Choba tapaphiwa

17001055
EXPERIMENT 2
CHEM 408
ADSORPTION OF ACETIC ACID ON TO ACTIVATED CHARCOAL
 1. ABSTRACT

Adsorbents have been commonly used to solve some environmental and related
issues. Activated carbons are widely used as adsorbents due to their extraordinary large
specific surface areas, well-developed porosity (their porous structure) and accessibility of
their surface. Adsorption is usually described through adsorption isotherms such as
Langmuir, Freundlich and Temkin. The main purpose of this study was test the validity of the
Langmuir adsorption isotherm and to measure the surface area per gram of a sample of
activated charcoal. From this experiment, it was found out that the adsorption of acetic acid
in charcoal follows the Langmuir theory of adsorption isotherm which shows that the
adsorption decreases as the concentration of the acetic acid solution decreases and from
the experimental results, the surface area of charcoal was found to be 3.280 x 10^3m2g-1

2. AIM
To test the validity of the Langmuir adsorption isotherm and to measure the surface area
per gram of a sample of activated charcoal.
3. INTRODUCTION
Activated carbons are carbon containing materials that can be differentiated from elemental
carbon by the oxidation of the carbon atoms found on the outer and inner surfaces. These
materials are categorized by their extraordinary large specific surface areas, well-developed
porosity (their porous structure) and accessibility of their surface. Activated carbon has an
exceptionally high surface area of approximately 400-1000 m 2 in 1 gram due to a high
degree of micro porosity [1]. For these unique features, activated carbons are widely used
as adsorbents for water treatment and in industrial applications such as in the extraction of
metal ions, air handling and purification, the discoloration of food in the food industry and
in the pharmaceutical industry [2]. Adsorption is the physical adherence or bonding of ions
and molecules onto the surface of another molecule and the matter that is attracting to the
surface is called adsorbate and the matter that attract or where others matters adhere on is
called adsorbent.

There are a wide variety of adsorbent materials such as silica gel, zeolites, synthetic
adsorbents (resins), clays, activated alumina, bio adsorbents and activated carbon.
Adsorption is highly recommended for elimination of organic and inorganic pollutants at low
concentrations and it requires a micro porous adsorbent, capable of exchanging ions and
creating chemical bond [3]. Acetic acid is an organic pollutant with a specific surface area
close to that of nitrogen most often used in adsorption experiments, hence it is used in this
study to characterize ACs samples. Adsorption is usually described through adsorption
isotherms, that is, functions which connect the amount of adsorbate on the adsorbent with
its pressure (if gas) or concentration (if liquid) and the equilibrium relationship of
adsorbent and adsorbate at constant parameter like temperature is normally very
informative with their isotherm models such as: Langmuir, Freundlich and Temkin in a
variety of studie [1].

In this experiment Langmuir Isotherm plot will be used to estimate the surface area of
activated carbon. This isotherm assumes that adsorption takes place at specific
homogeneous sites within the adsorbent, and has found successful applications for many
sorption processes of monolayer adsorption. Langmuir Isotherm relates the coverage or
adsorption of molecules on a solid surface to gas pressure or concentration of a medium
above the solid surface at a fixed temperature. The Langmuir introduced an equation for
adsorption isotherm as follows;

C C 1
= +
N N m KN m
C 1
A plot of versus C will give a straight line with a slope of . If the cross section area
N Nm
(σ) of the absorbed molecule is known (which area occupied by each adsorbate molecule on
the surface of adsorbent). The specific surface area, A (m 2g-1) can be calculated using the
following equation: A = N m N O σ x 10-20 m2g-1

Where, A = specific surface area of 1 g of solid (m 2) , N O = Avogrado number ,N m =

1 C
from the graph versus C and σ = cross sectional area of the adsorbate
gradient N
molecule.

EXPERIMENTAL
REAGENTS AND CHEMICALS
• Powdered activated charcoal 
• Acetic acid
• Sodium hydroxide 
• Phenolphthalein

