ENGINEERING CHEMISTRY LABORATORY EXPERMENTS

B.Tech I YEAR

EXP...No. 1

TITRIMETRY

AIM: Estimation of hardness of water by EDTA method

APPARATUS: - Burette, Pipette, beakers, Standard flask, Conical flask etc.

CHEMICALS: - 0.1 M EDTA, Eriochrome, Blacke-T, water sample buffer solution.

THOERY:- Estimation of hardness by EDTA method is based on the following principles.
1. First, the indicator Eriochrome Black-T, which is a blue colored dye, forms an unstable
complex with calcium or Magnesium ions in hard water at
H
P of 9 to 10. The complex is
wine red in color.

2 2
/ Mg Ca
+ +
+Eriochrome Black-T [Mg/CaEriochrome black-T)
Unstable Complex (Wine Red)

2. As this solution is titrated against EDTA, the free
2
Ca
+
and
2
Mg
+
tones in water from
stable metal ion EDTA [Mg/Ca-EDTA] Stable Complex. Colorless
Once the free metal ions are complexed, the EDTA replaces Ca and Mg ions from the
unstable indicator complex also, to form a stable complex, with the result, the indicator is
set free. Since the free indicator is blue in colour at the above mentioned PH, the end
point is the appearance of blue color
[Mg/Ca-Eriochrome Black-T] +EDTA [Mg/Ca-EDTA] + Eriochrome Black-T(Blue)
The temporary hardness is removed by boiling and after the removal of precipitate by
filtration; the permanent hardness in the filtrate is determined by titration with EDTA as
above.




Procedure:-
1 .Rinse and fill the burette with EDTA solution.
2. Pipette out 25 ml of hard water into volumetric flask and add 20 ml of distilled water and
10 ml of buffer solution
3. Add 2-3 drops of Eriochrome Black-T indicator.
4. Titrate against 0.01M EDTA solution till the color of the solution changes from wine red to
Blue.
5. Note the final reading and repeat to get three concordant readings.

Observation Table:
Sl.No
Volume of the solution
taken in the titration flask
(nl)
Burette Readings Volume of the
titrant used
2 1
V V nl
Initial
Reading(V
1
nl)
Final Reading
(V
2
nl)







Volume of hard water taken for each titration = 25 ml
Volume of 0.01 M EDTA used [from titration] = V
1
ml

Calculation: - 100 ml of 1 M EDTA = 100 gm of CaCo
3
= 1 mg of CaCo
3

1 ml of 0.01M EDTA =
1 1
100
1000 100gm
of CaCo
3
= 1 mg of CaCo
3
V ml of 0.01M EDTA = IV Mg of CaCo
3
= x mg of CaCo
3

25 ml of hard water contains=x mg of CaCo
3

1000 ml of hard water contains = x/25100 mg of CaCo
3
= y Mg/L
RESULT: The Total hardness of water= y Mg/L
Precautions:-
1. The burette and pipette, conical Flask should be rinsed with distilled water.
2. The color change near the end point is very slow and this should be observed carefully.



EXPERIMENT NO.2

DETERMINATION OF Cu
2+
THROUGH IODOMETRIC TITRATION
AIM: Determination of Cu percentage in Copper one (Brass)
APPARATUS: Burette, Pipette, Beakers, Titration flask
CHEMICALS: Copper One, Hypo, KI, Br
2
Solution, Acetic Acid, Nitric and HCl, H
2
So
4
INDICATOR: Starch solution
END POINT Blue to Colourless
PROCEDURE:
Preparation of Solution of ore
1. Take about 1 g of the finely ground copper ore in a beaker and warm with 15-20 ml of conc.
HNO3 until the copper passes into solution.
2. Evaporate to a volume of 5 ml and add 10 ml of conc. HCl and equal volume of 1: 1 H
2
SO
4
.
Again evaporate till dense fumes of SO
3
appear indicating complete removal of nitrogen
oxides.
3. Heat the mixture with 15 ml of bromine solution and an equal volume of water to complete
oxidation of any As and Sb to the Pentavalent state.
4. Boil off excess of bromine and dilute the resulting solution to 100 ml in a measuring flask.
Titration:
1. Rinse and fill the burette with 0.1 N Na2S2O4 solution
2. Measure 20 ml of the ore solution into a conical flask
3. Neutralize any free acid present by adding Na2CO3 solution drop by drop till a faint
permanent precipitate remains even on shaking.
4. Add dil. Acetic acid drop wise until precipitate just dissolves
5. Add 1 gm of solid Kl, cover the mouth of conical flask by filter paper and allow the
mixture to stand for 2 to 5 minutes in the dark the solution becomes brown due to
liberated iodine
6. Titrate the liberated iodine with hypo solution added from the burette, the brown colour
of iodine becomes fainter as the addition by hypo solution proceeds and when only a faint
yellow colour remains add 2 ml starch solution. This immediately form a deep blue iodo-
starch complex
7. Now add hypo solution further, drop by drop when only milky white colour remains.




