Experiment no.

Adsorption Experiment using Activated Carbon

In Partial Fulfilment of the Requirements of the Course

Chemical Engineering Laboratory 2 for Chemical Engineers

Submitted by:

GROUP 1

Cusipag, Jonelou A.

Decena, Clarissa H.

Donato, Redfield M.

Lozano, John Harvey S.

Odrunia, Christine Joy P.

Tuliao, Jon Yoshe S.

Ubi n~ a, Kate Hyacinth G.

Submitted to:

Engr. Angelica Corpuz

October 2018
 Abstract

Adsorption of activated carbon as the adsorbent with a reference solution was

performed to test the effectiveness of a packed bed in purifying varying amounts of a dye
solution. The experiment started with the preparation of a five reference dye solutions namely
0, 0.2, 0.4, 0.6, 0.8 and 1.0% (w/w) using corresponding mass of dye and 250 mL ± 0.1 ml onto
which their individual densities in room temperature using a hydrometer or make use of a
density formula. The R2 value for the density versus concentration plot is 0.9923 which does
not approaches 1 close enough, so the graph was subdivided onto three parts with the
corresponding equation holding certain density limits. The next key figure for this experiment
is the determination of adsorption isotherm. Among the adsorption isotherms, the Langmuir
model and Freundlich isotherm was compared. Based from the R2 values generated, the ____
model showed the best fit model of adsorption isotherm which was R2=____. Lastly, the design
of fixed bed adsorption was determined. A new set of reference solutions of 1% (w/w) and
0.5% (w/w) was again used as an inlet to a burette loaded with activated carbon representing
the bed height. The bed height used and compared was H=10 cm and H=5 cm with a loading
concentration (Co) of 1% (w/w) and 0.5% (w/w) respectively. The effect of average volumetric
flow rate, the determination of density of the effluent and the plot of breakthrough curve was
compared per bed height and Co. The results showed that for both H=10 cm and H=5 cm, the
average volumetric flow rate using Co=0.5% (w/w) dye solution was higher compared to that
of the 1% (w/w). But individually using H=5 cm generates a higher flow rate than that of
H=5cm. This is due to the low adsorbance as the solution flows down the adsorbent which is
the greater the bed height, the higher is the adsorbance which yields to a lower flow rate. The
density of the effluent is correlated using the equations generated in the first part of the
experiment holding certain density limits to get the concentration (C). This is necessary for the
construction of the breakthrough curve (C/Co) versus the time and from which the results
indicate that at smaller bed height the effluent concentration ratio increased more rapidly than
for a higher bed height. Steeper breakthrough curve is observed for each graphs which means
that the contact time between the activated carbon and the dye solution is minimized, leading
to early breakthrough. Increasing the flow rate gave rise to a shorter time for saturation.
 Table of Contents

I. Introduction ...................................................................................................................... 1

A. Objectives .................................................................................................................... 2

II. Review of Related Literature ....................................................................................... 2

III. Materials and Methodology ......................................................................................... 5

A. Materials and Chemicals ............................................................................................ 5

B. Experimental Procedure ............................................................................................. 7

IV. Results and Discussion................................................................................................ 15

V. Conclusions and Recommendations .......................................................................... 30

A. Recommendations...................................................................................................... 30

B. Conclusions ............................................................................................................... 30

VI. References .................................................................................................................... 30

VII. Appendix ...................................................................................................................... 31

List of Figures

Figure 1.Activated carbon, a) milled carbon which is powder, b) granulated active carbon .... 3
Figure 2. Fixed bed adsorber ..................................................................................................... 4
Figure 3.Preparation of Reference Solutions setup.................................................................... 9
Figure 4. Adsorption Isotherm Determination setup ............................................................... 10
Figure 5. Design of Fixed-bed Adsorption schematic diagram ............................................... 11
Figure 6. Schematic diagram for preparation of reference solutions ....................................... 12
Figure 7.Schematic diagram for adsorption isotherm determination....................................... 13
Figure 8. Schematic diagram for design of fixed-bed adsorption ............................................ 14
Figure 9.Density versus Concentration .................................................................................... 16
Figure 10. Subdivided Equations for Density-Concentration .................................................. 17
Figure 11. Breakthrough curve for Height =10 cm at 1% (w/w) dye solution ........................ 25
Figure 12. Breakthrough curve for Height =10 cm at 0.5% (w/w) dye solution ..................... 26
Figure 13. Breakthrough curve for Height =5 cm at 1% (w/w) dye solution .......................... 28
Figure 14. Breakthrough curve for Height =5 cm at 0.5% (w/w) dye solution ....................... 29
 List of Tables

Table 1: Laboratory Materials ................................................................................................... 6

