A Study of Phenol Adsorption Using Activated Carbon in a

Packed Bed Column

Nursyahira Ishak, Mohd. Irfan Hatim Mohamed Dzahir

School of Bioprocess Engineering, Universiti Malaysia Perlis, Perlis, Malaysia.

Abstract - The aim of this work was to present research on the removal of phenol by adsorption process
in activated carbon packed bed column. The removal of phenols from water was carried out using
activated carbon as adsorbent in the batch and column adsorption system. The parameters that was
manipulated were initial concentrations of phenol and the flow rate of the solution through the
columns. On the other hand, three isotherm models, which are Langmuir, Freundlich and Temkin
isotherm were used to investigate on the performance of curves that show the best absorption process.
Meanwhile, the breakthrough curve is used to assess the performance of the column in the adsorption
process. It has been noted that as the concentration of initial phenol solution increases, the
breakthrough curve becomes steeper and the breakthrough time decreases from 25 to 20 minutes.
Meanwhile, when the flow rate of phenol solution through the column increases, it gave rise to a
shorter time for the bed to be saturated with the adsorbate solution.

I. INTRODUCTION
Phenol which is also known as carbolic acid is one of the chemically active compounds. It is a pollutant
compounds that can be establish in the waste product of different ventures for example in oil refineries
industry, gasification industry and chemical plants [1]. In previous research by of article on phenol
biodegradation state that the annual production of this phenol compounds was more than 700 million ton
for essential and basic raw component in various ventures of chemical, pharmaceutical, petroleum and
leather [2]. Besides that, phenols which is in low concentration are generally used in household products
such as an antiseptic for home cleaning agent and as medicated solution for rinsing the mouth [3]. The
eliminating of pollutants from the industrial waters and wastewaters appeared as a crucial issue during the
last decade. Nevertheless, due to environmental laws, the efficient degradation of the pollutants from the
industrial waste has become a challenging task [4]. All types of the phenol and phenolic components get a
great concerned among others various organic pollutants that are found in the wastewater due to their high
toxicity level that may be harmful to living organisms.

There has been numerous treatment technique of these type of harmful pollutants removal which
includes biological, physical, and chemical phenol treatments method in order to discharge the an
environmentally companionate sewer water [5]. Among all of those treatment, adsorption has been
effectively used for the eliminating of organic as well as inorganic compounds from wastewater because of
its simplicity and safety [6].

In general, adsorption is the process that not target only on the volume but on the surface. It is one of
the physical treatment method of an effluent that includes the adhesion of specific particles at surface of the
particular adsorbent. Besides that, this adsorption process is one of the essential physical technique that is
classified as a low-price method in order to be used for the treatment method for the harmful effluent of
wastewater [7].

The adsorption methods by using solid adsorbent have been generally utilized to eliminate definite
groups of synthetic poisons from the waste-water for example, the phenolic compounds [8] [9]. The most
well-known adsorbent among the other adsorbent is the activated carbon due to its adsorption quality as the
most efficient adsorbents for organic synthesize particularly for phenolic component [10]. Consequently,
the adsorption process with granular adsorbents was done by using either batch technique or packed
adsorption column by continuous flow method [11].

Packed-bed column systems are employed for adsorption, desorption, rectification and direct heat
transfer processes in several industries. It can be comparatively simple scaled up for laboratory experiment
and it is also an easy to handle system. Besides that, because of the packed bed column adsorption process
has the best utilization of distinction known to be a main thrust for adsorption process and permits, more
productive use of the sorbent limit that outcomes in a superior nature of the effluent, thus the packed bed
column adsorption process is more efficient than the batch adsorption process technique [12].

II. MATERIALS

A. Chemicals
The crystallized phenol was obtained from Panreac. Sodium thiosulfate, iodine, potassium iodate and
sodium carbonate were purchased from HmBG. Meanwhile, the commercialized granular activated carbon
was purchased from Bendosen.

B. Equipments
The equipment used were the PTFE column to prepare the activated carbon packed bed column,
refractometer, vacuum oven, peristaltic pump and shaker that were located in laboratory of School of
Bioprocess Engineering, Universiti Malaysia Perlis.

III. PROCEDURES

A. Characterization of commercialized granular activated carbon

Commercialized granular activated carbon was characterized by using Scanning Electron Microscope
(SEM), Fourier Transform Infra-Red (FT-IR) and iodine number analysis.

