EXPERIMENT

Determine the viscosity of the given liquid and calculate t s

3.1 rheochor value.

. Theory: Viscosity is the resistance to flow of the liquid due to friction between the moving layers of the
liquid. Viscosity is thus defined as the force or internal frietion which opposes the displacement of different
another.
layers relative to one
The SI unit for absolute viscosity is the Pascal-sec. A more commonly used unit is the cgs unit poise (P) which
is a dyne-s/cm (10 kg m s).
Rheochor Value: According to Newton Friend if molecular volume of the liquid is multiplied by the
root of the coefficient of viscosity, a constant is obtained which is called Rheochor Value.
eighth
Mathematically, Rheochor value,
R =M/D xn* where M is molecular mass and D is density n is coefficient of
Hence Rheochor value is defined as the molecular volume of the liquid at the temperature at which
viscosity.
its viscosity is unity. Rheochor is both additive and constitutive property.
The viscosity of the liquids is measured by comparing the rate of flow of the fixed volume of the liquids
tube. The instrument used is called Ostwald's Viscometer. The viscosity is
caleulated as:
through a capillary

1P1t
2 P22
Here n1and 2 are the viscosities of standard liquid(water) and liquid under examination. pi and pare
the density of water and test liquid.
Rheochor is calculated as:
Rheochor value, R = M/Dxn
Where M is molecular mass and D is density n is coefficient of viscosity.
and beakers, etc.
Apparatus: Viscometer, stop watch, specific gravity bottle, pipette
Procedure
1. Wash the viscometer with chromic acid solution, distilled water and finally with acetone/ether. Dry it by

keeping it in oven or using up to room temperature.

hot air blower. Cool the viscometer
water is suflicient to fill the bend of tube and
2. Fill the viscometer with distilled water in such way that
more than half of the lower bulb B1
3. Allow the viscometer to stand for 10-15 minutes to attain the room temperature.
with pinch cork to the upper end of the limb of the
viscometer having
4. Now attach a rubber tubing
capillary tube.
5. Suck the water until it rises 2-3 cm above the mark A on the viscometer by using the rubber tubing.
tube into lower bulbB, and
6. Keep the stop ready. Allow water to flow back through capillary watch when the
watch
determine the time required to pass between points A and D. Start
the stop liquid passes
mark A and stop the watch when it touches the mark D.
The reading should not differ by
7. Repeat this procedure 2-3 times and take the mean of the measurements.
0.2% more than the mean values.
of flow for the
it with hot air bower. Measure the time
.
Clean the viscometer with acetone or ether and dry
liquid under examination as described above.
9. Determine the density of water and liquid under examination at room temperature.
10.Record your observations in tabular form.
11.Calculate the viscosity and rheochor values using the formulas.
X n1
Viscosity of the given liquid
=
n2
P1t1
and liquid.
the density of water
are the viscosities of water and liquid. p1 and pz are
a n d n2
eochor value, R = M/Dxn where M is molecular mass and D is density n is coeficient of viscosity.
 OBSERVATIONS AND CALCULATIONS

= 30"C
Room temperature

Molar mass
Viscosity (n) Rheochor
Liquids
Time of flow t Density R M/D x8
(seconds) (D) (M) g mol

1 2 3Mean
water
2012122
Liquid
A)
Mass of empty specific gravity bottle Xg
Mass of specific gravity bottle + water yg
Mass of water (y-x)gmg
0.995646. 10° kg m
Density of water m/vg cm°=z =
Mass ofspecific gravity bottle +given liquid
=
Lg
Mass of the liquid L-x) g
Mass of the liquid x Density of water
Specific gravity of the liquid =
Mass of water

Specific gravity of the liauid

- x )x Density of water
Mass of water
P2tzX n1
Viscosity of the given liquid = n2 P1t1

Parachor of the given liquid = M/D x

Friedrich Wilhelm Ostwald (September 2, 1853-April 4, 1932)

was Russian-German physical chemist. He moved to Germany in
1887 to take the chair of physical chemistry at Leipzig in 1887.
With Jacobus H. van't Hoff in 1887 he founded the Zeitschrift für
physikalische Chemie, which became for many years the most
important journal in the field. In 1888 he discovered Ostwald's law
of dilution of an electrolyte. He gave the first modern definition of a
catalyst in 1894 and was awarded the Nobel Prize in 1909 for his
work on catalysis. His process for the conversion of ammonia
to
nitric acid proved of great industrial importance. He is
one of the founders of the field of
regarded as
physical chemistry.
He was a
great teacher and built up an
important research school at Leipzig
through which most major chemists passed at some time in
career.
their

