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1. DETERMINATION OF MOLECULAR WEIGHT OF THE


POLYMER BY VISCOSITY MEASUREMENTS

AIM:
To determine the molecular weight of a polymer using Ostwalds
viscometer a 1% polymer solution is provided

MATERIALS REQUIRED:
Polymer material, solvent, viscometer, 50 ml std flask, 20 ml graduated
pipette, stop watch.

THEORY:
Molecular weight of a polymer is nothing but average molecular weight.
Of all the methods used for determination of molecular masses of polymers
viscosity method introduced by H.Staudinger is most commonly employed in
research. Accurate measurement of absolute viscosity being difficult it is
convenient to measure relative viscosity.

rel = /o

where and o are viscosity of solution and viscosity of the solvent.The


relative viscosity is related to other quantities as follows,
sp = rel -1
red = sp/c
i = lim sp/c
A series of samples of same polymer in a given solvent the intrinsic viscosity is
related to molar mass of the polymer by the following equation,

i = kMa
i Intrinsic Viscosity
K and a Constants
M Average Molecular weight.

Important Viscosity Definitions :

Relative viscosity (rel) =/o = t/to


Specific viscosity (sp) =/o -1
Reduced viscosity (red) = sp/c
Intrinsic viscosity(i) = lim sp/c
co
2

PROCEDURE:

Step 1: Preparation of polymer solutions of different concentrations


Polymer solutions of different concentrations say 0.2%,0.4%,0.6% and 0.8%
are prepared by dissolving 20 ml,40 ml ,60 ml and 80 ml of polymer solutions
in 80 ml, 60,40 and 20 ml of water respectively.

Step 2: Flow time of solvent 20 ml of the solvent is taken into the viscometer
and is sucked through capillary tube.Now note the time of flow of solvent to
the lower mark.

Step 3: Flow time of the polymer solution. Fill the viscometer with 20 ml of
one of the polymer solution and determine the flow time as before.Similarly the
flow time of other polymer solutions are found.From the flow times the
reduced viscosity can be calculated.Graph is plotted and i is found out.

TABULATIONS:

Preparation of Various Polymer Solutions

Vol of 1% Polymer Volume of Water Concentration(c)


SNo. Solution (ml) %

Flow time of the solvent (to) =


3

Preparation of viscosity data for a polymer solution

Concentration Flow rel= /o sp=t/to-1 red=sp/c


SNo. gm/100 ml Time = t/to
Sec

CALCULATIONS:

i=kMa

log i= log k + a log M

log M = 1/a ( log i - log K)

k= 20x10-5 ; a = 0.76

RESULT:

The molecular weight of the given polymer solution = gms


4

2. PARTITION COEFFICIENT OF IODINE BETWEEN TWO


IMMISCIBLE SOLVENTS
AIM:
To determine the distribution coefficient of iodine between carbon
tetrachloride and water at room temperature

MATERIALS REQUIRED:
A stoppered bottle, Burette, conical flask, separating funnel, Iodine,
carbon tetrachloride, sodium thiosulphate, starch indicator

THEORY:
When solute like sodium is added to a mixture of two immiscible liquids
iodine distributes itself between the liquids. The ratio of the concentration in
the two immiscible layers is called partition coefficient. It is independent if the
amounts of the substance added to the liquid pair.
Partition coefficient = Concentration of iodine in organic layer
Concentration of iodine in aqueous layer
Cd = Corg
Caq

PROCEDURE:
1. The bottle are held thoroughly. 40ml of pure water is taken in each
of the four bottles.
2. In the 1st bottle 30ml of CCl4 and 10ml of iodine are added.
3. Similarly in the second bottle 25ml of CCl4 and 15ml of iodine, to
the 3rd bottle 20ml of CCl4 and 20ml of iodine, in the 4th bottle15ml
of CCl4 and 25ml of iodine is added.
4. All the bottles are stoppered and vigorously shaken for about
30mins.
5. From the 0.1N thio provided 10ml is pipette out and made upto
100ml in a standard flask to prepare 0.01N thio.
6. The above 2 thio sulphate solutions are taken in bottles and allowed
to stand atleast for 15 mins.
7. When the contents of the bottle will separate into two layers the
lower layer will be organic and the upper layer will be aqueous.
8. The first bottle is taken and its contents are transferred to a
separating funnel.
9. When the contents of the separating funnel settle thelayers are
separated after slightly opening the cork.
5

10. 5ml of the aqueous layer is pipette out into a clean conical flask
11. 10ml of 10%KI and a drop of freshly prepared starch indicator is
added.
12. The contents are titrated with 0.01N thio sulphate and volume is
noted
13. Then 5cc organic layer is pipette into a conical flask containing
about 10ml of 10%KI solution. To that a drop of starch indicator is
added.
14. The above solution is titrated with 0,1N thio sulphate and volume is
noted.
15. The above procedure is repeated for each bottle and Corg and Caq
were calculated.