For analysis on the surface texture and the morphology of the adsorbent which is the commercialized
granular activated carbon, scanning electron microscope was used. A small amount of sample was coated
before been tested with the scanning electron microscope. After that, the sample was fitted on the aluminum
stub utilizing carbon conductive tape. At that point, the stub was mounted on the stub holder and stacked
into the chamber before the analysis was begun. The pictures result was recorded with a Quanta 200 FEI
magnifying instrument and was appeared on the screen.

The structural groups which are present in the commercialized granular activated carbon sample was
characterized by using Fourier transfer infra-red (FT-IR) was used. A small amount of sample was placed
under a thin disc which placed in the analysis chamber and exposed to the light of the infra-red which
wavelength that was set from range 650-4000 cm−1 .
 Iodine test by adsorption of iodine from the aqueous solution was utilized to decide on the relative
initiation level of unused or reactivated carbons. Firstly, three different weight of the commercialized
granular activated carbon sample was prepared before treated by 10ml of 5% hydrochloric acid solution.
The mixture was boiled for 30 seconds and then was cooled at room temperature. After that, 100 ml of
0.1 N iodine solution was added to the mixture and stirred for 30 seconds. The solution was then filtered
and 50 ml of filtrate was titrated with 0.1 N sodium thiosulphate solution utilizing thyodene as the
indicator. The measure of the iodine that was adsorbed per gram of adsorbent was plotted against the
carbon at residual iodine concentration.

B. Preparation of phenol solution

The crystallized phenol sample was obtained from Analytical Laboratory of School of Bioprocess
Engineering, UniMAP, that was used in preparing the phenol solutions. The solution of phenol at range
1% to 8% mass of phenol (g)/volume of distilled water (ml) were prepared by dissolving the crystallized
phenol sample in distilled water by using following equation:

M1 V1 = M2 V2

Where M1 is the high or original concentration and M2 is the low or new concentration. Meanwhile, V1 is
the volume needed of original concentration and V2 is the total volume of new concentration.

C. Preparation of calibration curve and standard solutions of phenol

Calibration curve was prepared by plotting known concentration of phenol solutions ranging from 1 to
8% mass of phenol (g)/volume of distilled water (ml) versus corresponding refractive index values. The
refractive index values of these known phenol solution concentrations were measured with calibrated
refractometer. Meanwhile, the series of the sample solutions at the concentration of 2, 4, 6 and 8 % mass
of phenol (g)/volume of distilled water (ml) were prepared to be used for batch and column adsorption
process.

D. Batch equilibrium of phenol adsorption

Batch equilibrium of phenol adsorption study was performed in a packed bed column made from
polyvinyl chloride (PVC) tubing at room temperature. A fixed amount of activated carbon of 10 g was put
into the PVC tube. A sponge was set at the top and base of the section of the bed with the goal that the
activated carbon will not flow out together with the solution and to make sure of good distribution of liquid
flow into the column throughout the experiment. Phenol solution of different concentration of 2, 4, 6 and
8 % mass of phenol (g) /volume of distilled water (ml) was pumped to the column in a downward and
recycle flow by using calibrated peristaltic pump. The influence of the interaction time and inlet
concentration were investigated. The treated phenol solution that come out from bottom of the column was
taken at fixed interval time from 0.5, 1, 2, 4, 6, 9, 12, 24 and 48 hours and then were filtered with filter
paper. After filtration, the refractive index of the filtrated were measured by using the calibrated
refractometer.

i. Determination of phenol concentration

The total concentrations of the phenol after the adsorption process were calculated by measuring the
refractive index by using calibrated refractometer where the calculation from the calibration curve was
done automatically. Amount of the phenol adsorbed at equilibrium, q (mg/g) was measured by using
following equation:
 (Co − C)V
q= W

Where q is the amount of phenol adsorbed (mg/g) while Co and C are the liquid phase concentrations of
phenol at initial times and sampling times. The other two parameters are the volume of the solution, V (ml)
and mass of dry adsorbent, W (g).

ii. Isotherm studies of phenol adsorption

The interaction under the equilibrium conditions between the adsorbate and the adsorbent which is in
optimizing the use of adsorbent amount was studied by developing the isotherm model. In this study, there
are three types of isotherm models that was used which are Langmuir, Freundlich and Temkin isotherm.

E. Column adsorption studies

The column was set up by using the PTFE column of 2.5 cm internal diameter and 10 cm height. In
order to obtain the desired height of the column, the column was packed with desired amount of
commercialized granular activated carbon. Other than that, the height of the activated carbon bed was
estimated before the tests with a specific end goal to observe the variety that will be cause by the bed height.
The bed was hold set up between two attachments of sponge.

