Journal of Environmental Protection, 2011, 2, 729-735 729

doi:10.4236/jep.2011.26084 Published Online August 2011 (http://www.SciRP.org/journal/jep)

Cr(VI) Ions Removal from Aqueous Solutions

Using Natural Adsorbents—FTIR Studies
Biswajit Singha, Tarun Kumar Naiya, Ashim Kumar Bhattacharya, Sudip Kumar Das
Department of Chemical Engineering, University of Calcutta, Kolkata, India.
Email: drsudipkdas@vsnl.net

Received March 22nd, 2011; revised May 6th, 2011; accepted June 15th, 2011.

ABSTRACT
The ability of eight natural adsorbents were investigated for adsorptive removal of Cr(VI) from aqueous solutions.
Various physico-chemical parameters such as pH, initial metal ion concentration, adsorbent dose level and equilibrium
contact time were optimized in batch adsorption technique. A detailed Fourier Transform Infrared spectra (FTIR) study
of adsorbents and Cr(VI) loaded adsorbents at the optimized condition was carried out to identify the different func-
tional groups that were responsible for the adsorption. The important functional groups like hydroxyl, alkene, aromatic
nitro, carboxilate anion, silicon oxide, sulphonic acid etc. were present in the natural adsorbent and were responsible
for the chemical adsorption of Cr(VI) from aqueous solutions. The sorption energy calculated from
Dubinin-Radushkevich isotherm indicated that the adsorption process were chemical in nature.

Keywords: FTIR, Chromium(VI), Rice Straw, Hyacinth Roots, Saw Dust

1. Introduction In recent years, several natural or agricultural wastes

[8-11] have been used for the removal of heavy metal
Cr(VI) containing waste water discharged from various from industrial waste water. In general natural or agri-
industries, including mining, tanning, cement, production cultural waste contains different functional groups like
of steel and other metal alloys, electroplating operations, hydroxyl, aldehyde, aliphatic acid, alkene, amide, aro-
photographic material and corrosive painting industries matic nitro, silicate, sulphonate etc. The present paper
[1,2]. It is carcinogenic, mutagenic and toxic; thus, its deals with the identification of functional groups which
presence in the environment poses a significant threat to are responsible for Cr(VI) ion adsorption in the eight
aquatic life and as well as public health [3]. bio-adsorbents.
The maximum permissible limit of Cr(VI) for the dis-
charge to inland surface water is 0.1 mg/L and in potable 2. Experimental Methods
water is 0.05 mg/L [4,5]. The Ministry of Environment
and Forest (MOEF), Government of India has set mini-
2.1. Preparation of Adsorbents
mal national standards (MINAS) of 0.1 mg/L for safe Rice straw, rice bran, rice husk, hyacinth roots, neem
discharge of effluent containing Cr(VI) in surface water bark, saw dust of teakwood origin, neem leaves and co-
[6]. To comply with this limit, industries have to treat conut shell were used as low cost natural or agricultural
their effluents to reduce the Cr(VI) concentration in wastes for Cr(VI) removal from aqueous solutions. All
wastewater to acceptable levels. In waste water treatment the adsorbents were collected from local area near
various technologies are available such as chemical pre- Kolkota, West Bengal, India.
cipitation, ion exchange, electrochemical precipitation, Rice straw, rice bran, rice husk and hyacinth roots
solvent extraction, membrane separation, concentration, were boiled for 6 hr. to remove color materials. Coconut
evaporation, reverse osmosis, emulsion per traction, ad- shell was crashed in roll crusher and then grinded. Saw-
sorption etc. [7]. Among these technologies, adsorption dust, neem bark, neem leaves and coconut shell were
is an user-friendly technique for the removal of heavy treated with 0.1 N NaOH to remove lignin based color
metal. This process includes the selective transfer of sol- materials followed by 0.1 N H2SO4. Finally all the ad-
ute components in the fluid phase onto the surface or sorbents were washed with distilled water several time
onto the bulk of solid adsorbent materials. and dried at 105˚C for 6 hr to remove the adherent mois-

