the different adsorbates during the
adsorption process were monitored by the use of Shimadzu AA650 Double Beam Atomic Absorption/Flame
spectrophotometer. Thermodynamic parameters such as ∆H and ∆S were calculated from Van’t Hoff plots
which subsequently lead to the computation of ∆G. At high adsorbate concentrations, ∆H varied from 292,
754, 180 and 1,868Jmol-1 respectively for Cr, Ni, Fe and Cd. While ∆S varied in the form 2.89, 10.04, 0.83
and 35.66Jmol-1K-1 respectively for the same set of adsorbates. Whereas at the highest temperature studied
∆G changes according to the order -666.45, -2,590.26, -96.69 and -10,006.20Jmol-1respectively. This shows
that the adsorption process is endothermic and spontaneous, with spontaneity increasing as the temperature
increases. Equilibrium data were tested using Freundlich, Langmuir and Dubinin-Radushkevich adsorption
isotherms. The adsorptions of Cr, Ni and Fe onto sawdust were found to be a favourable physical
adsorption process which fitted well to the Freundlich adsorption isotherm. However, the adsorption of Cd
having RL value of 1.0000 is a linear process as suggested by Langmuir isotherm.
Key words: Adsorption; Adsorbate; Adsorbent; Thermodynamics; Isotherm; Sawdust

