Adsorption

0
1. OBJECTIVE

1.) To study the adsorption of iodine from solution

2.) To identify the surface area of activated charcoal sample using Langmuir
equation.

2. INTRODUCTION

Adsorption is a process of free moving of gaseous or solutes molecules of a solution come

close and attach themselves onto surface of solid. The adsorption can be strong or weak
depends on the nature of forces between solid surface (adsorbent) and the gas or dissolves
solute (adsorbate). There are two types of adsorption which is chemical and physical
adsorption. Chemical adsorption is when it involve the chemical bond between adsorbend
and the adsorbate. It require activation energy, very strong and not reversible. The physical
adsorption is due to the Van der Waals forces between adsorbent and adsorbate . it is
reversible, non specific and can occur at any condition. Chemical adsorption will produce
one layer of the adsorbate while physical adsorption will produce multilayer of the
adsorbate. It also can happen where the chemical adsorption is followed by the physical
adsorption. The partial pressure of the gas and the concentration of adsorbate will affect the
degree of adsorption from the solution. Adsorption isotherm is the relationship between
degree of the adsorption and the partial pressure of concentration. The characteristic of the
solid form and the reaction involve will be different if there are changes of the isotherm in
the temperature. surface area if the factor that govern the rate of dissolution and the
bioavailability of drug that will determine the rate of absorption of the drug thought
gastrointestinal tract. The surface area of the solid can be determined by the adsorption
measurement. Base on the experiment that has been done, we had study the adsorption of
the iodine from the solution and Langmuir equation had been used to estimate the surface
area of the activated charcoal.

3. PERALATANAPPARATUS

Conical flask, centrifuge tubes, measuring cylinder, analytical balance, Beckman J6M/E
centriguge, burettes, retort stand and clamps, pastuer pippetes

4. MATERIALS

Iodine solutions( Table 1), 1% w/v starch solution, 0.1 M sodium thiosulpahte solution,
distilled water,activated charcoal.
5. PROCEDURE

VOLUME OF SOLUTION A VOLUME OF SOLUTION

(ml) B(ml)
FLASK
10 40
1 and 7
15 35
2 and 8
20 30
3 and 9
25 25
4 and 10
30 20
5 and 11
50 0
6 and 12
Table 1

Solution A: Iodine (0.05M)

Solution B: Potassium iodide (0.1M)

Using burette or measuring cylinders, fill 12 conical flask (labeled 1-12) with 50 ml
mixtures of solution A and B as stated in Table 1.

Set 1: Actual concentration of iodine solution A (X)

For flask 1-6:

1) 1-2 drops of starch solution were added as an indicator

2) 0.1 M sodium thiosulfate solution was titrated until the colour of the solution changed
from dark blue to colourless.

3) The volume of the sodium thiosulpahate used was recorded.

Set 2: Concentration of iodine in solution A at equilibrium (C).

For flask 7-12:

1) 0.1 g of activated charcoal was added.

2) The flasks was cap tightly. The flask was swirled or shaked every 10 minutes for 2
hours.

3) The solution was transferred into centrifuge tube after 2 hours and were labeled
accordingly.

4) The solution was centrifuged at 3000 rpm for 5 minutes and the resulting supernatant
was transfered into new conical flask. Each conical flask was labeled accordingly.

5) Steps 1,2 and 3 were repearted as carried out as carried out for flasks 1-6 in Set 1.

Results
Set 1

Flasks Initial reading(mL) Final reading(mL)

Volume of Na2S2O3 used (mL)
1 0.0 4.8 4.8

2 4.8 12.7 7.9

3 12.7 23.4 10.7

4 23.4 36.9 13.5

5 0.0 16.3 16.3

6 3.2 30.2 27.0

Set 2 :

Flasks Initial reading(mL) Final reading(mL)

Volume of Na2S2O3 used (mL)
7 9.2 10.3 1.1

8 12.5 14.1 1.6

9 10.3 12.5 2.2

10 14.1 16.9 2.8

11 5.8 9.2 3.4

12 0.0 5.8 5.8

Question
1. Calculate N for iodine in each flask.