Observation Table:


Sl.No
Volume of the
solution taken in
the titration
flask(ml)
Burette Readings

Volume of the
titrant used
(final-Initial
reading((ml)
Initial Reading Final Reading
1.
2.
3.


Calculations:
(Ore Soln.) (Na
2
S2O
3
)
N1V1 = N
2
V
2

N
1
20 = 0.1V
2

N
1
=
63.5
100
StrengthofSolution

2
0.1
20
V

N(
2
Cu
+
) =
2
200
V
Strength of
2
Cu
+
=
2
200
V
63.5g/L
Percentage of Cu in ore solution =
2
200
V 63.5
100
StrengthofSolution

RESULT: The amount of Cu present in copper ore solution is .













EXPERIMENT NO.4
COLORIMETRY
ESTIMATION OF COPPER BY COLORIMETRIC METHOD
AIM: Estimation of Copper by Colorimetry
APPARATUS: - Colorimeter, Test tubes, Burettes.
PRINCIPLE: - Colorimeter measures the optical density of an absorbing substance where optical
density (O.D) is defined as O.D = log 1
o
I
I

Where
o
I = Intensity of incident light
I = Intensity of transmitted light
As per beers law, optical density of an absorbing substance is related to the concentration by the
equation. . . . OD ECl =
. ( . ). 2 OD El C =
Where C is the concentration of the substance, l is the path length, which represents the width
of the cell used and is constant for a given cell used, E is the molar absorption coefficient and is
a constant for given substance. Equation 2 may be written as O.D. o C 3
Equation 3 represents the quantitative form of Beers law . if the optical density of a substance is
determined at varying concentration. A plot of O.D.vs C gives a straight line.
PROCEDURE:- take the sample solution of CuSo4 and prepare the following 10 sample
solutions in test tubes as 1 to 10
1. 1 ml 0.1 m CuSo
4
+ 9 ml Distilled water
2. 2 ml 0.1 m CuSo
4
+ 8 ml Distilled water
3. 3 ml 0.1 m CuSo
4
+ 7 ml Distilled water
4. 4 ml 0.1 m CuSo
4
+ 6 ml Distilled water
5. 5 ml 0.1 m CuSo
4
+ 5 ml Distilled water
6. 6 ml 0.1 m CuSo
4
+ 4 ml Distilled water
7. 7 ml 0.1 m CuSo
4
+ 3 ml Distilled water
8. 8 ml 0.1 m CuSo
4
+ 2 ml Distilled water
9. 9ml 0.1 m CuSo
4
+ 1 ml Distilled water
10. 10 ml 0.1 m CuSo
4
+ 0 ml Distilled water

The ten sample solutions prepared above have a varying concern from 0.01m to 0.1m, choose the
filter in the colorimeter with maximum absorbance. Tabulate the result of filter and O.D with a
given CuSo
4
sample solutions.
After selecting filter, determine the O.D. of the above mentioned ten sample solutions and
tabulate the results.
Observation:
Table-1
Filter No -Range (nm) Peak (nm)
Optical
Density(OD)
1
2
3
4
5
6
7
8






Table-II Selected Filter--------------------
Sl.No
Volume of
4
CuSo (ml)
Volume of
2
H O (ml)
Concentration
of
4
CuSo
Optical
Density
1
2
3
4
5
6
7
8
9
10
9
8
7
6
5
4
3
2
0
1
2
3
4
5
6
7
8

10 1 9


GRAPH: - Plot a graph of O.D Vs [CuSo4]. A straight line passing through origin is
obtained the slope of which gives El, E is the molar absorption coefficient.