Table 2. Determination of density of individual solution ........................................................ 15
Table 3. Concentration VS. Density ........................................................................................ 16
Table 4. Average volumetric flow rate for height 10 cm and 1% (w/w) dye solution ............ 20
Table 5. Average volumetric flow rate for height 10 cm and 0.5% (w/w) dye solution ......... 20
Table 6. Average volumetric flow rate for height of 5 cm and 1% (w/w) dye solution .......... 21
Table 7. Average volumetric flow rate for height of 5 cm and 0.5% (w/w) dye solution ....... 21
Table 8. Density of effluent for height 10 cm and 1% (w/w) dye solution ............................. 22
Table 9. Density of effluent for height 10 cm and 0.5% (w/w) dye solution .......................... 22
Table 10. Density of effluent for height 5 cm and 1% (w/w) dye solution ............................. 22
Table 11. Density of effluent for height 5 cm and 0.5% (w/w) dye solution .......................... 23
Table 12. Breakthrough table for H=10 cm, Co= 1% (w/w) dye solution .............................. 24
Table 13. Breakthrough table for H=10 cm, Co=0.5% (w/w) dye solution ............................ 26
Table 14. Breakthrough table for H=5 cm, Co=1% (w/w) dye solution ................................. 28
Table 15. Breakthrough table for H=5 cm, Co=0.5% (w/w) dye solution .............................. 29
I. Introduction
Adsorption is a process in which a component of a gas or a liquid stream is removed and
adsorbed by a solid adsorbent. In this process, one or more components of a gas or liquid stream
are adsorbed on the surface of a solid adsorbent and a separation is accomplished. It involves
the transfer and resulting distribution of one or more solutes between a fluid phase and particles.
The partitioning of a single solute between fluid and sorbed phases or the selectivity of a
sorbent toward multiple solutes makes it possible to separate solutes from a bulk fluid phase or
from one another. (Wankat, 2016)

In general, adsorption involves the accumulation or depletion of solute molecules at an

interface. Gas-solid and liquid-solid interfaces with solute distributed selectively between the
fluid and solid phases are considered. The accumulation per unit area is small. Most adsorbents
are highly porous materials, and adsorption takes place primarily on the walls of the pores or
at specific sites inside the particle. Because the pores are generally very small, the internal
surface area is orders of magnitude greater than the external area. (Perry & Green, 2008)

Separation occurs because differences in molecular weight, shape, or polarity cause some
molecules to be held more strongly on the surface than others because the pores are too small
to admit the larger molecules. In many cases, the adsorbing components, or adsorbate, is held
strongly enough to permit complete removal of that component from the fluid with very little
adsorption of other components. (McCabe, Smith, & Harriott, 1993)

Adsorption can also be defined based on the strength of interaction between the adsorbent
and adsorbed molecules. The first definition is through a process that includes intermolecular
forces specifically, Van der Waals, interaction between the substrate and the adsorbate. It
would be easy to recognize this when the phenomenon is a general one and it occurs in any
fluid/solid system and when the evidence for the perturbation of the electronic states of
adsorbent and adsorbate is minimal. Also, when the adsorbed species are chemically identical
with those in the fluid phase, so that the chemical nature of the fluid is not altered by adsorption
and desorption. This is called physisorption. The other definition of adsorption lies as
chemisorption which is defined as chemical bonds involved in sticking the adsorbate to the
adsorbent. When the phenomenon is characterized by chemical specificity and when the
changes in the electronic state may be detectable by suitable physical means, it is known to be
chemisorption.

1
 The process opposite of adsorption is known as desorption or stripping. This is
characterized by the release of a substance from another from the surface or through the surface.
When an equilibrium situation between a bulk phase and an adsorbing surface is altered,
desorption occurs. After adsorption, the adsorbed chemical will stay on the substrate
indefinitely, if the temperature remains low. However, as temperature rises, desorption is meant
to occur. (Geankoplis, Hersel, & Lepek, 2018)

In this experiment, performance of a packed bed of activated carbon adsorbent to purify or

cleanse varying concentrations of dye solution is evaluated.

A. Objectives
Generally, the objective of this experiment is to evaluate the performance of a packed bed
of activated carbon adsorbent to purify or cleanse varying concentrations of dye solution.
Specifically, it aims to:

a. Determine the best adsorption isotherm model

b. Design of a fixed bed adsorption
i. Determine the effect different parameters such as volumetric flow rate, compacted
bed height and initial concentration on the adsorption process

II. Review of Related Literature

Adsorption has been extensively studied as a cost effective method for removing a wide
variety of hazardous materials, such as dyes and heavy metals, from aqueous solutions. The
most widely used adsorbent for separating the pollutants is activated carbon. Most adsorption
research focused on the isotherm, kinetic, and thermodynamic processes. For the adsorption
process, an analysis of the isotherm data is important because the isotherms describe
equilibrium relationships between adsorbent and adsorbate, usually the ratio between the
quantity adsorbed and that remaining in the solution at a fixed temperature at equilibrium. The
distribution of dye between the adsorbent and dye solution, when the system is in a state of
equilibrium, is important in establishing the capacity of the adsorbent for the dyes (Mall,
Srivastava, & Agarwal, 2006). The capacity of activated carbon for a given pollutant is usually
determined by carrying out an adsorption isotherm.

Adsorption isotherms show the dependence of the amount of adsorbed substance from the
solution concentration at constant temperature. The adsorption capacity of adsorbent is
determined by using the adsorption isotherm models. The most commonly used iso-therms for

2
modelling adsorption processes in liquid phase are the Freundlich and Langmuir isotherm
models. Adsorption isotherms help to design experimental system and to evaluate it, based on
isotherm models, such as Freundlich and Langmuir isotherm models, and to find out a deviation
between experimental data and isotherm models. Adsorption isotherms are helping to describe
surface processes of adsorbent, type of adsorbate monolayer or mul-tilayer and capacity of
adsorbent, which were used for this work. (Willis, 2009), (Repo, 2011)

The Langmuir isotherm derived from assuming a uniform surface applies well for gases
that are weakly adsorbed given by the relation W=Wmax (Kc/(1+Kc)); whereas Freundlich
equation W=bcm, where b and m are constants and m<1, fits well for liquids.

