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Lab report

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concentrations of dye solution was evaluated in this experiment. The equation correlating the

density and the weight-by-weight percent dye concentration of a reference solution was found

out be y=0.0849x-0.0784. The adsorption isotherm representing the dye adsorption with the

highest coefficient of determination equal to 0.9604 was Freundlich Isotherm and was

represented by the equation w 18.1472175c 0.9834117406 . On the other hand, the effect of bed

height, initial concentration of the solution, and volumetric flowrate on the adsorption process

was also determined. Based on the breakthrough curves obtained, it was said that the 10 cm

bed height, compared to 5 cm, took longer time to make the bed totally saturated due to more

mass transfer zones on the bed. As per the effect of the initial concentration, in 1.0 %w/w

solution, the time when the bed became saturated was reached earlier compared to that of the

0.5 %w/w solution. This was because there is high concentration gradient or driving force

between the bed and the fluid. However, both these can be affected by the volumetric flowrate.

The main reason observed is that the higher the volumetric flowrate, the more mass of solute

will be exposed to adsorbent, taking it lesser time for the bed to be saturated. This accounts to

the random errors propagated during the experiment. Finally, an adsorption column with a

breakthrough concentration of 0.01 capable of operating for 12 hours was designed. It was

found out that the bed height must be 809.32 cm and the bed’s saturation capacity was 0.3555

grams of dye per gram of activated carbon.

TABLE OF CONTENTS

I. INTRODUCTION ............................................................................................................... 1

II. THEORETICAL BACKGROUND ..................................................................................... 2

A. EQUILIBRIUM RELATIONS FOR ADSORBENTS ......................................................................... 2

B. FIXED-BED ADSORPTION COLUMNS ........................................................................................ 3

C. BREAKTHROUGH CONCENTRATION CURVE ............................................................................ 4

D. CAPACITY OF THE COLUMN...................................................................................................... 4

A. MATERIALS ................................................................................................................................ 6

B. SCHEMATIC DIAGRAM .............................................................................................................. 7

C. METHODOLOGY ....................................................................................................................... 12

A. DETERMINATION OF EQUATION CORRELATING THE DENSITY AND CONCENTRATION ....... 14

B. DETERMINATION OF ADSORPTION ISOTHERM ....................................................................... 16

C. DETERMINATION OF THE EFFECT OF DIFFERENT PARAMETERS SUCH AS VOLUMETRIC

FLOWRATE, COMPACTED BED HEIGHT, AND INITIAL CONCENTRATION ON THE

V. CONCLUSION ................................................................................................................. 32

VI. RECOMMENDATIONS ................................................................................................... 34

VII. STUDY QUESTIONS ....................................................................................................... 35

VIII. REFERENCES ................................................................................................................ 37

IX. APPENDIX ....................................................................................................................... 38

LIST OF FIGURES

Figure 1: Common Types of Adsorption Isotherms (Geankoplis, 1993) ............................................... 2

Figure 2: Concentration profiles for adsorption in a fixed-bed: profiles at various positions and times

in the bed (Geankoplis, 1993). ................................................................................................................ 3

Figure 3: Breakthrough concentration profile in the fluid at outlet of bed (Geankoplis, 1993) ............ 4

Figure 4: Determination of the capacity of column from the breakthrough curve (Geankoplis, 1993). 5

Figure 5: Plot of Density vs Concentration for Dye Solution .............................................................. 15

Figure 6: Plot of Freundlich Isotherm at t = 8 minutes ........................................................................ 19

Figure 7: Plot of Langmuir Isotherm at t = 8 minutes ......................................................................... 20

Figure 8: Breakthrough Curve for the 0.5% Solution and 10 cm Bed Height ..................................... 22

Figure 9: Breakthrough Curve for the 0.5% Solution and 5 cm Bed Height ....................................... 23

Figure 10: Breakthrough Curve for the 1.0% Solution and 10 cm Bed Height ................................... 23

Figure 11: Breakthrough Curve for the 1.0% Solution and 5 cm Bed Height ..................................... 24

Figure 12: Comparison of the Breakthrough Curves at 10cm and 5cm Bed Heights for 0.5% Dye

Solution ................................................................................................................................................. 25

Figure 13: Comparison of the Breakthrough Curves at 10cm and 5cm Bed Heights for 1% Dye

Solution ................................................................................................................................................. 25

Figure 14: Comparison of the Breakthrough Curves at 10cm Bed Height for the Adsorption of 1%

and 0.5% Dye Solutions ........................................................................................................................ 26

Figure 15: Comparison of the Breakthrough Curves at 5cm Bed Height for the Adsorption of 1% and

0.5% Dye Solutions .............................................................................................................................. 27

Figure 16: Schematic diagram of the adsorption column .................................................................... 31

LIST OF TABLES

Table 1: Density Raw Data Using Hydrometer ................................................................................... 14

Table 2: Reference Solutions ............................................................................................................... 14

Table 3: Final Data Used for Equation Determination ........................................................................ 15

Table 4: Density at 0.2 % w/w dye solution ........................................................................................ 16

Table 5: Density at 0.4 % w/w dye solution ........................................................................................ 16

Table 6: Density at 0.6 % w/w dye solution ........................................................................................ 16

Table 7: Density at 0.8 % w/w dye solution ........................................................................................ 16

Table 8: Density at 1.0 % w/w dye solution ........................................................................................ 17

Table 9: Summary of the final densities at different concentration (w/w %) dye solution .................. 18

Table 10: R2 values of the Freundlich and Langmuir Isotherm Plots at different time t ..................... 19

Table 11: Freundlich Isotherm Raw Data at t = 8 minutes .................................................................. 19

Table 12: Langmuir Isotherm Raw Data at t = 8 minutes .................................................................... 20

Table 13: Raw Data Summary for the Adsorption of 0.5% Dye Solution ........................................... 21

Table 14: Densities of Effluent for the Adsorption of 0.5% Solution Using 10 cm Bed Height ......... 21

Table 15: Densities of Effluent for the Adsorption of 0.5% Solution Using 5 cm Bed Height ........... 21

Table 16: Raw Data Summary for the Adsorption of 1.0% Dye Solution ........................................... 21

Table 17: Densities of Effluent for the Adsorption of 1.0% Solution Using 10 cm Bed Height ......... 21

Table 18: Densities of Effluent for the Adsorption of 1.0% Solution Using 5 cm Bed Height ........... 22

Table 19: Determination of the Unusable Heights for the Adsorption Columns ................................. 28

Table 20: Data Assumptions1 .............................................................................................................. 29

Table 21: Data Assumptions 2 ............................................................................................................. 29

Table 22: Mass of Dye Used in Part A ................................................................................................ 35

Table 23: Mass of Dye Used in Part B ................................................................................................. 35

Table 24: Equation Determination Data .............................................................................................. 38

Table 25: Error Calculation Data for Equation Determination ............................................................ 38

Table 26: Error Bars Data .................................................................................................................... 39

Table 27: Final Density at 0.2 % w/w dye solution ............................................................................. 41

Table 28: Final Density at 0.4 % w/w dye solution ............................................................................. 42

Table 29: Final Density at 0.6 % w/w dye solution ............................................................................. 42

Table 30: Final Density at 0.8 % w/w dye solution ............................................................................. 42

Table 31: Final Density at 1.0 % w/w dye solution ............................................................................. 42

Table 32: Summary of calculated data at 0.2 % w/w dye solution ...................................................... 43

Table 33: Summary of calculated data at 0.4 % w/w dye solution ...................................................... 43

Table 34: Summary of calculated data at 0.6 % w/w dye solution ...................................................... 43

Table 35: Summary of calculated data at 0.8 % w/w dye solution ...................................................... 44

Table 36: Summary of calculated data at 1.0 % w/w dye solution ...................................................... 44

Table 37: Calculation of Concentrations in Figure 8 ........................................................................... 48

Table 38: Calculation of C/Co in Figure 8 ........................................................................................... 49

Table 39: Calculation of Concentrations in Figure 9 ........................................................................... 51

Table 40: Calculation of Concentrations in Figure 10 ......................................................................... 51