Introduction light, radiation, or sound), which interferes with the

Although water is abundant on earth, and since development of animals or plants. A pollutant on the other
almost 97% of the water contains salts, it is not suitable for hand is any substance produced by human activities, which at
drinking or for the various industrial purposes. Of the an unacceptable level, causes damage to the environment or is
remaining 3%, two thirds is in the form of ice and snow harmful to living systems. In general, pollution is usually
leaving only about 1% of the total water as fresh water. Of this harmful to one or more species of animal or plant. As such in
ground water accounts for about 98% and the surface water is order to maintain a healthy living environment, a careful study
only about 2%. Thus, of the total amount of water present on on the sources and nature of pollution and the ways of
earth, only about 0.02% is available in the lakes and streams pollution control should be considered.
[1]
. Therefore such a limited resource is very precious and Most of the reported work on the use of agricultural
needs conservation. Industrial effluents contains significant by-products for removal of heavy metals has to do with the
levels of toxic substances, and since the final destinations of capability of such materials in adsorbing heavy metals [3] The
effluents are the streams, rivers and the lakes, these toxic principle behind exploring agricultural by-products in this
substances are finally transported therein and the health risk work is the fact that most agricultural by-products are
become more wide. Hence keeping the effluents free of these composed of cellulose in the plant cell walls.
toxic substances is by extension keeping the environment The IR spectrum of sawdust according to Abdel-
healthier, and this is the target of this research work. Ghani et al., [4] showed small absorption bands at 3726.2,
Pollution has been defined by Wong et al., [2] as a 3618.2 and 3525.6 cm-1 assuming the presence of H-bridges
harmful change in the natural environment caused by human and crystal water. A medium band at 2908.5 cm-1 was also
activities which may be as a result of the release of substances,
that are toxic to either animals or plants, or energy (heat,
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attributed to H- bridges, the weak band at 2125.4 cm-1 may be in sunlight until almost all the moisture evaporated, then it was
attributed to (C=CH) while the band at 1639.4 cm-1was due to washed several times with distilled water in order to remove
(C=C).The strong band observed at 1033.8 cm-1 indicated the the water soluble tannins, after which it was dried in air and
stretching of the many C-OH and C-O-C bonds. then in an oven at 80 °C. The material was allowed to cool and
The work of Igwe and Abia [5] on the effect of it was then ground to the working particle size (850µm) and
temperature and particle size on bioremediation of As(III) kept in a plastic container for subsequent use.
from aqueous solution using modified and unmodified coconut Static adsorption experiments (studied at four
fiber reported ∆G values which are less than -15kJmol-1 different temperatures viz; 303, 313, 323 and 333K) in which
indicating a spontaneous and physical adsorption process, with the same solution remains in contact with a given quantity of
the modified fiber showing higher remediation of the adsorbent till equilibrium between the adsorbate concentration
adsorbate. in solution, and the adsorbate adsorbed per unit weight of
The work of Rajmond [6], utilised a mixed bed ion adsorbent, is reached was employed in this work. This type of
exchange column for the simultaneous determination of equilibrium established is static in character, as it does not
Cr(III) and Cr(VI) using UV detector at a wavelength of change further with time. Procedures described by
365nm from environmental samples such as rainwater and Bhattacharya, et al., [12] and El-Nemr, et al., [13] for testing the
galvanic sediments. The performance of his method was adsorption properties of the adsorbent were followed. The
established for the linearity, limit of detection, limit of procedure involved shaking a fixed amount of the adsorbent (8
quantification and the influence of sample pH. g) with 100 cm3 of the aqueous solutions of the adsorbates (in
Activated carbon from cassava peel was found to be a screw capped Erlenmeyer flasks) with initial loading
effective for the removal of nickel from aqueous solution [7] concentrations ranging from 20 – 60mg/L on an Innova 4000
and the equilibrium sorption isotherm were found to fit well to shaker from New Brunswick Scientific at a speed of 290 rpm
three isotherm models, with the Temkin model having the for an equilibrium period of one hour [14]. Immediately after
highest correlation coefficient. Their result also indicated that the shaking process, the samples were separately filtered using
Ni(II) uptake by the adsorbent followed pseudo 2nd-order rate Whatman number 1 filter paper, and the filtrates collected in
expression. polyethylene bottles were taken for AAS measurements for
The use of new commercially available superflow the residual adsorbate level using Shimadzu AA650 Double
chelating resin with Nitriloacetic Acid (NTA) - type functional Beam Atomic Absorption/Flame spectrophotometer.
groups for concentration of trace metals (such as iron and
copper) from seawater has been described by Lohan et al., [8]. Results and Discussion
The technique made use of inductively coupled plasma-sector A Thermodynamic Parameters for the Adsorption
field mass spectrometry (ICP – SFMS) for the determination Process
of low concentrations of dissolved iron and copper in Thermodynamic studies play an important role in
seawater. Trace metal recoveries were found to be pH determining the spontaneity and the heat change for the
dependent such that at pH ≤ 2, only iron (III) and copper are adsorption process. The adsorption of the metallic ions (Mn+)
quantitatively recovered. onto a given adsorbent is a typical example of a heterogeneous
The effect of agitation rate on the % adsorption of equilibrium for which the equilibrium constant for the
cadmium was studied by Ibrahim et al., [9] for cadmium in distribution of the metal ions between the liquid and solid
aqueous solution by using sugarcane bagasse. Results showed phases Ka, changes in enthalpy (∆H) entropy (∆S) and Gibbs
that highest Cd2+ adsorption was achieved at agitation rate of free energy (∆G) can be calculated from thermodynamic
150rpm and the adsorption process was relatively fast and relations [15 – 17] such as
equilibrium was achieved after about 90 mins of contact.
………………………………… (1)
Methodology
Material and Methods
All glasswares and plastic containers were washed …………………………………. (2)
with detergents, rinsed with distilled water and then soaked in //………………………. (3)
a 10% HNO3 solution for 24hrs. They were then washed with taking the adsorption process to be represented as
deionised water and dried in an oven for 24hrs at 80°C [10].
Distilled-deionised water, and AnalaR grade reagents Mn+(aq) + A(s)⇌A– M(ad) ………………………………. (4)
were employed for the preparation of all stock solutions.
1000mg/L of Cr(VI), Ni(II), Fe(II) and Cd(II) were Relevant data calculated from the thermodynamic
respectively prepared by dissolving 2.8290g of K2Cr2O7, relations were tabulated in Tables 1 (a & b) respectively. It is
4.0503g of NiCl2.6H2O, 4.9780g of FeSO4.7H2O and 2.1930g evident that the values of ∆Had were mostly positive, i.e.
of CdSO4.8/3H2O in small volumes of distilled deionised endothermic, especially at higher adsorbate concentration.
water in separate beakers and the solutions were transferred to One possible interpretation of the endothermicity of the
a 1.0litre volumetric flasks followed by the addition of 100cm3 adsorption process was that the metal ions were highly
of 6M HNO3 and they were made to mark with more water solvated in water. In order for these ions to be adsorbed, the
[11]
. Lower working concentrations were prepared daily from hydration sphere most be removed, and this process requires
the stock solution by appropriate dilution. energy intake. This energy of dehydration supersedes that
Hardwood sawdust material of Mahogany (Khaya required for getting the ions attached to the surface of the
senegalensis) tree collected from a local sawmill was air dried adsorbent [15], hence resulting to an overall endothermic
nature.
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Also evident from the Tables is the positive nature of Langmuir Adsorption Isotherm
the ∆Sad values at higher ionic strength i.e. suggesting The Langmuir model represents one of the first
spontaneous process. This occurs as a result of redistribution theoretical treatments of non-linear sorption and suggests that
of energy between the adsorbate and the adsorbent. Before the uptake occurs on a homogeneous surface by monolayer
adsorption occurs, the metallic ions near the surface of the sorption without interaction between the adsorbed molecules
[24]
adsorbent were more ordered than in the subsequent adsorbed . The constants k from Langmuir isotherm represents the
state. This increase in randomness at the adsorbent – adsorbate adsorption equilibrium constant (dm3/mg) and was computed
interface during the adsorption process leads to the increase in from the intercepts of the Langmuir plots (Figs. 2) and are
entropy and hence an overall positive ∆S. The adsorption presented in Table 2.
process is therefore likely to occur spontaneously at normal The essential characteristics of the Langmuir
and at high temperatures because ∆H > 0 and ∆S > 0 [18 – 20]. isotherm may be expressed in terms of the dimensionless
The Gibbs free energy change (∆Gad) was negative as separation parameter RL, computed from the relation;
expected for a spontaneous process under the applied
conditions. The decrease in ∆Gad (i.e. increase negative)
values with increase in temperature indicated more efficient
adsorption at higher temperature. This is because at higher ………………………………………………..…………… (8)
temperatures ions are easily desolvated and therefore their where k is the adsorption equilibrium constant while Co is the
adsorption becomes more favourable [21, 15, 18]. initial metal ion concentration. The value of the RL indicates
the type of the isotherm to be either (i) unfavourable if RL > 1,
B. Adsorption Isotherms (ii) linear if RL = 1, (iii) favourable if 0 < RL < 1 and
Adsorption isotherm studies were carried out with a irreversible if RL = 0. The calculated values of the RL for the
fixed initial adsorbent dose (8g) and varying adsorbate different ions onto the adsorbent (Table 3) under the different
concentrations [22] and the applicability of the data were tested conditions studied are in the negative range. This condition
for the Freundlich, Langmuir and Dubinin – Radushkevich(D- indicates that the adsorptions process does not fit to the
R) adsorption isotherms respectively according to the Langmuir model. However, the case of adsorption of cadmium
following relations, onto sawdust (RL = 1.0000) points to a linear situation [25, 9, 7].

