Journal of Colloid and Interface Science 251, 39–45 (2002)
doi:10.1006/jcis.2002.8395
Methylphenols Removal from Water by Low-Cost Adsorbents
A. K. Jain,1 Suhas, and A. Bhatnagar
Department of Chemistry, Indian Institute of Technology Roorkee, Roorkee 247667, India
E-mail: akjaincy@iitr.ernet.in
Received January 17, 2002; accepted March 25, 2002
A comparative study on the adsorption of methylphenols on
adsorbents prepared from several industrial wastes has been car-
ried out. The results show that extent of adsorption on carbona-
ceous adsorbent prepared from fertilizer industry waste has been
found to be 37.3, 40.5, 65.9, and 88.5 mg/g for 2-methylphenol,
4-methylphenol, 2,4-dimethylphenol, and 2,4,6-trimethylphenol,
rspectively. As compared to carbonaceous adsorbent, the other
three adsorbents viz. blast furnace sludge, dust, and slag adsorb
methylphenols to a much smaller extent. This has been accounted
for due to the carbonaceous adsorbent having a larger porosity and
consequently higher surface area. The adsorption of phenols on this
carbonaceous adsorbent as a function of contact time, concentra-
tion, and temperature has been studied by the batch method. The ad-
sorption has been found to be endothermic and data conform to the
Langmuir equation. The analysis of data indicates that adsorption is
a first-order process and pore diffusion-controlled. The efficiency of
the carbonaceous adsorbent was assessed by comparing the results
with those on a standard activated charcoal sample. It was found
that the carbonaceous adsorbent is about 45% as efficient as stan-
dard activated charcoal and can therefore be employed for the re-
moval of methylphenols from wastewaters. C 2002 Elsevier Science (USA)
Key Words: adsorption; industrial wastes; low cost adsorbents;
methylphenols.
INTRODUCTION
As a result of rapid industrialization, water is getting adversely
affected by both inorganic and organic pollutants. These pollu-
tants are often toxic and cause harmful effects to human and
animal life. It is, therefore, desirable that wastewater from in-
dustries be treated for the removal of toxic materials before be-
ing discharged into bodies of water. The nature of contaminants
present in effluents varies from industry to industry but some of
the common contaminants are metal ions, phenols, dyes, pesti-
cides, detergents, etc. (1). Effluents from gas and coke manu-
facture, tanneries, chemical plants, textile industries, petroleum
industries, etc., contain phenol and substituted phenols. Phenol
and substituted phenols are considered as priority pollutants (2)
since they impart bad taste and odor and are potential health haz-
ards even at low levels. Among the various methods employed
1 To whom correspondence should be addressed. Fax: 91-1332-73560.
39
(3) for the removal of toxic substances from industrial effluents,
the adsorption process has emerged as the best for removing
both inorganics and organics. Activated carbon, which is used to
remove organic molecules that cause taste, odor, and color
toxicity, is the most common adsorbent (4, 5). However, due
to the high cost of activated carbon, its use is restricted some-
times on economical considerations. In view of the importance
of effluent treatment, attention has, therefore, been directed to-
ward the development of low-cost adsorbents. For this purpose,
various solid waste materials of different industries like bottom
ash (6), slag (7), red muds and fly ashes (8), and blast furnace
sludge (9) have been investigated for the removal of toxic mate-
rials from water. These materials tend to remove inorganic con-
taminants more than organics. On the other hand, carbonaceous
slurry waste from fertilizer plants has been found to be a good
adsorbent for many organic molecules (10). No report dealing
with a comparative study of the adsorption of organic molecules
on both carbonaceous waste and waste of an inorganic nature is
available. In the present paper, we attempt to investigate the ad-
sorption of methyl-substituted phenols, a common contaminant,
on several inorganic wastes viz. blast furnace sludge, dust, and
slag from the steel industry and a carbonaceous slurry waste from
a fertilizer plant. The results have been compared with those on
standard activated charcoal in order to know the efficacy of the
adsorbents developed.
EXPERIMENTAL
Materials
Four methyl-substituted phenols viz. 2-methylphenol (2-MP),
4-methylphenol (4-MP), 2,4-dimethylphenol (2,4-DMP), and
2,4,6-trimethylphenol (2,4,6-TMP) were procured from SRL
(India), Merck (Germany), Eastman Kodak (New York), and
Fluka (Switzerland), respectively. Double distilled water was
used throughout.
Methods
Preparation of Adsorbents
The wastes obtained from fertilizer and steel plants were used
for preparing the adsorbents.
0021-9797/02 $35.00

