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ADSORPTION

Adsorption is the attachment of molecules to the surface of solids, where

one solute may be absorbed selectively from a mixture. The adsorption refers for

the substance that is absorbed whereas the underlying materials of a substrate

refer to the adsorbent. The amount of adsorbate for a given quantity of adsorbent

increases with concentration of the solution.

Freundlich adsorption isotherm, an adsorption isotherm, is an empirical

relation between the concentration of a solute on the surface of an adsorbent to

the concentration of the solute in the liquid with which it is in contact. In

1909, Herbert Freundlich gave an expression representing the isothermal variation

of adsorption of a quantity of gas adsorbed by unit mass of solid adsorbent with

pressure. This equation is known as Freundlich adsorption isotherm or Freundlich

adsorption equation. As this relationship is entirely empirical, in the case where

adsorption behavior can be properly fit by isotherms with a theoretical basis.

The amount of reactant for a given temperature is described by adsorption

isotherm.

[1] x/m = kCn

Definite masses of the adsorbent is brought in contact with a series of

solutions varying initial amount of reagent to be absorbed, after equilibrium has

been established, liquids are filtered and analyzed to determine the degree of

adsorption in each case. The amount of adsorbed in each case is equal to


difference of the initial and final concentration. The equation for the adsorption

isotherm may be written in the logarithm form as follows;

[2] log x/m = log k + n log C

where

x = mass of adsorbate

m = mass of adsorbent

p = Equilibrium pressure of adsorbate

c = Equilibrium concentration of adsorbate in solution.

K and n are constants for a given adsorbate and adsorbent at a particular

temperature.

At high pressure 1/n = 0, hence extent of adsorption becomes independent

of pressure.

I. Objective

The determination of data necessary to draw an adsorption isotherm for a

substance absorbed from the solution onto a porous solid.

II. Materials and procedures

Erlenmeyer flask, Analytical balance, Volumetric Flask, Rubber stopper, 50-

mL base burette, pipette, iron stand, burette holder, filter paper, 2.0 N acetic acid,

0.3 M NaOH, and phenolphthalein indicator.


Procedure

The 0.3 M Sodium Hydroxide solution was


prepared and standardized against KHP.

cleansed and dried Erlenmeyer flask was labeled


from 1 to 6. These labels corresponded to the
successive dilution of acetic acid ( N/2, N/4, N/8,
N/16, N/32, N/64 ) solutions.

The flasks were stoppered and were shaken for


several min.. It was then allowed for equilibrium for
at least 20 minutes.

three 2 mL aliquots of the original 2.0N acetic acid


were titrated with 0.3 M NaOH solution. , using
phenolphthalein as an indicator. The exact
concentration of 2.0N acetic acid was determined.

.After the equilibration period, the solution were


filtered using filter paper

a 10 ml aliquot of solution (filtered) from each


flask were titrated with 0.3 NaOH using
phenolphthalein as an indicator

The volume of NaOH was used and the


volume of samples CH3COOH were
recorded.
III. Data and Results.

