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Department of Chemical Engineering

School of Engineering and Architecture


Saint Louis University

LABORATORY REPORT EVALUATION SHEET


Laboratory Course:ChE 414L Schedule: 7:30-10:30 TTH
Experiment Number: 5
Experiment Title: The Study of an Adsorption Isotherm: Acetic Acid Solutions on Activated Carbon
Group Number: 4 Date Performed: 02, 09 March 2017
Group Members: Dacanay, John Lester P. Date Submitted: 16 March 2017
Jimenez, Jhon Paul B.
Robleza, John Kristoffer S.
Caw-is, Imee A.

TOTAL
CONTENTS REMARKS SCORE
POINTS
I. Abstract 10
II. Chapter 1 : Introduction 15
III. Chapter 2: Design and
10
Methodology
IV. Chapter 3: Results and
20
Discussion
V. Chapter 4: Conclusion and
10
Recommendation
VI. References 5
VII. Appendices
a List and Uses of
Apparatus
b Definition of Terms
15
c Computations
d Documentation
e Problems
f MSDS
VIII. Table of Contents/List of
5
Tables/List of Figures
IX. Format and Neatness 10

TOTAL POINTS: 100 SCORE: __________


Evaluated by: Engr. Gizelle Pascua Date: _____________
THE STUDY OF AN ADSORPTION ISTOTHERM:
ACETIC ACID SOLUTIONS ON ACTIVATED CARBON

An Experimental Study Presented to the

Faculty of the Department of Chemical Engineering

School of Engineering and Architecture

Saint Louis University

In Partial Fulfillment of the Requirements for the Degree

Bachelor of Science in Chemical Engineering

by

John Lester P. Dacanay

Jhon Paul B. Jimenez

John Kristoffer S. Robleza

Imee A. Caw-is

March 2017
ACKNOWLEDGEMENT

This experimental study took a tedious process to accomplish. It took us about a week to
finish, for we have to wait until equilibrium state was achieved. Moreover the procedures weren't
easy, especially titrating multiple concentrations of acetic acid. Nonetheless, these were all done
smoothly because of the following personalities involved.
Our instructor, Engr. Gizelle Pascua, was very approachable towards us. She was always
there to guide us whenever we have questions about the experiment. We appreciate all her efforts
in attending to our needs.
The custodians, as always, were very accommodating. They made sure that we were
using the equipment properly and taking safety precautions towards the reagents. They were very
kind and patient.
We also thank our dear classmates for rendering their materials that we don't have and for
helping us in the computations.
And of course to our parents, thank for your never ending support and unconditional love.
God bless!

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TABLE OF CONTENTS

TITLE PAGE i

ACKNOWLEDGEMENT ii

TABLE OF CONTENTS iii

LIST OF TABLES iv

LIST OF FIGURES v

ABSTRACT vi

Chapter 1: INTRODUCTION
1

Chapter 2: DESIGN AND METHODOLOGY 4

Chapter 3: RESULTS AND DISCUSSION 9

Chapter 4: CONCLUSION AND RECOMMENDATION 15

REFERENCES 16

APPENDICES 17

Appendix A 18

Appendix B 19

Appendix C 20

Appendix D 24

Appendix E 26

Appendix F 34

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LIST OF TABLES

Table 5.1: Data collected at original concentration, during titration, and


at equilibrium for the first trial. 9
Table 5.2: Data collected at original concentration, during titration, and
at equilibrium for the second trial. 10

4
LIST OF FIGURES

Figure 5.1: Flow chart for the preparation of 0.1000N NaOH solution 5
Figure 5.2: Flow chart for the standardization of 0.1000N NaOH solution 6
Figure 5.3: Flow chart for the preparation of 0.5000N acetic acid solution 6

Figure 5.4: Flow chart for the standardization of acetic acid solution 7

Figure 5.5: Flow chart for the preparation of adsorption solutions 7

Figure 5.6: Flow chart for the determination of the equilibrium

concentrations of the adsorption solutions 8

Figure 5.7: Graphical solution for the Freundlich equation to obtain

constants k and n for the first trial 12

Figure 5.8: Graphical solution for the Freundlich equation to obtain

constants k and n for the second trial 12

Figure 5.9: Graphical solution for the Langmuir isotherm to obtain

constants a and b for the first trial 13

Figure 5.10: Graphical solution for the Langmuir isotherm to obtain

constants a and b for the first trial 14

Figure D.1: Weighed Activated Carbon inside Weighing Bottle Containers 24

Figure D.2: Pipetting Separately the Clear Liquid from the Twelve Flasks 24

Figure D.3: Titration of the created Solutions 25

5
ABSTRACT

This experimental study is about the adsorption isotherm. It is a graph between the