Table 41: Calculation of Concentrations in Figure 11 ......................................................................... 51

Table 42: Calculation of C/Co in Figure 9 ........................................................................................... 51

Table 43: Calculation of C/Co in Figure 10 ......................................................................................... 51

Table 44: Calculation of C/Co in Figure 11 ......................................................................................... 52

I. INTRODUCTION

Adsorption is a unit operation that exploits the attraction of solutes in a liquid or gas to a

solid surface (Gabelman, 2017). In adsorption, the atoms, ions or molecules adheres from a

gas, liquid or dissolved solid to a surface which creates a film of the adsorbate on the surface

of the adsorbent. This process differs from absorption, in which a fluid (the absorbate) is

dissolved by or permeates a liquid or solid (the absorbent), respectively. Adsorption is a

surface phenomenon, while absorption involves the whole volume of the material. The term

sorption encompasses both processes, while desorption is the reverse of it.

all the bonding requirements (be they ionic, covalent or metallic) of the constituent atoms of

the material are filled by other atoms in the material. However, atoms on the surface of the

adsorbent are not wholly surrounded by other adsorbent atoms and therefore can attract

adsorbates. The exact nature of the bonding depends on the details of the species involved, but

the adsorption process is generally classified as physisorption (characteristic of weak van der

Waals forces) or chemisorption (characteristic of covalent bonding). It may also occur due to

electrostatic attraction (Ferrari et. al., 2010).

Adsorption is present in many natural, physical, biological and chemical systems and is

widely used in industrial applications such as heterogeneous catalysts, activated charcoal,

adsorption chillers, synthetic resins, increasing storage capacity of carbide-derived carbons and

water purification (Czelej et. al., 2016).

In this experiment, the adsorbate used is activated carbon. Activated carbon is the

collective name for a group of porous carbons, manufactured by the treatment of a char with

oxidizing gases or by carbonization of carbonaceous materials impregnated with dehydrating

chemicals. All these carbons are prepared to exhibit a high degree of porosity and an extended

internal surface area (F.Rodriguez, 2015). It is widely used throughout a number of industries

to remove undesirable components from liquids or gases. It can also be applied to various

number of applications that require the removal of contaminants or undesirable materials,

ranging from water and air purification, to soil remediation, and even gold recovery (Carrie

Carlson).

1

II. THEORETICAL BACKGROUND

interface (including gas-liquid interfaces, as in foam fractionation, and liquid-liquid interfaces,

as in detergency) (Perry & Green, 2008). Here we consider only liquid-solid interfaces, with

solute distributed selectively between the fluid and solid phases.

In commercial processes, the adsorbent is usually in the form of small particles in a fixed

bed. The fluid is passed through the bed and the solid particles adsorb components from the

fluid. When the bed is almost saturated, the flow in this bed is stopped and the bed is

regenerated thermally or by other methods, so desorption occurs. The adsorbed material

(adsorbate) is thus recovered and the solid adsorbent is ready for another cycle of adsorption

(Geankoplis, 1993).

1. The classical isotherm for a homogeneous flat surface, and most popular of all nonlinear

isotherms, is the Langmuir isotherm

wis K i ci

wi (1)

1 K i ci

equilibrium constant. These parameters are often determined by plotting 1/wi versus

1/ci. The derivation of the isotherm assumes negligible interaction between adsorbed

molecules (Perry & Green, 2008).

2

2. For a heterogeneous flat surface, a classical isotherm is the Freundlich isotherm

wi K i cimi (2)

approximately to an exponential distribution of heats of adsorption. Although it lacks

the required linear behavior in the Henry’s law region, it can often be used to correlate

data on heterogeneous adsorbents over wide ranges of concentration (Perry & Green,

2008). Also according to Geankoplis (1993), this isotherm is particularly useful for

liquids.

A widely used method for adsorption of solutes from liquid or gases employs a fixed

bed of granular particles. The fluid to be treated is usually passed down through a packed

bed at constant flow rate. Mass transfer resistances are important in the fixed-bed process

and the process is unsteady state. The concentrations of the solute in the fluid phase and of

the solid adsorbent phase change with time and also with position in the fixed bed as

adsorption proceeds. At the inlet to the bed the solid is assumed to contain no solute at the

start of the process. As the fluid first contacts the inlet of the bed, most of the mass transfer

and adsorption takes place here. As the fluid passes through the bed, the concentration in

this fluid drops down very rapidly with distance in the bed to zero way before the end of

the bed is reached. The concentration profile at the start at time t1 is shown in Fig. 2, where

the concentration ratio c/co is plotted versus bed length. The fluid concentration co is the

feed concentration and c is the fluid concentration at a point in bed.

positions and times in the bed (Geankoplis, 1993).

3

The dashed line for time t3 shows the concentration in the fluid phase in equilibrium

with the solid. The difference in concentrations is the driving force for mass transfer

(Geankoplis, 1993).

At a given time t3, when almost half of the bed is saturated with solute, the outlet

concentration is still approximately zero, as shown in Fig. 3. This outlet concentration

remains zero until the mass-transfer zone starts to reach the tower outlet at time t4. Then

the outlet concentration starts to rise and at t5 the outlet concentration has risen to cb, which

is called the break point.

The break-point concentration represents the maximum that can be discarded and is

often taken as 0.01 to 0.05 for cb/co. The value cd/co is taken as the point where cd is

approximately equal to co (Geankoplis, 1993).

1993)

D. Capacity of the Column

The total or stoichiometric capacity of the packed-bed tower, if the entire bed comes to

equilibrium with the feed, can be shown to be proportional to the area between the curve

and a line at c/co = 1.0 as shown in Fig. 4.

4

Figure 4: Determination of the capacity of column from the breakthrough curve

(Geankoplis, 1993).

The total shaded area represents the total or stoichiometric capacity of the bed as follows:

∞ 𝑐

𝑡𝑡 = ∫0 (1 − 𝑐 ) 𝑑𝑡 (3)

𝑜

where tt is the time equivalent to the total or stoichiometric capacity. The usable capacity

of the bed up to the break-point time tb is the crosshatched area.

𝑡 𝑐

𝑡𝑢 = ∫0 𝑏 (1 − 𝑐 ) 𝑑𝑡 (4)

𝑜

where tu is the time equivalent to the usable capacity or the time at which the effluent

concentration reaches its maximum permissible level.

The ratio of tu / tt is the fraction of the total bed capacity or length utilized up to the break

point. Hence, for a total bed length of HT m, HB is the length of bed used up to the break

point,

𝑡𝑢

𝐻𝐵 = 𝐻𝑇 (5)

𝑡𝑡

The length of the unused bed HUNB in is then the unused fraction times the total length.

𝑡

𝐻𝑈𝑁𝐵 = (1 − 𝑡𝑢) 𝐻𝑇 (6)

𝑡

𝐻𝑇 = 𝐻𝑈𝑁𝐵 + 𝐻𝐵 (7)

5

Note that HUNB represents the mass-transfer section or zone. It depends on the fluid velocity

and is essentially independent of the total length of the column (Geankoplis, 1993).

A. Materials

i. Reagents

REAGENT AMOUNT

Activated carbon 45 grams

Dyeing agent 16.5 grams

Distilled water 2 liters

Filter paper 1 piece

ii. Apparatus

300 g ± 0.0001 g

Analytical balance 300 g ± 0.005g

50 kg ± 0.01 kg

Beaker 250 mL ± 5 mL

Erlenmeyer flask 250 mL ± 5 mL

Burette 50 mL ± 0.02 mL

25 mL ± 0.5 mL

Graduated cylinder

250 mL ± 0.1 mL

Hydrometer - ± 0.0005

Ruler 30 cm -

Funnel - -

Stirring rod - -

Stopwatch - -

6

B. Schematic Diagram

i. Preparation of Reference Solutions

temperature.

7

ii. Adsorption Isotherm Determination

Pour 200 mL of 0.2, 0.4, 0.6, 0.8 and 1% w/w dye in each beaker, respectively.

Measure the density of each setup by determining the weight of the solution every 2

minutes.