lnqe = lnKF + alnCe, …………………………. (5) Dubinin – Radushkevich (D – R) Adsorption Isotherm

The D – R model was applied to the adsorption data
…………………….. (6) to determine if sorption had occurred by physical or chemical
processes. The constant K obtained from the slope of the D - R
and lnqe = lnqm – Kε2 ………………….……… (7)
isotherm is a constant related to adsorption energy having
units of mol2kJ-2 and it gives an idea about the mean free
Freundlich Adsorption Isotherm
energy E(kJmol-1) of adsorption per molecule of the adsorbate
The various adsorption data for the metal ions onto
when it is transferred to the surface of the adsorbent from
the adsorbent were tested against the Freundlich model as
infinite distance in the solution calculated for the relation
represented in Fig. 1. Freundlich isotherm gives an expression
encompassing the surface heterogeneity and the exponential [13, 26, 27, 28].
distribution of active sites and their energies. The numerical In the D – R isotherm, the sorption energy is
values of the constants nF and KF for the corresponding plot independent of the working temperature but varies depending
were determined from the slopes and intercepts of the on the nature of the adsorbent and adsorbate [24]. The
respective graph (Table 2). The constant KF is indicative of the magnitude of E provides information on the nature of the
relative adsorption capacity of the adsorbent related to the sorption process, i.e., whether it is chemisorptions or
bonding energy and can be defined as the adsorption or physisorption. If the values of E are in the range of less than
distribution coefficient. It represents the quantity of the metal 8kJmol-1 the sorption process is physical in nature, otherwise
ion adsorbed onto the adsorbent for unit equilibrium it is a chemical adsorption process [28]. From the D – R plots
concentration. While the constant a = 1/nF where nF is the (Figs. 3) the sorption energies were calculated and tabulated as
heterogeneity factor, represents deviation from linearity of the in Table 4. All the calculated energy values were found to be
adsorption process. Also for all values of 1/nF less than unity, in the range of less than 8kJmol-1, which according to Mataka
adsorption is the predominant process taking place otherwise et al., [28] corresponds to physical adsorption process.
desorption becomes predominant [23].
The observed values of nF > 1 for the adsorption of
Cr, Ni and Fe onto the sawdust material, the values of the
Conclusion
Conclusively, it can be observed that the adsorption
coefficient of variation (R2) and the linearity of their plots are
of the different ions studied is thermodynamically spontaneous
indicative of the fact that the result of the experimental data in
and feasible, with spontaneity increasing with increase in
this study fitted well to the Freundlich isotherm. Hence the
temperature and the mean free energy E, of the adsorption
adsorption of these metal ions onto the adsorbent can be said
suggested that the sorption process is physical in nature and is
to be a favourable physical adsorption process.
best defined by Freundlich adsorption isotherms.