amounts of adsorbate adsorbed on the surface of the adsorbent and pressure at constant

temperature to study the process of adsorption. The absorbate and absorbent in this experiment is

acetic acid and activated carbon, respectively. Its objectives are to determine the equilibrium

expressions of acetic acid solutions, to prepare adsorption solutions using activated carbon as the

adsorbent, and to study the adsorption of acetic acid on activated carbon at an approximately

constant temperature environment. From the results obtained both from the computations and the

graphical solutions, it is concluded that the adsorption of acetic acid solutions on activated

carbon follows the Freundlich adsorption isotherm. It is also evident that the adsorption

decreases as the concentration of the solution decreases, thus, the value of k remains constant at a

given temperature. It is recommended that precautions should be closely observed so as to

obtain more accurate results, thus having more precise computations for the constants.

KEYWORDS: Adsorption, adsorption isotherm, adsorbent, adsorbate, chemical equilibrium

6
Chapter 1

INTRODUCTION

Adsorption refers to the phenomena of binding of molecules to a surface. It occurs

because the atoms or ions at the surface of a solid are extremely reactive. Adsorption has two

classifications, namely physisorption and chemisorption. Physical adsorption, or physisorption,

is a type of adsorption where there is a van der Waals interaction between the adsorbate and the

substrate. Van der Waals interactions have a long range but are weak, and the energy released

when a particle is physisorbed is of the same order of magnitude as the enthalpy of condensation.

A molecule bouncing across the surface will gradually lose its energy and finally adsorb to the

surface. A physisorbed molecule retains its identity, although it might be distorted by the

presence of the surface. On the other hand, the second type of adsorption is chemical adsorption

or chemisorption. This is a process where the molecules or atoms stick to the surface by forming

a chemical (usually covalent) bond, and tend to find sites that maximize their coordination

number with the substrate. A chemisorbed molecule may be torn apart at the demand of the

unsatisfied valences of the surface atoms. In comparison, the enthalpy of chemisorption is very

much greater than that for physisorption. The distance between the surface and the closest

adsorbate atom is also typically shorter for chemisorption than for physisorption.

The rate of adsorption is determined by observing the change of fractional coverage with

time. It is also known to be the rate of change of surface coverage. The extent of surface

coverage is normally expressed as the fractional coverage θ , which is the ratio of the number

of adsorption sites occupied to the number of adsorption sites available. In addition, the rate of

adsorption is affected by several factors such as the nature of the adsorbate and adsorbent, the

1
surface area of the adsorbent, the activation of adsorbent, and some experimental conditions

(such as temperature, pressure, etc.).

2
3

The process of adsorption is usually studied through graphs known as adsorption

isotherms. These describe the variation of the fractional coverage of adsorption with pressure at a

chosen temperature. Adsorption isotherms are graphs between the amounts of adsorbate adsorbed

on the surface of the adsorbent and pressure at constant temperature.

For this experiment, it is being determined whether the adsorption of acetic acid on

activated carbon obeys either of the two adsorption isotherms, which are the Freundlich isotherm

and the Langmuir isotherm.

In 1916, Irving Langmuir proposed the Langmuir adsorption isotherm. This isotherm was

based on different assumptions:

a. Adsorption cannot proceed beyond monolayer coverage.


b. All sites are equivalent and the surface is uniform (that is, the surface is perfectly flat on a

microscopic scale).
c. The ability of a molecule to adsorb at a given site is independent of the occupation of

neighboring sites (that is, there are no interactions between adsorbed molecules).

The Langmuir isotherm is given by the equation:

Kp
θ=
1+Kp

Where θ is the surface coverage, p is is the partial pressure of adsorbate, and K is a constant

ratio given by:

ka
K=
kd

ka kd
In which and are the rate constants for adsorption and desorption, respectively.

Furthermore, the second isotherm called the Freundlich isotherm, which was introduced

by Herbert Freundlich, corresponds to a logarithmic change. This isotherm attempts to


4

incorporate the role of substrate-substrate interactions on the surface. The following equation

gives the Freundlich isotherm


1
c2
θ=c1 p

Where c1 and c2 are the Freundlich constants.