8

Repeat step 3 and 4 until the density of the liquid remains constant with respect to time.

Correlate the measured density to concentration using the equation obtained from Part A.

reaches a compacted height of 10 cm.

9

Set-up the burette in the iron stand.

Fill the graduated cylinder with 1% w/w solution. Note: Stock adequate amount of

1% w/w solution.

Set the stopcock of the burette quarterly open. Start the timer.

10

Determine the average volumetric flow rate.

Collect a measurable volume of the effluent every ten minutes from the outlet of the burette.

Note: Don’t get the samples from the bulk of the effluent.

Repeat steps 7 and 8 until the density of the effluent remains constant.

Compute for the height of used bed (HB) and height of unused bed (HUNB).

11

C. Methodology

i. Preparation of Reference Solutions

A 0, 0.2, 0.4, 0.6, 0.8 and 1% w/w dye solution was prepared using distilled water as

the solvent. The solutions were prepared by weighing 0.5, 1.0, 1.5, 2.0 and 2.5 grams of

blue colored dye using an analytical balance with ±0.01 g uncertainty and adding it to

249.50, 249.00, 248.50, 248.00 and 247.50 grams of distilled water in a 500 mL beaker.

After the preparation, the densities of each solution was determined using a hydrometer

(with ±0.0005 g/mL error) starting from the blank solution up to the 1% w/w dye solution.

The actual concentrations were determined by using the blank solution as the reference and

adding the correcting value to the relative density of the solutions. A plot of concentrations

as a function of densities was made including the errors propagated and the best equation

that represents the experimental data was determined by obtaining the coefficient of

determination (R2) of the possible equations. The best equation was selected on the criterion

of which line will pass through 70% of error bars.

Five sets of five grams of activated carbon were weighed in analytical balance with

±0.01g uncertainty and was placed in five 250 mL beakers. The procedure started by

pouring 200 mL of 0.2% w/w dye solution in the first beaker with 5 grams of activated

carbon. The solution was stirred for 1 minute and was allowed to rest for 1 minute. Then,

the density of the set-up was determined by obtaining the mass and the volume of the

solution from a sample. The mass of the solution was obtained using an analytical balance

with ±0.0001 g error and subtracting the mass of solution plus the mass of the graduated

cylinder to the mass of the graduated cylinder used. The volume of the solution was

determined using a graduated cylinder with ±0.5 mL uncertainty. After which, the density

of the sample was obtained by dividing the mass of the solution over its volume.

Consequently, the sample was returned to the solution and the process was repeated until

the density of the liquid remained constant. Due to the unavailability of the analytical

balance, the measurement of the mass of the solution every 2 minutes was not met. The

same procedure was performed using 0.4, 0.6, 0.8 and 1 % w/w dye solution. After all set-

up was finished, the amount of dye adsorbed per unit adsorbent was determined. Lastly, a

plot of W and equilibrium concentration was made to determine the best isotherm that

represents the experimental data.

12

iii. Design of Fixed Bed Adsorption Column

Two solutions with concentrations of 1 and 0.5% w/w dye solutions were prepared by

weighing 7.0000 and 4.0000 grams respectively for each concentration using an analytical

balance with ±0.0001g uncertainty. The weighed dye were added to 693(±0.0001g) and

796(±0.0001) grams of distilled water to produced 700 and 800 grams of dye solutions.

The bed for the 1% dye solution was prepared by putting the granulated activated carbon

inside the burette until the bed height reached 10 cm using a ruler as guide. The activated

carbon was removed from the burette and its mas was determined. The same procedure was

done to prepare a bed with height of 10 cm for the 0.5% dye solution. Two more beds were

prepared for each solution, this time having a height of 5 cm.

The experiment was performed by setting up the burette on the iron stand and then

pouring the 1% solution into the burette, the stopcock was opened and the timer was started.

The average volumetric flowrate was determined by reading the change in the volume of

the fluid inside the burette for a specific time range. This was performed three times then

the average volumetric flowrate was calculated. After 10 minutes, the effluent was

collected and its mass and volume were determined with the use of analytical balance and

graduated cylinder. From these information, the density of the effluent was calculated.

Effluents were collected every after tem minutes until its density becomes constant. The

bed was replaced with the activated carbon having a height of 5 cm. The same procedure

was performed but opening of the stopcock was changed, thus having a different volumetric

flowrate. This whole experiment was repeated for the 0.5% dye solution for both a bed

height of 10 cm and 5 cm.

13

IV. RESULTS AND DISCUSSION

A. Determination of equation correlating the density and concentration

Table 1: Density Raw Data Using Hydrometer

Concentration w/w%, (g/g) Density of dye (g/mL), ±0.0005 g/mL

0 0.9900

0.5 0.9865

1.0 0.9855

1.5 0.9975

2.0 0.9938

2.5 0.9951

The equation correlating the experimental data of the density and concentration was

determined by plotting the density versus concentration in consideration of all errors

propagated during the experiment. In this part, the raw data of densities obtained during the

experiment as tabulated in Table 1, is determined by using a hydrometer. However, the next

parts of the experiment proceeded by using mass over volume in determining the densities.

Since the equation obtained in this step will affect the succeeding calculations, it must be

considered that the inconsistent determination of the densities of the solutions will result to

more error. In solving this problem, a reference data provided is used and tabulated as follows.

%w/w Weight of Volume of Sample of Mass of

Density

Dye Dye Water Solution Sample

(±0.025g/mL)

Solution (±0.0001g) (±0.1mL) (±0.5 mL) (±0.01 g)

0.0 0.00 200.0 20.0 19.57 0.9650

0.2 0.40 199.6 20.0 19.72 0.9785

0.4 0.80 199.2 20.0 19.77 0.9860

0.6 1.20 198.8 20.0 19.80 0.9885

0.8 2.60 198.4 20.0 19.99 0.9900

1.0 2.00 198.0 20.0 19.30 0.9995

Consequently, the data above was analyzed to determine the equation correlating the

density and the concentration. All calculations and propagated errors are shown in the

Appendix. In obtaining the equation that best represents the experimental data, error bars are

used, according to the Lab Manual presented by University of Pennsylvania, the line must pass

through 70% of the error bars. The final density errors are shown in Table 3 to determine the

final equation.

14

Table 3: Final Data Used for Equation Determination

70 % error range

w/w Concentration, g/g Density, g/mL Error bar

Min Max

0.000 0.924 0.924 1.01 0.0591

0.002 0.947 0.937 1.02 0.0595

0.004 0.971 0.944 1.03 0.0597

0.006 0.994 0.947 1.03 0.0597

0.008 1.018 0.948 1.03 0.0598

0.01 1.042 0.958 1.04 0.0600

0.012

y = 0.0849x - 0.0784

R² = 1

0.01

Concentration, w/w%

0.008

0.006

0.004

0.002

0

0.88 0.9 0.92 0.94 0.96 0.98 1 1.02 1.04 1.06 1.08

Density, g/mL

It can be observed that the densities obtained by using the equation of the line fell within

the range of 70% error bar and the line’s coefficient of determination is equal to 1. It can be

said from Table 3 that as the density increases, the concentration also increases. This accounted

to the fact that adding more solute to a solvent changes the composition of particles in a given

volume or mass of solution. This results in the change of concentration that is derived by using

the mass of the solution over the mass or volume of the solvent. The equation obtained as

y=0.0849x-0.0784 in this part will be used in the succeeding calculations.

15

B. Determination of adsorption isotherm

As stated from the procedure in Methodology II, the density of the samples was obtained

by dividing the mass of the sample taken from the prepared solutions in Methodology I to its

volume. Once the density at a certain time is approximately equal to its subsequent density

after 2 minutes, the determination of density stops. The following results are shown in the

tables below.