TABULATION:
Standardisation of 0.1N thiosulphate

S.no Volume of Burette reading Volume of Concordant


K2Cr2O7 Initial Final thio value
(ml) (ml) (ml) (ml) (ml)

CALCULATIONS:
Volume of K2Cr2O7 = 10ml
Strength of K2Cr2O7 = 0.1N
Volume of thiosulphate = V1ml
Normality of thiosulphate = 10 * 0.1N/v1

Standardisation of 0.01N thiosulphate:


S.No Volume of Burette reading Volume of Concordant
K2Cr2O7 Initial Final thiosulphate value
(ml) (ml) (ml) (ml) (ml)
6

Volume of K2Cr2O7 = 10ml


Strength of K2Cr2O7 = 0.1N
Volume of thiosulphate = V2ml
Normality of thiosulphate = 10 x 0.1N/v2

TITRATION OF AQUEOUS LAYER:

S.no Volume of Burette reading Volume of Concordant


Aqueous Initial Final N/100 value
layer (ml) (ml) thiosulphate (ml)
(ml) (ml)

TITRATION OF ORGANIC LAYER:

S.no Volume of Burette reading Volume of Concordant


organic Initial Final N/10 value
layer (ml) (ml) thiosulphate (ml)
(ml) (ml)
7

MODEL CALCULATION:
Aqueous solution
Volume of 0.01N thiosulphate = V3ml
Concentration of iodine in aqueous layer = 0.5x N2/5
= geq/lit
Organic solution
Volume of 0.01N thiosulphate = V4ml
Concentration of iodine in aqueous layer = V4 x N4/5
= geq/lit

Bottle no Concentration of I2 Concentration of I2 Cd = Corg/Caq


in aqueous layer in organic layer
1
2
3
4

RESULT:
The partition coefficient for I2 between CCl4 and water is =
8

3. DETERMINATION OF PARTITION CO-EFFICIENT OF BENZOIC


ACID BETWEEN TWO IMMISCIBLE SOLVENTS

AIM:
To determine the association factor of benzoic acid between benzene
and water

MATERIALS REQUIRED:
Benzene, Benzoic acid, Distilled Water, N/10 and N/100 NaOH
solution, Separating funnel, Phenopthalein indicator, Reaction bottle, Pipette
and conical flask

THEORY:
When a solute like benzoic acid is placed between two immiscible
liquids such as benzene and water the solute tends to associate itself in benzene
while it is present in a single molecule in water. The dissociation coefficient for
equilibrium is given by,
K=C1/C2
Where C1 Benzoic acid in aqueous layer
C2 Benzoic acid in organic layer

PROCEDURE:
1. In a clean dry reaction bottle 50 ml of distilled water,50 ml of benzene
are added followed by 2 gms of benzoic acid.
2. In the same way in another reaction bottle 40 ml of benzene and 60 ml
of distilled water are added followed by 2 gms of benzoic acid.
3. The content of the bottle are heavily shaken for one hour and kept inside
to attain equilibrium.
4. In the reaction bottle organic layer and aqueous layer are distinctly
separated
5. Use a separating funnel to separate the organic and aqueous layer.
6. Exactly 10 ml of organic layer is pipetted out into a clean conical flask
and a drop of phenopthalein indicator is added and is titrated against std
N/10 NaOH
solution and the end point is appearance of pale pink colour.
7. Again 10 ml of aqueous layer is carefully pipetted out and titrated
against
N/100 NaOH solution using phenopthalein indicator.
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8. From the values of concentration of benzoic acid in each layer its


association factor is calculated.
TABULATIONS:

Volume Volume Burette Reading Volume of Volume of


of of (ml) N/100 N/10
aqueous Organic NaOH NaOH
layer layer Initial Final
(ml) (ml)
50 ml of
Benzene
+ 50 ml
H2O +
2 gms of
benzoic
acid

50 ml of
Benzene
+ 50 ml
H2O +
2 gms of
benzoic
acid

CALCULATIONS:

Caq = V1xN1/V2

Corg= V1xN1/V2

Caq / Corg =

Caq/Corg

Caq / Corg / Caq/Corg =


10

CALCULATION OF ASSOCIATION FACTOR

Bottle No. Benzoic Benzoic Caq/Corg Caq/Corg Caq/Corg


acid in acid in / Caq/Corg
aqueous Organic
Layer Caq Layer
Corg

Association Factor=

RESULT:

Association factor of benzoic acid between benzene and water =


11

4. DETERMINATION OF Ka OF THE WEAK ACID

AIM:
To determine the equivalent the equivalent conductance of the weak
electrolyte at various concentrations its dissociation constants and verify
Ostwald dilution law

MATERIALS REQUIRED:
KCl, N/10 CH3COOH, Conductivity bridge, Conductivity cell, burette,
pipette, glass rod, Standard flask.

THEORY:
The equivalent conductance is the product of observed specific
conductance and volume in ml containing one gram equivalent of electrolyte.
The equivalent conductance of strong electrolytes do not vary much with
concentration. In case of Weak electrolytes equivalent conductance increases
and specific conductance decreases with dilution. The equivalent conductance
of weak electrolyte at different concentrations is determined by measuring the
resistance of these solutions. The degree of dissociation of the electrolyte at
different concentration can be obtained from the equation.
= m/
The dissociation constant of weak electrolyte is given by Ostwald dilution law.
Ka = C 2 / 1-

PROCEDURE:
1. Exactly N/10 KCl solution is prepared and its resistance is measured.
2. From the value the cell constant of conductivity cell is calculated.
3. The solution of acetic acid is prepared.
4. From this solution solutions of 2, 1, 0.5, 0.25 and 0.125 M are prepared.
5. Each of the solution is taken in a beaker and conductivity cell is dipped
into it and its resistance is calculated.
6. With the known cell constant the specific conductance and the
equivalent conductance are calculated.
7. Using equivalent conductance at infinite dilution the degree of
dissociation is calculated at different concentrations.
8. The dissociation constant of weak acid is calculated using Ostwald
dilution law.
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TABULATIONS

Determination of Cell Constant

SNo. Conc of KCl R1 L1 L2 Rx


(M) () (mm) (mm) ()

CALCULATIONS:

Cell constant = Specific conductance / Measured conductance

Measured conductance = 1/ Measured Resistance

Cell Constant = Specific Conductance x Measured Resistance

Rx = L1/L2 x R1 =

Cell constant = 1.2886x Rx


13

S. Conc of R1 L1 L2 Rx 1/Rx Kx m Ka
No CH3COOH Sm2
(M) () (mm) (mm) () X10-3 Sm-1 mol-1 Mol
m-3

Mean =

CALCULATION:

Rx = l1/l2 x R1

1/Rx =

Kx= l/a x1/Rx

m = k/C

= 390.07x10-4 sm2mol-1

Ka = C 2/1-

RESULT:

The dissociation constant of the weak electrolyte was found to be =


14

5. CONDUCTIVITY MEASUREMENT AND VERIFICATION OF


OSTWALDS DILUTION LAW

AIM:
To verify Ostwald dilution law and to determine dissociation constant
for acetic acid

MATERIALS REQUIRED:
Conductivity cell, Conductivity bridge, beaker, electrodes, acetic acid

THEORY:
Consider the following equilibrium reaction for the dissociation of weak
electrolyte.

HA H+ + A-

Ka = [H+ ][A-] / [HA]

Where Ka is the dissociation constant for the weak electrolyte.The dissociation


of HA is given by c(1- ) and the formation of H+ and A- is given by c2 2.Then
Ka is given c2 2/1- . The equation represents the relationship between k,
and c. This is known as Ostwald dilution law and can b calculated from
equivalent conductance and equivalent conductance at infinite dilution.

= / c

PROCEDURE:
1. The beaker is filled with acetic acid of known concentration.
2. The conductivity cell was dipped into it.
3. Necessary connections were made.
4. Resistance was measured using the conductivity bridge.
5. Using the resistance and the cell constant the specific conductance was
determined.
6. The equivalent conductance was determined from the specific conductance.
7. The value of and Ka were calculated.
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TABULATION:

S Conc of C R1 L1 L2 Rx 1/Rx Kx m Ka
No. CH3COOH Sm2
(M) () (mm) (mm) () *10-3 Sm- mol-1 Mol
1
m-3

Mean =

CALCULATIONS:

k = l/a x1/Rx
=
Rx = l1/l2 xR1 =

m = k/C
=
= m/

Ka = c 2/1-

RESULT:

The Ostwald dilution law was verified and the dissociation constant =
16

6. CONDUCTOMETRIC TITRATION OF STRONG ACID WITH


STRONG BASE

AIM:
To determine the amount of NaOH present in 200 ml of the given solution by
conductometric titration using std HCl of 0.1 N.

MATERIALS REQUIRED:
1.Conductivity Bridge 2.Conductivity Cell 3.Beaker4.Std N/10 HCl 5.Given
NaOH solution 6.Burette ,Pipette ,Glass Rod.

THEORY:
Conductance measurements are frequently employed to find end points of
acid alkali number and mobility of ions. Consider for first instance the titration
of strong acid like HCl with a strong base like NaOH. The acid is taken in the
conductivity vessel and alkali is taken in the burette. The conductance of HCl is
due to presence of Hydrogen and Chlorine ions.
As alkali is added gradually the hydrogen ions are replaced by slow moving
sodium ions. Hence on continued addition of NaOH the conductance will go on
decreasing until the acid is completely neutralised. Any subsequent addition of
alkali will result in introduction of fast moving hydroxyl ions. The conductance
therefore after reaching a certain minimum value will begin to increase. On
plotting conductance vs volume of alkali added the points will lie on two
straight lines AB and CD. The point of intersection of these two lines gives the
volume of alkali required for neutralization

PROCEDURE:
1. Burette is filled with NaOH solution upto zero level.
2. 20 ml of standard HCl is pipetted out in a clean 100 ml beaker.
3. The cell is placed in it.
4. The two terminals of the cell are connected to the conductivity bridge.
5. 1 ml of the NaOH solution from the burette is added to the solution
taken in the beaker and stirred for some time and conductivity is
measured.
6. The process is repeated until atleast five readings are taken after end
point is reached.
7. Now a graph is plotted by taking volume of NaOH in the X-axis and
Conductance in Y-axis.
8. The end poinr is noted from the graph and amount of NaOH present in
250 ml Of the solution was calculated.
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SIMPLE PROCEDURE:

SNo. Contents Titration


1 Burette solution Sodium Hydroxide
2 Beaker solution 20 ml of 0.1 N HCl
3 Electrode Conductivity Cell
4 End Point Determined from the graph

TABULATIONS:

SNo. Volume of NaOH added(ml) Conductance (mho)


18

CALCULATION:

Volume of HCl taken = 20 ml


Strength of HCl = 0.1 N
Volume of NaOH =
Strength of NaOH = 20 x0,1/V1
Amount of NaOH present in 1000 ml of the solution =40xN1
Amount of NaOH present in 200 ml of the given solution =40xN1x200/1000

RESULT:

1. The strength of NaOH solution was found to be =

2. The amount of NaOH present in 200 ml of the given solution was found to
be=
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7. TITRATION OF MIXTURE OF STRONG ACID WEAK ACID Vs


STRONG BASE

AIM:
To determine the amount of strong acid and weak acid present in 1 lit of
given acid mixture.

MATERIALS REQUIRED:
Conductivity Bridge,Conductivity cell,Beaker,Std N/10 NaOH,N/10
HCl,N/10 CH3COOH.Burette-Pipette,Glass Rod.