Activated carbon, also called activated charcoal or activated coal, is a general term that

includes carbon material mostly derived from charcoal. For all three variations of the name,

"activated" is sometimes substituted by "active." By any name, it is a material with an

exceptionally high surface area. Just one gram of activated carbon has a surface area of

approximately 500 m² (for comparison, a tennis court is about 260 m²). Activated carbon is

frequently used in everyday life, in: industry, food production, medicine, pharmacy, military, etc.

The adsorbate used in this experiment was acetic acid. Acetic acid is an organic pollutant

with a specific surface area close to that of nitrogen most often used in adsorption experiments,

hence its is used in this study to characterize ACs samples. Acetic acid like phenol, iodine, p-

nitrophenol, methylene blue, caffeine and halophenols are reference substances for adsorption in

aqueous phase.

The main objectives of this experiment are to determine the equilibrium expressions of

acetic acid solutions, to prepare adsorption solutions using activated carbon as the adsorbent, and

to study the adsorption of acetic acid on activated carbon at an approximately constant

temperature environment.
Chapter 2

DESIGN AND METHODOLOGY

This experiment made use of the experimental research design in order to determine how

much of the acetic acid was adsorbed by the activated carbon. Adsorption isotherms were also

utilized to be able to attain the experiment’s objectives.

Two solutions were first prepared for the experiment. First, 1000 mL of 0.1000 N NaOH

solution was made. It was done by weighing 4 grams of sodium hydroxide pellets in an

analytical balance. The pellets were first dissolved with a small quantity of water in a beaker

before being transferred into a 1000 mL volumetric flask. The solution was then diluted by

adding distilled water until it reached the mark on the volumetric flask. This prepared solution

was mixed thoroughly and transferred into a properly labeled reagent bottle.

The second solution prepared was 250 mL of 0.5000N acetic acid. By using the dilution

equation to compute for the amount of glacial acetic acid needed for the required concentration

of the solution, 29.4 mL of glacial acetic acid was drawn using a pipette and transferred into a

250 mL volumetric flask. Distilled water was added to dilute it until the mark was reached in the

volumetric flask. The solution was mixed thoroughly and then transferred to a reagent bottle. The

bottle was labeled properly for easier identification.

After preparing the two solutions, they were standardized. The NaOH solution was

standardized by using a solution of potassium hydrogen phthalate (KHP). 0.4084g of KHP was

weighed and dissolved in 20mL of distilled water. This solution was titrated using the prepared

NaOH solution. The amount of titrant obtained from titration was used to calculate for the exact

concentration of the prepared NaOH solution. On the other hand, the acetic acid solution was

titrated by using the standardized NaOH solution. The exact concentration of the acetic acid

solution was obtained in the same manner as the NaOH solution.


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6

In the preparation of the adsorption solutions, 100 mL of NaOH solution with different

concentrations (N/2, N/4, N/8, N/16, N/32, N/64) was prepared. 80 mL of each solution was then

transferred in properly labeled Erlenmeyer flasks. Approximate 1 gram of activated carbon was

then weighed using an analytical balance and added to each Erlenmeyer flask. The flasks were

covered with a cork and shaken for 10 to 20 minutes. This preparation was repeated for a second

trial. The solutions were then properly stored and left to settle for one week for the solution

adsorbed by the activated carbon to reach equilibrium.

After one week, the solutions were titrated with the 0.1000N solution of NaOH. 10 mL of

the solutions with concentrations N/2 and N/4 were carefully drawn and titrated. However, for

those with concentrations of N/8, N/16, N/32, and N/64 30 mL of the solutions were obtained for

titration. This was done for both trials. The data obtained were used to determine the exact

equilibrium concentrations of the adsorbed solutions.

The above methods are summarized in the following schematic diagrams.

4 grams of NaOH pellets were weighed in an analytical balance

The pellets were dissolved in a small quantity of water

The solution was transferred to a 1000 mL volumetric flask

Distilled water was added until the flask is filled to the mark.

Solution was mixed thoroughly and transferred into a properly labeled reagent bottle
Figure 5.1: Flow chart for the preparation of 0.1000N NaOH solution
7

0.4084g of KHP were weighed in an analytical balance and dissolved in 20 mL of


distilled water

3 drops of the indicator phenolphthalein were added

The KHP solution was titrated with 0.1000 N NaoH solution until it turned light pink
in color.

The volume of NaOH solution used was recorded.

The standardized concentration of NaOH solution was computed from the data
collected.

Figure 5.2: Flow chart for the standardization of 0.1000N NaOH solution

29.4 mL of gracial acetic acid was drawn using a pipette and transferred into a 250 mL
volumetric flask

Distilled water was added until the mark in the flask was reached.