Mass of Sample (g) Volume of Sample (mL)

Time, min Density, g/mL

(±0.0001 g) (±0.5 mL)

2 23.8011 24.5 0.971

4 24.1042 25.0 0.964

6 22.9829 24.0 0.958

8 23.4442 24.5 0.957

10 22.9516 24.0 0.957

Mass of Sample (g) Volume of Sample (mL)

Time, min Density, g/mL

(±0.0001 g) (±0.5 mL)

2 23.7699 24.5 0.970

4 23.5209 24.5 0.960

6 23.4521 24.5 0.957

8 22.9204 24.0 0.955

10 22.9314 24.0 0.955

Mass of Sample (g) Volume of Sample (mL)

Time, min Density, g/mL

(±0.0001 g) (±0.5 mL)

2 24.6025 25.1 0.926

4 24.0780 24.9 0.913

6 24.0808 25.0 0.910

8 24.0840 25.0 0.909

Mass of Sample (g) Volume of Sample (mL)

Time, min Density, g/mL

(±0.0001 g) (±0.5 mL)

2 24.0017 24.8 0.969

4 22.6296 23.9 0.947

6 22.6042 24.0 0.942

8 22.7964 24.2 0.942

16

Table 8: Density at 1.0 % w/w dye solution

Mass of Sample (g) Volume of Sample (mL)

Time, min Density, g/mL

(±0.0001 g) (±0.5 mL)

2 23.8011 24.5 0.971

4 24.1042 25.0 0.964

6 22.9829 24.0 0.958

8 23.4442 24.5 0.957

10 22.9516 24.0 0.956

To put things simply, the density of the dye solution changes with time as adsorption

proceeds. As time passes by, it can be observed that the density in each concentration (0.2%,

0.4%, 0.6%, 0.8% and 1.0 %) is decreasing. The reason for this is that the dye that was

dissolved in the water is slowly being adsorbed in the activated carbon, causing its mass to

gradually decrease. However, certain factors can also be considered like the adsorption

capacity of the filter paper used in the separation of the sample from the solution and small

losses of activated carbon granules during this process. It was due to this that the densities

obtained are assumed to be inaccurate.

Another observation is that at the initial times from 2 to 4 minutes, sudden changes in

densities at two significant figures are shown, while the next passing minutes have small

changes, having difference only at 3 significant figures. According to Geankoplis (1993), when

the fluid is passed through the bed, the solid particles adsorb components from the fluid. When

the bed is almost saturated, the concentration would remain almost constant and the flow in the

bed is stopped. This is of somewhat similar case with that of obtained densities in the

experiment. At time 2 to 4 minutes, the activated carbon just continuously adsorbs dye solute

in the solution, however at the subsequent minutes; the adsorbent slowly becomes saturated

causing a decreasing change in the densities. Once it is fully saturated, the density remains

almost constant from its previous density, hence stopping the whole process. In the 0.2%, 0.4%

and 1.0% w/w dye solutions, the density became constant at 10 minutes, while it was 8 minutes

for both 0.6% and 0.8% w/w dye solutions.

according to him the removal of dye is rapid in initial stages but when it approaches

equilibrium, it slows down gradually. This is due to the availability of vacant surface sites

during the preliminary stage of adsorption, and after a certain period of time the vacant sites

are occupied by dye molecules, which lead to create a repulsive force between the adsorbate

on the adsorbent surface and in bulk phase. In the experiment, the attainment of equilibrium

17

takes place after agitating the solutions containing the adsorbent up to 8-10 minutes and once

equilibrium was attained, the percentage of adsorption of dye did not show any appreciable

change with time. This suggests that after equilibrium is attained, further treatment does not

provide more removal.

However, since the hydrometer is not used in determining the densities, certain errors can

be derived in its calculation, proving them inaccurate. To compensate for this, the propagation

of errors, as shown in Appendix B, were calculated, acquiring the density error and its

minimum and maximum corrected value. With the help of this data, the final density is

determined from the corrected range of errors.

Table 9: Summary of the final densities at different concentration (w/w %) dye solution

Time (min) 0.20% 0.40% 0.60% 0.80% 1.00%

2 0.939 0.941 0.944 0.948 0.945

4 0.932 0.931 0.931 0.925 0.938

6 0.925 0.928 0.927 0.928 0.931

8 0.92 0.925 0.927 0.928 0.930

10 0.924 0.926 ------- ------- 0.929

Note that the final density is merely an approximate. This density is used to determine the

final concentration of the dye solution after the adsorption process using the equation

correlating the density and concentration in Results A. Ideally, in an adsorption process, the

concentration obtained must be less than the initial concentrations (0.2%, 0.4%, 0.6%, 0.8%

and 1.0 %) of the solution. Nevertheless, by approximately calculating the final density through

the corrected range of errors using Excel®, the final density that is less than its initial value

can be obtained, creating a decreasing trend in concentration. Another basis of this is also the

percentage removal of the adsorbent. In the study of (Chattopafhyahya, 2017), it was stated

that when the initial concentration of dye solution increases, the percentage removal of the

adsorption process decreases. The same goes in the study of (Sharma & Uma, 2009), stating

that for low concentration ranges, the percentage removal of the dye is higher. That said,

assuming that the optimum percentage removal to be greater than 95%, the initial assumption

from 0.2% is greater than 95% followed by a decreasing trend up to 1.0%. Overall, by using

this method, the final concentrations obtained has approximately ±0.0016 error.

18

Afterwards, the mass of dye per volume of solution, c, and the mass of dye adsorbed per

mass of activated carbon, w, were calculated. A plot of c versus w was done to determine

whether it is a Freundlich Isotherm. Alternatively, a plot of 1/c versus 1/w was also done for

Langmuir Isotherm. This was done on time 2, 4, 6, and 8 minutes. Since both 0.6% and 0.8%,

w/w dye solutions became constant at 8 minutes, the data from time t = 10 minutes are not

considered.

Table 10: R2 values of the Freundlich and Langmuir Isotherm Plots at different time t

Time (minutes) Freundlich Isotherm Langmuir Isotherm

2 0.7444 0.6829

4 0.0044 0.1054

6 0.7729 0.8558

8 0.9604 0.8541

Optimum results were shown at t = 8 minutes, having high values of R2 for both Freundlich

and Langmuir Isotherm. Others, especially at t = 4 minutes, have points that are too far away

from each other to form a line, thus, only t = 8 minutes will be further discussed.

Concentration of Dye c w

Solution, w/w % ( g dye/mL solution ) ( g dye adsorbed/g AC )

1 0.000532887 0.010134648

0.8 0.000389761 0.008164909

0.6 0.000280309 0.006146290

0.4 0.000151895 0.004145200

0.2 0.000123100 0.002018277

19

Table 12: Langmuir Isotherm Raw Data at t = 8 minutes

Concentration of Dye Solution, 1/c 1/w

w/w % ( mL solution/g dye ) ( g AC / g dye adsorbed )

1 1876.571 98.67140835

0.8 2565.677 122.4753418

0.6 3567.489 162.6997654

0.4 6583.494 241.2428659

0.2 8123.466 495.4722064

Comparing both plots, the isotherm with the highest R2 is the Freundlich isotherm, having

a value equal to 0.9604, while Langmuir isotherm has only 0.8541, thus, the Freundlich

isotherm fitted better since it is more accurate. Taking this into consideration, the adsorption

isotherm involved in the process is hence the Freundlich Isotherm. This is considered

reasonable since Geankoplis (1993) stated that this isotherm is particularly useful for liquids.

By further calculations and simplifications, the Freundlich Isotherm equation is determined to

be w 18.1472175c 0.9834117406 .