Flask 1
Volume of Na2S2O3 used = 4.8mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =4.80.1/1000
= 4.8 10-4 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,4.8 10-4 mol Na2S2O3 react with 2.410-4 mol I2.
Concentration of I2(X) =mole/volume
=2.410^-4mol/0.05L

= 4.810-3M

Flask 7

Volume of Na2S2O3 used = 1.1mL

Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =1.10.1/1000
= 1.1 10-4 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,1.1 10-4 mol Na2S2O3 react with 5.510-5 mol I2.
Concentration of I2(C) =mole/volume
=5.510^-5mol/0.012L

= 4.5810-3M
N = (X-C)

= (4.810-3M-4.5810-3M)
= 1.1 10-4
Flask 2
Volume of Na2S2O3 used = 7.9mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =7.90.1/1000
= 7.9 10-4 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,7.9 10-4 mol Na2S2O3 react with 3.9510-4 mol I2.
Concentration of I2(X) =mole/volume
=3.9510^-4mol/0.05L

= 7.910-3M
Flask 8
Volume of Na2S2O3 used = 1.6mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =1.60.1/1000
= 1.6 10-4 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,1.6 10-4 mol Na2S2O3 react with 810-5 mol I2.
Concentration of I2(C) =mole/volume
=810^-5mol/0.012L

= 6.6710-3M
N = (X-C)

= (7.910-3M-6.6710-3M)
= 6.15 10-4
Flask 3
Volume of Na2S2O3 used = 10.7mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =1.070.1/1000
= 1.07 10-3 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,1.07 10-3 mol Na2S2O3 react with 5.3510-4 mol I2.
Concentration of I2(X) =mole/volume
=810^-5mol/0.012L

= 0.0107M
Flask 9
Volume of Na2S2O3 used = 2.2mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =2.2xo.1/1000
= 2.2 10-4 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,2.2 10-4 mol Na2S2O3 react with 1.110-4 mol I2.
Concentration of I2(C) =mole/volume
=5.3510-4mol/0.05L

= 9.1710-3M
N = (X-C)

= (0.0107M-9.1710-3M)
= 7.65 10-4
Flask 4
Volume of Na2S2O3 used = 13.5mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =1.350.1/1000
= 1.35 10-3 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,1.35 10-3 mol Na2S2O3 react with 6.7510-4 mol I2.
Concentration of I2(X) =mole/volume
=6.7510^-4mol/0.05L

= 0.0135M

Flask 10
Volume of Na2S2O3 used = 2.8mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =2.80.1/1000
= 2.8 10-4 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,2.8 10-4 mol Na2S2O3 react with 1.410-4 mol I2.
Concentration of I2(C) =mole/volume
=1.410^-4mol/0.012L

= 0.0117 M

N = (X-C)

= (0.0135M-0.0117M)

= 9.0 10-4

Flask 5
Volume of Na2S2O3 used = 16.3mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =1.630.1/1000
= 1.63 10-3 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,1.63 10-3 mol Na2S2O3 react with 8.1510-4 mol I2.
Concentration of I2(X) =mole/volume
=8.1510^-4mol/0.012L

= 0.0163M

Flask 11
Volume of Na2S2O3 used = 3.4mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =3.40.1/1000
= 3.4 10-4 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,3.4 10-4 mol Na2S2O3 react with 1.710-4 mol I2.
Concentration of I2(C) =mole/volume
=1.710^-4mol/0.012L

= 0.0142 M

N = (X-C)

= (0.0163M-0.0142M)

= 1.05 10-3
Flask 6
Volume of Na2S2O3 used = 27.0mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =2.70.1/1000
= 2.7 10-3 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,2.7 10-3 mol Na2S2O3 react with 1.3510-3 mol I2.
Concentration of I2(X) =mole/volume
=1.3510^-3mol/0.05L

= 0.027M

Flask 12
Volume of Na2S2O3 used = 5.8mL
Molarity of Na2S2O3 = 0.1M
Number of moles of Na2S2O3 =5.80.1/1000
= 5.8 10-4 mol
1 mol Na2S2O3 react with 0.5 mol I2. So,5.8 10-4 mol Na2S2O3 react with 2.910-4 mol I2.
Concentration of I2(C) =mole/volume
=2.910^-4mol/0.012L

= 0.0242 M

N = (X-C)

= (0.027M-0.0242M)

= 1.4 10-3

1. Plot amount of iodine adsorbed (N) versus balance concentration of solution at

equilibrium to obtain adsorption isotherm.

Balance concentration of solution (C) Amount of iodine adsorbed (N)

4.5810-3M 1.1 10-4

6.6710-3M 6.15 10-4
9.1710-3M 7.65 10-4
0.0117 M
9.0 10-4
0.0142 M
1.05 10-3
0.0242 M
1.4 10-3
 Graph of N against C

1. According to Langmuir theory, if there is no more than a monolayer of iodine

adsorbed on the charcoal,
C/N = C/Nm + 1/KNm
Where C = concentration of solution at equilibrium

Nm= number of mole per gram charcoal required

K = constant to complete a monolayer

Plot C/N versus C, if Langmuir equation is followed, a straight line with slope of 1/Nm and
intercept of 1/kNm is obtained.
Obtain the value of Nm, then calculate the number of iodine molecule adsorbed on the
monomolecular layer. Assume that the area covered by one adsorbed molecule is 3.2 10-
19 m2, Avogadro no. = 6.023 1023 molecule, calculate the surface area of charcoal in m2g-1.