Slope
2 1
2 1
y y
x x

1
slope
slope El E
l
E mole cm

= =
=


RESULT: - Amount of copper present in given CuSo
4
solution is _________grams?




















EXP.NO.5

CONDUCTOMETRY

Aim: - To determine strength of given HCl Solution Conductometrically

APPARATUS: - Conductivity meter, conductivity cells, Beakers, Pipette, Burette

CHEMICALS:- Oxalic acid Solution (0.1N), NaOH Solution, HCl, Phenolphthalein Indicator.

Preparation of Standard Oxalic acid Solution (o.1N)
About 1.6g of Oxalic acid dehydrate is weight accurately and dissolved in small amount of
distilled water and made up to the mark in 250 ml volumetric flask.


PRINCIPLE: - The conductivity of HCl is very high due to mobility of H+ ions in it. When a
solution of strong alkali is added to the solution of strong acid, the highly conducting H
+
ions are
replaced by Na
+
ions is considerably smaller than H
+
and hence addition of alkali to the acid
always accompanied by a decrees in conductivity. When all the H
+
are replaced that is after the
end point, further addition of NaOH results in increase in conductivity. from the plot of the
conductive Vs Volt NaOH added, the end point can be calculated

PROCEDURE: - 20 ML OF Oxalic acid is pipette out into a conical flask and is diluted to 30 ml
with distilled water. To the solution, two drops of phenolphthalein indicator is added and the
titrated against sodium hydroxide taken in a burette. The endpoint colorless to pale pink. The
experiment is replaced till correct reading are obtained





Determination of Strength of Given HCl Solution:-
The given unknown HCl solution is 100 ml volumetric flask is made up tot the mark and then
10ml of given unknown HCl Solution is taken in a 100 ml beaker. To this 40ml of distilled water
is added, the electrode of the cell is dipped in the solution. The conductivity of solution is noted
before adding the alksli. The standardized sodium hydroxide is added from a burette with 1ml of
increment and by shaking thoroughly, the contents of the beaker the conductivity values are
noted. The values of observed conductivities are plotted against volume of sodium hydroxide
The concentration of hydrochloric acid is determined using the end point from the graph.

PRECAUTIONS: - after 2 each addition of titrant from the burette the solution should be
thoroughly stirred and then the reading should be taken.

RESULT: - The Strength of Hydrochloric Acid is __________ g/lit.

Calculation:-
Standardization of Sodium Hydroxide Solution
S.No
Volume of Oxalic Acid
(V
1
ml)
Burette Readings
Volume of NaOH Solution
(
2
V =F-I)
Initial Final
1
2
3
20
20
20







WE know that
1 1 2 2
VN V N =
V1 is Volume of Oxalic Acid = 20ml
N1 is Normality O Oxalic Acid= 0.1N
V2 is Volume of Sodium Hydroxide=- -ml
N2 is Normality of Sodium Hydroxide N
1 1
2
2
V N
N
V
= Normality NaOH = -------N


Determination of Strength of Hcl:-

Sl.No Volume of NaOH Conductivity (ohm
-1
)
1
2
3






20







40



Volume of NaOH Solution from graph Ph V2 = -ml GRAPH:
Normality of NaOH Solution N2= -N
Volume of Hudrochloric acid solution V3= 10ml
Normality of HCl in mixture N3= -----N.
2 2 3 3 V N V N =
2 2
3
3
V N
N
V
=
Strength of HCl Solution = Normality of HCl Solution eg.Wt of HCl
= N3 36.5
=n ________ g/Lit


EXP.NO.6

POTENTIOMETRY

TITRATION OF STRONG ACID Vs STRONG BASE
AIM:- To Determine the concentration of a strong acid by a Potentiometry titration given a
strong base of known concentration.
APPARATUS: - Potentiometer, Pt-electrode, Calomel electrode, Salt bridge, 150 ml beakers,
Stirrer, Pipette, Burette.
CHEMICALS: - 0.1m NaOH, 0.1m HCL, Quinhydrone solid, KCl Solution.
PRINCIPLE: - The quinhydrone electrode is prepared by taking saturated solution of
quinhydrone in a known quantity of strong acid whose concentration is to be determined. This
electrode is combined with the calomel electrode to make the cell. Pt, Hg,
Hg
2
Cl
2
(s)/Saturated//H
+
/QH
2
/Pt
In acid medium quinhydrone exist in two forms.