C 2002 Elsevier Science (USA)
All rights reserved.
40 JAIN, SUHAS, AND BHATNAGAR
Carbonaceous adsorbent. In India, carbon slurry is pro-
duced as a waste in fertilizer plants using fuel oil/LSHS as a
feed stock. This waste slurry is available at a very cheap rate
(US $7 ton−1 ) and can be a good adsorbent for organics in view
of its porous nature. This slurry produced in plants is dumped
into huge tanks and allowed to dry. The dried cake material
was procured from NFL, Panipat (India) and powdered. It was
found to consist of small, black, and greasy granules and treated
(11) with H2 O2 to oxidize the adhering organic material. It was
then washed with distilled water and heated at 200◦ C till the
evolution of black soot stopped. The activation of this material
was done at different temperatures in a muffle furnace for 1 h
in the presence of air. After the activation, the ash content was
removed by treating the material with 1 M HCl and washed with
distilled water and dried. The yield of the finished product was
found to be ∼90%, and it is now called carbonaceous adsor-
bent. Different mesh sizes were obtained after sieving and kept
in the desiccator for further use. It was found after preliminary
adsorption studies that the activation at 500◦ C imparts maxi-
mum adsorption characteristics, and therefore, all investigations
were carried out on the samples activated at this temperature
only.
Blast furnace slag, dust, and sludge adsorbents. Among the
various wastes produced in steel plants, the blast furnace slag is
in the largest amounts. Besides this, blast furnace dust and sludge
are also waste products of the steel-making industry. During the
manufacture of pig iron, a dust load is carried by the gases gen-
erated in this process. This dust load is removed before their
release into the atmosphere. The gases are passed through a
large brick-lined chamber for the removal of coarse particles in
the exhaust gases. The chamber where some dust settles down
is called the dust catcher, and the waste material collected here
is termed as “blast furnace dust.” The finer particles that still
remain in the gas are removed in wet scrubbers, wherein the gas
is subjected to water sprays. The waste material collected here
is referred to as “blast furnace sludge.” The blast furnace (BF)
dust and sludge were procured from Malvika Steels, Jagdishpur
(India). The BF dust and sludge wastes were also treated sim-
ilar to carbon slurry treatment and then activation was done.
The temperature of 400◦ C was found to be optimum for activa-
tion. After activation, wastes were washed with water and dried.
Among the blast furnace slags procured from the same plant,
only foamed slag having some porosity was studied as adsor-
bent. To remove the impurities (if any), foamed slag was treated
with H2 O2 and washed with water and dried. The product was
sieved and kept in the desiccator.
Instrumentation
A Shimadzu 1601 UV-VIS spectrophotometer was used for
spectrophotometric determination of the phenols. The pH of the
solutions was measured with an Elico LI 127 pH meter and a
Leo 435 VP model was used for scanning electron microscopy
(SEM).
TABLE 1
Chemical Analysis of Blast Furnace Sludge, Dust, and Slag
BF sludge (%) BF dust (%) BF slag (%)
Loss on ignition 40.5 24.6 0.6
Insoluble residue 3.2 4.3 4.1
SiO2 12.7 15.8 32.7
R2 O3 35.4 44.9 22.8
CaO 3.5 4.7 31.7
MgO 3.0 4.2 6.8
Analysis
The blast furnace slag, dust and sludge were analyzed (12)
to determine the nature of the wastes, and the results are sum-
marized in Table 1. The analytical data of carbonaceous slurry
waste indicate the ash content to be 0.9%, volatile matter 3.2%,
and the rest to be mainly carbon. The N2 gas adsorption method
was used to determine the surface area of the adsorbents, and
their porosity was observed by scanning electron microscopy.
The iodine and methylene blue numbers were also determined
by standard methods (13) in order to determine the adsorption
characteristics of the prepared adsorbents.
Adsorption Studies
A series of batch adsorption experiments was conducted to
determine adsorption of phenols on the prepared adsorbents.
For this, a fixed amount of the adsorbents (0.01 g) was added
to 10 ml of phenol solution of varying concentrations taken in
50-ml stoppered glass tubes, which were placed in a thermostat
cum shaking assembly. The solutions were stirred continuously
at constant temperature to achieve equilibrium. After equilib-
rium, the adsorbent was allowed to settle and then filtered using
Whatman Filter Paper 42. The concentration of the adsorbate in
the residual solutions was subsequently analyzed spectrophoto-
metrically at the λmax values of 271 for 2-MP, 277 for 4-MP, 278
for 2,4-DMP, and 277.5 nm for 2,4,6-TMP. The adsorption was
also studied as a function of time at two concentrations in order
to have kinetic information.
RESULTS AND DISCUSSION
Characterization of the Prepared Adsorbents
The blast furnace slag, dust, and sludge were chemically an-
alyzed, and the results are compiled in Table 1. It is seen that
silica and calcium oxides are the main constituents of BF slag,
whereas coke, silica, and R2 O3 (mainly iron oxide) are the
prominent components of BF sludge and dust. Thus, BF slag
is inorganic in nature, whereas, BF sludge and dust are inor-
ganic but with partial organic character (carbon content). On
the other hand, carbonaceous adsorbent consisting of mainly
carbon is organic in nature. The organic content generally im-
parts porosity to the adsorbent. This is reflected in the surface
area of the four adsorbents given in Table 2. As the carbon
 METHYLPHENOLS REMOVAL FROM WATER BY LOW-COST ADSORBENTS 41