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730 Cr(VI) Ions Removal from Aqueous Solutions Using Natural Adsorbents—FTIR Studies

ture. After drying, all the adsorbents were sieved to ob- shaker with 120 - 125 strokes/minute at 30˚C. The time
tain particle size of 250 - 350 μm prior to being used for required to reach the equilibrium was estimated by with-
adsorption studies. drawing conical flask containing treated solution at
regular intervals of time (simultaneously 8 conical flasks
2.2. Reagents and Equipments with same concentrations of all items). The content of
All the necessary chemicals used in the study were of these flasks were filtered through filter paper (Whatman
analytical grade and obtained from E. Merck Limited, no.1). UV-visible spectrophotometer was employed to
Mumbai, India. The pH of the solution was measured determine the remaining Cr(VI) concentration in the
with a EUTECH make digital microprocessor based pH sample solution using 1,5-diphenylcarbazide method as
meter previously calibrated with standard buffer solu- laid down in standard methods for examination of water
tions. UV-Spectrophotometer (U-4100 spectrophotome- and wastewater, APHA, AWWA, WEF, 1998 edition
ter, Hitachi, Japan) was used to determine the Cr(VI) [13]. All the investigations were carried out in triplicate
content in standard and treated solutions after adsorption to avoid any discrepancy in experimental results with the
experiments. FT-IR (Jasco FT/IR-670 Plus) studies were reproducibility and the relative deviation of the order of
carried out to determine the type of functional group re- ±0.5% and ±2.5% respectively. The solution pH adjusted
sponsible for Cr(VI) adsorption. The surface area was to 1.0 ± 0.1 to 9.0 ± 0.1 under thermostated conditions of
measured on Micromeritics Surface Area Analyzer 30˚C ± 0.5˚C.
(ASAP 2020). The moisture content determination was 3. Results and Discussion
carried out with a digital microprocessor based moisture
analyzer (Metteler LP16). The point of zero charge was 3.1. Optimum Operating Condition and Cr(VI)
determined by solid addition method [12] and reported in Adsorption Mechanism
Table 1. Metal sorption is depends on the solution pH. The range
2.3. Preparation of Standard Cr(VI) Solution of variables investigated to obtain the optimum condition
is shown in Table 2. In general adsorption of anion is
The stock solution containing 1000 mg/L of Cr(VI) was favored at pH < pHpzc. At very low pH, chromium ions
prepared by dissolving 3.73 g of A. R. grade K2CrO4, exist in the form of HCrO 4 , at higher pH up to 6 differ-
2H2O in 1000 ml double distilled water. Required initial ent forms such as Cr2 O72  , HCrO 4 , and Cr3 O10
2
, coex-

concentration of Cr(VI) standards were prepared by ap- ists, of which HCrO 4 predominates. As the pH increa-
propriate dilution of the above stock Cr(VI) solution. ses equilibrium shifted form HCrO 4 to CrO 24  and
Cr2 O72  [14]. At very low pH values, the surface of ad-
2.4. Batch Adsorption Studies
sorbent would be surrounded by the hydronium ions
Using the necessary adsorbents in a series of 250 ml which enhance the Cr(VI) interaction with binding sites
stopper conical flask containing 100 ml of Cr(VI) solu- of the biosorbent by greater attractive forces. As the pH
tion batch adsorption were carried out. pH of the solution increased, the overall surface charge on the biosorbents-
adjusted by adding 0.1 N HCl or 0.1 N NaOH solution as became negative and adsorption decreased [2]. The fol-
required. Then the flasks were shaken for the desired lowing equilibrium may be written for the Cr(VI) anions
contact time in an electrically thermostated reciprocating present in aqueous solutions [9].

Table 1. Different physical characteristics of natural adsorbents.

