Adsorption Studies on the Removal of Hexavalent Chromium (Cr (VI)) from Aqueous Solution using Black Gram Husk

Journal of Environmental Treatment Techniques

2020, Volume 8, Issue 3, Pages: 1144-1150

J. Environ. Treat. Tech.

ISSN: 2309-1185

Journal web link: http://www.jett.dormaj.com

Adsorption Studies on the Removal of Hexavalent

Chromium (Cr (VI)) from Aqueous Solution using

Black Gram Husk

Sunil Rajoriya*, Ahlaam Haquiqi, Bhawna Chauhan, Girish Tyagi*, Avdesh Singh Pundir*,

Ajay Kumar Jain, Divya Agarwal

Chemical Engineering Department, Meerut Institute of Engineering and Technology Meerut-250005

Received: 17/06/2020

Accepted: 09/07/2020

Published: 20/09/2020

Abstract

In the current work, black gram husk (BGH) as an effective adsorbent was used to remove the hexavalent chromium (Cr (VI)) from

aqueous solution in the batch mode. The characterization of adsorbent was done by Fourier transform infrared spectroscopy (FT-IR) to

identify the functional groups present on the surface of BGH. The study was done with synthetic wastewater having a Cr (VI)

concentration of 100 mg/L. Batch experiments were conducted to study the effects of various process parameters such as solution pH (1

–

7), adsorbent dosage (0.5 – 1.5 g/100 mL), initial Cr (VI) concentration (100 – 200 mg/L), and contact time (0 – 30 min) on the

efficiency of the adsorption process. The maximum % removal of Cr (VI) was 65.23% at the optimized set of process parameters i.e.

solution pH of 3, adsorbent dosage of 1 g/100 mL, contact time of 15 min. Freundlich and Langmuir adsorption isotherms were applied

to investigate adsorption data, The observed experimental data fitted well to Langmuir isotherm (R = 0. 9804 and qmax = 9.19 mg/g).

The reusability study showed that BGH material is recyclable up to only one cycle with 45.19% Cr (VI) removal efficiency. The obtained

experimental results revealed that BGH as an efficient adsorbent may be used for the Cr (VI) removal from aqueous solutions.

Keywords: Black gram husk (BGH); Cr (VI); Adsorption; Reusability; Isotherms

Introduction¹

cost, incomplete metal removal, large quantity of toxic sludge,

high energy requirement (16). However, Adsorption process

has been found to be suitable process to remove toxic metals

from wastewater using low cost adsorbents due to its high

efficiency, simple to operate, low cost, reusability of adsorbent

In recent years, the polluted water containing heavy metals

has led to serious issues due to the random discharge of heavy

metals in to the water bodies (1). Among the heavy metals,

chromium has the harmful effects on the aquatic environment

(

17). In the recent years, many authors have utilized the various

(

2). Chromium occurs in two stable oxidation states i.e.

trivalent chromium (Cr(III)) and hexavalent chromium

Cr(VI)) in aqueous solution. Cr (VI) compounds are 500 times

adsorbents towards the removal of chromium from wastewater

such as modified groundnut hull (2), paper mill sludge (3), tea

waste (5), neem leaves (18), husk of Bengal gram (19),

modified corn stalks (20), fertilizer industry waste material

(

more toxic as compared to Cr(III) because of its high water

solubility, carcinogenic, mutagenic properties (3). According

to the World Health Organization (WHO), the maximum

acceptable limit of hexavalent chromium concentration is 0.05

mg/L in wastewater (4). United States Environmental

Protection Agency (US EPA) has recommended the acceptable

level of Cr(VI) is 0.05 mg/L for potable water and is 0.1 mg/L

for inland surface waters (5). If hexavalent chromium is present

in water beyond the acceptable limit which causes skin

irritation resulting in ulcer formation, liver damage and

pulmonary congestion (6). Hence, it is necessary for industries

to decrease the Cr(VI) concentration from their wastewaters to

acceptable limit before discharging it into the aquatic

environment. There have been various processes implemented

to remove the chromium from industrial wastewater including

ion exchange (7,8), electro-dialysis (9), chemical coagulation

(

21), distillery sludge (22), coconut husk and palm pressed

fibers (23).