The solution was mixed thoroughly and transferred to a properly labeled reagent
bottle.

Figure 5.3: Flow chart for the preparation of 0.5000N acetic acid solution
8

20 mL of the prepared acetic acid was placed in an erlenmeyer flask.

3 drops of the indicator phenolphthalein were added

The solution was titrated with the standardized NaoH solution until it turned light pink
in color.

The volume of NaOH solution used was recorded.

The standardized concentration of acetic acid solutionwas computed from the data
collected.

Figure 5.4: Flow chart for the standardization of acetic acid solution

100 mL of acetic acid solution with concentrations N/2, N/4, N/8, N/16, N/32, N/64
were prepared

80 mL of each solution were drawn and transferred into separate erlenmeyer flasks.

Approximately 1 gram of activated carbon was weighed and added to each


earlenmeyer flask.

The flasks were corked and shaken for 10-20 minutes

The solutions were stored for 1 week.

Figure 5.5: Flow chart for the preparation of adsorption solutions


9

Pipette and filter 10 mL of the solutions with concentration of N/2 and N/4. For those
with concentrations from N/8 to N/64, 30 mL of each solution were used.

3 drops of the indicator phenolphthalein were added

The solutions were titrated with the standardized NaoH solution until it turned light
pink in color.

The volume of NaOH solution used was recorded.

The concentration of acetic acid at equilibrium were computed.

Figure 5.6: Flow chart for the determination of the equilibrium concentrations of the adsorption

solutions
Chapter 3

RESULTS AND DISCUSSION

Table 5.1 Data collected at original concentration, during titration, and at equilibrium for the first

trial.

Vol of Sol’n Wt. of HAc in Vol. of HAc in Vol. of NaOH


Orig. Conc. N
(mL) orig. sol’n (g) titration (mL) used (mL)
N/2 0.5129 80 2.4619 10 49.8
N/4 0.2565 80 1.2312 10 31
N/8 0.1282 80 0.6154 30 42.4
N/16 0.0641 80 0.3077 30 17.3
N/32 0.0321 80 0.1541 30 7.1
N/64 0.0161 80 0.0773 30 2.4
W. of HAc
Wt. of
Wt. HAc at Wt. of HAc per g of
Eq. Conc. (N) activated
eq. (g) adsorbed Activated
carbon (g)
Carbon
N/2 0.3332 1.5514 0.9105 1.00 0.9105
N/4 0.2012 0.9658 0.2654 1.03 0.2577
N/8 0.2752 1.3210 -0.7056 1.00 -0.7056
N/16 0.1123 0.5390 -0.2313 1.02 -0.2268
N/32 0.0461 0.2213 -0.0672 1.04 -0.0646
N/64 0.0156 0.0749 2.4 x 10-3 1.05 3.8095 x10-3

10
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Table 5.2 Data collected at original concentration, during titration, and at equilibrium for the

second trial.

Vol of Sol’n Wt. of HAc in Vol. of HAc in Vol. of NaOH


Orig. Conc. N
(mL) orig. sol’n (g) titration (mL) used (mL)
N/2 0.5129 80 2.4619 10 48.4
N/4 0.2565 80 1.2312 10 35.2
N/8 0.1282 80 0.6154 30 31.6
N/16 0.0641 80 0.3077 30 16.4
N/32 0.0321 80 0.1541 30 6.3
N/64 0.0161 80 0.0773 30 2
W. of HAc
Wt. of
Wt. HAc at Wt. of HAc per g of
Eq. Conc. (N) activated
eq. (g) adsorbed Activated
carbon (g)
Carbon
N/2 0.3141 1.5077 0.9542 1.03 0.9264
N/4 0.2284 1.0963 0.1349 1.06 0.1273
N/8 0.2051 0.9845 -0.3691 1.05 -0.3515
N/16 0.1064 0.5107 -0.2030 1.03 -0.1971
N/32 0.0409 0.1963 -0.0422 1.03 -0.0410
N/64 0.0130 0.0624 0.0149 1.01 0.0148

The data as shown in Table 5.1 and Table 5.2 was obtained by computing the

standardized concentration of Acetic Acid solution and dividing the concentration by 2 to get