Adsorbents Surface area (m2/g) Moisture content (%) Point of zero charge Ash content (%)

Rice straw 1.21 7.26 6.85 9.40

Rice bran 0.12 10.68 6.10 11.72

Rice husk 0.54 9.02 6.05 11.80

Saw dust 3.85 8.63 3.90 12.35

Neem bark 3.47 9.23 4.50 10.62

Hyacinth roots 5.78 11.25 6.59 10.74

Neem leaves 0.57 8.33 6.94 13.58

Coconut shell 0.52 6.16 6.62 9.23

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 Cr(VI) Ions Removal from Aqueous Solutions Using Natural Adsorbents—FTIR Studies 731

Table 2. Range of variables for batch experiment.

Adsorbent Initial pH Initial Cr(VI) concentration (mg/L) Contact time (min) Adsorbent dosage (g/L)

Rice straw 1-9 5 - 300 0 - 420 2.5 - 12.5

Rice bran 1-9 5 - 300 0 - 420 2.5 - 12.5

Rice husk 1-9 5 - 300 0 - 420 2.5 - 12.5

Saw dust 2-8 3 - 300 0 - 300 2.5 - 30.0

Neem bark 2-8 3 - 300 0 - 300 2.5 - 30.0

Hyacinth roots 1-9 5 - 300 0 - 420 2.5 - 12.5

Neem leaves 1-9 5 - 300 0 - 300 2.5 - 12.5

Coconut shell 1-9 5 - 300 0 - 360 2.5 - 12.5

H 2 CrO 4  HCrO 4  H  k1  1.21 (1) adsorption capacity of adsorbent (mmol/g),  is con-

stant related to sorption energy. The Polanyi potential [18]
Cr2 O 72   H 2 O  2HCrO 4 k2  35.5 (2) which is equal to,
HCrO 4  CrO 42   H  k3  3  107 (3)  1 
  RT ln 1   (6)
Adsorption of Cr(VI) was not significant at pH values  Ce 
more than 6 due to dual complexation of the anions R is the ideal gas constant in kJ/mol/K and T is the
( CrO 24  , Cr2 O72  and OH  ) to be adsorbed on the sur- temperature in Kelvin. From the plot of ln Cabs vs.  2
face of the adsorbents, of which OH  predominates [15]. gave a straight line from which the values of  and
The optimum adsorbent dosage, equilibrium contact time, X m for all the adsorbents were calculated. Using the
optimum initial Cr(VI) ion concentration and maximum value of  , the mean sorption energy, E, is evaluated as
adsorption capacities of different natural or agricultural
waste adsorbent using Langmuir adsorption isotherm 1
E (7)
model [16] were experimentally determined in batch 2
process and the results are shown in Table 3.
The mean sorption energy, E, which indicated the in-
Ce 1 C formation about adsorption mechanism. If E  8 kJ/mol,
  e (4)
qe qmax b qmax the adsorption process was physical in nature and in the
ranges from 8 to 16 kJ/mol, it was chemical in nature
Equation (4) represents the Langmuir adsorption model [19-21]. The estimated values of E were 14.142 kJ/mol,
where Ce is the concentration of Cr(VI) in solution at 13.921 kJ/mol, 13.558 kJ/mol, 9.341 kJ/mol, 9.205
equilibrium (mg/L), qe is the amount adsorb per gram of kJ/mol, 12.845 kJ/mol, 14.712 kJ/mol and 15.394 kJ/mol
the adsorbent at equilibrium, qmax is the maximum ad- for rice straw, rice bran, rice husk, saw dust, neem bark,
sorption capacity (mg/g) and b is the Langmuir constant
hyacinth roots, neem leaves and coconut shell respec-
(L/mg). Linear plots of Ce/qe vs. Ce were employed to
tively which suggested the adsorption process was che-
determine the value of qmax (mg/g). The maximum ad-
mical in nature i.e. the indication of chemical bond for-
sorption capacity along with correlation coefficient (r2)
mation between metal ion species and the functional
obtained were listed in Table 3.
group of the adsorbents.
3.2. Calculation of Sorption Energy 3.3. FTIR Analysis for Cr(VI) Adsorption
The Dubinin-Radushkevich [17] isotherm model was Fouier transform infrared spectra (FTIR) was used to inves-
used to predict the nature of adsorption processes as tigate the changes in vibration frequency in the functional
physical or chemical by calculating sorption energy. The groups of the adsorbents due to Cr(VI) adsorption. Each
linear from of the model is described as, fresh and Cr(VI) loaded adsorbents were mixed sepa-
ln Cabs  ln X m   2 (5) rately with KBr of spectroscopic grade and made in the
form of pellets at a pressure of about 1 MPa. The pellets
where Cabs is the amount of Cr(VI) adsorbed onto ad- were about 10 mm in diameter and 1 mm thickness. Then
sorbent surface (mol/g) and Xm represents the maximum the adsorbents were scanned in the spectral range of 4000 -