As NaOH is added to a solution of H+ ions with quinhydrone the H+ ions are consumed steadily
and the relative concentration of QH2 and Q changes with the titration. At the end point where
all the ions are consumed, QH2 gets completely converted to Q. the electrode potential of the
electrodes is given as per the nearest equation.
2
0
2 2
2
0.059 .
/ / 10
aQa Qh
EQH Q E QH Q g
aQH
+
=

0
2
0.118
/ log E QH Q aH
n
= [ aQ Q and
2
1] aCH =
At the endpoint, which aH o
+
; there is a sudden fall in the cell emf
2
/ cell calomel aH Q
E E E = +
Since calomel is constant the variation of
cell
E is a measure of the variation of
2
/ aH Q
E . The
endpoint is the titration is the point where there is a maximum full in potential with a small
addition of NaOH.
Procedure: - Pipettes out 10 ml of the given HCl solution into a clean100ml beaker add a pinch
of quinhydrone and stir it well to make a saturated solution of quinhydrone is H+. dip a platinum
electrode. Take a second beaker with saturated KCl solution in it. Dip the calomel electrode in it.
Connect two beakers with a salt bridge; connect the terminals of the potentiometer with the two
electrodes. Note the emf of the cell. fill a burette with 0.1 NaOH, add 0.5ml of NaOH into the
beakers containing acid, stir well for equilibrium to establish. Note the emf of the cell once
again. The variation of emf by successive addition of 0.5 ml of NaOH. Each time will be about
10-20mv, as the endpoint approaches, the fall in the emf would increase from 10-20 mv to 40-50
mv. At this stage add NaOH in batches of 0.2 ml and note emf after each addition. At the end
point the emf falls suddenly by about 100-150 mv. Continue the titration with 0.2 ml of NaOH
and note 5-6 emf values. Now the variation is emf gets smaller and takes 4-5 emf readings, after
the endpoint by adding batches of 1ml of NaOH each time, tabulate the results.

GRAPH: - Plot a graph of emp Vs volume of NaOH added and a second graph of / E V V V Vs
Volume of NaOH added. Note the point of Neutralization from both the graph and calculate the
cone of given HCl using the concern of given NaOH as 0.1m








RESULT: - At the Neutralization point 10 ml of given HCl =? And concern of given HCl=____

Sl.No Volume of Alkali (ml) Emf (mv)
' Poly n

E
V
A
A

1
2
3

.
.
.

30


CALCULATION: -

HCl NaOH
1
10 V ml =
2
_____ V = (From Graph)
1
? N =
2
0.1 N =

1 1 2 2
V N V N =
1
1
2 2 V N
N
V
=

Concentration of given HCl (
1
N ) = ____N.

EXPERIMENT 9
IDENTIFICATION OF FUNCTIONAL GROUPS IN ORGANIC COMPUNDS
SYSTEMATIC PROCEDURE
EXPERIMENT OBSERVATION INFERENCE

PHYSICAL CHARACTERSTICS:
a)Physical state i) Liquid (or) Solid)
ii) Amorphous (or)
crystalline
b) Odour i) Pale yellow Nitro compounds
ii) Reddish orange Nitro amines
iii) Brownish yellow Aniline
iv) Pale pink Phenol
v) Colourless Carbohydrates, aldehydes,
ketones, carboxylic acids,
esters and some simple
hydrocarbons.
c) Odour i) Odourless Carbohydrates, aromatic
acids
ii) Bitteralononds Nitrobenzene, benzaldehyde
are absent
Aromatic amines
iii) Fishy smell Acetamide
iv) Mouse like smell Formaldehyde, formic acid
v) Pungent smell Esters
vi) Pleasant fruites Phenols
(Phenolic) Carbolic smell Acetic acid
Vinegar like Cinamon like Cinnamaldehyde
d) Melting point/ Boiling point
II. Solubility : Take a small amount of compound in a test tube and add 3-ml of solvent
a)Water Soluble in cold water i) Carbohydrates, glucose,
Fructose
ii) Amides, urea acetamide
b) 5% NaOH Soluble in 5% NaOH and May be week acid like
phenols
regerated with HCl
c) 5% NaHCO
3
Soluble in 5% NaHCO
3
and May be strong acids,
benzolic,
regenerated with HCl salicylic acids.
d) 5% HCl Soluble in 5% HCl regenerated May be amines like aniline
with NaOH.
e) Ether Soluble in ether May be nautral compounds
like, chlorobenzene,
Aldehydes, Ketones,
Nitrobenzene etc.
III. Ignition Test :
Heat a small amount 1) Burns with non-luminous Aliphatic compound
Of given compounds and non-smoky flame.
On spatula
2) Burns with Luminous Aromatic compound
And smokes flame
3) Burns with sugar smell Carbohydrates