C C/N

41.64
4.5810-3
 10.85
6.6710-3
11.99
9.1710-3
0.0117 13.0

0.0142 13.52

0.0242 17.29

From the graph C/N versus C, 1/KNm obtained is 8.

Gradient, m = 1/Nm =18-8/210^-3 0

= 416.67

Nm =1/416.67
= 2.410-3
Number of iodine molecule adsorbed on the monomolecular layer
= Nm 0.1g charcoal Avogadro no.
= 2.410-3 0.1 6.023 1023
= 1.45 1020molecules
Nm = 2.410-3 mole/gram ; 1 mole iodine = 2126.9g
Weight of iodine = Nm 0.1g (2126.9g)
= 2.410-3 0.1 (2126.9)
= 0.0609g

Thus, surface area of charcoal can be calculated. Since surface area covered by one
adsorbed molecule is 3.2 10-19 m2,
Surface area of charcoal =3.210-19m2x1.451020/ 0.0609g
= 761.90m2g-1
1. Discuss the results of the experiment. How do you determine experimentally that
equilibrium has been reached after shaking for 2 hours?
Deviation might occur when plotting graph and caused by period of time shaking may be
not enough, so equilibrium have not achieved. We can determine the concentration of
iodine. Equilibrium was reached when the solution becomes homogenous and there is no
more colour changed.

Discussion:

Adsorption is the sticking of molecules from the gas or liquid phase onto the surface of a
solid. A molecule that undergoes adsorption is referred to as the adsorbate, and the solid is
the adsorbent. Adsorption occur when particles such as ion, atom, or molecules on the
surface of solids are capable of attracting other molecules due to the instability of energies
around the particles resulting to the adsorption phenomena. For example, nitrogen and
oxygen gas being adsorbed by charcoal cooled in liquid air.

Besides, adsorption is a consequence of surface energy, just like the surface tension. In a
bulk material, all the bonding requirement of the constituent atoms are filled. But the atom
on the clan surface may experience a bond deficiency. Hence, it is more favourable for them
to bond with whatever happen to be available. However, the exact nature of the bonding
depends on the details of species involved. The adsorption can be physical adsorption or
chemisorptions generally.

Physical adsorption or van der waals adsorption may occur at low temperature when
shaking of thermal molecule is not enough to cause complete evaporation at adorbed layer
on the surface of solid. It may occur depending on surface area of the adsorbed substance
and the properties of adsorbent and adsorbate as well.

On the other hand, chemisorption involves the combination of chemical substances

adsorbed to the surface of adsorbent. Chemisorption also occur as opposed to the Van der
Waals forces which cause physisorption.
Activated charcoal 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 m (for comparison, a tennis
court is about 260 m). The three main physical carbon types are granular, powder and
extruded (pellet). All three types of activated carbon can have properties tailored to the
application. Activated carbon is frequently used in everyday life, in: industry, food
production, medicine, pharmacy, military, etc. In pharmacy, activated charcoal is
considered to be the most effective single agent available as an emergency decontaminant
in the gastrointestinal tract. It is used after a person swallows or absorbs almost any toxic
drug or chemical.

If the adsorption of the adsorbate leads to a maximum of a single monomolecular layer

when the adsorption is complete, it is possible to calculate the area of the adsorbent. When
a monomolecular layer is adsorbed, it may be assumed that the area of an adsorbent equals
the total area of the adsorbed molecules.

Solid surfaces can adsorb dissolved substances from solution. When a solution of iodine is
shaken with activated charcoal, part of the iodine is removed by the charcoal and the
concentration of the solution decreased. From the results gathered, it is realized that K
increases as the concentration of iodine is decreased with respect to time. Hence, the
degree to which a solid will adsorb material depends on a number of things including
temperature, nature of molecule being adsorbed, degree of surface pore structure, and,
solute concentration & solvent. Other factors are important factors dealing with the
process of adsorption of solutes from aqueous solution by highly porous solids

Regarding the result, the number of molecules adsorbed per gram of solid, N (mol/g),
depends on the specific surface area of the solid, S(m2/g), the final liquid phase
concentration Cf (mol/L) or equilibrium gas phase pressure p (atm or kPa), and the specific
molecules undergoing adsorption. A plot of N versus Cf or N versus p, where the
temperature is held constant, is referred to as an adsorption isotherm. There are a variety
of equations used to relate the moles adsorbed to the concentration of adsorbate molecules
actually.

Conclusion

The rate of adsorption increases with increasing concentration of absorbate.

References

1.) en.wikipedia.org/wiki/Adsorption
2.) link.springer.com/journal/10450
3.) http://www.howstuffworks.com/adsorption-info.htm