[Course title]

National Institute of Technology Calicut Department of Chemical Engineering

Experiment No:1 Date: 01-01-2025

SIMPLE DISTILLATION

OBJECTIVE
To verify Rayleigh’s equation for simple distillation of methanol-water mixture. To
verify material balance equation, FxF = DyD,avg + WxW

APPARATUS

1. Simple distillation apparatus.

2. Density bottle
3. Measuring cylinder (10 mL)
4. Burette (2 No.s)
5. Conical flask (100 mL)

CHEMICALS

1. 50 mole% methanol-water mixture.

2. Pure methanol

THEORY

Distillation is a method of separating the components of a solution. This makes use of the
fact that when part of a liquid mixture is vaporized by addition of heat, the composition of
the new phase may be different from the composition of the original solution. Let us
consider the addition of heat at constant pressure to a completely miscible liquid mixture A
and B. The temperature of the mixture rises. If it had been pure A, the vapour pressure of A
rises with increases in temperature and finally equals the pressure at which the operation is
carried out. If further heat is added, this is utilized in converting A from liquid to vapour
state at a constant temperature. Similar is the casefor a component for liquid B also. In
other words, we can say that a pure Component has only one degree of freedom at the two-
phase equilibrium condition. But when there are two components, phase rule suggests two
degrees of freedom for the same situation, which means that there is a range temperature
through which the

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Figure 1: Simple Distillation experimental setup

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transition from liquid to vapour state occurs. The temperature at which vaporization starts
is called ‘bubble point’ and the temperature at which the vaporization ends is called ‘dew
point’. In the figure, the mole fraction of more volatile component (here A) is used to
denote the compositions of the mixtures. Consider the mixture to be initially in the liquid
phase denoted by point G. On addition of heat, the temperature of the mixture rises. Let us
consider that two components, the state of the system have reached point H when the
vapour pressure of the solution equals the constant pressure exerted. The liquid mixtureis at
the point of vaporization, or the liquid mixture has reached its bubble point. When more
heat is added, the temperature further rises to point P. Now the system exists in two phases;
a liquid phase represented by point L and a vapour phase represented by point K. The
composition of the liquid phase suitably changed so that the vapor pressure of the solution
is equal to the pressure maintained. This is the property made use of in distillation to effect
a separation between A and B. On further addition of heat the state of the system reaches
point M where the mixture gets completely vaporized. The system at this state said to beat
at its dew point. The bottom line is saturated liquid line and the top curve is the saturated
vapour curve. Vapour phase K and liquid phase L coexist and hence they said to be in
equilibrium. While the mole fraction of A in the liquid phase is denoted by x, the mole
fraction of A in the vapour phase in equilibrium which is denoted by y*. If there is a
separation by distillation, y* has to be different from x.
Differential or Simple distillation

With reference to the figure, let us consider that the state of the system has reached the
point H. A drop of vapour forms which has compositions represented by J. By some
method this vapour is removed from the vessel in which the equilibrium distillation is
carried out and is condense elsewhere. The composition of liquid phase moves up along
the saturated liquid line. Addition of more heat forms more vapour, but all vapour is
removed from the region of distillation immediately on the formation. The process of
distillation is stopped when the composition of the liquid phase has changed to the extent
required. In practice, this can only be approximated since,

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OBSERVATIONS

Volume Volume of Weight of mix

Mix Density Mol % of
of water with specific
No methanol (g/ml) Methanol
(ml) gravity bottle(g)
(ml)
1 0 30 24.03 0.9612 0

2 3 27 23.84 0.9536 5.886

3 6 24 23.41 0.9364 12.329

4 9 21 23.1 0.924 19.424

5 12 18 22.56 0.9024 27.273

6 15 15 22.35 0.894 36.000

7 18 12 21.76 0.8704 45.763

8 21 9 21.16 0.8464 56.757

9 24 6 20.59 0.8236 69.290

10 27 3 19.78 0.7912 83.505

11 30 0 19.17 0.7668 100

Specific Gravity Bottle + Bottle + Bottle +

Item
Bottle Feed Distillate Residue
17.22 38.07 37.99 40.18

Weight (g)

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 Removal of differential amounts if vapour makes the process infinitely slow.