Activated carbon (Fig. 1) is the well-known adsorbent which is widely used in many
industries, such as water treatment and medical production. It has exceptionally strong
adsorption properties and complicated structure. Activated carbon can be produced by physical
or chemical activation from material such as coal, lignite, nutshells, peat, wood and petroleum
pitches.

Figure 1.Activated carbon, a) milled carbon which is powder, b) granulated active carbon

A fixed-bed adsorption system is a widely used method for the adsorption of solutes
from fluids. Granular particles are packed inside a fixed-bed. The liquid to be treated is passed
down through the packed bed at a constant flow rate. But in cases of gases, it works as the
opposite, it starts from the bottom and with the use of a blower, it would go up. Resistance to
mass transfer are important in the process and this would be in an unsteady state. The efficiency
of the process is determined by the overall dynamics of the system rather than just the
equilibrium considerations.

3
 Figure 2. Fixed bed adsorber

The major part of adsorption takes place in a relatively narrow adsorption or mass-
transfer zone at any time. As the solution continues to flow, the S-shaped mass-transfer zone
moves down the column. The concentration in the outlet becomes zero until the mass-transfer
zone starts to reach the tower outlet at a given time t4. Then, an outlet concentration starts to
rise and at time t5, the outlet concentration has risen to a point called the break-point.

Breakthrough concentration curve

A breakthrough curve in adsorption is the course of the effluent adsorptive

concentration at the outlet of a fixed-bed adsorber. This is important for adsorptive separation
technologies and for the characterization of porous materials.

After the break-point time is reached, the concentration rises rapidly up to the end of
the breakthrough curve where the bed is considered ineffective. The break-point concentration
represents the maximum that can be discarded and is often taken as 0.05 to 0.1.

4
III. Materials and Methodology
A. Materials and Chemicals
The materials used for this experiment are shown in Table 1 as follows:

Materials/ Equipment Description

1. Beaker Beaker is a common container in most labs.
It is used for mixing, stirring, and heating
chemicals. Most beakers have spouts on their
rims to aid in pouring. They also commonly
have lips around their rims and markings to
measure the volume they contain, although
they are not a precise way to measure liquids.
In this experiment, beaker sizes of 25 mL and
250 mL are used.
2. Stirring Rod A glass stirring rod, glass rod, stirring
rod or stir rod is a piece of laboratory
equipment used to mix chemicals and liquids
for laboratory purposes. They are usually
made of solid glass, about the thickness and
slightly longer than a drinking straw, with
rounded ends
3. Graduated Cylinder This is a primary measuring tool for the
volume of a liquid. There are several
markings up and down the length of the
container with specific increments. The
smaller they are in diameter, the more
specific the volume measurements will be.
Graduated cylinder of sizes 250 mL and 25
mL are used.

4. Funnel A funnel is a pipe with a wide (often conical)

mouth and a narrow stem. It is used to
channel liquid or fine-grained substances
into containers with a small opening.

5
 Without a funnel, spillage may occur. a tube
or pipe that is wide at the top and narrow at
the bottom, used for guiding liquid or powder
into a small opening.

5. Burette A burette (also buret) is a laboratory

equipment used in analytical chemistry for
the dispensing of variable amount of a
chemical solution and measuring that amount
at the same time. It is a long, graduated glass
tube, with a stopcock at its lower end and a
tapered capillary tube at the stopcock's outlet.
A 50 mL burette is used in this experiment.
6. Balance A balance is used to weigh chemicals. The
chemicals are always in some form of
container and never placed directly on the
balance. It is important not to move a balance
because they have been calibrated for the
exact position they are in.

Table 1: Laboratory Materials

Other materials not mentioned in the table are the following: filter paper, funnel, stop watch
and ruler. The chemical used in this experiment are activated carbon which is the adsorbent in
granular form of about 200 grams, a dyeing agent, the adsorbate, in powder form (of about 15-
20 packs, each pack consisting 2 grams) and distilled water as the solvent (we used at most 6L
for the whole procedure) which is used for the preparation for the different dye concentrations.

6
 B. Experimental Procedure
i. Preparation of Reference Solutions
For the preparation of reference solution, prepare 250 ± 1 mL with 0, 0.2, 0.4, 0.6, 0.8 and
1% w/w dye solution using distilled water as the solvent, to do this 0 g of dye must be added
to 250 ± 1 mL distilled water to produce 0% w/w dye solution, 0.510 ± 0.01 g of dye must be
added to 250 ± 1 mL distilled water to produce 0.2% w/w dye solution, 1.01 ± 0.01 g of dye
must be added to 250 ± 1 mL distilled water to produce 0.4% w/w dye solution, 1.51 ± 0.01 g
of dye must be added to 250 ± 1 mL distilled water to produce 0.6% w/w dye solution, 2.02 ±
0.01 g of dye must be added to 250 ± 1 mL distilled water to produce 0.8% w/w dye solution,
2.53 ± 0.01 g of dye must be added to 250 ± 1 mL distilled water to produce 1.0% w/w dye
solution. After that, determine the density of the individual solution at room temperature using
the hydrometer, this is done by placing the solution in a 250 ± 1 mL graduated cylinder then
let the hydrometer float in it and then read the measurement. Next, make a plot with the
concentration as a function of density using Microsoft excel. Then, determine the best equation
that represents the experimental data by getting the equation with R value nearest to 1.