THEORY:
When a mixture of strong and weak acid is titrated against a strong
alkali a combination of curves is obtained.Suppose a mixture of HCl and
CH3COOH is titrated against NaOH,HCl being a strong acid will get titrated
first.The titration of CH3COOH will commence only after HCl has been
completely neutralized.Hence a combination of curves is obtained.While point
B corresponds to neutralization of HCl point C corresponds to neutralization of
NaOH.

PROCEDURE:
1. The burette is washed well with water and mixed with given std solution
of NaOH.
2. It is then filled with NaOH with zero mark.
3. The given mixture of acids is pipetted out into a clean beaker.
4. The conductivity cell is placed in it.
5. The two terminals of the cell are connected to a conductivity bridge.
6. Now 0.5 ml of NaOH from the burette is added to the solution.
7. Then the beaker is stirred and the readings are noted.
8. After the end point the NaOH is again added which causes increase in
conductance.
9. After the second end point sudden increase in conductance is observed
on further addition of NaOH.
10. Now the graph is plotted between vol of NaOH vs conductivity.
11. From the end points the amount of CH3COOH and HCl present in 1 lit
of the solution are calculated.
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TABULATIONS

SNo. Volume of NaOH added Conductance


(ml) (mho)
21

CALCULATION:

Volume of HCl = 20 ml
Strength of HCl = N1
Volume of NaOH = V2 ml
Strength of NaOH =0.1 N
Strength of HCl = V2x0.1/20 =

Amount of HCl in 1 lit =Strength of HCl x Eqwt of HCl=W1 gms


Amount of HCl in 100 ml = W1x100/1000

Volume of CH3COOH = 20 ml
Strength of CH3COOH =N1
Volume of NaOH=B-A
Strength of NaOH= 0.1 N
N1 = (B-A)x0,1/20 =
Amount of CH3COOH in 1 lit = Strength of CH3COOHx Eqwt of CH3COOH
= W2 gms

Result :

1. The amount of HCl in 1lit=


2. The amount of CH3COOH in 1 lit=
22

8. TITRATION OF WEAK ACID AND WEAK BASE

AIM:
To determine the amount of Na2CO3 present in 200 ml of the given
solution by conductometric titration using std Acetic Acid of 0.1 N.

APPARATUS REQUIRED:
Conductivity Bridge,Conductivity Cell,Beaker,Std N/10
CH3COOH,Na2CO3 Solution,Burette,Pipette Glass Rod.

THEORY:
Conductance measurements are based on principle that electrical
conductance depends upon number and mobility of ions.For instance in the
titration of weak acidlike CH3COOH and weak base Na2CO3 the acid is taken
in the conductivity vessel and alkali in the burette.
As Na2CO3 is added the salt is formed which is fully ionised.Hence on
continued addition of Na2CO3 the conductance will go on increasing until the
acid is completely neutralised.Any subsequent addition will result in
introduction of partially dissociated carbonate ions.The conductance thus
increases at a slower rate. On plotting conductance vs volume of Na2CO3 added
two straight lines with their Intersection giving end point is obtained.

PROCEDURE:
1. Burette is filled with Na2CO3 solution upto zero level.
2. 20 ml of std acetic acid is pipetted out in a clean 100 ml beaker.
3. The cell is placed in it.
4. Two terminals are connected to the conductivity bridge.
5. 1 ml of Na2CO3 solution from the burette is added to the solution taken
in beaker and stirred for sometime and conductivity is measured.
6. The process is repeated until five readings are taken after the end point
is reached.
7. Graph is plotted by taking vol of Na2CO3 in X-axis and conductance in
Y-axis.
8. End point is noted from graph and amount of Na2CO3 in 200 ml of the
solution is calculated.
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TABULATIONS

SNo. Volume of Na2CO3 added Conductance (mho)


(ml)
24

CALCULATION:
Volume of CH3COOH = 20 ml
Strength of CH3COOH = 0.1 N
Volume of Na2CO3 =V1 ml
Strength of Na2CO3 =N1 Normal.
= 20x0.1/V1
Amount of Na2CO3 = Strength of Na2CO3 x 53
=
Amount of Na2CO3 in 200 ml of the given solution =200/1000xW1
=

RESULT:
The amount of Na2CO3 in 200ml of the solution is given =
25

9. DETERMINATION OF RATE CONSTANT


(ACID CATALYSED HYDROLYSIS OF AN ESTER)

AIM:
To determine the specific velocity constant for acid catalyzed hydrolysis
of methyl acetate at room temperature using HCl.

MATERIALS REQUIRED:
Burette, Pipette, Conical Flask,Methyl acetate, 0.5 N HCl,N/10
NaOH,Phenopthalein indicator, Ice Cold Water.

THEORY:
Esters are hydrolyzed by dilute mineral acid solutions.The reaction is
pseudo unimolecular when water is present in large excess.

CH3COOC2H5 + H2O CH3COOH + C2H5OH

Since the concentration of H2O remains constant the rate equation is given by

Rate = k1[Ester ]

Where c represents the concentration of ester at any time t.k id the specific
velocity constant.As the reaction proceeds the formation of CH3COOH
increases.It can be followed by drawing a known volume of reaction mixture at
regular intervals of time and titrating against std NaOH solution.