To the best of our knowledge, none study has been reported

in literature on the utilization of the husk of black gram for the

removal of chromium from industrial wastewater. Therefore, in

the present work, the possible use of the black gram husk for

the removal of chromium (VI) has been investigated for the

efficient removal of chromium (VI). The characterization of the

BGH adsorbent was done by Fourier transform infrared

spectroscopy (FTIR) analysis. Proximate analysis of the BGH

was also carried out. The influence of the different process

parameters like solution pH, adsorbent dosage, initial

chromium (VI) concentration and contact time was studied.

Reusability of the prepared adsorbent was also investigated in

order to check the efficiency of BGH. Besides, the adsorption

isotherms were also illustrated in the current work.

(

10), nanoparticles (11), membrane filtration (12),

electrochemical technologies (13), and adsorption (14, 15).

These processes have many disadvantages such as high capital

Corresponding authors: (a) Sunil Rajoriya, Chemical Engineering Department, Meerut Institute of Engineering and Technology

Meerut-250005, E-mail: sunilrajoriya@gmail.com. (b) Girish Tyagi, Chemical Engineering Department, Meerut Institute of Engineering

and Technology Meerut-250005, E-mail: girish.tyagi@miet.ac.in. (c) Avdesh Singh Pundir, Chemical Engineering Department, Meerut

Institute of Engineering and Technology Meerut-250005, E-mail: 2013rch9513@mnit.ac.in.

144

Journal of Environmental Treatment Techniques

2020, Volume 8, Issue 3, Pages: 1144-1150

major process parameters such as solution pH, adsorbent

dosage and initial Cr(VI) concentration on the removal

efficiency of Cr (VI). The mixture was stirred at 150 rpm for a

fixed period of time. The adsorbent laden Cr (VI) was separated

by Whatman filter paper and the clear solution was analyzed

for Cr (VI) concentration. Experimental set-up with range of

process parameters is shown in Fig.2. To optimize the pH

value, the effect of solution pH on the removal of Cr (VI) was

investigated over a pH range of 1.0–7.0. The effect of adsorbent

dosages from 0.5 to 1.5 g/100mL was carried out. Effect of

initial Cr (VI) concentration was studied by varying the

concentration of Cr (VI) from 100 to 200 mg/L. Adsorption

isotherm was studied with different initial concentrations of

Cr(VI) from 100 to 200 mg/L at the constant adsorbent dosage

of 1g/100 mL, temperature of 25°C and pH of 3. The observed

results were analyzed by two isotherm models such as

Freundlich and Langmuir.

Materials and methods

.1 Materials

2 2 7

Potassium dichromate (K Cr O ) was purchased from

Central Drug House (P) Ltd. India. The stock solution

comprising 1,000 ppm of Cr(VI) was prepared by dissolving

.4134 g of K

concentrations were prepared by appropriately diluting of the

stock solution. 0.1 M NaOH and 0.1 M H SO were used to

2 2 7

Cr O in 500 ml of distilled water. All desired

adjust the required pH of solution before starting the

experiments. Distilled water was used throughout all the

experiments.

.2 Preparation of adsorbent

Black gram (Vigna Mungo) Husk (BGH) was collected

from flour mill located at Gajraula, UP, India. Initially, the

BGH was washed thoroughly in running tap water followed by

distilled water to remove color and dirt particles. It was then

dried in oven at 110°C for 2 h. After drying, BGH was crushed

in mixer grinder to make fine powder and sieved through a 25

mesh sieve tray. Synthesized adsorbent was kept in air-tight

polythene bag for future use. Flow diagram for the presentation

of the absorbent is shown in Figure 1. The proximate analysis

of the adsorbent was carried out and the obtained results are

shown in Table 1.

.5 Analytical procedure

The remaining concentration of Cr(VI) in the solution after

experiments was determined by UV–visible spectrophotometer

JASCO, V-530) at 540 nm. Solution pH was determined by

(

digital pH meter. Reproducibility of experimental results was

examined by performing the experiments at least two times to

obtain an average value and the experimental errors were found

to be within ± 4%. The percentage removal efficiency of Cr

.3 Characterization of BGH

(VI) was determined by following Eq. (1).

The BGH adsorbent was characterized using FTIR spectra.