TABLE 2
Characteristics of Adsorbents Used

Standard activated Carbonaceous BF BF BF

charcoal adsorbent sludge dust slag

Surface area 710 380 28 13 4

(m2 /g)
Methylene 198 90 6 3 2
blue no.
Iodine no. 635 330 24 11 3

content decreases, the surface area correspondingly decreases.

The higher surface area is due to the porous nature of the adsor-
bents, and SEM results showed that porosity order is carbona-
ceous adsorbent > BF sludge > BF dust > BF slag. In order to
further evaluate the adsorption characteristics, methylene blue
and iodine numbers were also determined and given in Table 2.
It is seen that these two numbers decrease in the order carbona-
ceous adsorbent > BF sludge > BF dust > BF slag. This order
of adsorption is parallel to the surface area of the adsorbents,
which reflects that the adsorption of organic molecules is ex-
pectedly a surface phenomenon, and the carbonaceous adsorbent
having the largest surface area is the best. In order to compare
the efficacy of the adsorbents, the results were compared with FIG. 1. Effect of contact time on uptake of phenols on carbonaceous Ad-
sorbent (temperature, 25◦ C; particle size, 200–250 mesh).
a standard activated charcoal (E. Merck). Table 2 shows that
the carbonaceous adsorbent has about 50% of the surface area
of activated charcoal. Thus, it is expected that it would be half of concentration. The adsorption isotherms of 2-MP on various
as efficient as the activated charcoal in removing organics. This adsorbents are shown in Fig. 3. Simlar adsorption isotherms
conclusion is supported by relative values of methylene blue and were also obtained for the other three phenols. The maximum
iodine numbers. The other three adsorbents, BF sludge, dust, and adsorption from these adsorption isotherms has been calculated
slag, are not good materials for this purpose.