DETECTION OF FUNCTIONAL GROUPS
TEST FOR PHENOLS
i)With neutral FeCl
3
test :
The compound to dissolved Violet (or) Blue Phenol is present
In alcohol and add 1 (or) 2 colour is observed
Drops of 5% Fec
6
5 3 3 6 5
6 [ ( )] 3 C H OH FeCl H Fe OC H HCl + +
ii) Liebermanns nitroso reaction:
Take the compound in a dry A blue colour is obtained Phenol is present
Test tube add sodium nitrite the solution turns red on
And conc sulphuric acid(1ml) dilution with water and blue
Mix well and heat gently on basification with dil
Sol of NaOH






Test for Carboxylic Acids:
1.NaHCo3 Test
To a saturated solution Brisk effervescence Carboxylic acid is present
Of sodium bicarbonate is observed
in water (1ml) add the
given compound
3 2 2
R COOH NaHCO RCOONa H O CO + + + |
ii) Ester Test:
Heat the mixture Fruity smell is observed Carboxylic acid is present
Of the acid, ethanol (1ml)
And concentrated sulphuric acid
in a dry test-tube in a water bath.
Pour the reaction mixture carefully into a
Beaker containing Na
2
Co
3
Solution.
2 4
. 1 1
2
Conc H SO
Heat
R COOH R OH RCOOR H O + +
iii) Fe Cl
3
Test:
Neutralise0.5 gm of the i) A buff (or) brownish coloured Aromatic acids
Acid with excess of ammonia ppt is obtained
In a boiling test tube. Boil the ii) An intense yellow colour is o -Hydroxy acids
Solution to remove excess obtained
Of ammonia, cool and add a few iii) A violet (or) fleshy colour is | -substituted aromatic
Drops of neutral ferric chloride obtained hydroxy acid
Solution.
Test for Carbonyl Compounds:
I) Reaction with 2,4 DNP1
Dissolve the carbonyl compound a yellow or orange colour may be a
(100 mg (or) 1-2 drops) in ethanol (2-3ml) ppt is formed carbonyl compound
To this add an alcoholic solution of
2,4 di nitro-phenyl hydrazine (2 ml)
and Shake the mixture well.



ii) Tollens Test:
To the tollens reagent (1ml) a grey black ppt(or) silver May be aldehyde is
Add a solution of the aldehyde mirror deposits on the inner present
(2 drops (01) 50 mg) dissolved walls of a test tube
In aldehyda free alcohol
(-2-3 ml) and warm the solution
in a hot water bath.

iii) Fehling Test:
Add Fehling solution (2-3 ml Red precipitate of may be aldehyde is
By mixing equal amounts of cuprous oxide is formed present
Fehling A+ Fehling B0 to the
Organic compound .and warm the mixture
2 2 2
2 ( ) 2 CHO Cu OH COOH Cu O H O + + + +
2 2 2
2 ( ) 2 CHO Cu OH COOH Cu O H O + + + +
Fehling Solution Red
iv) Schiffs Test
To a solution organic Violet (or) purple colour (pink) may be aldehyde is
Compound add Schiffs is observed present
Reagent (2-3 drops) and
Shake the contents
v) Iodo form test:
Dissolve the given compound A yellow ppt lodo form may be ketone
(2-3 ml (or) 100 mg) in water is observed
(2-3ml) in a test tube and add
2-3ml NaOH (10%). To this add
A saturated solutaion of iodine-in Kl
with stirring until the dark colour of
iodine persists. Heat the solution in a
boiling water bath for 1-2 minutes.
2
3 3 3
I NaOH NaOH
CH COR Cl COR CHl RCOONa
+
+ Iodo form yellow solid
Test for Carbohydrates:

i).Molischs Test:
Add an alcoholic solution of A violet ring is observed at the may be carbohydrate
o -NaPhthol (10%) to an aqueous junction of two layers
Solution of substance. Then add
Conc
2 4
H So (1ml) carefully along
the sides of the test tube allow to stand
for 2 minutes.