20

C. Determination of the effect of different parameters such as volumetric flowrate,

compacted bed height, and initial concentration on the adsorption process

i. Raw data for 0.5 %w/w dye solution

Table 13: Raw Data Summary for the Adsorption of 0.5% Dye Solution

Flowrate (ml/sec) 10 cm bed height 5 cm bed height

Trial 1 0.1143 0.1220

Trial 2 0.1111 0.1027

Trial 3 0.1010 0.0877

Average Flowrate 0.1088 0.1041

Table 14: Densities of Effluent for the Adsorption of 0.5% Solution Using 10 cm Bed Height

Mass of Solution, g Volume, mL

Time(min) Density(g/mL) Density error(±)

(±0.0001 g) (±0.5 mL)

10 48.6454 52.5 0.927 0.00882

20 65.9183 69.0 0.955 0.00692

30 73.8450 75.5 0.978 0.00648

40 91.8353 93.5 0.982 0.00525

50 86.0423 87.6 0.982 0.00561

Table 15: Densities of Effluent for the Adsorption of 0.5% Solution Using 5 cm Bed Height

Mass of Solution, g Volume, mL

Time(min) Density(g/mL) Density error(±)

(±0.0001 g) (±0.5 mL)

10 50.5915 54.5 0.928 0.00852

20 51.603 53.5 0.965 0.00901

30 60.3173 61.5 0.981 0.00797

40 57.4055 58.5 0.981 0.00839

Table 16: Raw Data Summary for the Adsorption of 1.0% Dye Solution

Flowrate (ml/sec) 10 cm bed height 5 cm bed height

Trial 1 0.0980 0.0816

Trial 2 0.2041 0.0758

Trial 3 0.1887 0.0717

Average Flowrate 0.1636 0.0764

Table 17: Densities of Effluent for the Adsorption of 1.0% Solution Using 10 cm Bed Height

Mass of Solution, g Volume, mL

Time(min) Density(g/mL) Density error(±)

(±0.0001 g) (±0.5 mL)

10 55.1610 61.1 0.9028 0.0074

20 84.5213 89.9 0.9402 0.0052

30 84.6612 84.5 1.0019 0.0059

40 103.1106 102.1 1.0099 0.0049

21

Table 18: Densities of Effluent for the Adsorption of 1.0% Solution Using 5 cm Bed Height

Mass of Solution, g Volume, mL

Time(min) Density(g/mL) Density error(±)

(±0.0001 g) (±0.5 mL)

10 50.0552 55.0 0.91009455 0.0083

20 49.2982 49.5 0.99592323 0.0101

30 58.8783 58.1 1.01339587 0.0087

40 61.0800 60.2 1.01461794 0.0084

The tables above show the raw data for 0.5 and 1.0 %w/w dye solution comprising of the

volumetric flowrates and densities obtained after carrying the steps specified in Methodology

III. Due to the error incurred by using the relationship of mass over volume, the relative error

on the calculated densities were also determined. It can be said based on Tables 14, 15, 17 and

18 that a common trend is observed in the densities obtained in both 5 and 10 cm bed height.

The densities showed an increasing trend until densities obtained on two consecutive time

periods became constant or approximately equal to each other. The reason for this phenomena

is explained and discussed on the generation of breakthrough curves for each process.

HEIGHT

1.2

0.8

0.6

C/Co

0.4

0.2

0

0 10 20 30 40 50 60

-0.2

Time(min)

Figure 8: Breakthrough Curve for the 0.5% Solution and 10 cm Bed Height

22

BREAKTHROUGH CURVE FOR 5CM BED

HEIGHT

1.2

0.8

C/Co

0.6

0.4

0.2

0

0 5 10 15 20 25 30 35 40 45

Time(min)

Figure 9: Breakthrough Curve for the 0.5% Solution and 5 cm Bed Height

HEIGHT

1.2

0.8

C/Co

0.6

0.4

0.2

0

0 5 10 15 20 25 30 35 40 45

Time(min)

Figure 10: Breakthrough Curve for the 1.0% Solution and 10 cm Bed Height

23

BREAKTHROUGH CURVE FOR 5 CM BED

HEIGHT

1.2

0.8

C/Co

0.6

0.4

0.2

0

0 5 10 15 20 25 30 35 40 45

Time(min)

Figure 11: Breakthrough Curve for the 1.0% Solution and 5 cm Bed Height

The figures above show the breakthrough curves for the adsorption of dye solutions using

fixed beds with known heights. These figures show the change in the concentration of the

effluent from the burette with time by determining first the concentration of the effluents with

the use of its correlation with density and plotting the solid concentration ratio versus time. It

can be observed that it shows the same trend as the change in the density of the effluent shown

in the raw data table where the values calculated continue to rise until they reach a point where

they become constant. This is due to the linear relationship between density and concentration

as previously determined on the first part of this experiment.

For the adsorption process, it can be observed from the curves that at the start of the

operation, the ratio of the concentration of the effluent and feed is equal to zero which denotes

that during this period no solute is present on the effluent, at the same time, none was also

adsorbed on the column. In the beginning, the layer of the bed which comes in contact with the

fluid called the Mass Transfer Zone adsorbs the solute from the fluid. As time passes, this

previous layers will be saturated and less effective for further adsorption so whatever escapes

from this will be trapped on the next zones. A plot showing the change in the concentration of

the solute is given by Figure 4, where at a given time, the concentration of the solute decreases

until it reaches zero as it flows through the bed. It is also shown on the plot that there will come

a time when the concentration of the effluent is no longer zero. The time when the concentration

starts to rise is called the breakpoint for which C/Co is set to be 0.01 to 0.05. After this period,

the effluent’s concentration will continue to rise rapidly until it reaches the time when the

24

concentration of the feed and effluent will be equal. For the generated breakthrough curves

above, the appearance of the curve and their breakpoints depend on the total length of the bed

and initial concentration. The effect of bed height and initial concentrations will be discussed

separately.

BED HEIGHT

1.2

0.8

0.6

C/Co

5 cm

0.4

10 cm

0.2

0

0 10 20 30 40 50 60

-0.2

Time(min)

Figure 12: Comparison of the Breakthrough Curves at 10cm and 5cm Bed Heights for 0.5%

Dye Solution

BED HEIGHT

1.2

0.8

C/Co

0.6

10cm

0.4 5cm

0.2

0

0 10 20 30 40

Time (min)

Figure 13: Comparison of the Breakthrough Curves at 10cm and 5cm Bed Heights for 1%

Dye Solution

25

Figures 12 and 13 show the comparison between the generated breakthrough curves for

different bed heights at the same feed concentration. As discussed on the breakthrough curve

of each solution, most of the bed will be saturated by the time that the C/Co reaches 1. Based

on the graph on Figure 12, the bed having a height of 5 cm reached its saturation point earlier

compared to the bed with 10 cm height. The concentration profile given by Figure 3 can be

used to describe this situation where it showed that a bed with larger height can actually be

used longer given that the feed concentration and flow rate is held constant. This is due to more

mass transfer zones on the bed that it would take longer to make the bed totally saturated. On

the other hand, Figure 13 didn’t show the same trend. This is because it was affected by the

volumetric flowrate. Due to the small volumetric flow rate on the 5 cm bed, it took a longer

time to start becoming saturated. The main reason is that the higher the volumetric flowrate the

more mass of solute will be exposed to adsorbent and it will take lesser time for the bed to be

saturated.

ADSORPTION OF 1% AND 0.5% SOLUTION

1.2

0.8

0.6

C/Co

0.5% Soln

0.4

1% Soln

0.2

0

0 10 20 30 40 50 60

-0.2

Time (min)

Figure 14: Comparison of the Breakthrough Curves at 10cm Bed Height for the Adsorption

of 1% and 0.5% Dye Solutions

26

BREAKTHROUGH CURVES FOR THE

ADSORPTION OF 1% AND 0.5% SOLUTION

1.2

0.8

C/Co

0.6

5% Soln

0.4

1% Soln

0.2

0

0 10 20 30 40 50

Time (min)

Figure 15: Comparison of the Breakthrough Curves at 5cm Bed Height for the Adsorption of

1% and 0.5% Dye Solutions

These figures show the effect of the initial concentration of the feed on the breakthrough

curve. It can be observed based on Figure 14 that in the bed for the 1.0 %w/w solution, the time

when the bed became saturated is reached earlier compared to that of the 0.5 %w/w solution.

This is accounted that for the lower concentration feed, there is lower concentration gradient

or driving force between the bed and the fluid. This causes a slower transport due to the

decrease in the mass transfer coefficient. It should be seen from the graphs that the breakpoint

time for the 1% solution is faster because of a higher concentration gradient which would result

to a faster mass transport from the fluid to the bed. However, in Figure 15, during the time that

the fluid is fed, the bed got disturbed where some granules floated and some blocked the exit

of the fluid. This caused a difference in the flowrate of the effluent which affected the

breakthrough curve.