Ostwald probably did more than

anyone else to
chemistry. He was a great teacher anaDult up an important establish the new discipline of physica
most major chemists passed at research school at Leipzig
some time in
their career. He translated through whic
phvsical chemist Josiah Willard the writings of the American
GiDDS nto German in 1892, and also
volume textbook on the subject, Lenrpuen
Chemistry).
aer
algemeinen Chemie (1885,produced an inspiring two
1887: Textbook of Genera
 EXPERIMENT
Determine the heat of solution of ethanol in water
S4.3
solution. Heat of
Theorv: Heat is
absorbed or evolved on addition of the solute to solvent to form the
absorbed or evolved when one gram moleçule of a solute is dissolved in the large
is defined as heat
solution
evcess of the that further dilution produces no heat change in the system. Heat is evolved when
solvent such
ethanol is added to water.
Calorimeter with stirrer, decimal thermometer, balance, NaOH,
Apparatus and Chemicals:
pipette, etc.
HCL, beakers, and
Procedure:
Take a clean and dry calorimeter and weigh it along with lid and stirrer and put it in outer jacket.
1.
thermometer in the calorimeter through the hole as shown
2. 100 mL of distilled water and fix a
Take
in the figure.
Note the temperatureT1 of the distilled water.
Add 5 mL of ethanol to the calorimeter at once and cover the lid and start stop watch simultaneously.
after each 30 seconds.
Stirrer the solution and note the temperature of the solution
and time along x-axis of a graph.
Plot the temperature changes along y-axis
record observations in tabular form.
Determine the rise in temperature from the graph and

OBSERATIONS AND CALCULATIONS

Sr. No Time in| Temperature Sr. No Time in Sec. Temperature

Sec. change change

Thermometer
Stirrer
Temperature of solution
after mixing
Wooden Lid

Temperature -Copper Calorimeter

change
Temperature of solution
before mixing (starting time)
Woede Cover

15 30 45 60 5 90
Time in seconds

Figure: Graph between Time and temperature changes Calorimeter

Mass of the calorimeter + stirrer+ Lid Ci8

Mass of the calorimeter + stirrer+ Lid+ water - C8
- C8
Mass of the calorimeter +stirrer+ Lid+ water + C,H,0H
Mass of water -(C C ) g
Mass of water CH,OH -(C - C)g-XK
Mass of solution - (C C)g

29
 tC
Initial temperature
of water t c
solution from the graph =(T2 -T)'C=0
Rise of temperature of
= S1 (for copper = 0.091
Rise of temperature
the calorimeter = S2 (1 for simplicity)
Specific heat of
Specific heat of the solution = 46 g per mol
Molar mass of C2H,OH = Xg
Mass of C,H,OH
these values in equation
By substituting (m1 S1+ m2 S2) x 4. 184 kJ
Heat of Solution =
t0 x
1000 x W
kJ per mol
Result: Heat of solution of ethanol:..

EXPERIMENT
Determine the transition point of NazSO4.10 H,0 by
4.4 thermometric meter method