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732 Cr(VI) Ions Removal from Aqueous Solutions Using Natural Adsorbents—FTIR Studies

Table 3. Optimum operating condition obtaining in the batch process.

Langmuir isotherm model

Adsorbent Initial pH Initial Cr(VI) concentration (mg/L) Contact time (min) Adsorbent dosage (g/L)
qmax (mg/g) r2

Rice straw 2 25 180 10 12.17 0.9801

Rice bran 2 25 300 10 12.34 0.9476

Rice husk 1.5 25 360 10 11.39 0.9869

Saw dust 3 50 240 10 20.70 0.9963

Neem bark 3 50 240 10 19.60 0.9959

Hyacinth roots 2 25 240 10 15.28 0.9790

Neem leaves 2 25 240 10 15.95 0.9652

Coconut shell 2 25 240 10 18.69 0.9530

400 cm−1. Figures 1-3 show the FTIR spectra of rice

straw, hyacinth roots and coconut shell respectively.
Similar type of spectra also occurred for other adsorbents.
These spectra indicated a number of absorption peaks
showing the complex nature of the adsorbent. The func-
tional group is one of the key factors to understand the
mechanism of metal binding process on natural adsorb-
ents.
Tables 4 and 5 represented the shift in the wave num-
ber of dominant peak associated with the fresh and Cr(VI)
loaded adsorbents in the FT-IR plots. These shifts in the
wave length showed that there was metal binding process
taking place at the surface of the adsorbents [12,22]. The Figure 2. FTIR spectra of (a) hyacinth roots and (b) Cr(VI)
spectra display a number of absorption peaks, indicating loaded hyacinth roots.
the complex nature of the natural adsorbents. There was
a clear shift from wave number of 3348.78 cm−1 (rice
straw) to 3417.24 cm−1 (metal loaded rice straw), 3342.03
cm−1 (rice bran) to 3328.53 cm−1 (metal loaded rice bran)
and 3385.42 cm−1 (rice husk) to 3421.10 cm−1 (metal
loaded rice husk), 3297.75 cm−1 (neem bark) to 3266.82
cm−1 (metal loaded neem bark), 3328.53 cm−1 (hyacinth

Figure 3. FTIR spectra of (a) coconut shell and (b) Cr(VI)

loaded coconut shell.

root) to 3305.39 cm−1 (metal loaded hyacinth roots)

which indicate surface -OH group is one of the functional
group responsible for adsorption Cr(VI) on rice straw,
rice bran, rice husk, neem bark and hyacinth root.
Though surface -OH present as functional group in saw
Figure 1. FTIR spectra of (a) rice straw and (b) Cr(VI) dust but it is not responsible for metal binding in case of
loaded rice straw. adsorption of Cr(VI) on saw dust. This can be inferred

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 Cr(VI) Ions Removal from Aqueous Solutions Using Natural Adsorbents—FTIR Studies 733

Table 4. Wave number (cm−1) for the dominant peak from FT-IR for Cr(VI) adsorption.