To check the presence of functional groups in BGH, Fourier-

transform infrared spectroscopy (FTIR) of the adsorbent was

done by infrared spectrophotometer (model: 8400S, Shimadzu)

^퐶0 ⁻^퐶

푒

Removal of Cr (VI) =

× 1ꢀꢀ

(1)

퐶0

−1

ranging from 400 cm to 4000 cm .

where, C is initial Cr (VI) concentration and Ce are the final

.4 Batch adsorption studies

The adsorption of Cr (VI) from aqueous solution was

concentration of Cr (VI) in the sample (when equilibrium was

achieved).

carried out in a batch system. The experiments were conducted

with 100 mL solutions of 100 ppm Cr (VI) concentration in 250

mL glass flasks at the temperature of 25°C. The batch

adsorption experiments were studied to check the effect of

Washed with

tap water

Then, washed with

distilled water

Black gram husk (BGH)

Crushed and

powdered

Dried for 2 h at

110°C in an oven

Sieved (mesh 25)

Prepared adsorbent

Figure 1: Flow diagram for the preparation of adsorbent

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Journal of Environmental Treatment Techniques

2020, Volume 8, Issue 3, Pages: 1144-1150

Adsorption capacity (q

2).

) was determined using following Eq.

Fig. 3) was measured within the range of 500-4000 cm^-¹wave

number. FTIR study indicated that functional groups like C=O,

C–O, O–H and N–H were present onto the BGH surface. The

(

퐶₀− 퐶_푒

푀

observed peak at 3745.50 and 3407.98 cm is assigned due to

the presence of O-H groups on the surface of BGH. A

푞_푒

× 푉

(2)

characteristic peak at around 3339.51 cm may be due to the

where, V is volume of the solution in L and M is the mass of

the adsorbent used in g.

N–H symmetric stretching vibration indicating the presence of

amino (-NH ) groups (16). The presence of peaks observed at

-1 -1 -1

899.78 cm , 2888.20 cm and 2833.24 cm may be due to

Table 1: Proximate analysis of adsorbent (BGH)

the stretching vibration of the –C-H group (5). The band

-1

363.60 cm is the result of stretching vibrations of C=O or N-

Parameters

Value (%)

6.80

H groups possibly due to amines and ketones (24). The peak at

Moisture Content

Volatile matter

Ash content

-1

around 1632.63 cm may be due to the stretching vibration of

70.80

14.10

8.30

amide groups. The absorption band near 1520.77 cm may be

assigned to the –C-H deformation vibration indicating the

presence of alkanes group. The characteristics peak at 1397.33

Fixed Carbon

-1

cm was due to the stretching vibration of –C–O. The peak

-1

observed at 1326.93 cm and 1088.74 cm may be assigned to

the C-OH stretching vibration of carboxylic acid and alcohols

(

Results and Discussions

.1 FTIR analysis

In the present study, the FTIR spectrum was obtained to

identify the functional groups present on the surface of

prepared adsorbent. FTIR spectrum of the adsorbent (Shown in

-1

5, 24). The absorption band between 600 and 900 cm

comprises several bands associated to the aromatic and out of

plane –C–H bending (5, 25).

Thermometer

Black Gram

Husk (BGH)

Wastewater

Range of Process parameters

5 C

Solution pH

1 to 7)

Adsorbent dosage

(0.5 to 1.5 g/100 mL)

Reaction vessel

(

Initial Cr (VI)

concentration

100 to 200 mg/L)

Contact time

0 to 30 min)

Magnetic Bid

(

rpm

Power supply

Magnetic Stirrer

Optimum conditions:

Solution pH = 3;

Adsorbent dosage = 1 g/100 mL;

Initial Cr (VI) concentration =100 mg/L

Contact time = 15 min

Maximum Cr (VI) removal

efficiency = 65.23%

Figure 2: Experimental set-up with range of process parameters

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2020, Volume 8, Issue 3, Pages: 1144-1150

Figure 3: FTIR spectrum of BGH

.2 Optimization of Solution pH

The solution pH is an important parameter in deciding the

for the adsorption of Cr (VI) is directly proportional to surface

area of the adsorbent (5). It was further observed that the

increasing amount of BGH had no noticeable effect on the

removal efficiency of Cr(VI).

removal efficiency of Cr (VI). To find the optimum pH,

experiments were conducted over a various range of pH values

from 1.0 to 7.0. Fig. 4 depicts the removal efficiency of Cr (VI)

versus solution pH. Figure 4 shows th at the % removal of

Cr(VI) was increased from 42.14 to 65.23% for an increase in

solution pH from 1 to 3. Then, the percentage removal was

reduced to 19.32% with more increase in the pH up to 7.0. The

obtained results showed that the maximum 65.23% of Cr(VI)

by the prepared adsorbent (BGH) was removed at the optimized

pH of 3.0. Hence, the optimum pH was selected as 3.0 to

achieve the suitable removal efficiency of Cr(VI) for all the

remaining experiments. Hexavalent chromium (Cr(VI)) may

occur in the aqueous medium in various anionic forms i.e.