PROCEDURE:
1. Exactly 100 ml of H2O is taken and 5 ml of ester is added followed by
few drops of concentrated HCl.( 2-3 drops)
2. Zero time is noted when half the volume of ester solution in the pipette
is transferred to reaction bottle.
3. After thorough mixing immediately 10 ml of the solution is pipetted
into a clean conical flask containing ice cold water.
4. It is again titrated against std NaOH solution in burette using
phenopthalein Indicator.
5. The end point is appearance of pale pink colour.
6. The same volume of the reaction mixture is withdrawn at regular
intervals and titrated against NaOH solution.
7. The reaction is allowed to go to completion by keeping the reaction
mixuture over hot water for 1 hr.The final reading is then noted.
26

8. Let Vo be the volume of alkali used at zero time and Vt be volume of


alkali used after time t mins.Let V be the reading when the reaction
is completed.The specific reaction rate constant is given by

K1 = 2.303/t log (V - Vo )/ (V-Vt)


9. The rate constant values are calculated at different time intervals which
should be nearly same.
10. A graph is drawn betweem log(V - Vo )/(V-Vt) vs time. From the
slope of the plot the rate constant was calculated and compared with
experimental one.

TABULATIONS

Sno. Time Vol of V - Vo (V-Vt) K=2.303/t xlog


(mins) NaOH (V - Vo )/
(V-Vt)(ml)
(ml)

CALCULATIONS:
K= 2.303/t log (V - Vo )/ (V-Vt)

RESULT:
The average value of rate constant for acid hydrolysis of methyl acetate
is Experimental Value K1 =
Graphical Value K1=
27

10. DETERMINATION OF ACTIVATION ENERGY

AIM:
To determine the activation energy of hydrolysis of methyl acetate in
presence of acid

APPARATUS REQUIRED:
Water bath, Burette, Pipette, Conical Flask, Wash bottle, 0.5 N HCl,
Methyl acetate, N/10 NaOH, Ice cold water, Phenopthalein indicator

THEORY:
Esters are hydrolyzed by dilute mineral acid solutions.The reaction is
pseudo unimolecular when water is present in large excess.

CH3COOC2H5 + H2O CH3COOH + C2H5OH

Since the concentration of H2O remains constant the rate equation is given by

Rate = k1[Ester ]

Where c represents the concentration of ester at any time t.k id the specific
velocity constant.As the reaction proceeds the formation of CH3COOH
increases. It can be followed by drawing a known volume of reaction mixture
at regular intervals of time and titrating against std NaOH solution.

PROCEDURE:

1. Exactly 100 ml of H2O is taken and 5 ml of ester is added followed by few


dropsof conc HCl (2 -3 drops)
2 .Zero time is noted when half the volume of ester solution in the pipette is
transferred to the reaction bottle.
3. After throrough mixing immediately 10 ml of the solution is pipetted into a
clean conical flask containing ice cold water.
4. It is again titrated std NaOH solution in the burette using phenopthalein
indicator.
5. End point is the appearance of pale pink color.
6. The same volume of the reaction mixture is withdrawn at regular intervals
and titrated against NaOH solution.
28

7. The reaction is allowed to go to completion by keeping the reaction mixture


over hot water bath for 1 hour.The final reading is then noted.
8.Let Vo be the volume of alkali used at Zero time and Vt be the volume of
alkali used after the time t mins.
Kc = 2.303/t log (V-Vo)/(V-Vt)

9. The above procedure is repeated for 60oC .Then activation energy is


calculated using the formula

Lnk1/k2 =Ea/R (1/T1 -1/T2)

TABULATIONS
At 60oC (333 K)

Sno. Time Vol of V - Vo (V-Vt) K=2.303/t xlog


(mins) NaOH (ml) (V - Vo )/
(ml) (V-Vt)(ml)
29

At 30oC (303 K)

Sno. Time Vol of V - Vo (V-Vt) K=2.303/t xlog


(mins) NaOH (V - Vo )/
(ml) (ml) (V-Vt)(ml)

CALCULATION:

Ln k1/k2 = Ea/R ( 1/T1 1/T2)

RESULT:

The activation energy Ea =


30

11. ESTIMATION OF FERROUS ION CONCENTRATION BY


POTENTIOMETRIC TITRATION

AIM:
To estimate the amount of ferrous ion present in whole of the given
solution

MATERIALS REQUIRED:
Potentiometer, Pt electrode, Saturated Calomel Electode, Std K2Cr2O7,
2+
Fe solution

PROCEDURE:
TITRATION-1: K2Cr2O7 Vs Ferrous Ion
Take 20 ml of given Fe2+ solution,10 ml of dil H2SO4 and 20 ml of
water.A Pt electrode is dipped in the solution and coupled with calomel
electrode.Then K2Cr2O7 Is added in portions of 1 ml.The end point is the
sudden increase in emf value.

TITRATION-2 : K2Cr2O7 Vs Ferrous Ion


Here the K2Cr2O7 is added in portions of 0.1 ml using micro burette
near the end point.The corresponding emf value is noted.The end point is
obtained by plotting E/V vs Volume of K2Cr2O7.From the end point the
strength of Fe2+ solution and amount can be calculated.

TABUALTIONS
TITRATION-1

SNo Vol of K2Cr2O7 (ml) Emf Volts


31

TITRATION-2

SNo Vol of Emf e E V E/ V


K2Cr2O7 Volts

CALCULATIONS:

Vol of Fe2+ solution = 20 ml


St of Fe2+ solution =N1
Volume of K2Cr2O7 =V2 ml
Strength of K2Cr2O7 = 0.1 N
N1 = V2N2/V1
Strength of Fe2+ solution = N1
Amount of Fe2+ in 1000 ml of given solution= N1x55.85
= W1 gms /lit

RESULT:

The amount of Fe2+ in 1000 ml of given solution =


32

12. DETERMINATION OF STANDARD ELECTRODE POTENTIALS(Zn, Cu,


Ag)

AIM:
To determine the std electrode potential of Zn and Cu electrodes.