Substance coexist in
Theory: The temperature at which two crystalline forms of the same crystaline
equilibrium with each other is called transition temperature. Below or above this temperature only one
crystalline form exists. Measurement of transition temperature is based on the fact that each form of matter
is associated with certain amount of energy. For example, a substance, A, changes to B on heating ta
transition temperature, then B must have higher energy content than A. If B is allowed to cool uniformly,
cooling is interrupted at transition temperature due to release of heat from B. Transition temperature can
be deduced from cooling curve.
Apparatus: Thermometer, beaker, large glass tube, cork, stirrer, iron stand etc.
Procedure:
1. Take about 40 mg of hydrated sodium sulphate
(Na,SO4. 10H,0) in a test tube and place it into a Thermometer ()
bigger test tube which serve as outer jacket. Fix
the tube with the help of iron stand.
2. Insert a thermometer and stirrer in the small tube
Stirrers
by mean of a two holes cork in such a way that
stirrer reaches the salt for stirring and bulb of the
thermometer completely dip in the salt.
3. Suspend this apparatus in beaker congaing water.
4. Note the initial temperature and start
heating
water with constant stirring the salt and water.
(A Test Tube(A
magnetic stirrer may be used for this purpose.)
5. Note the temperature after each minute.
6. Salt will be iquefied Air Jacket
Continue heating slowly and
partially on
heating.
uniformly
stirring the water until temperature becomes with Sodium Sulphate
steady (This is transition temperature).
7. Note time and this
temperature. Continue heating
and record temperature rise with
8. Now remove the burner and temperature.
allow the sodium
sulphate to cool. Keep
stirring and record the
on
fall of
temperature with time Temperature
becomes constant for a while
transition temperature. again. This is
9. Note the time for which it
10 Plot the remains constant.
temperature changes against Figure 4.2:
time and
caleulate the
Determination of transition temp ture

transition temperature.
 EXPERIMENT
of hydrolysis of ethyl by NaOH
acetate

6.2
constant
Determine the rate sponification of eth
constant for
at 25° C or determine the velocity
acetate.

reaction and rate equation

is given
is second order
Theory:Saponificationof ethyl acetate,
by equation CH,COONa +C2H,OH
CH,COOCHs +NaOH
k[CH,COOC,Hs][OH ] =k{ester][OH]
Rate of reaction dt
rate constant is calculated by
When the concentration of ester and NaOH are different,

using the equation given below.

b(a - x)
2.303
k=
t(a b) a(b-x
ethyl acetate respectively in the reaction mixture
where a and b stand for initial concentration of NaOH and
and xis the change in the concentration of ethyl acetateattime
The reaction is monitered by taking the definite volume of reaction mixture at regular intervals and titrating
volumes of the standard HCI
mixture immediately against standard solution of HCI. if V,, V, Vo are the
solution required to neutralize OH in the aliquot at the beginning, at time t and at the end of the raction,
then V a; V.-VtoXand, V-V» o b. Hence
(a-x)=V.(V.-V) =V
(b-) (V-V.H V.-V) =V-V.
(a-b)= V,(V,-V)=V»
Substituting these values in the above equation, Second order equation can be written. The rate equation can
be written as:
2.303
k = 1V(VV)
log
tVoo Vo(V,-V.)
Apparatus and chemicals:
Two conical flasks, pipettes, thermostat, beakers, burette, stand, HCI, methyl acetate and 0.1M
NaOH, phenolphthalein.

Procedure:
1. 200 mL of approximately 0.020M ethyl
acetate solution and 200 mL of 0.030M
NaOH solution were taken in the separate
flasks and placed in the thermostat at 25 °C
for an hour to attain the thermal1
(V-VoV-(V-V)
equilibrium. Log
2. 100 mL of ethyl acetate solution and 100 (V-V)(V-V)
mL of NaOH solution were mixed and
stirred well.
3. 10 mL of the reaction mixture was
transferred to a conical flask and
titrated 15 30 45 60 75 90 105 120
against standard HCI using
phenolphthalein.
This volume Time in minutes
Corresponds to Vo
The same
procedure was repeated to get six readings.
4. Aftertaking six readings, the reaction mixture was placed in water bath at
60 °C for two hour.
 mixture was transferred to a conical
flask
10 mLL of the reaction
reaction mixture was cooled;
5. The the value of Vo.
the standard solution to get
and titrated against line
6. The graph was plotted log va vst. Which is a straight
acetate in water at25 °C is calculated.
Sponification of ethyl
Rate of Bimolecular

off reaction mixture titrated each time

=
1Ocm
Volume = 10cm
HCI solution
Volume of standard used against reaction
=

Volume of standard HCI solution

V mL
mL
LogVeVo-Vo
V mL
Vol VV)
(Voo9 VV oc) |k Mean k
No V
Time(s) 1og Yo) (VoNO_ dm'molr's dm'mor's

9.3.
12:5
15 3
i6
16 2

Result:Rate constant,k: -- dm'mol's

EXPERIMENT
Determine the relative strength of HCl and H2SO4 by kinetic
6 . 3 method.
Theory: Relative strength of acid is given by the equation:
Relative strength of acids k/k =

Apparatus and chemicals: Two conical flasks, pipettes, thermostat, beakers, burette, stand,
HCL, methyl acetate and0.1M NaOH,phenolphthalein.
Procedure:
1. Standard solution of NaOH (0.1M) was prepared.
2. 50.0 mL of 0.1M HCI and methyl acetate were taken in separate conical flasks and placed in

thermostat at 25 °C and let the flasks to attain the temperature of 25 °C.