APPARATUS AND GLASSWARE

• Volumetric flasks
• Conical flasks
• Beakers
• Pipettes
• Burettes 
• Funnel
• White tile
• Stoppered 250 cm3 reagent bottles

4. PROCEDURE

1g of powdered activated charcoal was weighed into each of 5 clean, stoppered 250 cm 3
stoppered reagent bottles. 100ml of 0.2 M (stock solution) acetic acid was added to the first
flask and shaken. Then 100ml acetic acid was added to each of the other flasks at varying
concentrations of; 0.15, 0.10, 0.07 and 0.03 M. The loosely stoppered flasks were shaken
periodically for 30mins using an orbital shaker. The flasks were then allowed to stand for 1
hour at room temperature. The solutions were filtered using a fluted filter paper to remove
the charcoal particles. Two 10 ml portions of the filtrate for each flask was then titrated with
0.1 M NaOH using phenolphthalein as an indicator.

5. RESULTS

Table 1; Preparations of acetic acid solutions

Concentration Volume of acetic Volume of distilled

of Acetic acid acid added (ml) water added (ml)

0.15 75 25

0.10 50 50

0.07 35 65

0.03 15 85

Sample calculation for preparation of 100ml acetic acid solution

From the stock solution provided, each concentration of the solution were prepared by
dilution process; M1V1 = M2V2

0.15M of Acetic Acid

M1V1 = M2V2
(0.2M) (V1) = (0.15M) (100mL)
V1 =75 mL
25 ml of distilled water was added to make 100 ml of the solution.

Preparation of standard solution of NaOH by using the formula;

n = MV/ 1000

= 0.1 M x 250 mL
1000
= 0.025 mol

Mass of NaOH = n x molar mass , Mr of NaOH = 40g mol-1

=0.025 mol x 40 g mol-1

= 1.0 g

Table 2; Mass of activated carbon used

Concentration of Initial Final volume Average

Acetic acid(M) volume (ml) (ml) volume of
NaOH (ml)

0.20 0.00 43.92 43.92

0.15 0.00 30.96 30.96
0.10 0.44 18.86 18.42
0.07 31.12 41.12 10.00
0.03 31.52 32.94 1.42

Table 3; Volume of NaOH used for each titration

Concentration of Acetic acid(M) Mass of activated carbon(g)

0.20 1.0000
0.15 1.0010
0.10 1.0013
 0.07 1.0020
0.03 1.0010
 The final (equilibrium) concentration of each acetic solution after titrated with NaOH

1. 0.2M of Acetic Acid

M1V1 = M2V2
(M2) (10mL) = (0.10M) (43.92mL)
M2 =0.4392M

 The number of moles of acetic acid adsorbed by 1 g of activated solution of each

acetic acid

1. 0.2M of Acetic Acid

a) Initial concentration
M1 =0.2M

Initial mol = n = MV/ 1000

= 0.2 M x 100 mL = 0.02 mol

1000

b) Final concentration
M2 = 0.4392M
Final mol = n = MV/ 1000
= 0.4392M x 100 mL = 0.04392 mol
1000

c) Number of mole of CH3COOH adsorb

Initial mol – final mol =0.02mol – 0.004392mol
=0.0156 mol

d) N = Number of mole of CH3COOH adsorb per gram of activated carbon

N = number of mole of CH3COOH adsorb
Mass of activated carbon
= 0.0156 mol = 0.0156 mol/g
1.000g

Table 4; Values of C and N obtained for each initial concentration of acetic acid
Flasks Equilibrium C (mol/L) N (mol/g) C/N (g/L)

1 0.4392 0.0156 85.0292

2 0.3092 0.0346 89.1745

3 0.1842 0.0109 79.9877

4 0.1000 0.0858 69.9352

5 0.0142 0.0358 73.4784

GRAPH OF C/N Versus C

100
90
80 f(x) = 39.1774750262861 x + 71.3188038284967
R² = 0.690739751064564
70
60
C/N(g/L)

50
40
30
20
10
0
0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0.45 0.5
C(mol/L)

Figure 1; graph of C/N Vs C used to determine the value of Nm and the equilibrium constant

