EXPERIMENT No - 12

AIM: DETERMINATION OF ADSORPTION ISOTHERM OF ACETIC ACID ON

ACTIVATED CHARCOAL
OBJECTIVE: To determine the adsorption capacity of activated charcoal
APPARATUS:
6 boiling flasks (250 ml), 6 Erlenmayer’s flasks (250 ml), 6 funnels, 3 burettes (50 ml),
10 titrimetric flasks, 3 pipettes, holders for funnel, holders for burettes, filtering paper,
vessels for weighing coal, spoon, rubber stoppers
CHEMICALS:
activated charcoal
acetic acid solution
solution of NaOH (concentration = 1N),
phenolphthalein indicator
THEORY:
Activated carbon is a carbon based material having exceptionally high surface area. It is known
to possess very high adsorption capacity. Activated carbon is frequently used in everyday life,
in– industry, food production, medicine, pharmacy, military, wastewater treatment etc.
Adsorption is a process that occurs when a gas or liquid solute (adsorbate) accumulates on the
surface of a solid or a liquid (adsorbent), forming a molecular or atomic film. It is different from
absorption, in which a substance diffuses into a liquid or solid to form a solution. There are two
ways by which the adsorbate binds to the surface of the adsorbent: physisorption and
chemisorption. Physisorption or physical adsorption is a type of adsorption in which the
adsorbate adheres to the surface only through Van der Waals (weak intermolecular) interactions.
Chemisorption is a type of adsorption whereby a molecule adheres to a surface through the
formation of a chemical bond.
Adsorption is usually described through adsorption isotherms. An adsorption isotherm is a plot
of the concentration of adsorbate at equilibrium vs the amount of adsorbate adsorbed on the
surface of the adsorbent.
The linear form of the Langmuir isotherm is represented as:
1 1 1
= +
𝑞𝑒 𝑄𝑜 𝑏𝑄𝑜 𝐶𝑒

Where Ce is the concentration of adsorbate at equilibrium and qe is the amount of adsorbate

adsorbed at equilibrium per gram of adsorbent. Qo and b are Langmuir constants corresponding
to maximum adsorption capacity and energy of adsorption respectively. Langmuir isotherm is
based on four hypotheses:
1. The surface of the adsorbent is uniform, that is, all the adsorption sites are equal.
2. Adsorbed molecules do not interact.
3. All adsorption occurs through the same mechanism.
4. At the maximum adsorption, only a monolayer is formed: molecules of adsorbate do not
deposit on other, already adsorbed, molecules of adsorbate, only on the free surface of the
adsorbent.
PROCEDURE:
1. Prepare aqueous solutions of acetic acid into numbered flasks following the scheme given
in the Table 1. The total volume of each flask is 60 ml. Use flasks fitted with stoppers.
Table-1: Scheme for acetic acid dilution
Flask # Volume of acetic acid (mL) Volume of distilled water (mL)
1 6 54
2 12 48
3 18 42
4 30 30
5 42 18
6 60 0

2. Transfer defined volume of acetic solution into numbered titrimetric flask as given in
Table-2.
Titrimetric flask 1 2 3 4 5 6
Volume of solution (mL) 10 10 5 5 2 1