3. 5.0 mL of methyl ester was introduced into acid and time was noted. Flask was shaken at once and 5.0
mL reaction mixture was withdrawn and transferred to a beaker containing clean ice to stop the
reaction.
ce cooled solution was titrated against standard (0.1M) NaOH solution using phenolphthalein as
indicator
n sreadingat (V) correspond to the initial concentration of HCl before the beginning of hydrolysis.
.
Again 5.0 mL reaction mixture was transferred to a flask
containing clean crushed ice and titrated
against the same solution of NaOH. Similar titrations were performed after 15, 45, and 75 minutes.
The
volume of NaOH consumed at different times
corresponded to V
ADOut 20 mL reaction mixture was taken in a conical flask, stoppered lightly and placed in a water
Dath at about 70 °C for
3 hours. The flak cooled to 25°C and 5.0 mL reaction mixture was titrated1
against the same NaOH solution. This
8. Similar gave the value of Va
procedure was repeated with H2SO4
 EXPERIMENT
MT 8.3 Determine the rate constant for the inversion of
the presence of hydrochloric acid by
using
cane

polarimeter.
sugar in

Principle: The rate of the reaction depends upon the concentrations of sucrose and water and also upon
the concentration of H+, which acts as a catalyst. The concentration of water may be regarded as a constant
since a large excess is normally present. Under a fixed H concentration the reaction is thus 1st order with
respect to sucrose. Cane sugar solution is dextro- rotatory and invert sugar is levo-rotatory. Inversion of cane
sugar is accompanied by the change of rotation sign from right (+) to the left (-). The concentration of cane
sugar at any time during inversion is proportional to the difference between the angle of rotation at that time
and the angle of rotation at the end of reaction. Hence the progress of the reaction can be
monitored by
polarimetry.
Chemical Equation:
Ci2H201 H,O CHO+ CH120%
Glucose Fructose
Chemicals and Apparatus: Polarimeter, thermometer, beaker, measuring flasks, thermostat, sodium
lamp. sugar, 0.9 HCi
Procedure:
l. Sodium lamp was switched on 1 hour before starting the experiment.
. 20 cane sugar solution was prepared and one drop of thymol blue was added to it to preserve the
solution.
3. 100.0 mL can sugar solution and 100.0 mL 4M HCI solutions were taken in conical flasks, Stoppard
and placed in thermostat to attain the temperature of the thermostat.
4. Zero reading was noted by taking distilled water in the Polarimeter tube.
5. Two solutions were mixed stirred well. The solution was taken in the polarimeter tube and the angle
of rotation was noted.
6. Subsequent readings were taken after 3, 6, 10, 15, 20, 30, 40, 60 minutes.
7. The final reading was noted after 24 hours.

Measurenent of Angle of rotation by polarimeter

Switch on the sodiun lamp one hour before taking the measurenent. Wash the polarimeter tube
thoroughl. Fill it with distilled water and place it in the polarimeter jacket and close it. Rotate the scale of
the polarimeter clockwise or anticlockwise so that the two side bands are darker than the central one. 1f
the scale is moved little more at this stage, the position is reversed, i.e., sides bands become brighter than the
central. Here fir the scale with the screw

OBSERVATIONS AND CALCULATIONS

Let A initial angle of rotation,
At angle at any time 1 and
Au the angle after complete inversion occurred.
s the initial concentration of cane sugar (C,) is proportional to the total range of
g eLe (As- Au) and the concentration (C) at time t is proportional to the total range
of change i.e., (A-Au).
For the 1st order reaction,
K (2.303) log

where C initial concentration

concentration at time t and
velocity constant
 log(At- Aa) K = 2.303)
Scale reading
Rotation in (At-Aa) t log
Time in in degrees
degrees (A)
minutes