 Entrainment cannot be fully avoided.
 There will be cooling and condensing of the vapour before removal from the
region of distillation.

The amount of liquid that is distilled can be related to the initial and final liquid phase
composition using an equation called Rayleigh’s equation. For a binary mixture of A and B
assume that at any time during the course of distillation there are L moles of liquid in the
still of composition x mole fraction of A and the amount of distillate ( =dL) of mole
fraction y* in equilibrium with the liquid, is formed. Let us denote the corresponding
change in the liquid phase composition by dx.
Let us determine the corresponding material balance for A

Lx = y* L + (L - dL)(x - dx)

Expanding and neglecting dxdL, we get y*dL = Ldx + xdL

xf
dL
L
=ln ( )
F dx
=∫ ¿
W x y −x w

where F and W are the total number of moles of liquid at any instant during distillation

having composition xF and xW respectively. This equation can be used to determine F, W,

xF, and xW for simple distillation when any three of these are known.

PROCEDURE

1. Add 300 ml of given methanol-water mixture in a simple distillation flask after exactly
measuring the volume using a measuring cylinder. Assemble the distillation apparatus,
start circulation of water through condenser and switch on the heating.
2. Take distilled water in one burette and methanol in another. Determine the specific
gravity of pure methanol. Clean and dry a 100 mL conical flask. Prepare a 10 % by
volume mixture of methanol and water in this by mixing 3 mL methanol with 27 mL
water and find out the specific gravity of this mixture.
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3. Similarly, find the specific gravity values of several known compositions of methanol-

CALCULATIONS:
Volume of Methanol-Water mixture for distillation = 300ml

Volume of distillate collected = 149ml

Volume of residue after distillation = 136ml

Molecular wt. of methanol = 32 g/mol
Molecular wt. of water = 18 g/mol
24.03
Density of water = =¿0.9612 g/ml
25
19.17
Density of methanol =
25
=0.7668 g/ml
38.07−17.22
Density of feed mixture = =¿ 0.834 g/ml
25
37.99−17.22
Density of distillate =
25
= 0.8308 g/ml

Density of residue = (40.18−17.22)/25 =0.9184 g/ml

𝟏
The equilibrium relation between Methanol (A) – Water (B) system at 1 atm :

𝒚 −𝒙
∗
xA yA*
0 0 -
0.02 0.1 12.5
0.04 0.2 6.25
0.06 0.3 4.17
0.09 0.4 3.23
0.14 0.5 2.78
0.22 0.6 2.61
0.3 0.66 2.78
0.4 0.73 3.03
0.5 0.78 3.57
0.6 0.82 4.54
0.7 0.87 5.88
0.8 0.92 8.33
0.9 0.96 16.67

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1.0 1.0 -

water mixtures. It is better to do the experiment in increasing percentages of methanol

and to shake the dry bottle between successive densitydeterminations so that little
amount of solution remain in the bottle and will not affect much.
4. When required amount of distillate (50 % of feed volume) has been collected, stop
heating and disassemble the apparatus. Measure the volume of distillate collected in
that of residue remaining using a measuring cylinder. Determine the specific gravity of
this solution also

From graph:

Mole fraction of methanol in the distillate, yD,avg = 0.66

Mole fraction of methanol in feed, xF = 0.63

Mole fraction of methanol in residue, xW, =0.25

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For feed, F

From graph, xF = 0.63

xF × Molecular weight of methanol

fraction of methanol in feed =
Mass

xF × MWmethanol + (1 − xF) × MWwater

0.63× 32
= = 0.75
0.63 ×32+0.37 ×18

Mass of feed, F = Volume of feed × Density of feed

= 0.834 × 300 =250.2 g

mass of feed × mass fraction of methanol in feed

Moles of methanol in feed =
Molecular weight of methanol

250.2× 0.75
= = 5.86 moles
32

Mass fraction of water in feed = 1 – mass fraction of methanol in feed

= 1- 0.75

= 0.25

mass of feed ×mass fraction of water in feed

Moles of water in feed =
molecular weight of water

250.2× 0.25
= = 3.475 moles
18

Total moles in feed = moles of methanol in feed + moles of water in feed

= 5.86+3.475 =9.335 moles

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For Distillate, D

From graph, xD = yD,avg =0.66

yD,avg×Molecular Weight of methanol
mass fraction of methanol in Distillate =
yD,avg×MWmethanol+(1−yD,avg)×MWwater

0.66 ×32
= = 0.78
0.66 ×32+0.34 × 18

Mass of Distillate = volume of distillate × Density of distillate

= 149× 0.8308 = 124 g

mass of distillate×mass fraction of methanol in Distillate

Moles of methanol in Distillate=
=
molecular weight of methanol

124 ×0.78
= = 3.0225 moles
32

Mass fraction of water in Distillate = 1 - mass fraction of methanol in Distillate

= 1- 0.78 =0.22 =

mass of distillate×mass fraction of water in distillate

Moles of water in Distillate =
molecular weight of water

124 ×0.22
= = 1.515 moles
18

Total moles in Distillate, D = moles of methanol + moles of water in Distillate

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= 3.0225+1.515 = 4.538 moles

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For Residue, W

From graph, xw =0.25

mass fraction of methanol in Residue = xw×Molecular Weight of methanol

xw×MW of methanol+(1−xw)×MW of water

0.25× 32
= = 0.372
0.25 ×32+0.75 ×18

Mass of residue = volume of residue × Density of residue

= 136 × 0.9184 = 124.9 g

mass of residue×mass fraction of methanol in residue

Moles of methanol in Residue =
molecular weight of methanol

124.9× 0.372
= = 1.452 moles
32

Mass fraction of water in Residue = 1 - mass fraction of methanol in Residue

= 1-0.372 = 0.628

mass of residue×mass fraction of water in residue

Moles of water in Residue =
molecular weight of water

= 124.9× 0.628
= 4.357 moles
18

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Total moles in Residue, W = moles of methanol + moles of water in Residue

=1.452+4.357 = 5.808 moles

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GRAPH

xA vs 1/y*-x
18

16

14

12

10
1/y*-x

0
0.02 0.04 0.06 0.09 0.14 0.22 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
xA

Area under the curve:

xf
dx
∫ y ¿ −x
xw

1
For the first pair (xw = 0.25, xf = 0.63 , = 2.7)
y∗−x

2.7 ×(0.63−0.25) = 1.026

1
For the second pair (xw = 0.25, xf = 0.63, = 3.03-2.7)
y∗−x

(0.63−0.25)×(3.03−2.7) = 0.1254
1
For the third pair (xw = 0.4, xf = 0.63, = 3.57-3.03)
y∗−x

(0.63−0.4 ¿ ×(3.57−3.03) = 0.1242

1
For the fourth pair (xw = 0.5, xf = 0.63, = 3.03-2.7)
y∗−x
1
×(0.5−0.63 ¿×(3.57−3.03) = 0.08645
2
Total Area = 1.026+0.1254+0.1242+0.08645 =1.36205×10-1

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=0.136205

Material Balance:

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FxF = DyD,avg + Wxw

Total moles in feed, F = 9.335 moles

Total moles in distillate, D = 4.538 moles

Total moles in residue, W = 5.808 moles

Mole fraction of methanol in the distillate, yD,avg, = 0.66

Mole fraction of methanol in feed, xF, = 0.63

Mole fraction of methanol in residue, xW, = 0.25

Substituting the values in material balance we get,

LHS =9.335×0.63 = 5.88

RHS = 4.538×0.66 + 5.808×0.25 =4.45

xf
dx
The area under the curve between xF and xW gives the value of ∫ y ¿ −x
xw

Area under the curve from graph =0.136205

ln( WF )= ln( 9.335

5.808 )
= 0.47

Hence, the Rayleigh’s equation and material balance for the system has been verified.