N/4, N/8, N/16, N/32, and N/64. The volume of solution was obtained by using a graduated

cylinder and transferred into an Erlenmeyer flask. The weight of HAc in original solution was

computed using the formula of normality by multiplying the original concentration by volume of

the solution by the molecular weight of HAc and dividing it all with the factor which is 1 eq/mol

for HAc. 10 mL of the prepared solution was used for titration for N/2 and N/4 while 30 mL of it

was used for N/8, N/16, N/32 and N/64. During titration, the volume of the NaOH used to

standardize the HAc solution was obtained. The concentration of the HAc at equilibrium was

computed by the milliequivalence formula where the standardized concentration of NaOH

multiplied by the volume of NaOH used for titration dividing it all with the volume of HAc at

equilibrium. For the weight of HAc at equilibrium, the formula for Normality again was then
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used by multiplying the concentration at equilibrium by volume of the solution by the molecular

weight of HAc and dividing it all with the factor which is 1 eq/mol for HAc. The weight of HAc

adsorbed was obtained through the difference between the weight of HAc at original solution and

the weight of HAc at equilibrium. Negative values of weight of HAc adsorbed for N/8, N/16 and

N/32 maybe due to inaccurate measurement of water added to the original concentration of HAc

to be titrated with NaOH. It is also possible that during the preparation of the standardized

concentrations of HAc and NaOH were inaccurately evaluated or estimated. By dividing the

weight of HAc adsorbed by the weight of activated carbon used, the ratio of weight of HAc per g

of activated carbon was obtained.

The Freundlich equation constants were obtained by getting the linear form of the

Freundlich equation and substituting the values for the equation. By using linear regression, the

constants were obtained. Data with negative values were not plotted.
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0
-4.5 -4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5

-1

-2

ln Y -3

-4

-5

-6
ln C

Figure 5.7: Graphical solution for the Freundlich equation to obtain constants k and n for the

first trial.

0
-5 -4.5 -4 -3.5 -3 -2.5 -2 -1.5 -1 -0.5
-0.5

-1

-1.5

-2
ln Y
-2.5

-3

-3.5

-4

-4.5
ln C
14

Figure 5.8: Graphical solution for the Freundlich equation to obtain constants k and n for the

second trial.

The graphs shown in Figures 5.7 and 5.8 are the graphical solution of the Freundlich

equation. First, get the linear form of the Freundlich equation and then assign ln C for the x-axis

and ln Y for the y-axis. Where C is the HAc concentration at equilibrium and Y is the weight of

HAc adsorbed per g of activated carbon. For more accurate graphical solutions we recommend

Microsoft Excel for this graph. In the Microsoft Excel, the slope-intercept equation was obtained

which is located at the top right corner of the graph. By substituting y = mx + b in the linear

form of the freundlich equation, the constants of Freundlich equation were determined which are

k and n. For the first trial, n = 0.5737 and k = 5.1952, and for the second trial the constants are n

= 0.9241 and k = 1.4196.

4.5

3.5

2.5
ln Y 2

1.5

0.5

0
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35
ln C
15

Figure 5.9: Graphical solution for the Langmuir isotherm to obtain constants a and b for the first

trial.

2
1.8
1.6
1.4
1.2
1
ln Y
0.8
0.6
0.4
0.2
0
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35
ln C

Figure 5.10: Graphical solution for the Langmuir isotherm to obtain constants a and b for the

second trial.

The graphs shown in Figures 5.8 and 5.9 are the graphical solution of the Langmuir

isotherm. First, get the linear form of the Langmuir isotherm and then assign C for the x-axis

and C/Y for the y-axis. Where C is the HAc concentration at equilibrium and Y is the weight of

HAc adsorbed per g of activated carbon. For more accurate graphical solutions we recommend

Microsoft Excel for this graph. In the Microsoft Excel, the slope-intercept equation was acquired

which is located at the top right corner of the graph. By substituting y = mx + b in the linear

form of the Langmuir isotherm, the constants of Langmuir isotherm were obtained which are a
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and b. For the first trial, a = 0.2517 and b = -3.0557, and for the second trial, a = 0.8936 and b =

-0.5559.
Chapter 4

CONCLUSION AND RECOMMENDATION

From the results obtained both from the computations and the graphical solutions, it is

therefore concluded that the adsorption of acetic acid solutions on activated carbon follows the

Freundlich adsorption isotherm. It is also evident that the adsorption decreases as the

concentration of the solution decreases, thus, the value of k remains constant at a given

temperature. Solid surfaces can adsorb dissolved substances from solutions. When a solution of

acetic acid in water was shaken with activated carbon, some of the acid was removed by the

activated carbon and the solution’s concentration was decreased. The results obtained showed

that value of k increased as the concentration of the acetic acid solutions decreased. It can be

deduced then that the degree to which the adsorbent will adsorb materials will depend on some

parameters such as temperature, the properties of the adsorbate, the degree of surface pore

structure, and the concentrations of the solute and the solvent. It must also be noted that there

are numerous factors that could contribute to possible errors that may affect the results such as

sample contamination and the use of dirty apparatus, for both could affect the volume

measurements. The burette and pipet readings may also be not accurate, for the readings may

not have been taken at eye level. This experiment is an example of physical adsorption where

dipole and van der Waals forces are predominant sources of attraction. The amount of acetic

acid (adsorbate) will depend on the surface area of the activated carbon (adsorbent), the

temperature of the solution and the adsorbate concentration in the solutions. It is recommended

that precautions should be closely observed so as to obtain more accurate results, thus having

more precise computations for the constants.