12 0 60
0.25
5O
20OL
2.
Co AAo
Result: Value of k from graphh=
C At - Ax

2.0

00

-0.2

S0.4

-0.6
0
50 100 150
Time minutes

Figure: ln[succrose vs time

Result: Value of k from graph=

Questions for viva voce

Q.What is Polarimeter?
Ans: A Polarimeter is instrument used to measure
an
passing polarized light through an optically active substance. the angle of rotation caused Dy
Q. What is meant by
optical activity of a substance?
Ans: Ability of a substance to
rotate the plain
through the solution of the substance, is called polarized light to left or right, when sed

Q.What polarization of light?

is optical activity. light is
pass
Ans: Polarization describes the physical
cannot orientation of the
see
polarization directly. electromagnetic field in space. eyes
Q.What is Specifie rotation?
Ans: Specific rotation of
chemical
a
rotation
and a sample
a
plane-polarized ight iscompound
when
passed
[al is defined as
through the observed
angle or
concentration ofI gram per cm.
length of l dect r
a
sample with a path
TaN-
o OOo
 Slope 1/K2

X/m

Intercept = 1/kjk2

0.3M 0.4M 0.5M

0.1M 0.2M
Concentration Ce

between and Ce is a straight line, therefore,

0.5M solution of acetic acid valid..
the
Result: The plot /m
Langmuir adsorption isotherm.

EXPERIMENT) the adsorption of

Verify Freundlich isotherm by considering
RP 2 acetic acid from aqueous media by using activated Charcoal.

Principle: The Freundlich equation or Freundlich adsorption isotherm is an adsorption isotherm, which is
a curve relating the concentration of a solute on the surface of an adsorbent, to the concentration of the solute
in the liquid with which it is in contact. In 1909, Freundlich gave an empirical expression representing the
isothermal variation of Adsorption of a quantity of gas adsorbed by unit mass of solid adsorbent with
pressure. This equation is known as Freundlich Adsorption Isotherm or Freundlich Adsorption equation.
The simplified Freundlich Adsorption equation is given below.
X 1
logloga +logc
m n
Here x is the quantity of the solute adsorbed, mis the quantity of the adsorbent, a is the specific heat which
depends on the nature of adsorbent, c is the equilibrium concentration of the adsorbate and n is constant and
its value depends on the nature of adsorbate. A straight line is obtained when log x/m is plotted against log C.
The isotherm is empirical and found to be valid in the low pressure
concentration) is raised departure from the equation is found. (concentration) range. As pressure (or
Apparatus and Chemicals: Standard Oxalic acid solution (0.1 M), NaOH
Activated charcoal, Phenolphthalein solution, CH,COOH solutios,
indicator, Reagent Bottles (5 each), Burette (50 cm), Pipette (10 cmb
Conical flask (250 cm, 100 cm), filter
papers.
Procedure:
1. Standardize NaOH against standard Oxalic
acid (0.1M) solution and then with
Standardized NaOH. Standardize CHCo
2. Take five
clean and dry stoppered reagent bottles and
3. Take 0.5M acetic acid and numbered them as 1, 2,3, 4, and S.
distilled water in these bottles
as
given below.
Bottles Bottle 1 Bottle5
0.5M acetic acid in cm 50
Bottle 2 Bottle 3 Bottle 4 10
Water 40
30 20
Initial conc. of acetic acid 10
20 30
0.5M 0.1M

4.
0.4M 0.3M 0.2M
Take out 5 cm°
This is the blank
of the solution and titrate it
titration. against 0.1M NaOH using i n d i c a t o r .

phenolphtnae
 wsp
Plot of
EA/cl Absotbance va

No Conc. Concety.
KMnO4
0.01M

0.02M

0.03M
me
0.04M
Onst
0.05M

0.06M d i s t r n

0.07M
0.08M
Unknown Concentration
0.09M Ap
0.1M
funne

Unknown
7
pro
Result: Concentration of KMnO,from graph:.
value of the e is constant for KMn04. Hence
plot of A vs concentration is straight line and
As the
the Beer-Lamberd's law is verified.