From equation

C C 1
= +
N N m KN m

1
We know that = gradient from the graph C/N versus C
N m

From the graph

1
= 39.177
N m

Nm = 1 / 39.177 = 2.552 x 10^-2 mol/g

 By assuming that the cross sectional area of acetic acid is 21 A2, The specific surface
area of activated carbon used in this experiment

A = N m N O σ x 10-20 m2g-1
= 2.552 x 10^-2 x 6.02x 1023 x 21 x 10-20 m2g-1
= 3.280 x 10^3m2g-1

Intercept= 71.319 g/L

1/KNm=71.319

K= 5.49x10^-4 M-1

GRAPH OF NUMBER OF MOLES VS CONCEN-

TRATION figure 2;graph of
0.4 number of moles
0.35 vs concentration
number of moles(mol/g)

0.3
0.25 6. DISCUSSIO
0.2 N
0.15
0.1 The adsorption is
0.05
influenced by
0
0 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 0.09 0.1
various factors
concentration(M)
such as initial
acetic acid concentration, amount of adsorbent, nature of adsorbent, temperature, nature
of adsorbent and contact time[4]. From the results in table 3 above, it shows that the
equilibrium concentration was lower than the initial concentration thereby indicating that
adsorption took place. This is because solid surfaces can adsorb dissolved substances from
solution therefore when a solution of acetic acid in water is shaken with activated carbon,
part of the acid is removed by the carbon and then the concentration of the solution
decreases.

A graph of C/N versus C was plotted as shown by figure 1 above and the equation of the line
was y= 39.177 + 71.319 and from the slope of the line Nm was determined to be 2.552 x
10^-2 mol/g therefore this high coefficient guaranteed a good adsorption of acetic acid on
activated charcoal. There was a linear relationship between C and C/N for various
concentrations of the acetic acid as depicted by the graph above and since it is assumed that
the adsorption of acetic acid in charcoal follows the Langmuir theory of adsorption isotherm
which states that the adsorption decrease as the concentration of the acetic acid solution
decrease then adsorption was directly proportional to concentration [5]. From the obtained
results, some of the points in the graph slightly deviated from the best fit line and this
resulted in a poor representation and a low value of the regression coefficient.

R squared known to be the coefficient of determination, tells one how many points fall on
the regression line .From the graph above, r-squared was found to be 0.6907 so this means
that 69.07% of the variation of y-values around the mean are explained by the x-values. This
shows that there was low linearity because good linearity should have an r-squared of
above 0.95. The correlation coefficients reported and showed slightly good positive
evidence on the adsorption of acetic acid onto AC indicating that this follows the Langmuir
isotherm however the applicability of the linear form of Langmuir model to AC was slightly
proved by the correlation coefficients since the r-squared value was low [2]. The R-squared
parameter in many cases is considered as a more reliable indicator of adsorption and in this
experiment these value is found to be positive and less than one indicating thereby a highly
favorable adsorption.

The degree to which a solid will adsorb material depends on a number of things including
temperature, the nature of the molecule being adsorbed, degree of surface pore structure,
and, solute concentration & solvent [4]. Based on the calculations above, the surface area of
charcoal is 3.280 x 10^3m2g-1 so this imply that there is a high level of accessible area of solid
surface (activated carbon) per unit mass of material (acetic acid). However this value is
slightly big if compared to the area per gram of activated charcoal as determined by
nitrogen adsorption which is typically between 300-1000m2/g [6]. This may be due to the
errors that occurred during the experiment such as inaccurate reading of the volume of the
sodium hydroxide used for each titration due to parallax error and also overshooting. This
error can be avoided by taking the reading below the meniscus and also titrating slowly and
carefully to avoid overshooting.

The theoretical concept however behind the Langmuir are that; the adsorption is an
equilibrium process, the adsorption cannot proceed beyond monolayer coverage and all
sites are equivalent and the surface is uniform i.e the surface is perfectly flat on a
microscopic scale[1]. Hence, the ability of a molecule to adsorb at a given site is
independent of the occupation of neighboring sites therefore this is a confirmation of the
fitness of experiment data into Langmuir isotherm model which indicates the homogenous
nature of the adsorbent surface there this isotherm was successfully followed.