27

vi. Usable and unusable bed height determination

Table 19: Determination of the Unusable Heights for the Adsorption Columns

0.5% Solution 1.0% Solution

Bed Height 10 cm 5 cm 10 cm 5 cm

C/Co 0.05 0.05 0.05 0.05

Tb(mins) 9.18 9.65 10.62 10.32

Tu(mins) 9.53 10.36 10.47 11.15

Ttotal(mins) 13.08 19.48 16.00 16.81

Husable(cm) 7.29 2.66 6.54 3.32

Hunusable(cm) 2.71 2.34 3.46 1.68

These results show the breakpoint times, total time of adsorption and the usable and

unusable heights of the beds. From the previous discussions, it was discussed that the effective

operation of the adsorbent would be affected by the bed height and initial concentration. A

longer bed corresponds to greater mass transfer zones and a lower feed concentration

corresponds to weaker driving force which would cause slower mass transfer. As a result, the

bed with a larger height and fed with a less concentrated fluid will have longer time before

reaching its saturation point and higher adsorption efficiency. These results can only be attained

if the flowrate was controlled to be constant for the different operations. From the results above

in 0.5 % w/w solution, it can be observed that the breakpoint time for the 5 cm bed is higher

than that of the 10 cm bed. This is due to the small volumetric flow rate on the 5 cm bed that it

took a longer time to get to its break point. In this case, two concentrations exposed into two

different bed heights have different flow rates and that results into inconsistent Tb. This effect

is also true for the usable height of the beds. The determination of the usable height was based

on the time that the bed can be effectively used and therefore, the effect of flowrate on the

breakpoint time would also affect the height of usable bed. All calculations are shown in the

Appendix.

28

D. Design of Fixed-bed Adsorption Column

i. Design problem

Design a fixed-bed adsorber that is capable of operating for 12 hours. Target break through

concentration ratio is 0.01. State your assumptions clearly.

ii. Assumptions

The initial data will be based from the data of Results C and is tabulated as follows:

Bed Height 10

Weight of Activated Carbon (g) 4.4154

Feed Density (g/mL) 0.999

Volumetric Flowrate (mL/sec) 0.1636

Ttotal (min) 16

Basing on the breakthrough curve shown in Figure 8, we can determine the following data:

C/Co 0.05

Tb(mins) 10.62

Tu(mins) 10.47

Ttotal(mins) 16.00

Husable(cm) 6.54

Hunusable(cm) 3.46

Using the data determined from the breakthrough curve, solve for the new height of

adsorption bed:

T

Husable ( New ) b new ( H usable/ old )

Tb old

720 min utes

Husable ( New ) ( 6.54 cm )

5.85 min utes

H usable (New)= 805.86 cm

805.86 cm 3.46 cm

HT (New)=809.32 cm

29

iv. Saturation capacity determination

With the data assumed, the calculation of saturation capacity of the up-scaled

adsorption bed can be performed:

mL g

Flowrate ( 0.1636 )( 0.9995 )

sec mL

g

Flowrate=9.811

min

0.01 g dye g sol' n

Total Dye Adsorbed ( )( 9.811 )( 16 min)

g sol' n min

Total Dye Adsorbed= 1.56976 g dye

wt. dye adsorbed

Saturation Capacity

wt. activated carbon

1.56976 g dye

Saturation Capacity

4.4154 g AC

g dye

Saturation Capacity=0.3555

g AC

30

v. Schematic diagram of adsorption column

Flowrate = 9.811 mL/min

Husable = 805.86 cm

HTotal = 809.32 cm

Hunusable = 3.46 cm

C/C0 = 0.01

31

V. CONCLUSION

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

or cleanse varying concentrations of dye solution is evaluated. Starting with the determination

of relationship of the densities of the reference solution versus the concentration, a linear

relationship with the equation y=0.0849x-0.0784 is obtained. This equation was used to

determine the final concentrations after obtaining the final densities as shown in the appendix.

0.6, 0.8 and 1 %w/w solution were poured in 5 grams of activated carbon and the densities of

the solutions every after two minutes were determined. It was observed that, the density of dye

solution decreases with time as the adsorption proceeds. It was generalized that at the first two

to four minutes that the changes in density were two significant figures until it was observed

that the density changes became smaller and became constant. This observation proves the

theory specified by (Geankoplis, 1993) that when a fluid is passed through a bed, the solid

particles adsorb components from the fluid. When the bed is almost saturated, the concentration

would remain almost constant and the flow in the bed is stopped. Consequently, the mass of

dye per volume of solution, c, and the mass of dye adsorbed per mass of activated carbon, w,

were calculated. A plot of c versus w was done to determine whether it is a Freundlich Isotherm.

Alternatively, a plot of 1/c versus 1/w was also done for Langmuir Isotherm. It was found that

the optimum results of coefficient determination were determined at time equal to 8 minutes.

A Freundlich isotherm with the equation w 18.1472175c 0.9834117406 is chosen as the best

isotherm that fits the exprimental data with a coefficient of determination equal to 0.9604. This

is considered reasonable since Geankoplis (1993) stated that this isotherm is particularly useful

for liquids.

The effect of different parameters such as bed height, volumetric flowrate and initial

concentration on the adsorption process were determined. Breakthrough curves were generated

to show the relationship between the ratio of the concentration at a specific time over the initial

concentration versus time. It was concluded that a bed with larger height can be used longer

given that the feed concentration and volumetric flow rate are held constant. This is due to

more mass transfer zones on the bed that it would take longer to make the bed totally saturated.

As per the effect of the initial concentration, it was determined that for lower concentration of

the feed, there is lower concentration gradient or driving force between the bed and the fluid.

This causes a slower transport due to the decrease in the mass transfer coefficient. However,

the results obtained in Results C-v showed that the 0.5 %w/w dye solution reached the

32

breakpoint time faster which is unideal. This error is accounted to the fact that when the dye

solutions are fed, the bed got disturbed and some granules floated and blocked the exit of the

fluid.

In addition, in the calculation of the usable and unusable bed height, it was found out that

in the breakpoint times for 0.5 % w/w solution, the 5 cm bed was higher compared to that of

10 cm bed. This is due to the small volumetric flow rate on the 5 cm bed that it took a longer

time to get to its break point. It was also observed that for usable and unusable bed height, the

heights calculated were a function of flowrate and breakpoint time.

In the design problem specified, it was found out that for new operating time of 12 hours

with a target breakthrough of 0.01, the new bed height calculated was 809.32 cm. By assuming

that the operating conditions were the same with that of 1.0 %w/w dye solution at 10 cm bed

height, the flowrate of the feed is computed as 9.811 g/min and the bed’s saturation capacity is

0.3555 grams of dye/ grams of activated carbon.

33

VI. RECOMMENDATIONS

In view of more precise and accurate results, the researchers would like to recommend the

following:

This is very important for the accuracy of the data gathered in the experiment.

Throughout the experiment, the method for determining the densities varied from

using the hydrometer to using the relationship of mass over volume. In effect, the

data gathered in the Part A became unusable due to inconsistencies of results. If

possible, one method must be used and using the hydrometer is preferable.

All equipment must be properly calibrated and one equipment must be used to

measure the mass of all reagents and chemicals used. In the experiment, due to the

insufficient equipment, the determination of weights were made by using different

types of weighing scale with different uncertainties. For the sake of uniformity and

precision, one equipment must be used to measure one specific parameter.

This will remove the extra time the groups spend to wait for their turns to use an

equipment. In effect, the experimental procedures will be carried out based on

specific instructions and will not be delayed.

In the experiment, the source of activated carbon was not specific and its

commercial specifications were unknown. Due to this, it was difficult for the

researchers to identify if the activated carbon was properly activated and if it can

actually be used as an adsorbent.

To compare the adsorption efficiency of the activated carbon, other adsorbents may

be used to achieve this objective.