In this column study, there are two parameters that were being observed which are the initial
concentration of phenol of 2, 4 and 6% mass of phenol (g)/volume of distilled water (ml) and the flow rate
of phenol through the column of 1.0, 2.0 and 3.0 ml/min. The treated phenol sample was collected
immediately from the exit at time intervals and was measured by using the calibrated refractometer. The
change of phenol concentration in the column effluent was determined. In order to describe the packed
adsorption column performance, the breakthrough curves from the experimental data obtain was used.

F. Statistical analysis
All the shape of the curves that indicated the batch equilibrium and column adsorption process that
were used in this research study were analyzed by plotting the curves by using Microsoft Excel program.
This procedure also allowed exploring the adsorption isotherms and the breakthrough curves that involved
in this research study.

IV. RESULTS AND DISCUSSION

A. Characterization of commercialized granular activated carbon

i. Scanning electron microscope (SEM) analysis

In order to characterizing the surface morphology and fundamental physical properties of the adsorbent
used in this study which is the commercialized granular activated carbon, scanning electron microscope
(SEM) was used. Figure 1 (a-f) below shows the images from SEM analysis at three different
magnifications which are 500 x, 1000 x and 5000 x and two different spots on surface of the adsorbent.
Based on the figure obtained, there are many large pores that clearly found on the surface of the
commercialized granular activated carbon. Thus, the porous structure of the activated carbon from the well-
developed pores was led to a good possibility for phenol to be adsorbed into the pores of the adsorbent.

Other research for characterization on the surface morphology of the activated carbon also supported
this study where their finding also stated that the activated carbon was characterized by their well-
developed porosity structure in order to widely be used as adsorbents for removal of any organic chemicals
of environmental or economic concern from air, gases, potable water and wastewater [13].

a) b)

c) d)

e) f)

Figure 1: SEM images of commercialized granular activated carbon at three

different magnifications: (a) and (b): 500 x, (c) and (d): 1000 x, (e) and (f): 5000 x

ii. Fourier transform infra-red (FT-IR) analysis

In this study, the adsorbent used which is the commercialized granular activated carbon was observed
under FT-IR spectroscopy in order to figure out the functional groups of the activated carbon. Based on
Figure 2, the FT-IR spectra pattern of the commercialized granular activated carbon sample was figured
out. FT-IR spectra displaying peaks at around 2875.96, 2171.52, 1377.17 and 1001.69 cm−1 that are
characteristics of the activated carbon correspond to aromatic C-H stretching, aliphatic C≡C stretching, C-
O stretching and C-C stretching respectively.

This result has shown the similar pattern of spectra displayed as previous research on the same
adsorbent type which is an activated carbon [14]. They later found out that the FT-IR spectra of the
activated carbon have four major band which include C-H interaction with the surface of carbon at peak
2930 cm−1 and C-O stretching at 1125 cm−1 but the other two band at 3450 cm−1 are correspond to the
hydrogen bonded OH stretching mode of hydroxyl group and 1300 cm−1 amides groups at 1640 cm−1 .

From the other previous research study, the activated carbon used is very intense to aliphatic C-H
stretching absorption around 2800 cm−1 and the spectra displaying a broad band with peak around 1500
cm−1 due to C=O stretching [15]. Thus, these results are in good agreement with the findings of many
investigators from previous research study.
 Figure 2: FT-IR spectra recorded for commercialized granular activated carbon

iii. Iodine number analysis

The iodine number analysis was conducted on the commercialized granular activated carbon in order
to measure the porosity by adsorption of the iodine from solution. According to previous research, 1.0 m2
of the activated carbon internal surface area was considered by each of 1.0 mg iodine adsorbed from
solution [14].

From Table 1 below, the values of the iodine adsorbed per gram of carbon, X/M (mg/g) and the residual
filtrate, C (N) for three different weight of commercialized granular activated carbon sample were obtained.
Based on Table 1, the highest iodine adsorbed per gram of carbon is 1187.05 mg/g on the second adsorbent
sample with 0.0484 residual filtrate.