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Specific gravity of mixture vs Mole percentege of methanol

1.2 Specific gravity of mixture

1
xw
xf yDavg
0.8

0.6

0.4

0.2

0
0 20 40 60 80 100 120

Mole percentege of methanol

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RESULTS:
The Rayleigh’s equation and material balances for the given methanol - water system has
been verified with errors present within allowable limits.

DISCUSSION:
Although the experiment procedures are followed throughout, the incorrect measurement of
(bottle+distillate) weight resulted in an error of ≈ 20% in the material balance of methanol and
error in the Rayleigh equation.

SAFETY PRECAUTIONS:

For the simple distillation of the methanol-water mixture, ensure proper ventilation or
use a fume hood to avoid inhaling toxic methanol vapors. Wear safety goggles, a lab
coat, and gloves to protect against chemical exposure. Handle methanol carefully, as it
is flammable and toxic, and keep it away from heat sources. Use heat-resistant gloves
when dealing with hot apparatus, and ensure glassware is intact to prevent breakage.
Maintain proper water circulation in the condenser to avoid overheating. In case of
spills, clean immediately with absorbent materials, and dispose of chemicals according
to safety regulations. Keep a fire extinguisher nearby and label all containers correctly.

Handling Methanol: Methanol is toxic and flammable. Avoid skin contact, inhalation,
or ingestion. Always handle methanol with care, and keep it away from open flames or
heat sources

Spill Management: In case of a methanol or methanol-water mixture spill, clean it up

immediately using appropriate absorbent materials and dispose of it properly.

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Experiment No.: 2 Date: 08-01-2025

ADSORPTION ISOTHERM
OBJECTIVE

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

APPARATUS

Reagent bottles, conical flasks, filtering funnel, burette, pipette, and volumetric flask

CHEMICALS REQUIRED

Acetic acid, activated carbon, 0.1N NaOH solution, Oxalic acid

THEORY

Adsorption isotherm exploits the ability of certain solids preferentially to concentrate

specific substances from solution to their surfaces. In this, components of either liquid
or gaseous solution may be separated from each other. Some applications of adsorption
in gaseous separations are de-humidification of air and other gases, removal of
objectionable odours of impurities from industrial gases, recovery of valuable solvent
vapours from dilute mixtures with air and other gases and fractionation of mixtures of
hydrocarbon gases containing such substances like methane, ethane, and propylene.
Typical liquid separation is the removal of moisture dissolved in gasoline,
decolourisation of petroleum products and aqueous sugar solution, removal of
objectionable taste and odour from water and fractionation of a mixture of aromatics
and paraffinic hydrocarbons.

Adsorption can be physical or chemical. Physical adsorption or Vander Waal’s

adsorption can be readily reserved and is the result of intermolecular forces of
attraction between solid and the substance adsorbed. The equilibrium partial pressure of
the substance adsorbed equals that of contacting gas phase. This is lower than the
vapour pressure and so adsorption is not simple condensation. By lowering the pressure
of gas phase by raising the temperature, the adsorbate is readily removed or desorbed in
unchanged form, reversible adsorption is seen in liquids as well.

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OBSERVATIONS:
Room Temperature = 27 oC
Weight of acetic acid taken in 250 mL flask (F1) = 25 g
Normality of Oxalic Acid N1 = 0.1N

Standardization of NaOH
Indicator: Phenolphthalein
Colour Change: Pink to colorless

S No. Volume of NaOH (ml) Titre value of Oxalic Acid (ml) V1

V2
Titre 1 Titre 2

1 10 9.6 9.1

Preparation of mixtures

V12 Volume V2B Volume from F2 Weight of

Bottl
transferred from transferred to bottle Carbon
e No.
F1 to F2 (mL) (mL) added (g)

1 10 250 5

2 20 250 5

3 30 250 5

4 40 250 5

5 50 250 5

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Chemisorption or activated adsorption is the result of chemical interaction between the

solid and the adsorbed substance. The process is frequently irreversible and on
adsorption, the original substance will be found to have undergone a chemical change.
Chemisorption finds applications in catalysis. The usual adsorbents are fuller’s earth,
activated clays, bauxite, alumina, bone charcoal, decolourising carbon, gas adsorbent
carbon, silica gel, zeolites and metal alumino-silicates.