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REFERENCES

Adamson, Arthur W. (1979). “A Textbook of Physical Chemistry,” 2nd Ed. Academic Press, New

York.

Atkins, P., & De Paula, J. (2006). Physical Chemistry (8th ed.). Madison Avenue, New York:

Oxford University Press.

Brown, T. E., LeMay, H. H., Bursten, B. E., Murphy, C., & Woodward, P. (2014). Chemistry:

The Central Science (12th ed.). Singapore, Singapore: Pearson Education South Asia Pte

Ltd.

Castellan, Gilbert W. (1983). “Physical Chemistry,” 3rd Ed. Addison-Wesley.

Hansen, R. S., Craig, R. P. (1954). “The Adsorption of Aliphatic Alcohols from Aqueous

Solutions by Non-porous Carbons”. J. Phys. Chem. 58:211

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APPENDICES
APPENDIX A

List and Uses of Apparatus.

 Reagent Bottle (1000mL) was used as the container for the NaOH solution.
 Stirring Rod was used to stir solutions.
 Watch Glass was used as a container to weigh the solid reagents.
 Clamp was used to hold the buret in in titration.
 Iron Stand was used to support the titration process.
 Volumetric Flask was used to dilute the NaOH pellets to 1000 mL.
 Erlenmeyer Flask was used as receiver in titration and container for the different solutions.
 Pipetol was used to suck the liquids with the help of the pipette.
 Base burettes are used for base titrants. Basically this is used in titrations where the analyte

is an acid
 Funnels was used for guiding liquid or powder into a small opening.

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APPENDIX B

Definition of Terms

 Acetic Acid (C2H4O2) a colorless liquid with a strong and distinct pungent and sour smell.
 Sodium Hydroxide pellets [NaOH(s)] is a white, deliquescent, water-soluble solid that

upon solution in water generates heat.


 Phenolphthalein was used as an indicator in acid–base titrations.
 Potassium Hydrogen Phthalate (KHP) is an acidic salt compound. It forms white powder,

colorless crystals, a colorless solution and an ionic solid that is the monopotassium salt of

phthalic acid.
 Chemical Equilibrium is the state in which both reactants and products are present in

concentrations which have no further tendency to change with time.


 Adsorption is the phenomenon of accumulation of large number of species at the surface

of liquid or solid phase in comparison to the bulk.


 Adsorbent is the adsorbing medium. It is the substance on the surface of which

adsorption takes place.


 Adsorbate is the substance being adsorbed.

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APPENDIX C

Computations

GLACIAL ACETIC ACID

Dilution Equation: C1V1 = C2V2

(1000mL)(0.5N) = (V2)(17N)

V2 = 29.4118 mL

STANDARDIZATION OF HAc WITH NaOH

Concept of Milliequivalence: mEq base = mEq acid

(106.3mL)(0.0965N) = (20mL)(NHAc)