34

VII. STUDY QUESTIONS

1. How much dye is needed for the whole experiment?

A. Determination of densities of solution and adsorption isotherms

% w/w Concentration Mass of Dye ±0.01 g

0.2 0.50

0.4 1.00

0.6 1.50

0.8 2.00

1 2.50

Total mass of Dye 7.50 g ±0.01 g

adsorption

% w/w Concentration Height of Bed (cm), ±0.01 cm Mass of Dye(g), ±0.01 g

10.00 2.50

x1.00

5.00 2.50

10.00 1.25

0.5

5.00 1.25

Total mass of Dye 7.50 g ±0.01 g

Total mass of Dye =15.0 g

z x 2 y 2

z 0.012 0.012

z=0.01

Ideally, the amount of dye that must be used is 15.0g± 0.01 g, however, two sets of

concentrations (0.2 and 0.4 %w/w) was repeated due to random errors. The theoretical total

dye used is 16.5g ± 0.01g.

35

2. How do you separate powdered adsorbent from the fluid to get desired volume/density

of effluent?

In obtaining samples from the solution to determine the density of the effluent, the

researchers made used of two methods: decantation and filtration. However, the

methods posed two different disadvantages. The disadvantage of decanting a sample is

that some activated carbon were accidentally incorporated in the sample. Due to this,

when the researches tried to separate the activated carbon, some dye and solution

adhered to the fingers of the researches. Consequently, it must be noted that this

potentially deviates the results from correctly obtaining the density of the effluent. On

the other hand, using a filter paper filters the powdered dye and also creates errors in

obtaining the density of the samples. Although both methods poses disadvantages,

separating the powdered adsorbent must be done by decantation. This method is chosen

because it produces less error compared to filtration.

36

VIII. REFERENCES

[1] Carrie Carlson, W. H. (n.d.). FEECO international, inc. Introduction to Activated CArbon.

Retrieved from FEECO interntional: http://feeco.com/introduction-to-activated-carbon/

toxic dye, tartrazine from aqeous solutions by a low cost agricultural . Arabian Journal of

Chemistry.

[3] Czelej et. al., K. (2016). Czelej, K., Cwieka,CO2 stability on the Ni low-index surfaces:

Van der Waals corrected DFT analysis. 33-38.

[5] Ferrari et. al., L. (2010). Ferrari, L.; Kaufmann, JInteraction of cement model systems with

superplasticizers investigated by atomic force microscopy, zeta potential, and adsorption

measurements.

Minnesota: Prentice-Hall International, Inc.

[8] Perry, R. H., & Green, D. W. (2008). Perry’s Chemical Engineers’ Handbook (8th ed.).

United States of America: McGraw-Hill Companies, Inc.

[10] Sharma, Y., & Uma. (2009). Optimization of parameters for the adsorpton of Methylene

Blue on low cost activated carbon. Journal of Chemical & Engineering Data, 435-439.

37

IX. APPENDIX

A. Determination equation of line

Table 24: Equation Determination Data

%w/w Weight of Volume of Sample of Mass of

Density

Dye Dye Water Solution Sample

(±0.025g/mL)

Solution (±0.0001g) (±0.1mL) (±0.5 mL) (±0.01 g)

0.0 0.00 200.0 20.0 19.57 0.9650

0.2 0.40 199.6 20.0 19.72 0.9785

0.4 0.80 199.2 20.0 19.77 0.9860

0.6 1.20 198.8 20.0 19.80 0.9885

0.8 2.60 198.4 20.0 19.99 0.9900

1.0 2.00 198.0 20.0 19.30 0.9995

Not corrected Corrected

Corrected

min max min max

1.0135 0.9535 1.0035 0.9185 1.0385

1.0210 0.9610 1.0110 0.9260 1.0460

1.0235 0.9635 1.0135 0.9285 1.0485

1.0250 0.9650 1.0150 0.9300 1.0500

1.0345 0.9745 1.0245 0.9395 1.0595

1.0000 0.9400 0.9900 0.9050 1.0250

Error 0.0350

g g

Error 1.000 0.9650

mL mL

g

Error=0.0350

mL

i. Calculation of actual density error

2 2

z x y

z x y

2 2

x y

z z

x y

2 2

0.01 0.5

z 0.965

19.3 20

z=0.024

38

ii. Calculation of 70% error range

Error 0.70 density error correction factor

Error 0.70 0.024 0.0350

Error=0.024

Not corrected Corrected 70% error range

Density error Corrected density

min max min max min max

0.024 1.000 0.941 0.989 0.906 1.024 0.924 1.006

0.024 1.014 0.954 1.003 0.919 1.038 0.937 1.020

0.025 1.021 0.961 1.011 0.926 1.046 0.944 1.028

0.025 1.024 0.964 1.013 0.929 1.048 0.947 1.031

0.025 1.025 0.965 1.015 0.930 1.050 0.948 1.032

0.025 1.035 0.975 1.024 0.940 1.059 0.958 1.042

2 2

z x y

z x y

2 2

x y

z z

x y

2 2

0.0001 0.1

z 0

0 200

z=0.0

Since the concentration is equal to 0, it did not affect the vertical error and was

neglected.

The line was defined using two points, the maximum and minimum values that fell

within the range of 70% error. After obtaining the equation, it was used to determine

the densities given the concentration.

Equation of line:

y 0.0849 x 0.0784

Solving x in terms of y

39

y 0.0849 x 0.0784

y 0.0784

x

0.0849

Solving the density at 0.004 w/w concentration

y 0.0849 x 0.0784

0.004 0.0784

x

0.0849

x=0.971

To show that density accurately, the number of significant figures used in this

calculation is three.

v. Excel Files

40

B. Determination of the Adsorption Isotherm

i. Calculation of actual density error

At initial concentration of 0.2% w/w dye solution:

2 2

z x y

z x y

2 2

x y

z z

x y

2 2

0.0001 0.5

z 0.97147

23.8011 24.5

z=0.01982599

The same method is done in 0.4%, 0.6%, 0.8% and 1.0 % w/w concentrations.

At initial concentration of 0.8% w/w dye solution:

final density Corrected min (density factor ) density error correction factor

final density 0.91665 0.415 0.01982599 0.0350

g

final density=0.939400265

mL

Note that the density factor varies depending on the final concentration and

percentage removal of the adsorbent.

Not Corrected Corrected

Final Density, g/mL

Density error min max min max

0.019825990 0.951647 0.991299 0.916647 1.026299 0.939400265

0.019283360 0.944885 0.983451 0.909885 1.018451 0.932412234

0.019950434 0.93767 0.977571 0.90267 1.012571 0.925474829

0.019528697 0.937377 0.976435 0.902377 1.011435 0.925006835

0.019923264 0.936393 0.97624 0.901393 1.01124 0.924186557

41

Table 28: Final Density at 0.4 % w/w dye solution

Not Corrected Corrected

Final Density, g/mL

Density error min max min max

0.019800000 0.9504 0.99 0.9154 1.025 0.940608

0.019592587 0.940444 0.979629 0.905444 1.014629 0.930556738

0.019535277 0.937693 0.976764 0.902693 1.011764 0.927779522

0.019896181 0.93512 0.974913 0.90012 1.009913 0.925372729

0.019905730 0.935569 0.975381 0.900569 1.010381 0.925825906

Not Corrected Corrected

Final Density, g/mL

Density error min max min max

0.019525484 0.960654 0.999705 0.925654 1.034705 0.943647209

0.019417429 0.947571 0.986405 0.912571 1.021405 0.930528274

0.019264640 0.943967 0.982497 0.908967 1.017497 0.926874691

0.019267200 0.944093 0.982627 0.909093 1.017627 0.927000976

Not Corrected Corrected

Final Density, g/mL

Density error min max min max

0.019512309 0.948298 0.987323 0.913298 1.022323 0.946550684

0.019808477 0.927037 0.966654 0.892037 1.001654 0.925469882

0.019621702 0.92222 0.961463 0.88722 0.996463 0.928186241

0.019462810 0.922537 0.961463 0.887537 0.996463 0.928384297

Not Corrected Corrected

Final Density, g/mL

Density error min max min max

0.01982599 0.951647 0.991299 0.916647 1.026299 0.944608734

0.01928336 0.944885 0.983451 0.909885 1.018451 0.937569153

0.019950434 0.93767 0.977571 0.90267 1.012571 0.93069512

0.019528697 0.937377 0.976435 0.902377 1.011435 0.930187061

0.019923264 0.936393 0.97624 0.901393 1.01124 0.929404267

At initial concentration of 0.8% w/w dye solution:

y 0.0849 x 0.0784

final concentration 0.0849 final density 0.0784

final concentration 0.0849 0.946550684 0.0784

final concentration=0.001962153

The same method is done in 0.4%, 0.6%, 0.2% and 1.0 % w/w concentrations.

