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ADSORPTION ISOTHERM

Aim

To verify the application of freudlich equation for adsorption of acetic acid on activated carbon
and to determine the value of constants k and n in equation for adsorption at room
temperature.

Apparatus

Reagent bottles, beaker shaker, Burette, filtering funnel, conical flask, pipette, volumetric flask,
weighing balance.

Chemicals required

Acetic acid, activated carbon, 0.1 NaOH, Oxalic acid.

Theory

Adsorption is a surface phenomena. The amount of substance adsorbed depends on the


concentration of contacting gas or liquid phase temperature and pressure. A relationship
among the variables is calculated using adsorption equilibria. Data on adsorption equilibria are
essential for designing an adsorption unit. Equilibruim data expressed for a particular
temperature is called adsorption isotherm.

In liquids, adsorption isotherm are important since no appreciable volume change of the liquid
occurs, which might be used as measure of adsorption. Withdrawal of the solid and weigh

When an adsorbent is mixed with a binary solution adsorption of both solvent and solution
occurs. Since the total adsorption cannot be measured the relative or apparent adsorption is
determined instead. The customary procedure is to treat a known weight of adsorbent, V am3
of solution/ gm of adsorbent.

The solute concentration of the solvent is observed to fall from the initial value Co to the final
value C*in the liquid. (C is the concentration expressed in gm of solute/ cm 3 of solvent). The
apparent adsorption of solute, neglecting any adsorption of solvent is v (Co – C*) g of solute
adsorbed per gram of adsorbent. This is satisfactory for dilute solutions where the fraction of
original solvent which may be adsorbed is small. Over a small concentration range and
particularly for dilute solution. The adsorption isotherm may be described by an empirical
expression usually attributed to Freudlich C* = k[v(C0- C*)]n

K and n are constants at a particular temperature. It is noted that n is independent of units and
k has same units as that of C0 and C*.
Procedure

Prepare 0.5N oxalic acid solution by weighing accurately about 15.75g of crystalline oxalic acid
and transferring to a 500ml standard flask. Dissolve with distilled water and make up the mark.
Calculate its exact weight.

Standardization of approximately 0.1N KMnO4: Wash a 50ml burette first with distilled water
and then rinse it with given potassium permanganate solution. Fill the burette to a convenient
mark with the permanganate solution after ensuring that the tip of the burette is also
completely filled with solution.

Pipette out 5 ml of the 0.5N oxalic acid into a 250ml conical flask and add about 20ml of
distilled water followed by 20ml of 1:1 sulphuric acid. Heat the contents over a hot plate to
about 600 C and titrate the hot solution against the potassium permanganate solution from the
burette till the end point is reached (appearance of a permanent pink color). Note the burette
reading and determine the amount of permanganate used. Repeat the experiment till
concordant values are obtained. Calculate the exact normality of potassium permanganate.

Adsorption studies: Clean and dry six stoppered 350 ml bottles and label them from 1 to 6.
Weigh accurately into each of them about 2 grams of finely divided charcoal.

Add by means of a burette 50, 40, 30, 20, 10 and 5ml of 0.5N of oxalic acid and 0, 10, 20, 30, 40
and 45 ml of distilled water into the bottles numbered 1, 2, 3, 4, 5 and 6. Stopper the bottles
and shake them vigorously. Keep the bottles in a trough of water at room temperature and
leave them for one hour with intermittent shaking.

Set up 6 dry funnels with dry filter paper and filter the supernatant liquid separately into 100ml
beakers. Reject the first 10ml of the filtrate since the concentration of the first fractions are
likely to be changed due to the absorption by the filter paper.

Pipette out 5ml of the filtrate collected from the bottles 1, 2and 3and 10ml collected from the
remaining bottles. Titrate the filtrate with the standardized 0.1N KMnO4 as before. Conduct the
titrations in duplicate for the filtrate of each bottle till concordant values are obtained.

CALCULATIONS:

Calculate the values of (x/m) and C2 as shown in the calculations and also C2 / (x/m).

Plot (x/m) against C2 and get the adsorption isotherm

Freundlich Equation constants:


Plot (x/m) on the Y axis and C2 on the X axis of a log -log graph and the slope and the intercept.

Slope gives the value of n and the intercept gives log K.

OBSERVATIONS AND CALCULATIONS

Preparation of standard oxalic acid:

Weight of weighing bottle and oxalic acid (w1) =

Weight of weighing bottle (after transfer) (w2) =

Weight of oxalic acid transferred (w1-w2) =

Volume made up = 500 ml

(𝑤1−𝑤2)
Strength of oxalic acid = =
31.5

Standardization of potassium permanganate:

Indicator: self
End point: Appearance of permanent pale pink color

Volume of oxalic acid Burette reading Volume of KMnO4 used up


Pipette V2 ml
V1 ml
V1 X S oxalic acid = V2 X S potassium permanaganate

Strength of potassium permanganate (N2) = V1 X S oxalic acid


_________________
V2

Bottle No 1 2 3 4 5 6
Vol of
standard
oxalic acid
transferred
Volume of
water added

Total
volume
Initial conc
of solution

Bottle No Weight of Initial conc Volume of Volume of Final Con of Amount of


charcoal of acid sample KMnO4 used acid after acid
transferred pipetted out adsorption adsorbed
1
2
3
4
5
6

Calculations:
Initial concentration of the solution, C1 =
𝑉2 𝑋𝑁2
Final concentration of acid by adsorption C2 =
𝑉1

( 𝐶1−𝐶2)𝑋 𝑉 𝑋 𝐸𝑞 𝑤𝑡 𝑜𝑓 𝑎𝑐𝑖𝑑 (𝐶1−𝐶2)𝑋50 𝑋 63


The amount of acid adsorbed x = 1000
= 1000
Determination of Constants of Freundlich Adsorption isotherm

Bottle No Wt of C1 C2 x/m 𝐶2 Log C2 Log(x/m)


charcoal 𝑥/𝑚
transferred
1
2
3
4
5
6

Results:

Freundlich Equation

Constants k =

n=