MATERIALS REQUIRED:
ZnCl2 solution,Zn Electrode,CuSO4,Cu electrode, Potentiometer,
Saturated Calomel Electrode.

THEORY:
Ecell = EoCell 0.0591/n log[Zn2+]

Ecell = EoCell +0.0591/n log[Cu2+]

PROCEDURE:
1. Prepare 1 M solution of ZnCl2 and CuSO4
2. Dip Zn and Cu electrodes in their respective solutions.
3. Measure the emf using the given potentiometer.
4. Calculate the std electrode potentials using the equations

TABULATIONS

SNo. Electrode Conc of Salt Solution Emf Volts


33

CALCULATION:

Ecell = EoCell 0.0591/n log[Zn2+]


EoCell = EoR - EoL
EoR =0.2422
Ecell = (0.2422-EoL) 0.0591/2 log(Zn2+)
Ecell = (EoR-0.2422) + 0.0591/2 log(Cu2+)

RESULT:

The saturated electrode potential of electrode is


Zn =
Cu =
34

13. ADSORPTION STUDIES


(FREUNDLICH ADSORPTION ISOTHERM)
AIM:
To determine the adsorption of oxalic acid from aqueous solution by
activated charcoal and determine the constants of freundlich adsorption
isotherm.

MATERIALS REQUIRED:
0.5N Oxalic acid,N/10 NaOH,Activated Charcoal,Conical Flasks.

THEORY:
Solid surface can adsorb dissolved substance from a solution.When a
solution of oxalic acid or acetic acid in water is shaken with activated charcoal
part of the acid is removed by charcoal and the concentration of the solute leads
to the establishment of an equilibrium between concentration of adsorbed on
the surface and concentration of the substance in the solution.The extent of
adsorption is given by equation x/m = kC1/n where x is the amount of solute
adsorbed per gram of the adsorbent.Taking log on both sides eqn becomes log
x/m = log k +1/n logc.Hence log x/m vs log c should be a straight line with
slope 1/n and intercept log k.The value of n can be determined from the slope
of the line

PROCEDURE:
1. A 500 ml of 0.5 N oxalic acid solution is prepared.
2. Five clean dry bottles are taken and 2 gm of activated charcoal is added
to it.
3. Each of the bottle is filled with 100,80,60,40 and 20 ml of oxalic acid
followed by 0,20,40,60,80 ml of water.
4. The bottles are shaken for hour by means of mechanical shaker.
5. They are set aside to reach equilibrium.
6. The supernatant liquid of each of bottle is treated with filter paper and
the filterate is collected in a conical flask.
7. 10 ml of the filtrate is pipetted out in a clean conical flask a drop of
phenopthalein is added and the solution is titrated with std NaOH
solution.
8. The titration is repeated for concordant values.
35

TABULATIONS
STANDARDISATION OF NAOH

Volume of Burette Reading Volume of Concardant


Oxalic Acid (ml) NaOH Value
(ml) Initial Final (ml) (ml)

CALCULATION:

Volume of Oxalic Acid =10 ml


Strength of Oxalic Acid = 0.1 N
Volume of NaOH = V1
Strength of NaOH = 10x0.1/V 1 =

Oxalic Acid Vs NaOH

Bottle Volume of Oxalic Burette Reading (ml) Volume of


No. acid NaOH
Initial Final
(ml) (ml)

Volume of Oxalic acid =10 ml


Strength of Oxalic acid =
Volume of NaOH = V1
Strength of NaOH = N1
Strength of Oxalic acid = V1xN1 /10
36

Bottl Initial Final Adsorptio Weight X/m Log Log


e No. Concentrati Concentration n of of X/m C
on of Oxalic of Oxalic acid Oxalic Charcoal
Acid (N) (N) acid m gms
X=Co -CL

CALCULATION:

X= Co -CL

X/m =

Log X/m =

Log c =

RESULT:
The Freundlich adsorption is verified and the values of n and k were found to
be
n=
k=
37

14. TO STUDY THE ADSORPTION OF ACETIC ACID BY CHARCOAL


AND CONSTRUCT THE ISOTHERM

AIM:
To determine the adsorption of acetic acid from aqueous solution by
activated charcoal and determine the freundlich adsorption isotherm.

MATERIALS REQUIRED:
0.5 N acetic acid, N/10 NaOH, Activated charcoal, Conical Flask

THEORY:
Solid surface can adsorb dissolved substance from a solution when a
solution of CH3COOH in H2O is shaken with activated charcoal part of acid is
removed by Charcoal and conc of solute leads to the establishment of an
equilibrium between Conc of adsorbed on the surface and conc of the substance
in the solution. The extend of adsorption is given by equation x/m=kc1/n where
x is the amount where x is the amount of solute absorbed per gram of the
adsorbed Taking log on both sides of the above equation log x/m =log k
+1/nlogc. Here the plot of log x/m vs log c should be a straight line with slope
=1/n and intercept =log k. The value of n can be determined from the slope of
the line.