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Table 1(a): Thermodynamic Parameters for the Adsorption of the various Metal ions
onto Sawdust
Ka ∆G = ∆H - T∆S ∆H ∆S
(Jmol-1) (Jmol-1) (Jmol-1K-1)
303K 313K 323K 333K
Cr 0.5708 6199.57 6422.88 6646.19 6869.51 -566.8485 -22.3314
Ni 0.0875 3055.09 3147.46 3239.82 3332.19 256.3206 -9.2369
Fe 0.2375 4249.23 4393.14 4537.06 4680.97 -111.4076 -14.3915
Cd 0.0299 -406.07 -448.81 -491.54 -534.27 888.7666 4.2734
Conditions: 8g Adsorbent, 20mg/L metal ion concentration and 1hr Agitation time

Table 1(b): Thermodynamic Parameters for the Adsorption of the various Metal ions
onto Sawdust
Ka ∆G = ∆H - T∆S ∆H ∆S
(Jmol-1) (Jmol-1) (Jmol-1K-1)
303K 313K 323K 333K
Cr 0.3156 -581.91 -610.76 -639.60 -668.45 292.2371 2.8850
Ni 0.1125 -2288.96 -2389.39 -2489.83 -2590.26 754.1629 10.0433
Fe 0.4696 -71.7498 -80.0638 -88.3778 -96.6918 180.1644 0.8314
Cd 0.0250 -8936.44 -9293.03 -9649.62 -10006.2 1868.1558 35.6587
Conditions: 8g Adsorbent, 60mg/L metal ion concentration and 1hr Agitation time

Table 2: Numeric Constants for the Adsorption of the Metal ions onto Sawdust Adsorbent

Ion Freundlich Langmuir D–R

nF KF k (L/mg) K (mol2kJ-2)
Cr 1.4514 0.4325 -0.1595 4 x 106
Ni 1.6556 0.2254 -0.0718 1 x 106
Fe 1.0627 0.5105 -0.0673 4 x 106
Cd 0.5627 0.0015 0.0000 250.9

Table 3: Variation of RL for the Sawdust Adsorbent with Increase in Initial Metal Ion
Concentration
Langmuir Separation Parameter (RL)
Co Sawdust
Cr Ni Fe Cd
20 -0.4565 -2.2941 -2.8947 1.0000
30 -0.2641 -0.8667 -0.9821 1.0000
40 -0.1858 -0.5343 -0.5914 1.0000
50 -0.1433 -0.3861 -0.4231 1.0000
60 -0.1167 -0.3023 -0.3293 1.0000

Table 4: Variation of the Sorption Energy (E) of the Adsorbates onto the Various
Adsorbents
Ion Sawdust
K E
Cr 4 x 106 0.0004
Ni 1 x 106 0.0007
Fe 4 x 106 0.0004
Cd 250.9 0.0446

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Figure 1: Freundlich Adsorption Isotherm for the Adsorption of the Metal Ions onto
Sawdust for 1hr Agitation

Figure 2: Langmuir Adsorption Isotherm for the Adsorption of the Metal Ions onto
Sawdust for 1hr Agitation

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Figure 3: Dubinin - Radushkevich Adsorption Isotherm for the Adsorption of the Metal
Ions onto Sawdust for 1hr Agitatio

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