Effect of Contact Time and Concentration

In order to find equilibrium time for maximum uptake of the
phenols, the adsorption of all the phenols at fixed concentration
on the carbonaceous adsorbent was studied as a function of con-
tact time, and the results are shown in Fig. 1. It is seen from Fig. 1
that rate of uptake of all the phenols is rapid in the beginning
and 50% adsorption in the case of all the phenols is completed
within 2 h. Figure 1 also indicates that the time required for
equilibrium adsorption is 8 h. Thus for all equilibrium adsorp-
tion studies, the equilibration period was kept at 10 h. The effect
of concentration on equilibrium time was also investigated at dif-
ferent concentrations in the case of 2-methylphenol and shown
in Fig. 2. Similar plots were also obtained for other phenols. The
plots in Fig. 2 show that time of equilibrium as well as the time
required to achieve a definite fraction of equilibrium adsorption
is independent of the initial concentration. These results indicate
that the adsorption process is first order, which is confirmed by
Lagergren’s plots discussed later under dynamic modeling.

Adsorption Isotherms
FIG. 2. Effect of contact time on the uptake of 2-methylphenol on carbona-
To determine the efficacy of the adsorbents prepared, the ceous adsorbent at different initial concentrations (particle size, 200–250 mesh;
equilibrium adsorption of phenols was studied as a function temperature, 25◦ C).
42 JAIN, SUHAS, AND BHATNAGAR

their inorganic nature resulting in poor porosity, are not good

materials for the removal of organics from wastewaters. It is
further seen from Table 3 that the extent of adsorption of vari-
ous methylphenols on different adsorbents follows the order 2,4,
6-trimethylphenol > 2,4-dimethylphenol > 4-methylphenol >
2-methylphenol. These results indicate that as the number of
methyl groups on the phenol molecule increases, adsorption also
increases. This appears due to the solubility of phenols in aque-
ous media. The phenols having a larger number of methyl groups
have a lower solubility and, therefore, adsorbed on the adsorbent
in increasing amount compared to phenols having a lesser num-
ber of methyl groups and consequently higher solubility (14, 15).
As the carbonaceous adsorbent is the best, its performance was
further assessed by comparing its results with those of standard
activated charcoal. The results on adsorption of these phenols on
standard activated charcoal are also incorporated in Table 3. It
is seen that carbonaceous adsorbent is about 45% as efficient as
standard activated charcoal in removing phenols and, therefore,
can be employed for effluent treatment. As the carbonaceous ad-
sorbent appears to be promising material with high adsorption
efficiency, all further studies were done with it only.

FIG. 3. Adsorption isotherms of 2-methylphenol on different adsorbents at Effect of Temperature

25◦ C (X, standard activated charcoal; 
· , carbonaceous adsorbent; 
· , BF sludge;
, BF dust; adsorption on BF slag negligible).
and compiled in Table 3. It is seen that the adsorption is in
the order carbonaceous adsorbent > BF sludge > BF dust > BF
slag. This order of adsorption is parallel to the surface area
and porosity of the adsorbents. The carbonaceous adsorbent,
which has maximum surface area and porosity, adsorbs all the
phenols to a maximum extent, whereas the other three adsor-
bents having low porosity and surface area show only little or
negligible adsorption. Thus, it is concluded from these stud-
ies that only carbonaceous adsorbent, which possesses high
surface area and porosity, is a potential material for the removal
of phenols (organics). The adsorption of phenols on the surface
of carbonaceous adsorbent appears to occur due to their interac-
tion through hydrogen bonding with hydrophilic sites or groups
formed at the time of activation. In addition to this, some ad-
sorption might also be occurring due to van der Waal’s forces.
The other three adsorbents, which show poor adsorption due to
In order to understand the effect of temperature on the adsorp-
tion of phenols, experiments were also conducted at 45◦ C and re-
sults are shown in Fig. 4. A comparison of adsorption isotherms
at 25 and 45◦ C shows that adsorption increases with increase in
temperature, indicating that the process is apparently endother-
mic. Similar results were also obtained by other workers (16, 17).
The effect of temperature can be explained on the basis of hy-
drogen bonding. In aqueous solutions of phenols, there exists
extensive hydrogen bonding between the phenol molecule and
water, resulting in appreciable solubility. These hydrogen bonds
get broken at higher temperatures, and this would cause phenols
to be less soluble and, therefore, exhibit a higher tendency to go
to the adsorbent surface and adsorbed rather remaining in the
solution. The adsorption data were further analyzed and found
to conform best to the Langmuir equation
1 1 1
= + , [1]
qe qm qm bCe