Precautions:
1. Solutions should be absolutely clear.
2. No air bubble should be present in the polarimeter tube.
3. Both ends of the polarimeter must be clean.
4. Polarimeter tubemust be rinsed 2-3 times with the solution to be measured each time.

EXPERIMENT
Verification of Beer-Lamberd's law and determination of
3B unknown concentration of K;Cr;07 solution
colorimeterically
Est

Please see experiment 7.1 at p.45 of this Mannua

EXPERIMENT
Determination of distribution coefficient of
4 H,O and CCl4 1, between
2 N S2O3 t ->
Na2
Principle: When a substance is partially solubleSy
in
Oc + 2Na
dissolved in two solvents on each of the two
immisicible s, it is
The adding
distribution ratio or partition to the mixture of
two immisccible solvc a
ay.
coefficient (D) equal to the solvent in a speci
he
organic phase divided by its is
concentration of a so the
concentration in the aqueous the
phase. Depending on the systo the
 distribution ratio can be a function of temperature, the concentration of chemical species in the
system, and a large number of other parameters.

Concentration of solute in organic layer

D:
Concentration of solute in water

It means that the ratio of concentration ration of solute in organic solvent and water is constant at
constant temperature irrespective of the amount of the solute dissolved. This is called
distribution ratio or partition coefficient (D).

Apparatus and Chemicals: Burette pipette, titration flasks, reagent bottles and separately
funnel, lodine and CCl4

Procedure:
1. Saturated solution of iodine was prepared in carbon tetrachloride.
2. Three reagent bottles (250 cm ) were filled as follows:

Bottle No Saturated I, solution in CCl4 Pure CCl4 Water

0.0 cm 100 cm
1 40cm
II 30 cm 10.0 cm 100 cm
III 20 cm 20.0 cm IO0 cm

flask shaker or by
3. All bottles were stoppered and shaken vigorously for 45minutes on a
hand.
4. Mixture in bottles was layers in all bottles.
allowed to separate into two
were separated by separatory funnel.
5. Organic layer and aqueous layers of each bottle
6. 10.0cH-efaqHeoustayer-from each-botte wastitrated-agaimst 6-8HFNazSz03

Estimation of I, in Aqueous layer

the iodine titration flask and 10.0 mL distilled
1. 10.0cm' iodine solution was taken in
water was added to it.
0.01M NazS203.5H20 solution taken in the
2. lodine solution was titrated with standard
burette until appearance of lemon yellow colour.
was added to the flask when
lemon yellow
3. Icm freshly prepared starch solution
titrated until end point.
colour appeared. This solution was again
4. Initial and final burette readings were noted.
initial burette reading from final burette
5. Volume used was found by subtracting
the concordant readings.
reading. Experiment was repeated thrice get were titrated.
to
6. Similarly Ih solutions from bottle-II and bottle-III
1omL disti
waas
addedded
Estimation of I2 in CCl, layer w COTer

taken in titration flask andl titrated

against
7. 1Ocm CCl4 layer of I2 solution was
Then
standard 0.01M NagS2O3.5H20 solution as described above.
 Observations and Calculations

C
Room Temperature

Titration with CCl4 laver

with aq. layer .R Vol
Titration
I.R F.R Vol. of Volume I.R
fina
Vol. of
of of I2 inti r e a d i nNaS :
Bottle Volume
I2 solution
NazS203 solutionead S,0
0,
No used
taken taken
1
2 2
II
2 301 21 2
302122

Molarity of iodine solution

M =?
Volume of iodine solution VI 0.0 cm
n =1
No. of moles of iodine
Molarity of NazS203.5H20
= M =0.01M
a ssumE)
Volume of Na2S2035H20 V2 =10 cm =

No. of moles of NazS20,5H20 = n2 2

Substituting these values in molarity equation,

M,V MV2(sodium thiosulphate)

n1 n2

M.
M2V2n1 0.01 x 10.0 x1= 0.005M
M1 2 xA0
nVi
Similarly determine molarity of iodine in CCl4is caleulated

Bottle Conc. oflh Conc. of Molarity of Iz in CCl4

No in CCl D =
in H2OO Molarity of I2 in H20

II
III
Result: The distribution ratio or
partition coefficient (D) = - -