Table 1: Values of the iodine adsorbed per gram of carbon and residual filtrate
Samples C, (N) X/M,
(mg/g)
1 0.0850 825.05
2 0.0484 1187.05
3 0.0445 647.98

Meanwhile, Figure 3 below shows the results on the iodine number for the activated carbon sample by
plotting the data in Table 1. Thus, from Figure 3, the iodine number obtained is 965.41 mg/g, which is
supported by the statement in previous research study that state the iodine number for the activated carbon
varies in the range 500-1200 mg/g in order for the sorbent to be able to adsorb even a small molecule [15].
 Figure 3: Iodine absorbed per gram of carbon and residual filtrate

B. Influence of interaction time and inlet concentration

Phenol adsorption onto the commercialized granular activated carbon at different inlet concentrations
was studies as a function in order to determine the necessary equilibrium time. From Figure 4 below, it
can be seen that the amount of the adsorbate that was adsorbed onto the activated carbon was increased
with time. The efficiency of the adsorbent was indicated by the rapid uptake and the quick establishment
of equilibrium time for its use in the treatment of phenol. All the curves increase sharply in the initial
stage, signifying that their plenty of readily vacant sites which means that there are large numbers of
vacant sites existing on the surface of commercialized granular activated carbon that are available for
adsorption during the initial contact stage.

Effects Initial Concentration and Contact Time

160
amount of phenol adsorbed, q

140
120
100
80
(mg/g)

2%
60 4%
40 6%
20 8%
0
0 10 20 30 40
time (h)

Figure 4: The relationships between the amount of phenol adsorbed on commercialized granular activated
carbon at different time and various initial concentrations of phenol at room temperature

The amount of phenol adsorbed onto the commercialized activated carbon elevated from 94.44 mg/g
to 146.68 mg/g as the concentration was increased from 2% to 8% of concentration. The same results were
reported by previous research study that state a higher initial phenol concentration will enhance in the
adsorption process [16] [17].
 C. Adsorption isotherm
The equilibrium adsorption isotherm is an important in the design of the adsorption system. Three
isotherms have been applied for this study which are the Langmuir, Freundlich and Temkin isotherm.

i. Langmuir isotherm
Linearized form of Langmuir is given in Figure 5 which express the adsorption of the phenol on
commercialized granular activated carbon. The parameter involved in Langmuir isotherm such as the
maximum adsorption capacity (qmax ), Langmuir constant (K L ) and correlation coefficient (R2 ) of the
adsorbent is clear listed in Table 2.

Graph of Linearized Langmuir Isotherms

500
y = 0.006x + 57.01
400 R² = 0.9956
300
Ce/qe

200
100
0
0 10000 20000 30000 40000 50000 60000 70000
Ce

Figure 5: Linearized Langmuir isotherms for the adsorption of phenol on

commercialized granular activated carbon at room temperature

ii. Freundlich isotherm

Based on the linearized form of Freundlich isotherm which is given in Figure 6, the Freundlich
constant value (K F ), was determined as 2.2952 at room temperature which can be defined as the adsorption
or distribution coefficient and represents the quantity of phenol adsorbed on the commercialized granular
activated carbon. From Table 2, the 1/n value was 0.2428 which is between 0 and 1, that indicates the
adsorption of phenol on the activated carbon was favorable.

Graph of Linearized Freundlich Isotherms

5.1 y = 0.2428x + 2.2952
5 R² = 0.9988
4.9
ln qe

4.8
4.7
4.6
4.5
9 9.5 10 10.5 11 11.5
ln Ce

Figure 6: Linearized Freundlich isotherms for the adsorption of phenol on the

commercialized granular activated carbon at room temperature
iii. Temkin isotherm
By plotting qe versus ln Ce in Figure 7, for the adsorption of phenol on the commercialized granular
activated carbon, the linear form of Temkin isotherm was obtained. Based on Table 2, the values of Temkin
parameters (K T , B1 ) with correlation coefficients R2 was listed. The R2 of Temkin model for the adsorption
of phenol on the commercialized granular activated carbon much less fit the experimental data than that
Langmuir which in turn Freundlich isotherm model was the best.

Graph of Linearized Temkin Isotherms

200
y = 28.555x - 171.44
150 R² = 0.9919
qe

100

50

0
9 9.5 10 10.5 11 11.5
ln Ce

Figure 7: Linearized Temkin isotherms for the adsorption of phenol on the

commercialized granular activated carbon at room temperature

Table 2: Langmuir, Freundlich and Temkin parameters for the adsorption of phenol
on the commercialized granular activated carbon
Isotherm Langmuir Freundlich Temkin
Parameters isotherm isotherm isotherm
𝐪𝐦𝐚𝐱 (mg/g) 166.70 - -
𝐊 𝐋 (L/mg) 0.0001 - -
𝐑𝐋 0.1020 - -
𝐊 𝐅 (mg/g)(𝐋/ - 2.2952 -
𝐦𝐠)𝟏/𝐧
1/n - 0.2428 -
n - 4.1186 -
𝐊 𝐓 (L/mg) - - 0.0025
𝐁𝟏 - - 28.555
𝐑𝟐 0.9956 0.9988 0.9919

Based on Table 2, the three models were represented the data equilibrium because correlation
coefficients (R2 ) of three of them are above 0.90%, but the Freundlich model effectively fits the
experimental data better than Langmuir and Temkin with correlation coefficients (R2 ) 0.9988%. Thus,
based on the results of the study, the best isotherm models fitted for phenol adsorption were determined
in the order of Freundlich > Langmuir > Temkin isotherms. This result was also supported by other
researchers in previous study on phenol adsorption process [16].