TABLE 3
Solubility (in Water) and Adsorbability of Methylphenols (mg/g) on Various Adsorbents

Adsorbability (mg/g)
Standard
Solubility activated Carbonaceous BF BF BF
Phenols (g/liter) charcoal adsorbent sludge dust slag

2-Methylphenol 25.9 86.5 37.3 12.9 7.6 Negligible

4-Methylphenol 23.3 91.9 40.5 16.2 12.9 Negligible
2,4-Dimethylphenol 8.8 140.5 65.9 21.9 18.3 Negligible
2,4,6-Trimethylphenol 1.00 197.5 88.5 30.6 25.2 Negligible
 METHYLPHENOLS REMOVAL FROM WATER BY LOW-COST ADSORBENTS 43

also obtained for other phenols. The values of monolayer capac-

ity (qm ) and equilibrium constant (b) have been evaluated from
the intercept and slope of these plots and given in Table 4. It is
seen from Table 4 that the monolayer capacity (qm ) of the adsor-
bent for the phenols is comparable to the maximum adsorption
(Table 3) obtained from adsorption isotherms. As b values reflect
equilibrium constant for the adsorption process, it reflects the
affinity of the adsorbent for phenol. Thus, b values indicate that
the adsorbent has maximum affinity for 2,4,6-trimethylphenol
and minimum for 2-methylphenol.
The influence of adsorption isotherm shape has been dis-
cussed (18) to determine whether adsorption is favorable in terms
of RL , a dimensionless constant referred to as separation factor
or equilibrium parameter. RL is calculated using the equation

1
RL = . [2]
1 + bC0

The values of RL calculated as per the above equation are incor-

porated into Table 4. As the RL values lie between 0 and 1, the
adsorption isotherm is favorable (18, 19).
The free energy change (G 0 ), enthalpy change (H 0 ), and
entropy change (S 0 ) were calculated using the equations

−G 0 = RT ln(b) [3]

FIG. 4. Adsorption isotherms of methylphenols on carbonaceous adsorbent  
at 45◦ C. H 0 1 1
ln(b2 /b1 ) = − − [4]
R T2 T1
where qe is the amount adsorbed at equilibrium concentration
G 0 = H 0 − T S 0 [5]
Ce , qm the Langmuir constant related to the maximum mono-
layer capacity, and b the Langmuir constant related to the energy
of adsorption. The plots between 1/qe and 1/Ce for the adsorp- for the adsorption process in order to know the nature of adsorp-
tion of 2-methylphenol are drawn in Fig. 5. Similar plots were tion and are summarized in Table 5. The H 0 values, which are
positive, are the only apparent heat of adsorption. They reflect the
effect of temperature on the breaking down of hydrogen bonds,
which resulted in increased adsorption. Thus, a preadsorption
process (breaking of hydrogen bonds at higher temperature)
gives rise to positive H 0 , which is called the only apparent
heat of adsorption as they do not reflect the physical forces of

TABLE 4
Langmuir Constants and Separation Factor for the Adsorption of
Phenols on Carbonaceous Adsorbent at Different Temperatures

Temperature qmax b
Phenol (◦ C) (mg/g) (L/mol) RL

2-Methylphenol 25 50.0 5.5 × 103 0.15

45 64.5 6.6 × 103 0.13
4-Methylphenol 25 52.6 5.6 × 103 0.15
45 66.7 6.7 × 103 0.13
2,4-Dimethylphenol 25 83.3 7.4 × 103 0.12
45 100.0 9.1 × 103 0.10
2,4,6-Trimethylphenol 25 117.6 9.8 × 103 0.09
FIG. 5. Langmuir adsorption isotherms of 2-methylphenol on carbonaceous
45 125.0 12.3 × 103 0.08
adsorbent at different temperatures.
44 JAIN, SUHAS, AND BHATNAGAR

TABLE 5
Thermodynamic Parameters for Adsorption of Phenols
on Carbonaceous Adsorbent at Different Temperatures

Temperature −G 0 S 0 H 0
Phenol (◦ C) (kJ/mol) (J/mol · K) (kJ/mol)

2-Methylphenol 25 21.3 95.6 7.2

45 23.2 95.5
4-Methylphenol 25 21.3 97.3 7.7
45 23.2 97.2
2,4-Dimethylphenol 25 22.1 101.7 8.2
45 24.1 101.6
2,4,6-Trimethylphenol 25 22.8 106.7 9.0
45 24.9 106.6

attraction occurring at the time of phenol molecule adsorption

at the adsorbent surface. Further, negative G 0 values indicate
a spontaneous process. Positive S 0 values indicate the affinity
of the adsorbent for phenols.