ii. Adsorption Isotherm Determination

To determine the most adequate adsorption isotherm certain steps are followed. First, weigh
5 sets of 5 ± 0.01 g of activated carbon using the analytical balance then place into 5 beakers
with a volume of 250 ± 1 mL each. After that, pour 200 ± 1 mL of 0.2, 0.4, 0.6, 0.8 and 1%
w/w dye solution in each beaker with the activated carbon, respectively. Stir the solution every
minute. Then, for every 2 minutes measure the density of each set-up by getting a certain
volume from the mixture then weighing that on the analytical balance then apply the mass over
volume approach. The determination of density is continued until the obtained density is
deemed constant with respect to time. After that, using the equation obtained in the first set of
procedures correlate the measured density to concentration. Then determine the amount of
solute adsorbed per unit amount of adsorbent used (W), to do this this is done by decanting the
mixture then weighing the decanted solution then subtract it from its original weight. After
doing this, plot the amount of solute adsorbed per unit amount of adsorbent used (W) as a
function of the equilibrium concentration (c). Lastly, determine the best isotherm that
represents the adsorption process by getting the equation with R value nearest to 1.

7
 iii. Design of Fixed-bed Adsorption

For the design of a fixed-bed adsorption, it was represented onto a burette loaded with a
predetermined amount of activated carbon until it reaches a compacted height of 10 cm. Then
the weight of burette and the weight of burette filled with 10 cm amount of activated carbon
was measured. The weight of activated carbon was obtained by subtracting the weight of the
loaded burette of 10 cm activated carbon minus that to the weight of burette. After the 10 cm
load of activated carbon in a burette, it was set-up in the iron stand.

A new 1% w/w dye solution was prepared by using 250 mL of distilled water and 2.54 ±
0.01 g of dye. The solution of 1 % w/w dye solution was filled in a graduated cylinder. After
that, the burette’s stopcock was set quarterly open. The 1% w/w solution was poured into the
burette containing the 10 cm load of activated carbon. The timer was started to about 10
minutes and the effluent volume was recorded using a 25 mL graduated cylinder. The mass of
the 25 mL graduated cylinder containing the effluent volume was measured using a balance.
The mass also of the 25 mL graduated cylinder was measured. The final mass of the effluent
was determined by subtracting the mass of the 25 mL graduated cylinder to the mass of the
empty 25 mL graduated cylinder. This is necessary to determine the average volumetric flow
rate and the density of the effluent. For the average volumetric flow rate expressed in mL/min,
it can be determined by dividing the effluent volume to that of the time which is 10 min. And
for the density expressed in g/mL, it is determined by dividing the final mass of the effluent to
that of the final volume of the effluent. The determination of density of the effluent was done
for number of trials of set of 10 minutes until the density of the effluent is constant.

The same set of procedures were done also for 0.5% w/w solution and using 10 cm of
burette-loaded activated carbon referring to the packed bed height , packed bed height of 5 cm
and 0.5% w/w dye solution and lastly packed bed height of 5 cm and 1% w/w dye solution.
The preparation of 0.5 % w/w solution was prepared by using 1.26 ± 0.01 g of dye and 250 mL
of distilled water. The density determined is correlated by plotting the density versus the
concentration of the effluent. The breakthrough curve is then generated by plotting C/Co versus
time. Lastly, height of used bed (HB) and height of unused bed (HUB) is determined by using
the formula indicated in the literature.

8
I. Preparation of Reference Solutions

dye dye dye dye dye

H2O H2O H2O H2O H2O

Determining density using a Hydrometer

Hydrometer

Decanted
solution

Figure 3.Preparation of Reference Solutions setup

9
II. Determination of Adsorption Isotherm

Preparation of solution with activated carbon

Decanting

Solution
Activated
carbon

Stirring Determining density using mass over

volume approach

Figure 4. Adsorption Isotherm Determination setup

10
III. Design of Fixed-bed adsorption

Adsorption bed setup

Bed height (height onto which activated

carbon is filled)

Effluent

Figure 5. Design of Fixed-bed Adsorption schematic diagram

11
1. Preparation of Reference Solutions

Prepare
0
0.2% w/w (0.501 g activated carbon + 250 ml water);
0.4% w/w (1.004 g activated carbon + 250 ml water);
0.6% w/w (1.509 g activated carbon + 250 ml water);
0.8% w/w (2.016 g activated carbon + 250 ml water);
1% w/w (2.525 g activated carbon + 250 ml water)
dye solution. Use distilled water as the solvent.

Determine the density of the individual solution at room

temperature. Take note that the density data in Table 1
was acquired by using a hydrometer. For the succeeding
densities, this formula is being used:
mass _ of _ solution

volume _ of _ solution

Plot the concentration as a function of density using

Microsoft Excel

Determine the best equation that represents the

experimental data using Microsoft Excel

Figure 6. Schematic diagram for preparation of reference solutions

12
2. Adsorption Isotherm Determination

Load 5 grams of activated carbon into 5 beakers (250 ml)

Pour 200 ml of 0, 0.2, 0.4, 0.6, 0.8, and 1% w/w dye

solution in each beaker, respectively.