ii).Barfoed Test:
Heat the aqueous solution i) red colour precipitate of Cu2O carbohydrate is present
of the compound (iml) with is formed present
barfoed reagent (1ml) in
boiling water bath for 1-2 minutes

iii).Test with Benedict solution:
Add Benedict solution (2ml) to the
Aqueous solution of organic substance Red ppt is observed Carbohydrate is present
(reducing suguar)

IV). TEST FOR
0 0 0
[1 , 2 , 3 ] AMINES:
1. Carbylamine test:
To the compound add few ml a foul smell is observed may be
0
1 amine
Of chloro form and then add 2 ml
of alcoholic KOH; mix well and gently warmed.
2 3 2 2
3 3 3
Heat
R NH KOH CHCl RNC KCL H O + + + +
2. Azodye Test:
Take 2 ml of compound, add 2 ml orange red dye is formed presence of
0
1 amine
Of HCl, coll in ice, and then add
2 ml of ice cold 10% Aq NaNo2
solution. Add to it cold solution of 0.4 gms
of 2-Naphthol in 4 ml of 5% NaOH solution is added.

EXPERMENT NO.10

Preparation of Aspirin

AIM : To Prepare Aspirin from salicylic Acid

APPARATUS: Conical flask, Water bath, beakers, glass rod

CHEMICALS: Salicylic acid, acetic anhydride, sulphuric acid, alcohol

PROCEDURE:
1. Take 5 gm of salicylic acid in a 100 ml conical flask. To this add about 10 ml of acetic-
anhydride and 1-2 ml of con.H
2
So
4
.
2. 2Shake the contents to 800C, because of exothermic reaction. Maintain the tem at 60-70
0

for about 15 minutes, keeping on a water bath.
3. Allow the solution to come to room temperature and the pour it in 100 ml cold water
taken in a 500 ml beaker with stirring (water is added to destroy the excess acetic
anhydride which gets converted to acetic acid.
4. To induce crystallization scratches the sides of the flask with glass rod.
5. Filter the solid and wash it with cold water. Press it in between the folds of filter paper.
6. Spread the solid on the filter paper to dry
7. To obtain colorless crystals, recrystallization can be done using equal volumes of ethanol
and water solvent system.

RESULT: - Yield=

Precautions:-1 Take acetic anhydride in excess as if acts as acetylating agent as well as
Solvent.
2. Make sure that all the salicylic acid is dissolved.
CHEMICAL EQUATION:




Experiment No.11
KINETICS:

To determine the rate constant of hydrolysis of methyl acetate catalysed by an acid also
the activation energy.

AIM: To determine the rate constant of hydrolysis of methyl acetate catalysed by two different
concentrations of acids.

APPARATUS: - Conical Flask, Beakers, Reagent bottles, Burette, Pipette.

CHEMICALS: - Methyl acetate, Hydrochloric acid (1M, 2M)
Oxalic acid solution (0.2N), NaOH, Phenol phthalein indicator

Preparation of Slandered oxalic acid solution (0.2N)
About 3.15 g of oxalic acid di hydrate is weight accurately and dissolved in small amount of
distilled water and made up to the mark in 250ml of volumetric flask.
1000
2. 250
W
N
E Wt
=
Principle: - The hydrolysis of methyl acetate in presence of an acid may be represented as
3 3
CH COOCH +
2 3
H o CH COOH +
3
CH OH
The rate of reaction is given by
2.303
log(
dx a
dt t a x
| |
=
|

\ .
(First Order)
As acetic acid is producing during the reaction, the reaction may be studied by the titration of
unknown concentration of reaction mixture with a standard alkali at suitable of time.

Standardization of NaOH Solution-
20 ml of Oxalic acid is pipette out into a conical flask and is diluted to 30 ml with distilled water.
To the solution two drops of phenolphthalein indicator is added and then titrated against sodium
hydroxide taken in a burette. The cold point is colorless to pale pink. The experiment is repeated
till concurrent readings are obtained.