A. Standardization of 1N NaOH against Oxalic acid

Trial I Trial II Trial III

Mass of oxalic 0.3103 g 0.3065 g 0.3023 g

Volume of NaOH used , mL 19.40 ml 19.00 ml 19.00 ml

Concentraion of NaOH, N 0.2538 M 0.2560 M 0.2525 M

Average conc’n of NaOH 0.2541 M

B. Standardization of 2.0 N acetic acid

Trial I Trial II Trial III

Volume of acetic acid, mL 2 mL 2 mL 2 mL

Conc’n of NaOH, N 0.2541 M 0.2541 M 0.2541 M

Volume of NaOH, mL 17.2 mL 16.4 mL 16.8 mL

Conc’n of acetic acid, N 2.1853 M 2.0836 M 2.1344 M

Average conc’n of Acetic Acid 2.1344 M


C. Titration Data

Solutions Wt.of Original Volume of Volume Final

activated conc’n of sample of NaOH conc’n of

charcoal, CH3COOH CH3COOH used, mL CH3COOH

g sol’n, N soln, mL soln, N

M/2 0.3011g 1.0672 M 10 mL 10.40 1.05664 N

mL

M/4 0.313 g 0.5336 M 20 mL 10.30 0.52324 N

mL

M/8 0.3024 g 0.2668 M 20 mL 5.10 mL 0.25908 N

M/16 0.3021 g 0.13340 M 30 mL 3.80 mL 0.12869 N

M/32 0.3014 g 0.06670 M 30 mL 1.90 mL 0.06434 N

M/64 0.3018 g 0.03335 M 40 mL 2.00 mL 0.05080 N

Solution MCH3CO Mass of Mass X/m Log(x/ C2 Log C2

s OH CH3CO of act. m)

Adsorb OH Charco

ed, adsorbe al (m),

mol d (x), g g
M/2 9× 0.5405 0.3011 1.7950 0.2540 0.5120 -

10-3 g g N 0.2907

M/4 2.2 × 0.1321 0.313 0.4220 - 0.1210 -

10-3 g g 0.3747 N 0.9172

M/8 9×10-4 0.0541 0.3024 0.1789 - 0.0460 -

g g 0.7474 N 1.3372

M/16 3×10-4 0.0180 0.3021 0.0596 - 0.0120 -

g g 1.2248 N 1.9208

M/32 4.95× 0.0297 0.3014 0.0985 - 0.0021 -

10-4 g g 1.0065 N 2.6778

M/64 5.55× 0.0333 0.3018 0.1103 - 0.00089 -

10-4 g g 0.9574 N 3.0477

IV. Calculations

For conc’n of NaOH

1 𝑚𝑜𝑙 𝑜𝑥𝑎𝑙𝑖𝑐 2 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻


Mass of KHP x x
𝑀𝑊 𝐾𝐻𝑃 1 𝑚𝑜𝑙 𝑂𝑥𝑎𝑙𝑖𝑐

Trial I

1 𝑚𝑜𝑙 𝑂𝑥𝑎𝑙𝑖𝑐 2 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻


0.3103 g x 126.05 𝑔/𝑚𝑜𝑙
x 1 𝑚𝑜𝑙 𝑂𝑥𝑎𝑙𝑖𝑐
= 4.92 mmol NaOH

4.92 mmol NaOH


M= = 0.2538 M
19.40 𝑚𝑙 𝑁𝑎𝑂𝐻

Concentration of CH3COOH

𝑚𝑚𝑜𝑙 𝑜𝑓 𝑁𝑎𝑂𝐻 1𝑚𝑚𝑜𝑙 𝑜𝑓 𝐶𝐻3𝐶𝑂𝑂𝐻


Vol. of NaOH x x
1 𝑚𝐿 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 1 𝑚𝑚𝑜𝑙 𝑁𝑎𝑂𝐻

𝑚𝑚𝑜𝑙 𝑜𝑓 𝑎𝑐𝑒𝑡𝑖𝑐 𝑎𝑐𝑖𝑑


CCH3COOH= 𝑣𝑜𝑙.𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛

0.2541 𝑚𝑚𝑜𝑙 𝑜𝑓 𝑁𝑎𝑂𝐻 1𝑚𝑚𝑜𝑙 𝑜𝑓 𝐶𝐻3𝐶𝑂𝑂𝐻


17.2 mL x x
1 𝑚𝐿 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 1 𝑚𝑚𝑜𝑙 𝑁𝑎𝑂𝐻

= 4.3705 mmol

4.3705 𝑚𝑚𝑜𝑙 𝑜𝑓 𝐶𝐻3𝐶𝑂𝑂𝐻


M= 2 𝑚𝐿 𝑜𝑓 𝑆𝑜𝑙𝑢𝑡𝑜𝑛

M= 2.1853 M

For final concentration of CH3COOH (C2)