Stir the solution every 1 minute

Measure the density of each set-up every 2 minutes. (Use

the formula indicated in the 2nd step in preparation of
reference solutions to get the density) Measured
Density is
not
Return the withdrawn liquid after measuring the density constant

Measured density is constant

Correlate the measured density to concentration using the

equation obtained from step 1.4

Determine the amount adsorbed per unit amount of

adsorbent W

Plot W as a function of the equilibrium concentration C

Determine the best isotherm that represents the

adsorption process

Figure 7.Schematic diagram for adsorption isotherm determination

13
 3. Design of Fixed-bed adsorption

Load a predetermined amount of activated carbon in the

burette until it reaches a compared height of 10 cm

Record the weight of the activated carbon

Set-up the burette in the iron stand

Fill the graduated cylinder with 1% w/w solution

Set the stopcock of the burette quarterly open then start

the timer.

Determine the average volumetric rate

Collect a measurable volume of the effluent every 10

minutes from the outlet of the burette

Determine the density of the effluent (Use the formula

indicated in the 2nd step in preparation of reference
solutions to get the density) Measured
density is
not constant
Measured density is constant

Correlate the densities in terms of concentrations

Plot the break through curve (c/co vs time)

Repeat the entire experiment for a compacted bed height

of 10 cm, stopcock half-open and loading concentration
of 0.1% and 0.5% w/w dye solution.

Figure 8. Schematic diagram for design of fixed-bed adsorption

14
IV. Results and Discussion
Gathered Data

I. Preparation of Reference Solutions

i. Determination of density of reference solutions
mwater (g) mdye (g) Wt % (g/g)  (g/ml)
(± 1 ml) (± 0.01) (±0.0005)
250 0.510 0.204 0.990
250 1.01 0.402 0.990
250 1.51 0.600 0.992
250 2.02 0.802 0.994
250 2.53 1 0.998
250 _ 0.000 0.985
Table 2. Determination of density of individual solution

Take note that the standard density of water at 1 atmospheric pressure and 25 oC is
approximately 1000 kg/m3 (1 g/ml). The volume of prepared water at each beaker is 250 ml
therefore, the mass of water being calculated for each beaker is 250 g. The mathematical
representation for mwater calculation is;

mass water
  * volume
1g
mass water
 * 250ml
ml
mass water
 250 g

This explains why the uncertainty for the mass of water is in terms of volume instead of
mass.

15
 ii. Concentration VS. Density Plot

Density Concentration
0.985 0
0.99 0.00204
0.993 0.00402
0.996 0.006
0.997 0.00802
0.999 0.01
Table 3. Concentration VS. Density

Density VS. Concentration

0.012
0.01
0.01 y = 37.359x2 - 73.412x + 36.065
R² = 0.9923
0.00802
0.008
0.006
0.006
0.00402
0.004
0.00204
0.002
0
0
0.984 0.986 0.988 0.99 0.992 0.994 0.996 0.998 1

Figure 9.Density versus Concentration

Since the R2 does not approaches 1 close enough, the data representing the graph will be
cut into three parts.

16
 iii. Determination of best equation that represents the experimental data using
Microsoft Excel

Subdivided Equations for Density-Concentration

0.012

0.01
0.01
y = 0.99x - 0.979
0.00802 R² = 1
0.008

0.006y = 2.02x - 2.0059

Concentration

0.006 R² = 1
0.00402
0.004 y = 0.66x - 0.6514
R² = 1
0.00204
0.002

0 y = 0.408x - 0.4019
0 R² = 1
0.98 0.99 1 1.01 1.02 1.03 1.04 1.05 1.06

-0.002
Density (g/ml)

Eqn 1 Eqn 2 Eqn 3 Eqn 4

Figure 10. Subdivided Equations for Density-Concentration

The corresponding equation of every part will be identified with respect to its interval. This
method will be used for the reason that the graphing by parts is more accurate than graphing
by whole. We take into consideration that for every equations hold, a corresponding density
limit must be applied.

Equation 1 …… y = 0.408x - 0.4019

Equation 2 …… y = 0.66x - 0.6514
Equation 3 …… y = 2.02x - 2.0059
Equation 4 …… y = 0.99x - 0.979

Therefore
At 0.985<density<0.99, Eqn 1 will be used
At 0.99<density<0.996, Eqn 2 will be used
At 0.996<density<0.997, Eqn 3 will be used
At 0.997<density<0.999, Equation 4 will be used

17
 Where y-concentration and x-density

II. Gathered Data for Adsorption Isotherm Determination

Density
Beaker Number
3 min 6 min 9 min

1 0.959 0.950 0.950

2 0.975 0.951

3 0.976 0.965

4 0.985 0.966

5 0.999 0.972

III. Gathered Data for the Design of Fixed-bed Adsorption

Raw Data
a. For bed height of 10 cm and loading concentration of 1% (w/w)
Height 10 cm activated carbon
mburette 0.1 kg ± 0.5 g
mburette + m10cm activated carbon 0.105 kg ± 0.5 g
m10cm activated carbon 0.005 kg (± 0.5 g)
1% (w/w) dye solution:
mdye 2.54 ± 0.01 g
vwater 250 ml
Bed Height: 10 cm