Dynamic Modeling
The kinetics of adsorption is important from the point of
view that it controls the process efficiency. Various kinetic mod-
els have been used by various workers, where the adsorption
has been treated as a first-order (16, 20), a pseudo-first-order
FIG. 6. Lagergren’s plot for phenols on carbonaceous adsorbent.
(17, 21) and a pseudo-second-order-process (22). Different sys-
tems conform to different models. Lagergren’s rate equation (23)
is the one most widely used (16, 20, 24) for the sorption of a the Bangham equation (25)
solute from a liquid solution. Thus this first-order equation    
C0
k0 m

log log = log + α log t, [7]

kads C0
− q
m
2.303V
log(qe − q) = log qe − t, [6]
2.303
where C0
is the initial concentration of the adsorbate in solution
(mmol/l), V is the volume of the solution (ml), m
is the weight
where qe and q are the amount of phenol adsorbed at equilibrium
and at time t, in milligrams per gram respectively, and kads is
the first-order rate constant, was applied to the present studies
of phenol adsorption. As such, the values of log(qe − q) were
calculated from the kinetic data of Fig. 1 and plotted against
time in Fig. 6. The plots are found to be linear with good corre-
lation coefficients, indicating that Lagergren’s equation is appli-
cable to the phenol adsorption on carbonaceous adsorbent and
the adsorption process is a first-order process. The first-order
rate constants calculated from the plots (Fig. 6) are found to
be 7.6 × 10−3 , 7.8 × 10−3 , 8.3 × 10−3 , and 8.5 × 10−3 min−1
for 2-methylphenol, 4-methylphenol, 2,4-dimethylphenol, and
2,4,6-trimethylphenol, respectively. A higher rate constant for
2,4,6-trimethylphenol indicates that the adsorbent has a higher
affinity for this phenol. This is consistent with higher adsorption
(qm ) observed for this phenol as compared to that of others. As
a matter of fact, the rate constants for phenols are in the order
parallel to their qm values.
The kinetic data were further used to learn about the slow step
occurring in the present adsorption system. The applicability of FIG. 7. Bangham’s plot for phenols on carbonaceous adsorbent.
 METHYLPHENOLS REMOVAL FROM WATER BY LOW-COST ADSORBENTS
of the adsorbent used per liter of solution (g/l), q
(mmol/g) is 3. Pontius, F. W., “Water Quality and Treatment,” 4th ed. McGraw-Hill,
the amount of adsorbate retained at time t, and α(<1) and k0
are constants, to present phenol adsorption studies was used. As
such log log[C0
/C0
− q
m
] was plotted against log t in Fig. 7. 5. Paprowicz, J. T., Environ. Technol. 11, 71 (1990).
The linearity of these plots confirms the applicability of the
Bangham equation and indicates that the diffusion into pores of
the adsorbent controls the adsorption process (17, 26).
CONCLUSIONS
It is reasonable to conclude from the results of adsorption of
methylphenols on various adsorbents prepared from industrial
wastes that (i) a carbonaceous adsorbent is appropriate for re-
moval of phenols, whereas adsorbents of an inorganic nature are
not, (ii) the adsorption process is first order and pore diffusion-
controlled, and (iii) the carbonaceous adsorbent studied is not
only a low-cost material but also about 45% as efficient as stan-
dard activated charcoal and thus can be used in its place for the
removal of phenols from effluents.
ACKNOWLEDGMENT
The authors are thankful to the Ministry of Environment and Forests,
Government of India for financial support.
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