C 141 (Expt. No. 7) NAME:________________________ ______ ROLL NO.

:___________________________ SIGNATURE:___________________ ______ BATCH: ____________ DATE: _____________

STUDY OF ADSORPTION OF ACETIC ACID ON CHARCOAL VERIFICATION OF FREUNDLICH'S ADSORPTION ISOTHERM

AIM
To study the adsorption of acetic acid on charcoal and to verify the application of adsorption isotherm. THEORY Absorption is a physical or chemical phenomenon or a process in which atoms, molecules, or ions enter some bulk phase gas, liquid, or solid material. This is a different process from adsorption, since molecules undergoing absorption are taken up by the volume, not by the surface (in case of adsorption). Adsorption is the adhesion of atoms, ions, or molecules from a gas, liquid, or dissolved solid to a surface. It is a surface phenomena occurs due to a tendency to lower free energy and entropy. The surface of any solid or liquid is in a state of strain due to unsaturated force. To lower this strain, they try to adsorb foreign particles on the surface. Extent of adsorption depends on (a) nature of adsorbent and adsorbate, (b) nature of surface, (c) temperature and (d) concentration of adsorbate. For a given pair of adsorbent and adsorbate and at a given temperature relation between extent of adsorption and concentration is called adsorption isotherm. Freundlich's isotherm is also applicable for absorption of gases on solid surface. The empirical equation for Freundlich's isotherm is : (x / m) = K Pn where 'P' is the pressure of adsorbate (i.e., gas). But, here the equation becomes: (x/m) = K. Cn freundlich's

where 'x' is the amount of adsorbate adsorbed by 'm' gm of the adsorbent; 'C' is the concentration of adsorbate and 'K' and 'n' are constants. By taking logarithm on both sides, we get log (x) - log(m) = log K + n log C log(x) = log (m) + log K + n log C Hence, a plot of log (x) against log C will be a straight line. The isotherm is empirical and found to be valid in the low pressure (concentration) range. As pressure (or concentration) is raised departure from the equation is found. At moderate to high pressure Langmuir's isotherm is valid and at still high pressure B.E.T. Equation is valid.

A different equation is more likely to describe adsorption where the adsorbate exceeds a monolayer. The Brunauer-Emmett-Teller (BET) equation is:

where Cs = concentration at which all layers are filled Kb = a coefficient Its assumptions are: Adsorbed molecules stay put Enthalpy of adsorption is the same for any layer Energy of adsorption is the same for layers other than the first A new layer can start before another is finished.

The function has an asymptotic maximum as pressure increases without bound. As the temperature increases, the constants 'k' and 'n' change to reflect the empirical observation that the quantity adsorbed rises more slowly and higher pressures are required to saturate the surface.

MATERIALS REQUIRED Standard Oxalic acid solution (0.1 N), NaOH solution, CH3COOH solution, Activated charcoal, Phenophthalein indicator, Reagent Bottles (5 each), Burette (50 ml), Pipette (10 ml), Conical flask (250 ml, 100 ml), filter papers. PROCEDURE
PART-I: Standardization of NaOH against standard Oxalic acid (0.1N) 1. 10ml of given 0.1N standard Oxalic acid is pipetted out into a 100ml conical flask. 2. This solution is titrated against the given unknown concentration of NaOH using 1-2 drops of phenolphthalein indicator until the end point is colorless to pale pink. 3. Tabulate the values and repeat the titration for concurrent readings and determine the concentration of supplied NaOH solution.

Table 1 _______________________________________________________________________ S.No Volume of Oxalic Acid Burette Readings (ml) Volume of NaOH taken (ml) Initial Final consumed (ml) _______________________________________________________________________ 1 2 3 _______________________________________________________________________ (HCOO)2 N1 V1 = N2 V2 (NaOH)

PART-II: Standardization of Acetic acid using standard NaOH solution. 1. 10ml of given acetic acid solution is pipetted out into a 100ml conical flask. 2. This solution is titrated against the standard NaOH using 1-2 drops of phenolphthalein indicator until the end point is colorless to pale pink. 3. Tabulate the values and repeat the titration for concurrent readings and determine the concentration of supplied NaOH solution.

Table 2 _______________________________________________________________________ S.No Volume of CH3COOH Burette Readings (ml) Volume of NaOH taken (ml) Initial Final consumed, 'V' (ml) _______________________________________________________________________ 1 2 3 _______________________________________________________________________ (CH3COOH) N1 V1 = N2 V2 (NaOH)

PART-III: Verification of Freundlich's Adsorption Isotherm 1. The different concentrations of the solutions are prepared in the reagent bottles of various proportions are given in the table 3 below . 2. 10 ml of the solution is pipetted out from bottle no. 1 into a conical flask and is titrated against NaOH solution using phenophthalein indicator and the reading is tabulated as 'V' ml. 3. The above process is repeated for the remaining bottles also. 4. Now, in each of these bottles, 2g of activated charcoal is added. 5. The bottles are shaken by mechanical shaker or by manual shaking using hands for about 30-45 minutes and then allowed to rest for 15 minutes. 6. A small filter paper is placed on a funnel and the content of the first bottle is filtered in a 250 ml conical flask. First 3-4 ml of the filtrate is rejected. This is to saturate the filter paper. 7. 10 ml of the filtrate from bottle no.1 is pipetted out into a 100 ml conical flask and is titrated against same NaOH solution using phenophthalein indicator. 8. Repeat the titrations for concurrent readings. 9. Similarly, repeat steps 5 & 6 for the remaining bottles also. 10. The readings are tabulated and the volume of NaOH consumed before and after adsorption are to be noted for each solution and concentration of solution in moles are to be determined.

Table 3 Bottle No. Content of the bottle Volume of NaOH Concentration of Extent of log(x) log C1 consumed by 10 ml solution in moles adsorption in Before After Before After terms of adsorption adsorption adsorption adsorption difference in (C1) (C2) concentration, x = (C1 - C2)

1. 2. 3 4

50 ml AcOH 30 ml AcOH + 20 ml H2O 25 ml AcOH + 25 ml H2O 10 ml AcOH + 40 ml H2O

OBSERVATIONS AND CALCULATIONS Room Temperature = __________________oC. Amount of Charcoal added, m = _________gm. Hence, a plot of log (x) vs log C1 gives a straight line, where 'x' is the extent of adsorption in terms of difference in concentration of solutions and 'C 1' is the concentration of each solution before adsorption. The slope (n) and intercept (log K) are to be determined from the graph. COMMENTS AND DISCUSSIONS The success of the above experiment requires patience on the part of the student, because attainment of adsorption equilibrium and also subsequent filtration is a very slow process as impatience may bring error in the experiment. Care should be taken while preparing the solutions and shaking the bottles also. Each and every calculation of the tables should be shown clearly with formulas, units, graph etc. RESULT 1. Strength(Concentration) of NaOH 2. Strength (Concentration) of AcOH 3. The value of the constant, n 4. The value of the constant, K

= = = =

__________________ __________________ __________________ __________________