Adsorption equilibria

The amount of substance adsorbed depends on the concentration of the contacting gas
or liquid phase, the temperature, and pressure. A relationship between these variables is
called “adsorption equilibria”. Data on equilibria are essential for designing adsorption
unit. Equilibrium data plotted for a given temperature is called “adsorption isotherm”.

Figure Adsorption Equilibria

In liquid adsorption, isotherms are important since no appreciable volume changes of

the liquid occur which might be used as a measure of adsorption. Withdrawal of the
solid and weighing it, as can be done in the case of gases, will not distinguish between
the adsorbed liquid and that which is mechanically occluded. When adsorbent is mixed
with a binary solution, adsorption in both solute and solvent occurs. Since the total
adsorption cannot be measured, the relative or apparent adsorption can be determined
instead. The customary procedure is to treat a known volume of solution with a known
weight of the adsorbent. V cm3 of solution/g of adsorbent. As a result of preferential
adsorption of solute, the solute concentration of the solution is observed to fall from
initial C0 to final Ce in the liquid (C-concentration in g of solute per cm3 of solution).

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Titration of the filtered solution

Indicator: Phenolphthalein

Colour Change: Pink to colorless

Titre value of
V4 Acetic Acid
V3 Volume of Makeu V5 Volume
Bottle of NaOH
filtrate taken for p V6 (mL)
No
dilution (mL) Volum taken (mL)
e (mL) Titr Titr
e1 e2

1 50 50 10 15.3 16.2

2 50 50 10 9.8 9.4

3 50 50 10 4.7 4.6

4 50 50 10 3.6 3.6

5 50 50 10 2.7 2.5

CALCULATIONS

9.35 ×0.1
Normality of given NaOH solution (N2) = V 1 × N 1 / V2 =
10

= 0.0935 N

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The apparent adsorption of solute, neglecting any adsorption of solvent is qe = V(C0-

Ce)/m g of solute adsorbed per gram of adsorbent. This is satisfactory for dilute
solutions where the fraction of the original solvent, which may be adsorbed, is small.
For dilute solutions, the adsorption isotherm may be described by an empirical
expression,

V ( C 0 −Ce )
q e= =KC 1/
e
n
m

In linear form of Freundlich isotherm, can be written as ln q e =ln k + ( 1n ) ln C where k

e

and n are constants at a particular temperature. It is to be noted that ‘n’ is independent

of units used and ‘ k ’ has units same as that used for C0 or Ce. Sometimes this curve
may show deviation from linearity. This may be due to appreciable adsorption of the
solvent or simply the general inapplicability of Freundlich isotherm.

PROCEDURE

1. Record the room temperature.

2. Weigh about 25 g of Acetic acid exactly in weighing bottle and transfer it

completely by repeated washings to a 250 ml volumetric flask (F1) and make up the
volume with distilled water.

3. Pipette out 10 ml of this solution into another 250 ml volumetric flask (F2) and the
volume is made up.

4. Weigh about 5 g of activated carbon into reagent bottle (B1) by differential

weighing.

5. Add 200 ml of solution from the flask (F2) to this bottle.

6. Repeat the same procedure with bottle numbers B2, B3, B4, B5 with the difference
that the volumes of solution pipette out from the flask F1 are 20 ml, 30 ml, 40 ml
and 50 ml respectively.