D. Column Studies
The effects of the inlet concentration of the adsorbate which is the phenol solution and the volumetric
flow rate through the column on the activated carbon packed bed column are presented by using the
experimental breakthrough curves.
i. Effects of flow rate on the breakthrough curves
The effect of the flow rate through the packed bed column for the adsorption of the phenol onto the
commercialized granular activated carbon at flow rates of 1, 2 and 3 ml/min, at an inlet adsorbate
concentration of 4% and bed height of 5 cm was shown in Figure 8 below.

Experimental breakthrough curves at different values of

flow rate
1

0.8

0.6
1 ml/min
C/Co

0.4 2 ml/min

0.2 3 ml/min

0
0 50 100 time (min)150 200
Figure 8: Experimental breakthrough curves at different values of
flow rate through the packed bed column

As the flow rate was increased, the breakthrough time decrease from 60 min for 1 ml/min to 20 min
for 3 ml/min without considering the velocity variety along the bed. Along these lines, the breakthrough
curve became steeper when the flow rate was increased that pointed by the shortened of the mass transfer
zone onto the activated carbon in the packed bed column thus indicating more effective intra-particle
diffusion effects as stated in the previous research [18]. Besides that, from the research on the other studies
of packed-bed adsorption, an increasing of the flow rate through the column past certain value will cause
the adsorption rate to decrease in the residence time of the adsorbate in the column [19].

ii. Effects of inlet phenol concentration on the breakthrough curves

The effect of the inlet adsorbate solution concentrations on the breakthrough curves was depicted on
Figure 9. The inlet concentration of the phenol solutions that flow through the packed bed column were
varied from 2, 4 and 6%, at the flow rate of 2 ml/min and fixed height of bed at 5 cm. In view of Figure
9, it is seen that the breakthrough curves were taken after the ideal "S" shape profile that is characteristic
for adsorbents of little sub-atomic sizes and also of adsorbents involved small sized particles as expressed
in previous studies.
Experimental breakthrough curves at different
values of inlet phenol concentration
1
0.8
0.6
2%
C/Co

0.4 4%
0.2 6%
0
0 50 100 150 200
time (min)
Figure 9: Experimental breakthrough curves at different values of
inlet phenol concentration through the packed bed column
 It is noticed that as the initial phenol solution concentration was increased from 2 to 6%, breakthrough
curves became steeper and the breakthrough volume decreasing due to the lower mass-transfer flux from
the bulk solution to the molecule surface because of the weaker driving force [20]. Besides that, at the point
when inlet concentration was increased, it was lead a shortening of both the breakthrough time and the bed
service time that make the adsorbent was more rapidly to soaked in the packed bed section. As the inlet
concentration was increased from 2% to 6%, the breakthrough time was shortened from 25 min to 20 min.
This is attributed to a higher concentration gradient that causing a faster transport and more successful
intra-molecule dispersion [20].

V. CONCLUSION

As a conclusion, phenol adsorption by using activated carbon had been successfully carried out in a
packed bed column. From the SEM analysis, FT-IR analysis and iodine test result that was obtained, the
first objective in this study which is to characterize the commercialized granular activated carbon was
achieved. In order to assess the interaction between the inlet flow rate and the initial phenol concentration
in the packed adsorption column, the effect of the variable parameters on the breakthrough time, saturation
time and C/Co ratio was evaluated. Therefore, the second objective in this study was achieved. The
Langmuir, Freundlich and Temkin isotherm models were used to express the sorption phenomena of the
phenol to the commercialized granular activated carbon. Consequently, the linear of the experimental data
showed that the Freundlich equation best represented of phenol adsorption data as confirmed by correlation
coefficient values obtained in this study. Moreover, the adsorption of phenol from the solution by
commercialized granular activated carbon was also investigated in a continuous-flow packed-bed column.
The experimental breakthrough curves presented the “S” shape, have been determined at various flow rates
and initial concentrations of adsorbate solutions. Thus, the experimental breakthrough curves fitted well to
the experimental data. Thus, the third objective which is to evaluate the adsorption process via isotherm
studies and experimental breakthrough curve with regards to the changing of parameter of interest was
achieved.

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