PROCEDURE:
1. A 500 ml of 0.5 N CH3COOH solution is prepared.
2. Five clean dry bottles are taken and 2 gm of activated charcoal is added
to it.
3. Each of the bottle is filled with 100 ml,80,60,40 and 20 ml of
CH3COOH followed by 0,20,40,60 and 80 ml of H2O.
4. The bottles are shaken for 1 hour by means of mechanical shaker.
5. They are set aside to reach equilibrium
6. The supertant liquid of each bottle is treated with filter paper and the
filter is colleceted in a conical flask.
7. 10 ml of filtererate is pipette and in a clean conical flask a drop of
phenopthalein is added and solution is titrated with std NaOH.
8. The titration is repeated for concordant values/.
38

TABULATIONS

Vol of Acetic Burette Reading Vol of NaOH Concardant


acid (ml) Initial Final (ml) Value

CALCULATION:
Volume of Acetic acid =10 ml
Strength of Acetic acid = 0.1 N
Volume of NaOH =V1
Strength of NaOH =10x0.1/V

Acetic Acid Vs NaOH

Bottle No, Volume Of Burette Reading (ml) Volume of


Acetic Acid Initial Final NaOH

Volume of Acetic Acid =


Strength of Acetic acid =
Strength of NaOH =
Strength of Acetic acid =
39

Log x/m vs Log c

Sno. Initial Final Adsorption Weight X/m Log Log C


Conc of Conc Of Acetic of X/m
Acetic Acetic acid Charcoal
Acid Acid

X=Co Cl
X/m
Log X/m
Log C =

RESULT:

The Freundlich adsorption is verified and the values of n and k were found to
be

N=
K=
40

15. PH METRY DETERMINATION OF STRENGTH OF HCL BY


NAOH

AIM:
To determine the strength of HCl by PH metry a std solution of NaOH
is provided.

MATERIALS REQUIRED:
PH meter, Glass Electrode, Beaker, Std N/10 NaOH, App N/10 HCl,
Burette, Glass Rod

THEORY
Since the Ph of the solution is related to H+ ions concentration by the formula
PH = -log[H+]
Measurement of PH of the solution gives the values when NaOH is added
slowly from the burette to the solution in HCl as a result PH of the solution
increases.
HCl + NaOH NaCl +H2O
The increase in PH takes place until all the H+ ions are completely
neutralized. After the end point further addiation of NaOH increases pH
sharply as there is an excess of fast moving OH- ions.

PROCEDURE:
1. The burette is filled with std NaOH solution.Exactly 20 ml of the given
HCl solution is pipetted out into a clean 100 ml beaker.
2. The glass electrode is dipped in it and connected with a PH meter.Now
NaOH is added in 1 ml gradually.
3. The PH is noted in each reading.
4. The process is repeated until 5 readings taken after the end point.
5. The observed PH values are plotted against the vol of NaOH added.
6. The point with max slope gives the end point
7. Before carrying and the experiment Calibrate the instrument by inserting
the glass electrode in water and set the PH to 7.
41

TABULATIONS
SNo. Volume of NaOH Added (ml) PH

CALCULATIONS:
Vol of HCl = V1
Strength of HCl = N1
Strength of NaOH , N2 =0.1 N
Strength of HCl N1=V2N2/V1

Amount of HCl in 1000 ml of the given solution = Strength of HCl x


Equivalent of HCL

TABULATIONS

SNo. Volume of NaOH V PH PH PH/ V


added (ml)

RESULT:

Strength of HCl =
Amount of HCl is 1000 ml of given solution =
42

16. ENZYME CATALYTIC REACTION BY VARYING pH


DETERMINATION OF MICHAELIS MENTEN PARAMETERS
AIM:
To verify the Michaelis Menten model for enzyme substrate reaction
and to determine Michaelis Menten parameters.
THEORY:
The relationship between substrate concentration x and the rate of reaction was
mathematically expressed by
V = Vmax [S]
Km + [S]

Where Vmax = maximum reaction rate


[S] = substrate concentration (mol/l)
Km = Michaelis Menten constant

There are three ways in which the hyperbolic relationship between three initial
rate of reaction x, initial substrate concentration can be obtained,

Line wearnerberg plot Line wearnerberg plot of 1/v against 1/[So] giring
intercepts at 1/Vmax and slope -1/Km. Eadie hofstee plot is the plot against
v/[s] giving intercepts at Vmax and Vmax/Km Haneswolt plot [s]/v against [s].
It is also called as half reciprocal plot. It gives intercept at Km/Vmax and Km

For the free enzymes , one unit of enzymatic activity corresponds to the
quantity of enzymes that produce 1M mol of glucoseand fructose in the
hydrolysis of 5% (W/M) sucrose solution at 55*c and PH 5.

REAGENTS REQUIRED:
1. Invertase
500 mg of intertase dissolved in 50 ml of distilled water.

2. Buffer solution
Solution A: 0.1 M acetic acid (PH5) 357 ml
Solution B: 0.1 M sodium acetate 643 ml

3. Sucrose Solution
3g of sucrose dissolved in 100 ml of distilled water
43

4. 40% sodium potassium tartarate


20g of sodium potassium tartarate dissolved in 50 ml of water.

5. DSNA reagent
To 1g of DSNA, add 0.2 ml of phenol solution and 50 mg sodium
sulphate dissolved in 100ml of 1% NAOH.

PROCEDURE:

1. Pipette out 0.5, 1.0, . 3 ml of sucrose solution in a series of test tube


and make up the volume as 3 ml with distilled water.

2. Add 0.1 ml of inverse solution and 2.9 ml of acetate buffer at PH 5.


Immediately, incubate the mixture at 55*c in a water bath for 5 min.

3. Take out 2 ml of reaction mixture in new set test tubes containing 3 ml of


DSNA reagent. Add 1 ml of distilled water to each of the test tubes; heat
the test tubes at 35*c for 5 min.

4. Add 1 ml of 440% sodium potassium tartarate solution to each of the test


tubes, immediately after removing from the water bath.

5. Cool the mixture and measure the optical density at 540 nm against blank.

6. Calculate the enzyme activity.

7. A graph was plotted between the reaction rate (v) and the substrate
concentration [s]; and (line weaver burk plot) reciprocal of substrate
concentration 1/[s] and reciprocal of reaction rate 1/v.