𝑉𝑜𝑙.𝑁𝑎𝑂𝐻 𝑥 𝑀 𝑜𝑓 𝑁𝑎𝑂𝐻
MCH3COOH= 𝑉𝑜𝑙.𝑜𝑓 𝐶𝐻3𝐶𝑂𝑂𝐻

For M/2:

10.40 𝑚𝐿 .𝑁𝑎𝑂𝐻 𝑥0.2541 𝑀 𝑜𝑓 𝑁𝑎𝑂𝐻


M= 10 𝑚𝐿 𝐶𝐻3𝐶𝑂𝑂𝐻

M= 1.05664 M

For mole of CH3COOH adsorbed at 50 mL solution

MCH3COOH= [c1-c2] x 0.05L

For M/2:

= (0.692 – 0.512) M x 0.05 L


M= 9.00 × 10-3 mole

For mass of CH3COOH adsorbed

mCH3COOH= MCH3COOH x MW of CH3COOH

For M/2:

= 9.00 × 10-3 mol x 60.06 g/mol

= 0.5405 g

0
-1.4 -1.2 -1 -0.8 -0.6 -0.4 -0.2 -0.2 0 0.2

-0.4
-0.6
-0.8
-1
y = 0.539x - 1.1272 -1.2
-1.4
-1.6
-1.8
-2

Series1 Linear (Series1) Linear (Series1)

y- intercept:

log(x/m)= log k + n log C

log k = -1.1272

k= 0.0746

slope:

m= 0.529
weight of the adsorbed material:

log(x/m)= log k + n log C

log(x/m)= -1.1272 + 0.539 log C

= 0.0746 C0.539

graph of absorbed materials


0.09
0.08
0.07
0.06
0.05
graph of absorbed
0.04 materials
0.03
0.02
0.01
0
1 2 3 4 5 6 7 8 9 10

V. Discussion

Solids have the property of holding molecules to their surfaces and this

property quite mark in the case of porous and finely solid. In the experiment,

activated charcoal was used as the adsorbent and acetic acid as the adsorbate.

The concentration of each solution (M/2, M/4, M/8, M/16, M/32, M/64) was

calculated from the calculation of the original 2N of HAc which has a value of

2.1853 M. From the titration data shown in table, the final concentration of
each filtrate were acquired using m1v1=m2v2 equation. The difference between

the original and the final concentration of acetic acid was used for the

calculation of amount adsorbed. This molar quantity was converted(X/M) by

multiplying it with the volume of the initial solution and molecular weight of the

acetic acid as well as by the mass of activated charcoal. The amount of acetic

acid that has adsorbed to a given mass of charcoal were 0.5405, 0.1321,

0.0540, 0.0180, 0.0297, 0.0333 or M/2, M/4, M/8, M/16, M/32, M/64

respectively. It decreases from N/2 to N/64 as the concentration of acetic acid

decreases. The adsorption isotherm of acetic- activated charcoal solutions

follows a linear function, when the logarithm of the ratio of the mass of acetic

acid adsorbed and the mass of the activated charcoal plotted versus the

logarithm of the concentration of the acetic acid at equilibrium.

Using the slope from excel, the n which is the slope of the line has a value

of 0.539. Extension of the line to y- axis the value of log k is -1.1272 which the

y- intercept of the equation. The value of k is 0.0746 which will be used to

create an empirical equation. The empirical equation is (x/m)=0.0746C0.529

which can predict the weight of activated charcoal and the concentration of

unadsorbed acetic acid solution.


VI. Conclusion

Adsorption is one of the most important separation techniques in any

chemical experiments and even the industrial processes. Many applications of

adsorption includes water purification and recovery of organic compound.

From the experiment, the adsorption isotherm of acetic- activated charcoal

solutions follows linear function. Concentration of the solution will affect the

adsorption. As the concentration of the adsorbate increases, the rate of

adsorption will increases too.


VII. References

https://vlab.amrita.edu/adsorption isotherm theory (august 2019)


https://www.sciencedirect.com/topics/earth-and-planetary-sciences/adsorption-isotherms
(august 2019)

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