Cr(VI) loaded Cr(VI) loaded Cr(VI) loaded Cr(VI) loaded

Functional Groups Rice straw Rice bran Rice husk Saw dust
rice straw rice bran rice husk saw dust
Surface O-H
3348.78 3417.24 3342.03 3328.53 3385.42 3421.10 3335.10 3328.53
stretching
Aliphatic C-H
2918.73 2916.81 2924.52 2924.52 2925.48 2925.48 2917.70 2920.66
stretching
Aldehyde C-H
x x 2854.13 2854.13 2854.13 2854.13 x x
stretching
Aliphatic acid C=O
x x 1709.59 1713.44 x x x x
Stretching
Unsaturated
1644.09 1633.41 1655.59 1644.02 1654.62 1638.23 x x
group like alkene
Amide C-O
x x x x x x 1594.04 1593.88
stretching
Aromatic C-NO2
1512.88 1505.17 1546.63 1514.81 1515.77 1509.99 x x
stretching
Carboxilate anion
1321.00 1371.14 x x x x x x
C=O stretching
Si-O stretching 1072.66 1058.73 1079.94 1055.84 1098.26 1075.12 x x
Sulphonic acid S=O
x x x x x x 1033.60 1031.73
stretching
Sulphonate
x x x x x x 693.28 651.82
S-O stretching

Table 5. Wave number (cm−1) for the dominant peak from FT-IR for Cr(VI) adsorption.

Cr(VI) loaded Hyacinth Cr(VI) loaded Cr(VI) loaded Coconut Cr(VI) loaded
Functional Groups Neem bark Neem leaves
neem bark roots hyacinth roots neem leaves shell coconut shell
Surface O-H
3297.75 3266.82 3328.53 3305.39 x x x x
stretching
Aliphatic C-H
x x 2924.52 2923.88 2920.28 2910.16 x x
stretching
Phosphite ester
x x x x x x 2353.97 2358.78
group
Aliphatic acid C=O
x x 1713.44 1713.44 1715.83 1715.67 1717.73 1715.75
Stretching
Unsaturated
x x 1644.02 1633.41 x x x x
group like alkene
Amide C-O
1606.40 1603.52 x x x x x x
stretching
Aromatic C-NO2
x x 1514.81 1505.17 1515.46 1515.80 1507.22 1507.19
stretching
Alkane group
x x x x 1455.88 1455.98 1472.91 1456.25
stretching

-SO3 stretching x x x x x x 1236.10 1226.83

Sulphonyl chlorides
x x x x 1163.39 1162.00 x x
stretching
Sulphonic acid
1032.91 1034.84 1055.84 1035.59 x x 1031.37 1032.23
S=O stretching
Sulphonate
756.92 658.57 x x x x x x
S-O stretching

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734 Cr(VI) Ions Removal from Aqueous Solutions Using Natural Adsorbents—FTIR Studies