7. CONCLUSION
From this experiment, it can be concluded that the adsorption of acetic acid in charcoal
follows the Langmuir theory of adsorption isotherm which shows that the adsorption
decreases as the concentration of the acetic acid solution decreases.  From the
experimental result, the surface area of charcoal was found to be 3.280 x 10^3m2g-1

 Answers to Post- Lab questions

1. Since acetic acid absorbs differently from nitrogen it was used in this experiment hence
the difference in the results ,also this may be due to some of the errors that occurred during
the experiment such as inaccurate reading of the volume of the sodium hydroxide used for
each titration due to parallax error and also overshooting.

2. Oxidation is used to increase the surface acidity of the carbon by introducing acidic
surface groups responsible for more specific adsorption forces and also some other surface
groups introduced can be heteroatoms such as oxygen. Typically the surface area for
activated carbon is approximately 1,000 square meters per gram (m 2/gm).

3. The most common use for the carbon-based substance is for the absorption of toxins in
the body, most notably in the digestive tract. Activated charcoal is administered as a slurry
to a patient to absorb and stop the harmful substance from being processed by the body.
Then the toxin can pass harmlessly from the system.

4. For a weak acid and a strong base (e.g. acetic or ethanoic acid and NaOH) a suitable
indicator is phenolphthalein. The pH of the mixture at the equivalence point is 8.73 and the
color expected is a permanent light pink. An alternative indicator would be thymol blue
indicator.

5. An equilibrium constant, designated by a upper case K, is the ratio of the equilibrium

concentrations of reaction products to reactants or vice versa. For bimolecular reactions,
the units of Kd are concentration (M, mM, µM, etc.) and the units of Ka are concentration -1
(M-1, mM-1, µM-1, etc.). However equilibrium constant, like unimolecular reactions, is unit
less.
 8. REFERENCES
[1] Dada, A.O, Olalekan, A. . (2012) ‘Langmuir, Freundlich, Temkin and Dubinin–
Radushkevich Isotherms Studies of Equilibrium Sorption of Zn 2+ Unto Phosphoric Acid
Modified Rice Husk’, IOSR Journal of Applied Chemistry, 3(1), pp. 38–45. doi: 10.9790/5736-
0313845.

[2] Berhe, A., Jeevan, A. and Lijalem, T. (2015) ‘Removal of Acetic Acid from Aqueous
Solution by using Activated Carbon’, International Journal of Innovation and Scientific
Research, 17(2), pp. 443–450. Available at: http://www.ijisr.issr-journals.org/.

[3] Elhussien, M. H. and Isa, Y. M. (2015) ‘Acetic Acid Adsorption onto Activated Carbon
Derived from Pods of Acacia nilotica var astringens (Sunt tree) by Chemical Activation with
ZnCl2’, Journal of Natural Sciences Research, 5(10), pp. 42–49. Available at:
http://citeseerx.ist.psu.edu/viewdoc/download?doi=10.1.1.892.6635&rep=rep1&type=pdf.

[4] Jalil, A. H. (2012) ‘Surface Area Determination of Activated Carbons Produced from
Waste Tires Using Adsorption from Solution Abstract ’:, Tikrit Journal of Pure Science, 17(2),
pp. 2–7.

[5] Itodo, A., Itodo, H. and Gafar, M. (2011) ‘Estimation of Specific Surface Area using
Langmuir Isotherm Method’, Journal of Applied Sciences and Environmental Management,
14(4), pp. 1–5. doi: 10.4314/jasem.v14i4.63287.

6. Nethaji, S., Sivasamy, A. and Mandal, A. B. (2013) ‘Adsorption isotherms, kinetics and
mechanism for the adsorption of cationic and anionic dyes onto carbonaceous particles
prepared from Juglans regia shell biomass’, International Journal of Environmental Science
and Technology, 10(2), pp. 231–242. doi: 10.1007/s13762-012-0112-0.