8. The values of Vmax and Km are found from the graph.

RESULT:
Thus Michaelis Menten kinetics for the enzyme substrate was verified
and the parameters were determined as
V max =
Km =
-1/Km =
44

Content B S1 S2 S3 S4 S5 S6
Volume of
sucrose (ml)

Concentration
of sucrose
solution (mg)

Volume of
distilled water
(mg)

Volume of the
enzyme (ml)

Volume of
acetate buffer
(ml)

Volume of
DNSA reagent
(ml)

Volume of
distilled water
(ml)

Volume of
sodium
potassium
tartarate (ml)

Optical density
at 540nm
45

S.No Concentration Optical 1/S 1/V


[S] density
V
46

17. APPLICATION OF PHASE RULE TO PHENOL WATER SYSTEM


DETERMINATION OF CRITICAL TEMPERATURE OF PARTIALLY MISCIBLE SOLUTION

AIM:
To construct a material solubility temperature for a pair of partially
miscible liquids namely phenol and water to determine critical temperature of
solution

MATERIALS REQUIRED:
Phenol, Beaker, Distilled water, 110oC, Sensitive thermometer

THEORY:
When partially miscible liquids such as water and phenol are mixed; two
mutually miscible layers are separated. The upperlayer is the solution of phenol
in water and the lower layer is water in phenol. At any given time and
temperature the two layers are mixed. However, such a system becomes
incompletely homogenous mixture alone in certain temperature. This
temperature is called critical temperature.

PROCEDURE:
1. Exactly 3 ml of phenol; freshly distilled water is taken in a flat bottomed test
tube.
2. It is fitted with a cork-carrying thermometer and stirrer.
3. The flat-bottomed test tube is placed in water bath and slowly heated.
4. The mixture is stirred well and the temperature at which the turbidity
disappears.
5. The two layers form a single layer is noted.
6. It is then allowed to cool and temperature at which the turbidity disappears.
7. It is then allowed to cool and temperature at which turbidity begins to appear
is noted.
8. The experiment is repeated by adding 3,4,5,6,7,8,9 ml of water of the
corresponding miscibility temperature plotted against % composition of phenol
by weight.
9. The maximum of the curve indicates the critical solution temperature of the
system under consideration.
47

TABULATIONS:

SNo. Volume of Vol of % Temperature Average


Phenol H2O Phenol

Calculation :

% Comp of Phenol = Volume of Phenol x p


= -------------------------
Volume of Phenol x p +Volume of H2OxH2O

RESULT:

The critical solution temperature of phenol water system is % phenol =


Miscible temperature =
48

18. TO STUDY THE INVERSION OF CANE SUGAR BY


POLARIMETER

AIM:
To study the inversion of cane sugar in the presence of dilute acids and
to determine the rate constants for the reaction

MATERIALS REQUIRED:
Polarimeter, 20% sucrose solution, 0.1N HCl, Pipette, Burette

THEORY:
Inversion of cane sugar is usually catalysed by a dilute acid as an
example of pseudo unimolecular reaction. The reaction takes place according
to the following reaction

C12H22O11 + H2O C6H12O6 + C6H12O6


As the concentration of water remains constant the reaction obeys 1st
order kinetics. Bothe cane sugar and glucose are dextrorotatory, but fructose id
leavorotatory. The laevorotation of fructose is 92 which counteracts the
dextrorotation of glucose which is 52. Hence the reaction is followed by
measuring the change in the angle of rotation. The change gives the amount of
sugar decomposed.

PROCEDURE:
1. 20% of sucrose solution is prepared and a drop of thymol is added
2. Exactly 20ml of sugar solution and 20ml of 0.1N HCl is mixed and
poured into polarimeter tube
3. The angle of rotation is measured at regular intervals of 10mins
4. Let the critical angle at the start of the reaction be 0
5. At the instant of rotation the angle be T and infinite reading is 00
6. At time t the concentration of sugar be T - 00
7. At the start the concentration is T - 00
8. Knowing the various values at different times the rate constant can be
calculated
49

TABULATION:

S.No Time Angle of rotation T - 00 K = 2.303/t log(0 - 00


/ T - 00)

CALCULATIONS:

K = 2.303/t log(0 - 00 / T - 00)

RESULT:
The rate constant for the inversion of sugar by theoretical method is

= by calculation
= by graph

TABLE OF CONTENTS
50

S.No TITLE OF THE EXPERIMENT PAGE No


1 Determination of molecular weight of a polymer by viscosity method.
2 Determination of partition co-efficient of iodine between two
immiscible solvents
3 Determination of partition co-efficient of benzoic acid between two
immiscible solvents
4 Determination of Ka of the weak acid
5 Conductometric experiments- Verification of Oswalds Dilution Law
6 Titration of Strong Acid Vs Strong Base
7 Titration of mixture of Strong Acid Weak Acid Vs Strong Base
8 Titration of Weak Acid Vs Weak Base
9 Determination of Rate Constant (K)
10 Determination of Activation Energy (E)
11 Estimation of Ferrous ion concentration by Potentiometric Titration
12 Determination of standard electrode potential (Zn, Cu, Ag)
13 Adsorption studies
14 To study the adsorption of Acetic acid on charcoal and construct the
isotherm.
15 Determination of pH metric titration of Strong Acid Vs Strong Base
16 Enzyme catalytic reaction by varying pH.
17 Application of Phase Rule to Phenol-Water system
18 To study the inversion of cane sugar by polarimeter