7. Shake the bottles well for one hour using bottle shaker for adsorption to come into
equilibrium.

8. Prepare a standard solution of Oxalic acid (0.1 N) and use this to standardize the
supplied NaOH solution.

After 1 h shaking, filter the solution and titrate in the five bottles. Take the solutions in
the burette and titrate it against 10 ml NaOH.

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For Bottle No: 3

The value of V (cm3 of solution/ g of adsorbent) and C0 in each of the five bottles are
calculated. The value of Ce in each of the original filtered solution is found out by

N NaOH × V 5 × Equivalent weight of acetic acid

C e=
V 6 × 1000

0.0935 ×10 ×60

= = 9.93×10-3 g/ml
5.65 ×1000

weight of acetic acid taken(g) ×V 12 (mL)

C 0=
V F 1 (mL )×V F 2 (mL)

25 ×30
= = 0.0129 g/ml
250× 250

V (C0 −Ce )
q e=
m

250(0.012−0.0093)
= = 0.135
5

ln Ce = ln(9.93×10-3 ) = -4.61227

ln qe = ln(0.135) = -2.0024

C0 Ce
Bottle V (cm3 of
solution/ g (g solute/ ml (g solute/ ml qe ln Ce ln qe
No
adsorbent) of solution) of solution)

1 50 0.004 0.0035619 0.023 -5.637 -3.772

2 50 0.008 0.005843 0.108 -5.1423 -2.225

3 50 0.012 0.009929 0.103 -4.612 -2.273

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4 50 0.016 0.01558 0.021 -4.161 -3.863

5 50 0.02 0.01939 0.031 -3.945 -3.473

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GRAPH:

ln Ce
0
-5.8 -5.6 -5.4 -5.2 -5 -4.8 -4.6 -4.4 -4.2 -4 -3.8
-0.5

-1

-1.5

(x 1 ,y 1 )

ln qe
-2

-2.5

-3

-3.5

-4

-4.5

y 2− y 1 −0.5−(−2.5)
Slope = = = 0.571
x 2−x 1 0−(−3.5)

From graph,

Slope = 1/n = 0.571

Thus, n = 1.751

Intercept = ln k = -0.5

Thus, k = 0.606

Thus, Freundlich isotherm is qe = k Ce1/n i.e. qe = 0.606 Ce0.571

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RESULTS:

The applicability of Freundlich isotherm for adsorption of acetic acid on activated

charcoal has been verified at room temperature and the Frendlich constant values are
found as

n = 1.751

k = 0.606

Thus, isotherm equation is qe = 0.606 Ce0.571

Error visible the graph plot inefficient shaking, or other parts of experiment.

DISCUSSION:

The experiment aimed to verify the applicability of the Freundlich adsorption isotherm
for acetic acid on activated carbon and to determine the constants k and n at room
temperature. Acetic acid solutions of varying concentrations were prepared, and 5 g of
activated carbon was added to each solution. After shaking for one hour to reach
equilibrium, the remaining acetic acid concentration was determined through titration
with standardized NaOH. The amount of acetic acid adsorbed per gram of activated
carbon was calculated, and a plot of ln Ce vs ln qe was used to determine k and n. The
results help characterize the adsorption process, indicating the adsorption capacity and
intensity of activated carbon for acetic acid.

SAFETY PRECAUTIONS:

For safety, handle acetic acid and sodium hydroxide with care, as both are corrosive
and can cause burns. Wear protective gear, including gloves, safety goggles, and lab
coats, and work in a well-ventilated area or under a fume hood to avoid inhaling
harmful vapors. Avoid direct contact with chemicals, and immediately clean up any
spills. Properly dispose of chemical waste following safety protocols. Ensure that an
eyewash station and first aid kit are accessible in case of accidental exposure.

Handle Chemicals with Care: Acetic acid is corrosive and can cause burns. Handle it
with care, and use gloves and safety goggles to protect your skin and eyes.

Handle NaOH with Caution: Sodium hydroxide is a strong base and can cause severe
burns. Ensure it does not come into contact with your skin or eyes, and always add it
slowly to avoid splashing

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