from the peak shift (Tables 4 and 5). Aliphatic C-H not for other adsorbents.
stretching may be responsible for Cr(VI) adsorption onto Crystal radius of Cr(VI) is 0.52 Å. It is moderately
neem leaves as wave number shift from 2920.28 cm−1 to large ion, fit into the binding site of the natural adsorb-
2910.16 cm−1. Unsaturated group like alkenes present ents and bind to several group present in the adsorbents
may also responsible for adsorption of Cr(VI) on rice simultaneously.
straw, rice bran, rice husk and hyacinth root which is
inferred from the shift of the peak more than 10 cm−1.
4. Conclusions
Aromatic nitro, C-NO2 stretching was found to have In this study batch adsorption experiments for the re-
major shift of wave number from 1546.63 cm−1 to moval of Cr(VI) from aqueous solutions has been carried
1514.81 cm−1 for the adsorption of Cr(VI) on rice bran. out using eight different natural adsorbents. The adsorp-
There were also minor shift of peak for the adsorption of tion characterestics have heen examined at different pH
Cr(VI) on rice straw, rice husk, hyacinth roots, neem values, initial metal ion concentrations, contact time and
leaves and coconut shell. So the aromatic nitro groups different adsorbent dosages. FTIR analysis confirmed the
are responsible for adsorption of Cr(VI) on rice bran not existence of different functional groups responsible for
for the adsorption on other adsorbents. Alkane group was the adsorption. The obtained results are summarized as
only responsible for Cr(VI) adsorption onto coconut shell follows
as indicated in Table 5. 1) The optimum pH for the removal of Cr(VI) was
FT-IR spectrum of rice straw also showed intense found to be 1.5 for husk and 2 for other adsorbents.
bands around 1321.00 cm−1 which shifted to 1371.14 2) Maximum uptake was obtained at adsorbent dosage
cm−1 for Cr(VI) loaded rice straw. This is to be attributed of 10 g/L for all the adsorbents.
that the carboxylate anion are responsible for the adsorp- 3) The equilibrium time for the adsorption of Cr(VI)
tion on rice straw. At 1072.66 cm−1 (rice straw), 1079.94 from aqueous solutions were varied from 3 hr to 6 hr for
cm−1 (rice bran) and 1098.26 cm−1 (rice husk) bands can adsorbents used.
be assigned Si-O stretching. Major shift of these band 4) The maximum monolayer adsorption capacities by
indicated that Si-OH group is responsible for adsorption. the adsorbents were measured using Langmuir adsorp-
Tables 4 and 5 also indicated that the minor shift for tion isotherm.
the other band (aldehyde C-H stretching, phosphate ester 5) Sorption energy calculated from Dubinin-Raduske-
group, aliphatic carboxylic acids) which showed that vich (D-R) shows the chemisorptions process for all the
these groups were not involved in the adsorption process. adsorbents.
SO3 stretching were found be to responsible for Cr(VI) 6) FTIR studies indicated the following functional
adsorption onto coconut shell. groups were responsible for adsorption,
The peak at 1033.60, 1032.91, 1055.84 and 1031.37 a) Rice straw—Surface hydroxyl, unsaturated group
cm−1 for saw dust, neem bark, hyacinth roots and coconut like alkene, Carboxilate anion, Silicate groups;
shell can be assigned to the S=O stretching mode of sul- b) Rice bran—Surface hydroxyl, unsaturated group
phonic acid group. S=O stretching was slightly shifted by like alkene, Aromatic nitro, Silicate groups;
Cr(VI) adsorption on saw dust, neem bark and coconut c) Rice husk—Surface hydroxyl, unsaturated group
shell while the adsorption on hyaceinth root resulted in a like alkene, Silicate groups;
large shift of functional group from 1055.84 cm−1 to d) Saw dust—Sulphonate groups;
1035.59 cm−1. This would be imply that S=O stretching e) Neem bark—Surface hydroxyl, Sulphonate groups;
of sulphonic acid group is available for the adsorption of f) Hyacinth roots—Surface hydroxyl, Unsaturated
Cr(VI) on hyacinth root, however not involved on other group like alkene, Sulphonic acid groups;
adsorbents used in our study. g) Neem leaves—Aliphatic group;
The observation for the sulphonate group revealed that h) Coconut shell—Alkane, -SO3 groups.
S-O stretching was highly occurred by Cr(VI) adsorption
on saw dust and neem bark. The S-O stretching group 5. Acknowledgements
was observed to shift clearly from wave number 756.92 Biswajit Singha wishes to thanks the University of Cal-
cm−1 to 658.57 cm−1 and 693.28 cm−1 to 651.82 cm−1 cutta for the Project Fellow (UPE/Science & Technol-
neem bark and saw dust respectively. This indicated that ogy), Ref. No. UGC/489/Fellow UPE (SC/T), dated the
there is a high potential of S-O stretching group from 16/4/2009.
sulphonate involved with Cr(VI) binding on neem bark The authors acknowledge to AICTE for financial sup-
and saw dust. So S-O stretching was only associated with port (Project No.- F. No.:8023/BOR/RID/RPS-72/2008-
the adsorption of Cr(VI) on neem bark and saw dust but 09).

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 Cr(VI) Ions Removal from Aqueous Solutions Using Natural Adsorbents—FTIR Studies 735

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