Experiment 8: Surface Chemistry

(Adsorption of acetic acid on activated carbon).

Objective

To study the adsorption isotherm of acetic acid by activated carbon.

Introduction

Surface chemistry is the branch of chemistry that deals with process of adsorption
that occurs on the surface of a liquid or solid. Adsorption is found in most natural
physical, biological, and chemical systems and it is very important particularly for
industrial purposes. The most common process involving adsorption process in
industry is waste water treatment. The term adsorption is used to describe the
process that occurs when a gas or liquid or solute called adsorbate accumulates on
the surface of adsorbent forming a molecular or atomic film. The adsorbent can be a
solid or more rarely a liquid. The adsorbate may be held on the surface either by
physical attraction forces or chemical forces. The adsorption due to physical
adsorption is called physisorption while the adsorption due to chemical affinity is
called chemisorption.

Adsorption is usually described through isotherms, that is, functions which relate the
amount of adsorbate on the adsorbent with pressure of gas or concentration of
liquid. There are several models of isotherms available in literature that can be used
to discuss the process of adsorption such as Langmuir isotherm, Freundlich
isotherm, BET isotherm and so on. Each isotherm differs from each other by the
assumptions that must be made while working with these models of isotherms. In
general, the amount of adsorption, Y is expressed as number of moles of adsorbate
per mass of adsorbent. The amount of adsorption increases with the concentration
or pressure of the adsorbate. The increase is rapid at first but as the surface of
adsorbent fills with adsorbate, the rate of adsorption, dY/dc decreases. As the
surface of the adsorbent becomes full, further increases in concentration would not
contribute in increase of the amount adsorbed. The amount adsorbed when the
surface is covered with a monolayer of the adsorbate is called Ymax. At a given
concentration, the amount adsorbed decreases with increasing temperature.

The Freundlich adsorption isotherm can be represented as

Y = kc1/n (1)

where
Y = the amount of adsorption in of moles of adsorbate per mass of adsorbent
c = concentration in mol dm-3
k and n are experimentally determined constants
linear form of Equation (1) is

1
log Y =log k + (2)
nlogc

To test the validity of the Freundlich isotherm, a plot of log Y against log c should
give a straight line with slope equal to 1/n and the y-intercept equal to log k.
The equation for the Langmuir isotherm is
c 1 c
= +
Y kYmax Ymax

If the system follows the Langmuir isotherm, then the plot of c/Y against c is a
straight line with a slope equal to 1/Ymax and the y-intercept equal to 1/kYmax

Apparatus

 250 cm3 conocal flask

 20 cm3 beaker
 Burette
 25 cm3 pipette
 100 cm3 measuring cylinder
 Filter funnel
 Retort stand
 Parafilm

Chemicals
 Activated charcoal (carbon)
 0.4 M acetic acid (CH3COOH)
 0.1 M sodium hydroxide (NaOH)
 Phenolphthalein indicator

Procedure

About 1.5 g of activated charcoal were weighed into each of the dry glass-stoppered flasks.
Then, series of acetic acid was prepared of various concentrations according to the Table 8.1.
A 100 cm3 measuring cylinder was used to measure the required amount of 0.4 M acetic acid
and then was diluted with distilled water to exactly the 100 cm3 mark. The prepared acetic
acid solution (100 cm3) were poured into each of the glass-stoppered conical flask containing
charcoal. The flask vigorously was swirled and let them stand for a week. Next, the solutions
were filtered. A suitable volume (refer to Table 8.2) of the filtrate were titrated with the
standard 0.1M NaOH using phenolphthalein as indicator.A pipette was used to measure
accurately the required aliquot. Lastly, the titration were repeated for three times for each
sample.
 Table 8.1 : Suggested volumes of 0.4 M acetic acid to be diluted to 100 cm3
Sample Volume 0.4 M acetic acid
(cm3)
1 100
2 75
3 50
4 25
5 10
6 5

Table 8.2 : Volume of filtrate required for analysis of sample

Sample Volume of filtrate
(cm3)
1 10
2 10
3 10
4 25
5 25
6 40

Result

Sample 1 2 3 4 5 6
Mass of activated carbon 1.5052 1.5047 1.5056 1.5056 1.5010 1.5052
(g)
Titration : Volume of
NaOH (cm3)
Trial 1 38.20 27.80 18.30 20.90 6.70 3.70
Trial 2 38.00 27.70 18.00 20.90 6.70 3.80
Trial 3 38.10 27.60 18.10 21.00 6.40
Average volume of NaOH 38.10 27.70 18.13 20.93 6.60 3.75
(cm3)
 Calculation

sample 1 2 3 4 5 6
Initial concentration of diluted acetic 0.40 M 0.30 M 0.20 M 0.1M 0.04M 0.02M
acid (mol dm-3) (c)