Loading Concentration: 1% (w/w) dye solution

Stopcock Opening: Quarterly open

b. For bed height of 10 cm and loading concentration of 0.5% (w/w)

Height 10 cm activated carbon
mburette 0.1 kg ± 0.5 g
mburette + m10cm activated carbon 0.105 kg ± 0.5 g

18
 m10cm activated carbon 0.005 kg (± 0.5 g)
0.5% (w/w) dye solution:
mdye 1.26 ± 0.01 g
vwater 250 ml
Bed Height: 10 cm
Loading Concentration: 0.5% (w/w) dye solution
Stopcock Opening: Quarterly open
c. For bed height of 5 cm and loading concentration of 1% (w/w)

Height 5 cm activated carbon

mburette 0.1 kg ± 0.5 g
mburette + m10cm activated carbon 0.103 kg ± 0.5 g
m10cm activated carbon 0.003 kg (± 0.5 g)
1% (w/w) dye solution:
mdye 2.54 ± 0.01 g
vwater 250 ml

Bed Height: 5 cm

Loading Concentration: 1% (w/w) dye solution

Stopcock Opening: Quarterly open

d. For bed height of 5 cm and loading concentration of 0.5% (w/w)

Height 5 cm activated carbon

mburette 0.1 kg ± 0.5 g
mburette + m10cm activated carbon 0.103 kg ± 0.5 g
m10cm activated carbon 0.003 kg (± 0.5 g)
1% (w/w) dye solution:
mdye 1.26 ± 0.01 g
vwater 250 ml

19
 Bed Height: 5 cm

Loading Concentration: 0.5% (w/w) dye solution

Stopcock Opening: Quarterly open

i. Determination of Average Volumetric flow rate

a. For bed height of 10 cm and loading concentration of 1% (w/w)

Time (min) Volume (ml) ± 0.1 ml Volumetric Flowrate (mL/min)

10 19.5 1.95
20 22.5 2.25
30 34.8 3.48
40 30.0 3.00
50 26.2 2.62
60 26.7 2.67
Average Volumetric Flowrate: 2.66 mL/min

Table 4. Average volumetric flow rate for height 10 cm and 1% (w/w) dye
solution

b. For bed height of 10 cm and loading concentration of 0.5% (w/w)

Volumetric Flow Rate

Time(min) Volume (±0.1 ml)
mL/min
10 38.6 3.86308
20 70.5 7.053
30 75.7 7.57
40 63.0 6.3
Average Volumetric Flow Rate: 6.19652 mL/min
Table 5. Average volumetric flow rate for height 10 cm and 0.5% (w/w) dye solution

Comparing Table 2 and Table 3, of the same bed height of 10 cm but of different initial
loading concentration, a higher volumetric flow rate is achieved for a loading concentration of
0.5% (w/w) than 1.0% (w/w) dye solution. For every loading concentration introduced into the
burette, it adsorbs as it flows down as it has contacted the adsorbent’s surface. When the flow
rate of the effluent’s solution for 0.5% (w/w) loading concentration is higher than 1% (w/w)

20
dye solution, less is adsorbed hence more flow rate flows. The same is also achieved for Table
6 and 7.

c. For bed height of 5 cm and loading concentration of 1% (w/w)

Volume of solution
Time(min) Volumetric Flowrate (mL/min)
(±0.1 ml)
10 83.9 8.394763343
20 70.0 7
30 60.4 6.03707
40 43.0 4.3025
Average Volumetric Flow Rate: 6.433583336 mL/min
Table 6. Average volumetric flow rate for height of 5 cm and 1% (w/w) dye solution

d. For bed height of 5 cm and loading concentration of 0.5% (w/w)

Volume of solution
Time(min) Volumetric Flowrate (mL/min)
(±0.1 ml)
10 115.0 11.5
20 144.0 14.4
30 122.0 12.2
40 116.5 11.65
50 119.8 11.98
Average Volumetric Flow Rate: 12.346 mL/min
Table 7. Average volumetric flow rate for height of 5 cm and 0.5% (w/w) dye solution

Comparing Table 2 and Table 3, of the same bed height of 10 cm but of different initial
loading concentration, a higher volumetric flow rate is achieved for a loading concentration
of % (w/w) dye solution.

ii. Determination of Density of Effluent

a. For bed height of 10 cm and loading concentration of 1% (w/w)

Mass of 25 mL Graduated Mass of Volume of Density of

Time(min)
Cylinder + Solution Solution solution Solution

21
 (±0.01 g) (±0.01 g) (±0.1 ml) (±0.1 g/ml)

10 55.4 19.31 19.5 0.990

20 58.88 22.32 22.5 0.992
30 68.02 34.52 34.8 0.993
40 66.09 29.89 30.0 0.996
50 62.4000 26.16 26.2 0.999
60 62.8700 26.686 26.7 1.000
Table 8. Density of effluent for height 10 cm and 1% (w/w) dye solution

b. For bed height of 10 cm and loading concentration of 0.5% (w/w)

Time(min) Mass of 25 mL Graduated Mass of Volume of Density of

Cylinder + Solution Solution solution Solution
(±0.01 g) (±0.01 g) (±0.1 ml) (±0.1 g/ml)
10 189.49 38.09 38.6 0.986
20 372.42 69.62 70.5 0.987
30 292.54 75.3215 75.7 0.995
40 282.93 62.874 63.0 0.998
Table 9. Density of effluent for height 10 cm and 0.5% (w/w) dye solution

c. For bed height of 5 cm and loading concentration of 1% (w/w)