−

7−

chromate (CrO

chromate (HCrO ) as per the following Eq. (3):

), dichromate (Cr

), or hydrogen

−4

ꢃꢂ

퐻 푂

퐻⁺ꢁ 2퐻퐶푟푂₄^ꢂ ↔ 2퐻 퐶푟푂 ↔ 2퐻 푂 ꢁ 퐶푟푂 ↔ 2퐶푟푂 ꢁ

Solution pH

Figure 4: Effect of solution pH on the removal efficiency of Cr (VI)

Experimental conditions: Adsorbent dosage = 1 g/100 mL; T = 25°C;

ꢃ

(3)

ꢃ

(

Time = 15 min; Initial Cr (VI) concentration = 100 mg/L, Solution

volume = 100 mL)

It is well reported in literature that the dominant form of

−4

Cr(VI) at lower pH is HCrO (5). When the solution pH

−

increases, the concentration of HCrO is shifted to other forms

7−

2 2

such as CrO2ꢀ4−ꢀandꢀCr O . It can be established that the

−4

The decrease in the adsorption efficiency is mainly because

of remained unsaturated sites during the adsorption process.

Maximum % removal of Cr (VI) was achieved with 1g/100 mL

of adsorbent dosage at solution pH of 3, temperature of 25°C,

time of 15 min and initial Cr (VI) concentration of 100 mg/L.

Hence, 1 g/100 mL of the BGH was chosen for all the

remaining experiments.

active form of Cr(VI) is HCrO that can be adsorbed by the

BGH in this work.

.3 Effect of Adsorbent dosage

The effect of adsorbent dosage was investigated by varying

the amount of adsorbent from 0.5 to 1 g/100 mL. The obtained

results of adsorbent dosage on the % removal of Cr (VI) are

depicted in the Fig. 5. It can be seen from figure 5, the

adsorption of Cr (VI) increases with an increase in adsorbent

dosage due to an increase in the number of adsorption sites and

enhance surface area (22). Number of adsorption sites available

.4 Effect of initial Cr(VI) concentration

The effect of initial Cr(VI) concentration on the removal

efficiency was studied under the optimum conditions i.e.

solution pH of 3, time of 15 min, temperature of 25°C and

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2020, Volume 8, Issue 3, Pages: 1144-1150

adsorbent dosage of 1 g/100 mL. The initial Cr (VI)

concentration was varied from 100 to 200 mg/L. The observed

results are shown in Fig.6.

equilibrium adsorption data were fitted to the Freundlich and

Langmuir as following.

.6.1 Freundlich isotherm

The linear form of Freundlich isotherm can be represented

by Eq. (4):

푙표푔푞_푒= 푙표푔푘 ꢁ 푙표푔퐶_푒

(ꢄ)

푓

푛

where C

is equilibrium concentration (mg/L), K

is the

Freundlich isotherm constant (L/mg) and n is the Freundlich

adsorption intensity. Freundlich isotherm model has been

plotted between log q against log C (shown in Fig. 8 (a)).

e e

0.5

1.5

Adsorbent dosage, g/100 mL

Figure 5: Effect of adsorbent dosage on the removal efficiency of Cr

VI) (Experimental conditions: Solution pH = 3; T = 25°C; Time = 15

(

min; Initial Cr (VI) concentration = 100 mg/L, Solution volume = 100

mL)

It was observed that percentage removal of Cr(VI) was

decreased from 65.23% to 41.25% when the initial Cr(VI)

concentration increased from 100 to 200 mg/L. This may be

attributed to enhance in the number of chromium ions for a

fixed dosage of the adsorbent, the total available adsorption

sites were restricted and therefore decreasing trend in %

removal of Cr (VI) (2, 5). The observed results are consistent

with the previous studies reported showing that the Cr (VI)

removal efficiency using adsorption is inversely proportional

to the initial concentration of Cr (VI) (2, 20-21).