NHAc = 0.5129 N

ORIGINAL CONCENTRATION

N/2 = 0.5129 N

N/4 = 0.5129 N/2 = 0.2565 N

N/8 = 0.2565 N/2 = 0.1282 N

N/16 = 0.1282 N/2 = 0.0641 N

N/32 = 0.0641 N/2 = 0.0321N

N/64 = 0.0321N/2 = 0.0161 N

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23

VOLUME OF SOLUTION

N/2:100 mL

N/4: (0.2565 N)(100 mL) = (0.5129 N)(V) ; V= 50.0097 mL

N/8: (0.1282 N)(100 mL) = (0.5129 N)(V) ; V= 24.9951 mL

N/16: (0.0641 N)(100 mL) = (0.5129 N)(V) ; V= 12.4976 mL

N/32: (0.0321 N)(100 mL) = (0.5129 N)(V) ; V= 6.2585 mL

N/64: (0.0161 N)(100 mL) = (0.5129 N)(V) ; V= 3.1390 mL

WEIGHT OF HAC IN ORIGINAL SOLUTION

m = [(N)(MW)(V)]/f

N/2: m= (0.5129)(60)(80/1000)/1 = 2.4619 g

N/4: m= (0.2565)(60)(80/1000)/1 = 1.2312 g

N/8: m= (0.1282)(60)(80/1000)/1 = 0.6154 g

N/16: m= (0.0641)(60)(80/1000)/1 = 0.3077 g

N/32: m= (0.0321)(60)(80/1000)/1 = 0.1541 g

N/64: m= (0.0161)(60)(80/1000)/1 = 0.0773g


24

TRIAL 1

EQUILIBRIUM CONC.

N/2: (0.5192)(49.8) = (NHAc)(80) ; NHAc = 0.3232 N

N/4: (0.5192)(31) = (NHAc)(80) ; NHAc = 0.2012 N

N/8: (0.5192)(42.4) = (NHAc)(80) ; NHAc = 0.2752 N

N/16: (0.5192)(17.3) = (NHAc)(80) ; NHAc = 0.1123 N

N/32: (0.5192)(7.1) = (NHAc)(80) ; NHAc = 0.0461 N

N/64: (0.5192)(2.4) = (NHAc)(80) ; NHAc = 0.0156 N

WEIGHT OF HAC AT EQUILIBRIUM

N/2: m = (0.3232)(60)(80/1000)/1 = 1.5514 g

N/4: m = (0.2012)(60)(80/1000)/1 = 0.9658 g

N/8: m = (0.2752)(60)(80/1000)/1 = 1.3210 g

N/16: m = (0.1123)(60)(80/1000)/1 = 0.5390 g

N/32: m = (0.0461)(60)(80/1000)/1 = 0.2213 g

N/64: m = (0.0156)(60)(80/1000)/1 = 0.0749


25

WEIGHT OF HAC ABSORBED

N/2: 2.4619 – 1.5514 = 0.9105 g

N/4: 1.2312 – 1.5514 = 0.2054 g

N/8: 0.6154 – 1.5514 = -0.7056 g

N/16: 0.3077 – 1.5514 = -0.2313g

N/32: 0.1541 – 1.5514 = -0.0672 g

N/64: 0.0773 – 1.5514 = 2.4x10-3 g

WEIGHT HAC / ACTIVATED

N/2: 0.9105 / 1.00 = 0.9105

N/4: 0.2654 / 1.03 = 0.2577

N/8: -0.7056 / 1.00 = -0.7056

N/16: -0.2313 / 1.02 = -0.2268

N/32: -0.0672 / 1.04 = -0.0646

N/64: 2.4X10-3 / 1.05 = 3.8095X10-4


APPENDIX D

Documentation

Figure D.1: Weighed Activated Carbon


inside Weighing Bottle Containers

Figure D.2: Pipetting Separately the Clear Liquid


from the Twelve Flasks

26
27

Figure D.3: Titration of the created Solutions


APPENDIX E

Problems

1. The following are data for the adsorption of CO on wood charcoal at 0 C. The pressure P is in

mmHg while x is the volume of the gas in cc, measured standard conditions adsorbed 2.964 g

of charcoal.

P, mmHg x,cc P, mmHg x,cc


73 7.5 540 38.1
180 16.5 882 52.3
309 25.1

Find graphically the constant k and n of the Freundlich equation.


Given: mcharcoal = 2.964 g
T=0 C

P, mmHg x, cc
73 7.5
180 16.5
309 25.1
540 38.1
882 52.3

Required: k and n (using Freundlich equation)


Solution: Using Freundlich Isotherm equation:
1
y = kP n

1
ln y = ln k + n (ln P) y = mx + b

ln P ln y (x/mcharcoal)
4.290459441 0.9283633131
5.192956851 1.716820673
5.733341277 2.136328139
6.29156914 2.553674575

28
6.782192056 2.870456664

29
30

3.5

2.5

2
ln y
1.5

0.5

0
4 4.5 5 5.5 6 6.5 7
ln P

1
n = 0.7816192885

n = 1.2794

ln k = -2.381354357

k = 0.09243

Answer: The values of n and k are 1.2794 and 0.09243respectively.

2. Find graphically the constants a and b in the Langmuir equation which fit the data given in

problem number 1.