PROCEDURE:
From standardized 1N and 2N HCl , p0 ml of IN HCl taken in a iodination flask and 10 ml of
pure methyl acetate is taken a test tube. Both the iodination flask and test tubes are placed in
water bath to bring them into room temperature. Measure exactly 5 ml of methyl acetate and add
to 90 ml 1N HCl in a iodination flask. When exactly half of the amount in the pipette is been
discharged, the stop watch is started. Mixture is shaken well and maintain at a constant
temperature. Now titrated with NaOH solution + using phenolphthalein indicator. The volume of
alkali required for titration is noted and is taken as V
O
. Similarly 10 ml of reaction mixture is
taken out in successive intervals of time 10, 20, 30, 40, 50 minutes. To obtain compute
hydrolysis the reaction mixture kept in a water bath maintained at for about half an hour.

After the hydrolysis completed and it is cooled at room temperature and titrated the 10 ml of
reaction mixture with NaOH solution and is taken as V .
Method of Calculation:-
The initial volume of titrate; NaOH is V
O
at

T
0
0
C is proporsonal to the amount of HCl present
in the reaction mixture at Zero time. When there is an acetic acid present as the hydrolysis
proceeds
0
V V

directly proportional to initial concentration of ester (a), at successive intervals

is proportional the concentration of esters at timet(a-x).

| |
=
|

\ .
1
80C

Same procedure and calculation is repeated for 2N HCl solution.
Relative strength of two acids is given by
2
1
K
K
=
Calculation of Activation Energy:-
2 2 1
1 2
log
2.303
K T T Ea
K R T

.

2 2
1 2 1
10 2.3.3
K T
Ea g R
K T T
=

Result:-Rate Constant for hydrolysis of methyl acetate by 1N HCl are
2
K = ------,
2
K = ----
Activation Energy Ea = -------------------


Observation Table:-
Table-1 Standardization of NaOH:-
Sl.No
Vol of Oxalic acid
(V1M1)
Burette Readings Vol of NaOH (V2)
V2= F-I Initial Final
1 20
2 20
3 20
Vol of Oxalic acid Solution V
1
= 20 ml
Normality of Oxalic Acid N1 = 0.2 N
Vol of NaOH Solution V2 = ---- M1
Normality of NaOH N2= -----N
N
1
V
1
=N
2
V
2

1 1
2
2
NV
N
V
=
Normality of NaOH N
2
= ----------------N


Calculations for determine rate constants
For 1N Hcl
Sl.No Time (t)
Minutes
Vol of
NaOH
(Vt)
t
V V
o

0
t
V V
V V
o
o

0
10
t
V V
g
V V
o
o

0
1
2.303
log
t
V V
K
t V V
o
o

1
2
3
4
5
6
7
8
9
0
10
20
30
40
50
60
Vo











Average K
1
=


0
V ml = GRAPH:
V
o
=
0
V V ml
o
=
From Graph
2 1
__________
2 1
1
2.303
1 2.303
y y
Slope
x x
K
Slope
K Slope

= =

=
=


For 2N HCl:
Sl.No Time (t)
Minutes
Vol of
NaOH
t
V V
o

0
t
V V
V V
o
o

0
10
t
V V
g
V V
o
o

0
2
2.303
log
t
V V
K
t V V
o
o

(Vt)
1
2
3
4
5
6
7
8
9
0
10
20
30
40
50
60
Vo











Average K
2
=
0
V ml = GRAPH:
V
o
=
0
V V ml
o
=
From Graph
2
2
2 1
__________
2 1
2.303
2.303
y y
Slope
x x
K
Slope
K Slope

= =

=
=

EXPERIMENT -12

AIM: - Preparation of Thiokol Rubber
Operators: - Beakers, Glass Rod, Funnel, Filter Paper
Chemicals: - Ethylene Dichloride, Na
2
S
2
(Sodium Ploy Sulphide)

Procedure: -
1. Place about 10 ml. of Ethylene dichloride solution in 100 m). beaker
2. Add about 5 gr. of sodium polysulphide and Heated to form poly sulphide rubber (solid)
3. Wash the above solid with water and dry it in the folds of filter paper
4. Calculate the yield of the product

Result:
The yield of Thiokol Rubber is _______ gr.
CHEMICAL EQUATION:
nCl-CH
2
-CH
2
-Cl + Na
2
S
2

' Poly n
----------
[CH
2
CH
2
-S-S-]
n

(Ethylene Chloride) (Sodium Poly Sulphide) (Poly Sulphide Rubber (or) Thiokol)