Final concentration of diluted acetic 0.381 M 0.277 M 0.1813M 0.2093M 0.066M 0.0375M
acid (mol dm-3)
Concentration of acetic acid 0.019M 0.023 M 0.0187M 0.0163M 0.0136 0.0106 M
(adsorbed) in equilibrium with the M
adsorbent (mol dm-3)

Amount in mole of adsorbed acetic 1.2644 X 1.526 X 1.242 X 1.0826 X 9.06 X 7.04 X
acid per g charcoal (y) 10-3 10-3 10-3 10-3 10-3 10-3

Log c -0.3979 -0.5229 -0.6990 -1.000 -1.3979 -1.6990

Log y -2.8996 -2.8153 -2.9066 -2.966 -3.043 -2.152

c/y 317.460 196.078 161.290 92.37 44.15 28.41

Discussion

This experiment was conducted to study the adsorption isotherm of acetic

acid by activated carbon. Activated charcoal with presence of 0.4 M acetic acid was
used to titrated by 0.1 M sodium hydroxide, NaOH with phenolphnathalein indicator.
Adsorption is the adhesion of atoms,ions,or molecules from a gas ,liquid or dissolved
solid to a surfeca. A molecule that undergoes adsorption is referred to as the
adsorbate, the solid is the adsorbent. Chemisorption is the process commonly known
as bond formation between the adsorbate and the surface. Physical adsorption
involves low heats of adsorption and is enhanced by lowering the temperature while
chemical adsorption involve higher heats of adsorption and is enhanced by raising
the temperature. Similar to surface tension, adsorption is a consequence of surface
energy.

The factors that decide the amount of substance that can be adsorbed
onto activated charcoal are nature of adsorbate and adsobent, the surface area of
adsorbent, activation of adsorbent and experimental condition such as temperature.
Adsorption process is studied through graphs known as adsorption isotherm. In this
experiment, Langmuir equation is used to estimate the surface area of activated
charcoal sample. Langmuir derived an equation which explained the relationship
between the number of active sites of the surface undergoing adsorption and
pressure.

The possible errors that occur while conducting this experiment is the
position of the eye would not perpendicular to meniscus line which cause the
amount of sodium hydroxide titrated recorded are inaccurate and it will changes
overall result of the experiment. Besides, the amount of charcoal is added is more
than needed and not distributed equally over the solution. This cause the solution
not achieved equilibrium. Next, the charcoal maybe included in supernatant that will
affect the amount of sodium hydroxide needed to change colour drom dark blue to
colourless.

Conclusion

From this experiment, the adsorption of acetic acid in charcoal follows the
Langmuir theory of adsorption isotherm which shows that the adsorption decrease
as the concentration of the acetic acid solution decrease.
References

1. Mashiah Domat Shaharudin, Nesamalar Kantasamy (2019), Introduction to

Physical Chemistry (3rd edtion), Pencetakan Tabah Sdn. Bhd. UiTM Press
2. Hofmann, A. (2016). Introduction to physical chemistry. Nathan, Qld.:
Structural Chemistry Program, Griffith University.
3. Atkins, P. W., & Paula, J. D. (2010). Physical chemistry. New York: W.H.
Freeman and Co

Question
The data below relate to the adsorption of N2 on rutile (TiO2) at 75 K. Confirm
that they fit a BET isotherm in the range of pressure reported, and determine
Vmon and c.

p/Torr 1.20 14.0 45.8 87.5 127.7 164.4 204.7

V/mm3 2.35 559 649 719 790 860 950
At 75 K, p* = 570 Torr. The volumes have been corrected to 1.00 atm and 273 K
and refer to 1.00 g substrate.

Answer:

Z=p/p* 2.11 24.50 80.35 153.51 224.04 288.42 359.12

(10-3)
z/(1-z)V 8.99x1 1.07x10- 1.35x10- 2.52x10- 3.65x10- 4.71x10- 5.90x10-
0-6 4 4 4 4 4 4

*Graph was plot at graph paper