Mass of 25 mL
Mass of Volume of Density of
Graduated
Time(min) Solution solution Solution
Cylinder + Solution
(±0.01 g) (±0.01 g) (±0.1 ml) (±0.1 g/ml)
10 374.88 83.36 83.9 0.993
20 288.24 69.6 70.0 0.994
30 278.89 60.25 60.4 0.998
40 188.79 43.03 43.0 1.000
Table 10. Density of effluent for height 5 cm and 1% (w/w) dye solution

d. For bed height of 5 cm and loading concentration of 0.5% (w/w)

22
 Mass of 25 mL Graduated Mass of Volume of Density of
Time(min) Cylinder + Solution Solution solution Solution
(±0.01 g) (±0.01 g) (±0.1 ml) (±0.1 g/ml)
10 477.43 113.85 115.0 0.990
20 577.33 143.136 144.0 0.994
30 483.91 121.268 122.0 0.994
40 477.62 116.1505 116.5 0.997
50 480.23 119.67 119.8 0.999
Table 11. Density of effluent for height 5 cm and 0.5% (w/w) dye solution

iii. Correlation of Density in terms of concentration

To correlate the density in terms of concentration, we use the 4 equations generated in part
A for which density limits are hold to determine the concentration for the analysis of
breakthrough curve which are the following:

Where:
Equation 1 …… y = 0.408x - 0.4019 y-concentration
Equation 2 …… y = 0.66x - 0.6514 x-density
Equation 3 …… y = 2.02x - 2.0059
Equation 4 …… y = 0.99x - 0.979

Therefore
At 0.985<density<0.99, Eqn 1 will be used
At 0.99<density<0.996, Eqn 2 will be used
At 0.996<density<0.997, Eqn 3 will be used
At 0.997<density<0.999, Equation 4 will be used

a. For bed height of 10 cm and loading concentration of 1% (w/w)

Density of Holds
Concentration
Time(min) Solution for Co C/co
(y)
(±0.1 g/ml) Equation
10 0.990 1 0.002124615 0.01 0.212462
30 0.992 2 0.00332 0.01 0.332

23
 40 0.993 2 0.003980818 0.01 0.39808
50 0.996 3 0.006693333 0.01 0.66933
60 0.999 4 0.012094348 0.01 1.20943
70 1.000 4 0.014024308 0.01 1.40243

Density VS. Concentration

0.016
0.014
R² = 0.9519
0.012
Concentration C

0.01
0.008
0.006
0.004
0.002
0
0.988 0.990 0.992 0.994 0.996 0.998 1.000 1.002
Density

Time(min) C/co
10 0.212462
20 0.332
30 0.39808
40 0.66933
50 1.20943
60 1.40243
Table 12. Breakthrough table for H=10 cm, Co= 1% (w/w) dye solution

24
 Breakthrough Curve @H=10 cm, 1% (w/w) dye solution
1.6
1.4
1.2
1
C/Co

0.8
0.6 2.491 mL/min

0.4
0.2
0
0 10 20 30 40 50 60 70
Time

Figure 11. Breakthrough curve for Height =10 cm at 1% (w/w) dye solution

Figure 4 shows the breakthrough curve for height of 10 cm at 1% (w/w) dye solution. Based
from the graph, of an average volumetric flow rate of 2.491 mL/min, there is a steady increasing
of breakthrough concentration at a time from 10 to 30 min which indicates a slow uptake of
dye. As time progresses, the breakthrough curve becomes steep and breakthrough is reached
quickly because of the residence time of the dye solution in the column, which is long enough
for adsorption equilibrium to be reached at high flow rate.

b. For bed height of 10 cm and loading concentration of 0.5% (w/w)

Density of
Holds
Solution
Time(min) for C Co C/Co
(±0.1
Equation
g/ml)
10 0.986 1 0.00038833 0.005 0.077666
20 0.987 1 0.000835857 0.005 0.167171
30 0.995 2 0.0053 0.005 1.06
40 0.998 4 0.00902 0.005 1.804

25
 Density VS. Concentration
0.01
0.009
0.008 R² = 0.9699

0.007
Concentration C

0.006
0.005
0.004
0.003
0.002
0.001
0
0.984 0.986 0.988 0.990 0.992 0.994 0.996 0.998 1.000
Density

Time(min) C/Co

10 0.077666
20 0.167171
30 1.06
40 1.804
Table 13. Breakthrough table for H=10 cm, Co=0.5% (w/w) dye solution

Breakthrough Curve @H=10 cm, 0.5% (w/w) dye

solution
2
1.8
1.6
1.4
1.2
C/Co

1
0.8 6.19652 mL/min
0.6
0.4
0.2
0
0 10 20 30 40 50
Time

Figure 12. Breakthrough curve for Height =10 cm at 0.5% (w/w) dye solution

26
 Figure 5 shows the generated breakthrough curve for a bed height of 10 cm at 0.5% (w/w)
loading concentration. As can be seen from the figure, breakthrough curve becomes steeper as
time progresses which means that the contact time between the activated carbon and the dye
solution is minimized, leading to early breakthrough.

c. For bed height of 5 cm and loading concentration of 1% (w/w)

