Professional Documents
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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
by
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!
2
TABLE OF CONTENTS
TITLE PAGE i
ACKNOWLEDGEMENT ii
LIST OF TABLES iv
LIST OF FIGURES v
ABSTRACT vi
Chapter 1: INTRODUCTION
1
REFERENCES 16
APPENDICES 17
Appendix A 18
Appendix B 19
Appendix C 20
Appendix D 24
Appendix E 26
Appendix F 34
3
LIST OF TABLES
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 D.2: Pipetting Separately the Clear Liquid from the Twelve Flasks 24
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
obtain more accurate results, thus having more precise computations for the constants.
6
Chapter 1
INTRODUCTION
because the atoms or ions at the surface of a solid are extremely reactive. Adsorption has two
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
2
3
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
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
In 1916, Irving Langmuir proposed the Langmuir adsorption isotherm. This isotherm was
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).
Kp
θ=
1+Kp
Where θ is the surface coverage, p is is the partial pressure of adsorbate, and K is a constant
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
incorporate the role of substrate-substrate interactions on the surface. The following equation
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,
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
temperature environment.
Chapter 2
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
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
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
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
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
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
The KHP solution was titrated with 0.1000 N NaoH solution until it turned light pink
in color.
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
The solution was titrated with the standardized NaoH solution until it turned light pink
in color.
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.
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.
The solutions were titrated with the standardized NaoH solution until it turned light
pink in color.
Figure 5.6: Flow chart for the determination of the equilibrium concentrations of the adsorption
solutions
Chapter 3
Table 5.1 Data collected at original concentration, during titration, and at equilibrium for the first
trial.
10
11
Table 5.2 Data collected at original concentration, during titration, and at equilibrium for the
second trial.
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
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
12
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
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.
13
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
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
16
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
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
17
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:
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.
Hansen, R. S., Craig, R. P. (1954). “The Adsorption of Aliphatic Alcohols from Aqueous
18
APPENDICES
APPENDIX A
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.
20
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
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
21
APPENDIX C
Computations
(1000mL)(0.5N) = (V2)(17N)
V2 = 29.4118 mL
(106.3mL)(0.0965N) = (20mL)(NHAc)
NHAc = 0.5129 N
ORIGINAL CONCENTRATION
N/2 = 0.5129 N
22
23
VOLUME OF SOLUTION
N/2:100 mL
m = [(N)(MW)(V)]/f
TRIAL 1
EQUILIBRIUM CONC.
Documentation
26
27
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
73 7.5
180 16.5
309 25.1
540 38.1
882 52.3
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
2. Find graphically the constants a and b in the Langmuir equation which fit the data given in
problem number 1.
P, mmHg x, cc
73 7.5
180 16.5
309 25.1
540 38.1
882 52.3
31
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
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.
mcharcoal = 5 g
NNaOH = 0.1N
Solution:
( 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 )
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 at equilibrium)
( m Acetic acid ∈original solution )− g of charcoal
m Acetic acid adsorbed
=¿
g of charcoal
Answer: a.) 0.048 grams of acetic acid was adsorbed per gram of charcoal.
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
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
5. The following data are obtained for the adsorption of acetone on charcoal from an aqueous
solution at 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.