Time, min

Figure 7: Effect of contact time on the removal efficiency of Cr (VI)

Experimental conditions: Adsorbent dosage = 1 g/100 mL; Solution

pH = 3; T = 25°C; Initial Cr (VI) concentration = 100 mg/L; Solution

volume = 100 mL)

(

.6.2 Langmuir isotherm

The linear form of Langmuir isotherm model is given by

the following Eq. (5):

퐶_푒

ꢁ

푞_푚_푎_푥퐾 푞

퐿 푚푎푥

(5)

^푞푒

where, q

equilibrium, qmax is the maximum monolayer adsorption

capacity (mg/g) and K is the Langmuir isotherm constant

L/mg) that is associated to adsorption energy. Langmuir plot

is the amount of the adsorbate adsorbed (mg/g) at

150

200

(

Initial Cr (VI) concentration, mg/L

of C

parameters K

v/s C

is depicted in Fig. 8(b). The values of Langmuir

Figure 6: Effect of initial Cr (VI) concentration on the removal

efficiency of Cr (VI) (Experimental conditions: Adsorbent dosage = 1

g/100 mL; Solution pH = 3; T = 25°C; Time = 15 min; Solution volume

andqmax were determined using the intercept and

slope. The isotherm parameters and correlation coefficient (R )

are presented in Table 2. The value of Freundlich constant (n)

was greater than 1 indicating a strong interaction between BGH

and Cr (VI). Amongst the correlation coefficient obtained from

different two isotherms, Langmuir isotherm model provided

the best fitted data for the adsorption of Cr (VI) giving the

100 mL)

.5 Effect of contact time

The experiments were conducted at the optimized

conditions such as adsorbent dosage of 1 g/100 mL, pH of 3,

initial Cr (VI) concentration of 100 mg/L and temperature of

higher value of regression coefficient (R = 0.9804).

5°C. It was observed that percentage removal of Cr (VI) was

.7 Reusability of the prepared adsorbent

Reusability of the any prepared new material is the most

improved from 29.54 to 65.23% in initial 15 min after that no

removal in chromium was seen. This is mainly because of the

fact that all the available adsorbing sites on the adsorbent

surface are engaged and no further adsorption is possible (5).

Therefore, time was selected as 15 min for all the experiments

in the present study.

notable advantage for the treatment of wastewater. Hence, a

reusability test of the adsorbent was conducted at the optimized

conditions (Initial Cr (VI) concentration = 100 mg/L; pH = 3.0;

Temperature = 25°C; Contact Time = 15 min, adsorbent dosage

1 g/100 mL) where the maximum removal efficacy was

achieved. In the present work, reusability of the used material

was examined by regenerating the adsorbent laden with Cr (VI)

using the method reported in literature (26). The regeneration

study for Cr (VI) adsorption was carried out using 1 M HCl and

found that the removal efficiency of Cr(VI) was reduced from

.6 Adsorption Isotherms

In order to optimize the design of an adsorption method, it

is necessary to create the most suitable correlation for the

equilibrium curve. Several isotherms are available for

analyzing experimental data but in this study the obtained

148

Journal of Environmental Treatment Techniques

2020, Volume 8, Issue 3, Pages: 1144-1150

5.23% to 45.19% after one cycle. Almost 31% reduction in

may be utilized efficiently in the removal of Cr (VI) from

aqueous solutions for the purposes of environmental cleaning.

the efficiency of Cr (VI) removal was obtained after one cycle.

Acknowledgement

.95

.85

.75

.65

.55

(a)

Authors are thankful to Chemical Engineering Department,

MIET, Meerut for providing the necessary facilities to conduct

the research work. The authors also acknowledge the

Department of Pharmacy, MIET Meerut for providing the

characterization facility of FTIR.

R² = 0.6168

Ethical issue

Authors are aware of, and comply with, best practice in

publication ethics specifically with regard to authorship

(avoidance of guest authorship), dual submission, manipulation

of figures, competing interests and compliance with policies on

research ethics. Authors adhere to publication requirements

that submitted work is original and has not been published

elsewhere in any language.

1.2

1.4

1.6

1.8

2.2

(b)

Competing interests

The authors declare that there is no conflict of interest that

would prejudice the impartiality of this scientific work.

R² = 0.9804

Authors’ contribution

All authors of this study have a complete contribution for

data collection, data analyses and manuscript writing.

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