Density of Holds
Time(min) Solution for concentration, C Co C/Co
(±0.1 g/ml) Equation
10 0.993 2 0.00398 0.01 0.398
20 0.994 2 0.004828571 0.01 0.482857
30 0.998 4 0.009020679 0.01 0.902068
40 1.000 4 0.011115049 0.01 1.111505

Density VS. Concentration

0.012
R² = 0.9964
0.01
Concentration, C

0.008

0.006

0.004

0.002

0
0.992 0.993 0.994 0.995 0.996 0.997 0.998 0.999 1.000 1.001
Density

Time(min)
C/Co

10 0.398000003
20 0.482857143
30 0.902067891
40 1.111504939

27
 Table 14. Breakthrough table for H=5 cm, Co=1% (w/w) dye solution

Breakthrough Curve @H=5 cm, 1% (w/w) dye solution

1.2

0.8
C/Co

0.6
6.43358 mL/min
0.4

0.2

0
0 10 20 30 40 50
Time

Figure 13. Breakthrough curve for Height =5 cm at 1% (w/w) dye solution

Figure 6 shows the measure of C/Co over time for height equal to 5 cm at 1% dye solution.
Slow uptake of dye is noticed in the initial stage and rate increased thereafter and finally
reached saturation. As flow rate increased, the breakthrough curve becomes steep and
breakthrough is reached quickly. This is because of the residence time of the dye solution in
the column, which is long enough for adsorption equilibrium to be reached at high flow rate.
Steeper breakthrough curve means that the contact time between the activated carbon and the
dye solution is minimized, leading to early breakthrough. Increasing the flow rate gave rise to
a shorter time for saturation.

a. For bed height of 5 cm and loading concentration of 0.5% (w/w)

Density of Solution
Time(min) Holds for Equation C Co C/Co
(±0.1 g/ml)
10 0.990 1 0.00202 0.005 0.404
20 0.994 2 0.00464 0.005 0.928
30 0.994 2 0.00464 0.005 0.928
40 0.997 3 0.00804 0.005 1.608
50 0.999 4 0.00992571 0.005 1.985142

28
 Density VS. Concentration
0.012

0.01
Concentration C R² = 0.977

0.008

0.006

0.004

0.002

0
0.988 0.990 0.992 0.994 0.996 0.998 1.000
Density

Time(min) C/Co

10 0.404
20 0.928
30 0.928
40 1.608
50 1.985141903
Table 15. Breakthrough table for H=5 cm, Co=0.5% (w/w) dye solution

Breakthrough Curve @ H=5cm, 0.5% (w/w) dye

solution
2.5

1.5
C/Co

1 12.346 mL/min

0.5

0
0 10 20 30 40 50 60
Time

Figure 14. Breakthrough curve for Height =5 cm at 0.5% (w/w) dye solution

29
 Based from Figure 7, it can be concluded that there is rapid uptake of the dye solution in
the initial stage, after 10 seconds the rate decreases and the rate increased thereafter and finally
saturation is reached. The results indicate that at smaller bed height the effluent concentration
ratio increased more rapidly than for a higher bed height. An increase in the flow rate decreases
the volume of dye solution treated; consequently, this decreases the service time of the
activated carbon bed. The data satisfies from the experiment proves the theoretical assumption
of a break through curve (when the slope at the center part of the S curve stays constant, this
means the column saturation is achieved).

V. Conclusions and Recommendations

A. Recommendations

B. Conclusions

VI. References
Geankoplis, C., Hersel, A. H., & Lepek, D. H. (2018). Transport Processes and Separation
Process Principles (5th ed.). Prentice-Hall International, Inc.

Mall, I., Srivastava, V., & Agarwal, N. (2006). Removal of Orange-G and methyl violet dyes
by adsorption onto bagasse fly ash kinetic study and equilibrium isotherm analyses.
Dyes and Pigments, 210-223.

McCabe, W., Smith, J., & Harriott, P. (1993). Unit Operations of Chemical Engineering, 5th
edition. McGraw-Hill, Inc.

Perry, R., & Green, D. (2008). Perry's Chemical Engineers' Handbook. McGraw-Hill.

Repo, E. (2011). EDTA- and DTPA- Functionalized Silica Gel and Chitosan Adsorbents
bents for the Removal of Heavy Metals From Aqueous Solutions. Thesis,
Lappeenranta Uni-versity of Technology.

Wankat, P. C. (2016). Separation Process Engineering: Mass Transfer Analysis, 4th edition.
Prentice-Hall International, Inc.

Willis, T. (2009). Sorbents – Properties, Materials and Applications. New York: Nova
Science Publishers, Inc.

30
VII. Appendix
Raw Data for Bed height = 10 cm, C=1% (w/w) dye solution

Density Error

Concentration Error

Raw Data for Bed height = 5 cm, C=1% (w/w) dye solution

31
Density error

Concentration

Raw Data for Bed height = 10 cm, C=0.5% (w/w) dye solution

32
Density error

Concentration

Raw Data for Bed height = 5 cm, C=0.5% (w/w) dye solution

Density error

33
Concentration

Design of Fixed Bed adsorption

i. Determination of density of the effluent

34
ii. Determination of the average volumetric flow rate

iii. Correlation of the density in terms of concentration

35
Construction of breakthrough curve

NOTE: Sample used is using Bed height of 10 cm at 1% (w/w) loading concentration

of dye

36