Given: mcharcoal = 2.964 g


T=0 C

P, mmHg x, cc
73 7.5
180 16.5
309 25.1
540 38.1
882 52.3
31

Required: a and b (using Langmuir equation)


Solution: Using Langmuir Isotherm equation:
aP
y=
1+bP

P 1 b
= + P
y a a y = mx + b

P P
P ( )
y x /m

73 28.8496
180 32.33454545
309 36.48908367
540 42.00944882
882 49.98562141

60

50

40

30
P/y
20

10

0
0 100 200 300 400 500 600 700 800 900 1000
P

1
a = 27.70199891

a = 0.03610
b
a = 0.02578543589

b = 9.3081 x 10-4
32

Answer: The value of a is equal to 0.03610 while b is equal to 9.3081 x 10-4.

3. In a laboratory experiment, 50 cc of a solution originally 0.2 molar in CH 3COOH was

permitted to come to equilibrium with a 5-g sample of charcoal. At equilibrium, 25 cc of the

CH3COOH solution required 30.0 cc of 0.1 N NaOH for neutralization. Calculate the weight

of CH3COOH adsorbed per gram of charcoal and the equilibrium concentration of the acid.

Given: VAcetic acid solution = 50 cm3

MAcetic acid = 0.2 molar

mcharcoal = 5 g

At equilibrium: VAcetic acid solution = 25 cm3

VNaOH = 30.0 cm3

NNaOH = 0.1N

macetic acid adsorbed


Required: a.) g of charcoal

b.) NAcetic acid at equilibrium

Solution:

at equilibrium: (VAcetic acid solution) (NAcetic acid) = (VNaOH) (NNaOH)


33

(25 cm3) (NAcetic acid) = (30.0 cm3) (0.1 N)

NAcetic acid at equilibrium = 0.12 N

( macetic acid )
( macetic acid )
60 g/mol eq
MW of acetic acid N= x1
N= x factor 1 L mol
L of acetic acid solution 50 cm 3 x 3
1000 cm

macetic acid at equilibrium=0.36 g

( macetic acid )
in original solution: MW of acetic acid
M Acetic acid=
L of acetic acid solution

( macetic acid )
60 g /mol
0.2 molar=
1L
50 cm3 x
1000 cm 3

m Acetic acid ∈original solution=0.6 g

m
( ¿¿ Acetic acid at equilibrium)
( m Acetic acid ∈original solution )− g of charcoal
m Acetic acid adsorbed
=¿
g of charcoal

mAcetic acid adsorbed 0.6 g−0.36 g


=
g of charcoal 5g
34

mAcetic acid adsorbed


=0.048 grams
g of charcoal

Answer: a.) 0.048 grams of acetic acid was adsorbed per gram of charcoal.

b.) The equilibrium concentration of acetic acid is 0.12 normal.

4. For the adsorption of a substance A from aqueous solution by charcoal at 25 the Freundlich

constants are n=3.0 and k=0.50 for y in grams per gram and C in grams per liter. What weight

of a W is adsorbed by 2 g of charcoal from 1 L of a solution containing originally 2 g of the

substance?

Given: T = 25 C

nF = 3.0

KF = 0.50

mcharcoal = 2 g

Vsolution = 1 L

msubstance = 2 g

Required: madsorbed

1
nF
Solution: y=K F C
35

m adsorbed 2 grams 1

2 g charcoal
=(0.50)( 1L ) 3.0

madsorbed = 1.2599 grams

Answer: The amount of mass adsorbed by charcoal is equal to 1.2599 grams.

5. The following data are obtained for the adsorption of acetone on charcoal from an aqueous

solution at 18 C:

Y, millimoles/g C, millimoles/L Y, millimoles/g C, millimoles/L


0.208 2.34 1.50 88.62
0.618 14.65 2.08 177.69
1.075 41.03 2.88 268.97

Evaluate graphically the constants k and n of the Freundlich equation.


Given: T = 18 C

Y, mmol/g C,mmol/L
0.208 2.34
0.618 14.65
1.075 41.03
1.50 88.62
2.08 177.69
2.88 268.97
Required: k and n (using Freundlich equation)
1
n
Solution: y = kC
36

1
ln y = ln k + n (ln C) y = mx + b

ln C ln Y
0.8501509294 -1.570217199
2.684440335 -0.4812668215
3.714303506 0.07232066158
4.484357566 0.4054651081
5.180040459 0.7323678937
5.594599849 1.057790294
1.5

0.5

0
ln Y 0 1 2 3 4 5 6
-0.5

-1

-1.5

-2
ln C

1
n = 0.5381963994

n = 1.8581
ln k = -1.982867807
k = 0.1377
Answer: The values of the constants k and n are 0.1377 and 1.8581 respectively.

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