3. Add 1-2 drops of phenolphthalein and titrate by NaOH.

4. Once the endpoint has been reached, read the burette. Let the volume of NaOH that was
required to reach the endpoint for titrimetric flask i be V1 (mL) and write down in Table
3.
5. Calculate the actual concentration of acetic acid before adsorption (Cif) in the flasks 1-6
respectively as per normality equation: N1V1 = N2V2
N2 = (N1V1)/V2
Where N1 = initial strength of NaOH before adsorption (1N)
V1 = volume of NaOH consumed during titration (mL)
V2 = volume of acetic acid taken in titrimetric flask (mL)(Table-2)
N2 = strength of acetic acid
Convert the N2 values thus obtained for each titrimetric flask to g/L by multiplying with
equivalent weight of acetic acid (60). This represents Co-ba for each flask
Put the values thus obtained in Table-3.
6. Using practical balance and vessels for weighing coal, weigh 6 portions of activated
charcoal, each portion 2 g. The accuracy of weighing must be with accuracy 0.01 g.
7. Put activated charcoal into numbered flasks with stoppers. The volume of acetic acid
used for adsorption in each flask is 50mL. Adsorbent dosage is 2g/50mL = 40g/L
8. Plug up the flasks, and shake them. Wait for 20 minutes, the process of adsorption is in
progress. Mix the mixtures for several times by flasks shaking within this period.
Remark: The process of adsorption is a function of time too. It is important to put
charcoal into flasks at the same time, to provide adsorption for the same period in each
flask.
9. Filter the mixtures into clean and dry flasks. To avoid disturbing effect of adsorption of
acetic acid into filtering paper, remove away the first portion of filtration, app. 5 ml.
10. Determine the final concentration of acetic acid (Ce) in each of the flasks after adsorption
by titration with 1N NaOH and using phenolphthalein as indicator by following step 2-5
Put the values thus obtained in Table-3.
11. After the finishing experiment, wash carefully used flasks, pipettes, etc
12. Determination of the amount of acetic acid adsorbed per gram of the charcoal
qe (g/g) in individual flask: 𝑞𝑒 = (Co-ba – Cf-ad) *V/m
 where: Co-ba is initial concentration of acetic acid before adsorption (from Table 3, unit
g/L)
Cf-ad is the concentration of acetic acid after adsorption (from Table 3, unit g/L)
V is the volume of the acetic acid used for adsorption (V= 50 ml)
m is the mass of the adsorbent – charcoal (2 grams)
13. Write down the obtained values of qe to the Table 3.
14. Calculate 1/qe and 1/Ce values and put in Table-3
15. Determination of Langmuir constants (Qo) maximum adsorption capacity and b from
1 1 1
Langmuir equation: 𝑞 = +
𝑒 𝑄𝑜 𝑏𝑄𝑜 𝐶𝑒
1 1
Use MS Excell file to create a scatter graph by plotting values vs values
𝑞𝑒 𝐶𝑒
1 1
The slope of the plot represents the value of and intercept corresponds to
𝑏𝑄𝑜 𝑄𝑜

Calculate Qo from intercept and b from the slope

OBSERVATION:
Flask No. Before adsorption After adsorption Amount 1/Ce 1/qe
burette Initial acetic Burette Final acetic adsorbed
reading acid conc reading acid conc (qe) (g/g)
[ml] (g/L) [ml] (g/L)
(Co-ba) (Ce-ad)
1 22.7 136.2 21.9 131.4 0.12 0.00761 8.33
2 41.5 249.0 40.0 240.0 0.225 0.00417 4.44
3 31.9 382.8 30.5 366.0 0.42 0.00273 2.38
4 49.0 588.0 47.0 564.0 0.60 0.00177 1.67
5 26.9 807.0 25.1 753.0 1.35 0.00133 0.74
6 18.5 1110.0 16.5 990.0 3.00 0.00101 0.33
Calculation:

3.50
amount adsorbed qe(g/g)

3.00
2.50
2.00
1.50
1.00
0.50
0.00
0.0 200.0 400.0 600.0 800.0 1000.0 1200.0
Equilibrium Concentration of acetic acid (Ce) (g/L)

Fig 1: Langmuir adsorption isotherm plot of adsorption of acetic acid onto activated carbon

10
y = 1203.5x - 0.7517
8 R² = 0.9962

6
1/qe

0
0 0.001 0.002 0.003 0.004 0.005 0.006 0.007 0.008
1/Ce

Plot of 1/qe vs 1/Ce

Slope = (1/bQo) = 1203
Intercept = (1/Qo) = 0.751
Qo (maximum adsorption capacity) = 1/0.751 = 1.332 g/g
b (energy of adsorption) = 0.006 L/g
RESULT:
Qo (maximum adsorption capacity) = 1.332 g/g
b (energy of adsorption) = 0.006 L/g