42

iv. Calculation of percentage removal

At initial concentration of 0.8% w/w dye solution:

initial concentration final concentration

% removal 100

initial concentration

0.002 0.001962153

% removal 100

0.002

%removal=1.8923%

The same method is done in 0.4%, 0.6%, 0.2% and 1.0 % w/w concentrations.

At initial concentration of 0.8% w/w dye solution:

Concentration error 0.0849 density error

\ Concentration error 0.0849 0.019512309

Concentration error=0.0017

The same method is done in 0.4%, 0.6%, 0.2% and 1.0 % w/w concentrations.

Final concentration, w/w dye solution Percentage Removal Concentration Error

0.001355083 32.2458731 0.00168323

0.000761799 61.910066 0.00163716

0.000172813 91.3593502 0.00169379

0.00013308 93.3459862 0.00165799

6.34387E-05 96.8280654 0.00169149

Final concentration, w/w dye solution Percentage Removal Concentration Error

0.001457619 27.119041 0.00168102

0.000604267 69.7866481 0.00166341

0.000368481 81.5759307 0.00165855

0.000164145 91.7927657 0.00168919

0.000202619 89.869029 0.00169

Final concentration, w/w dye solution Percentage Removal Concentration Error

0.001715648 14.2175999 0.00165771

0.000601850 69.9074757 0.00164854

0.000291661 85.416937 0.00163557

0.000302383 84.8808581 0.00163579

43

Table 35: Summary of calculated data at 0.8 % w/w dye solution

Final concentration, w/w dye solution Percentage Removal Concentration Error

0.001962153 1.8923484 0.00165659

0.000172393 91.3803501 0.00168174

0.000403012 79.8494061 0.00166588

0.000419827 79.0086575 0.00165239

Final concentration, w/w dye solution Percentage Removal Concentration Error

0.001797282 10.1359221 0.00168323

0.001199621 40.0189438 0.00163716

0.000616016 69.1992137 0.00169379

0.000572881 71.355926 0.00165799

0.000506422 74.678886 0.00169149

At initial concentration of 0.2% w/w dye solution:

c final concentration final density

c 0.001355083 0.939400265

g

c=0.001272965

mL

The same method is done in 0.4%, 0.6%, 0.8% and 1.0 % w/w concentrations.

At initial concentration of 0.2% w/w dye solution:

initial concentration final concentration

w

final density

0.002 0.001355083

w

0.939400265

g

w=0.00068652

g

The same method is done in 0.4%, 0.6%, 0.8% and 1.0 % w/w concentrations.

44

viii. Calculation of mass of dye per volume of solution error, c error

At initial concentration of 0.2% w/w dye solution:

2 2

z x y

z x y

2 2

x y

z z

x y

2 2

0.035 density error concentration error

z c

final density final concentration

2 2

0.035 0.019512309 0.00165659

z 0.001857277

0.946550684 0.001962153

z=0.00157

The same method is done in 0.4%, 0.6%, 0.8% and 1.0 % w/w concentrations.

Calculations and simplifications was done using fx-991ES Plus Casio Calculator.

The following commands were first clicked:

Mode 3 7

Equation 2, let y = w

A=k

x=c

B=m

Then put the following data on the table,

X y

( g dye/mL solution ) ( g dye adsorbed/g AC )

0.000532887 0.010134648

0.000389761 0.008164909

0.000280309 0.006146290

0.000151895 0.004145200

0.000123100 0.002018277

Shift 1 5 1 : For A

Shift 1 5 2 : For B

45

Simplifying these give the Freundlich Isotherm equation: w 18.1472175c 0.9834117406 .

x. Plotting of Isotherms

46

C. Design of Fixed Bed Adsorption Column

i. Density of Effluent

From the raw data Table 14, the density of the effluent is calculated using the

following:

(mass of solution)

density of solution =

(volume of solution)

density of solution

( volume of solution )

101.5931g - 52.9477 g

density of solution

52.5 mL

density of solution 0.927 g / mL

The same method is done in the determination of densities from Table 15.

2 2

z x y

z x y

2 2

x y

z z

x y

2 2

0.5

z 0.927

0.0001

101.5931 52.9477

52.5

z= ±0.00882

47

iii. Minimum and Maximum Densities

The maximum and minimum densities of the effluent were calculated by either adding

or subtracting the density error.

0.927 g / mL

min 0.927 0.00882 0.918 g/mL

max 0.927 0.00882 0.935 g/mL

The same method was used in calculating the densities of the effluents for the

succeeding time periods as well as those from Table 17 and 18.

Using the equation correlating density and concentration from part A, the concentration

of the effluent in each time period was calculated.

From Part A:

Concentration 0.0849density 0.0784

For the Effluent time t = 10 minutes:

Concentration 0.0849 0.927 0.0784

C oncentration=0.00027

Density(g/mL) Concentration(w/w%)

0.927 0.00027

0.955 0.00271

0.978 0.00464

0.982 0.00499

0.982 0.00499

In the Breakthrough curve, time was on the x-axis while c/co on the y-axis:

C0 = 0.005

At time t = 10 minutes:

C 0.00027

Co 0.005

C

= 0.053

Co

Hence, for the Breakthrough Curve at Figure 8, the following data are calculated,

48

Table 38: Calculation of C/Co in Figure 8

Time(min) C/Co

0 0

10 0.053

20 0.542

30 0.928

40 0.998

50 0.998

For the bed with a height of 10 cm:

1.2

0.8

0.6

C/Co

0.4

R² = 1

0

0 10 20 30 40 50 60

-0.2

Time(min)

where: y = c/co

x = time

Setting the Breakpoint time at c/co = 0.05

0.05 1 10 8 x 5 2 10 7 x 4 0.0001x 3 0.0058 x 2 0.0396 x 4 10 11

x 9.18

tb 9.18 minutes

vii. Calculation of Usable Time

tb C

tusable 0

1

Co

dt

9.18

tusable 0

1 1 108 x5 2 107 x 4 0.0001x3 0.0058 x 2 0.0396 x 4 1011 dt

t usable = 9.53 min

49

viii. Total time

tT A1 A2

A1 6( 1 )

A1 6.00

A2 ( 36 6 )( 1 ) 636 1 1108 x5 2 107 x4 0.0001x3 0.0058 x2 0.0396 x 4 1011

dt

A2 =7.07577

tT 6.00 7.07577

tT = 13.08 min

t

H u HT u

tT

9.53

H u 10

13.08

H u =7.29 cm

x. Unusable Height

HUNB HT HU

HUNB 10 7.29

HUNB = 2.71cm

50

xi. Other Tables of Concentration Calculated from Their Densities

Density(g/mL) Concentration(w/%)

0.928 0.000411346

0.965 0.003489621

0.981 0.004867297

0.981 0.004911572

Density(g/mL) Concentration(w/%)

0.9304 0.000591878

0.9699 0.003948009

1.0310 0.009130138

1.0400 0.009891968

Density(g/mL) Concentration(w/%)

0.9368 0.001136099

1.0209 0.008271303

1.0397 0.009868385

1.0412 0.009997106

xii. Other Tables for the Values of C/Co in the Generation of Breakthrough Curves

Time(min) C/Co

0 0

10 0.082269174

20 0.697924112

30 0.973459415

40 0.982314359

Time(min) C/Co

0 0

10 0.059187798

20 0.394800884

30 0.913013784

40 0.989196781

51

Table 44: Calculation of C/Co in Figure 11

Time(min) C/Co

0 0

10 0.11360994

20 0.82713028

30 0.98683849

40 0.99971058

52

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