Group A

1. Determination of viscosity of lubrication oil by Redwood viscometer no. 1

(At five different temperatures).
2. Determination of percentage of moisture in a coal sample
3. Determination of flash point of a given oil by Abel’s apparatus
4. Determination of flash point of a given oil by Pensky Martin’s apparatus
5. Determination of total solids in a water sample
6. Determination of aniline point of a given oil sample
7. Determination of Drop point of a semi-solid lubricant
8. Determination of acid value of an oil sample
9. Determination of viscosity of lubrication oil by Redwood viscometer no. 2.
(at five different temperatures)
10.Determination of Steam emulsification number (SEN) of a given lubricating oil sample
11. To study the Chemical oscillations (Iodine clock reaction )
12. Potentiometric estimation of Ferrous Ammonium Sulphate using standard Potassium
Dichromate Solution
13. Determination of the partition coefficient of a substance between two immiscible liquids.
14 Synthesis of polymer and nanomaterials
15 Verification of Beer- Lambert’s law by visible spectroscopy

Group B

1 Determination of hardness of water by EDTA method

2 Determination of carbonates, bica
rbonates and total alkalinity of a water sample
3 Determination of chloride content of water
4 Determination of percentage purity of iron alloy by internal indicator method
5 Determination of percentage purity of iron alloy by external indicator method
Course Outcomes: This course will illustrate the principles of chemistry relevant to the
study of science and engineering.The students will learn to Properties,prectical applications,
analysis and determination of engineering materials like

 Lubricants (liquids and semisolid )

 Fuel oil & Coal samples,
 Water in terms of hardness, chloride content and alkalinity
 Polymers
 Application of spectroscopic techniques for

1
 *******************
Exercise No. 1

Aim: To determine the viscosity of given sample of lubricating oil with Redwood
viscometer No.1 and to study the viscosity at various temperatures.

Articles required: Redwood viscometer No.1, Thermometers, Oil sample, 50ml

Measuring cylinder, etc.

Significance of determination: Viscosity is the property of a homogeneous liquid which

causes it to offer frictional resistance to its motion. Viscosity of lubricating oil tells about its
suitability for lubricating purpose.
The function of a lubricant is to reduce the friction between the moving parts and to avoid
the direct metal to metal contact. The moving parts remain apart due to extremely thin
liquid film in between. The frictional resistance therefore, is entirely on account of the
shearing of liquid which is in between the metallic surfaces. The viscosity of fluid measures
the amount of internal resistance of lubricating oil.
The object of this test is to ascertain, whether the lubricating oil is sufficiently viscous to
adhere to the bearings to which it is applied or is so thin that it may be squeezed out of the
bearing due to high pressure & temperature.

Theory: Viscosity is that property of a fluid which is due to the resistance to its flow. It is
expressed in 3 ways.
(a) Absolute dynamic viscosity expressed in C.G.S. unit as poise.
(b) Absolute kinematic viscosity expressed in C.G.S. unit as stoke.
(c) Time taken by the determining instrument in seconds noted by the name of
Instrument (Redwood viscosity).

(a)Absolute dynamic viscosity: It is the tangential force on unit area of either of two
parallel layers at unit distance apart when the space between the planes is filled with the
fluid and one of the planes moves relatively to the other with unit velocity in its own plane.
It is defined as the ratio of the shearing stress to the rate of shearing strain. If force F is
required to keep moving an article of surface area A, in contact with the fluid separated
from a stationary surface by thickness d with velocity v then,

Shearing stress =

Rate of shearing strain =

Absolute viscosity =

When u is in poise then = 1 dyne, = 1 sq.cm. = 1 cm. = 1 cm. per second.

(b) Absolute kinematic viscosity: It is obtained by dividing Dynamic viscosity by density.

The metric units are stoke and centistokes. Thus if ‘p’ is density, then kinematic viscosity
= stoke.

(c) Redwood Viscosity : The timing or the rate of flow of given quantity of liquid from a
given height through a calibrated capillary tube under its own weight may be used as a
means for measuring viscosity and called after the name of the apparatus used for its
2
determination. Thee time in se
seconds required for 50 ml. of oil to gravitate through the
Redwood viscometer at a given temperature is expressed as its viscosity in Redwood
seconds at that temperature.
Absolute dynamic and kinematic viscosities can also be determined from the Redwood
values by means of the following formula.

( )×
Absolute dynamic viscosity =

Kinematic viscosity = =

When A and B are constants known as instrument factors, t is Redwood

Redwood viscosity and p is
the density of fluid. The values of A and B for Redwood viscometer No.1 are as follows:-
follows:
A B
Between 34 – 100 seconds 1.79 0.00260
Above 100 seconds 0.50 0.00247
“Water bath must be filled with water before starting the experiment.

Difference between Redwood No.1 and No. 2:

Redwood viscometer is available in two types, No.1 and No.2. Redwood No.1 and No.2 are
similar in construction and working except that the jet of No.1 has a diameter of 1.62mm
and length 10 mm. whereas
hereas jet of No.2 has a diameter of 3.8mm and length 50mm and
Redwood viscometer No.1 is suitable for oils whose time of flow varies from 30 seconds to
2000 seconds and No.2 is suitable beyond 2000 seconds.

Figure:: Redwood Viscometer No. 1 (L. Section view)

3
 1. The oil cup: is a silvered copper cylinder which has stout stand. A pointer is fitted
inside the oil cup to indicate the level to which the oil is to be filled. The upper end
of the cup is open while the bottom of the cup is concave internally and cup has a
tapering central hole in which the jet (J) is fitted.

2. The jet: constructed of a gate, is provided with a concave depression which can be
covered, or uncovered with a ball valve for stopping or starting the flow of oil.

3. Water bath: is made up of brass and surrounds the oil cup. It is heated electrically,
is provided with a tap for emptying water. Stirring of the bath is affected by means
of cylinder surrounding the oil cup and is provided with 4 vanes.

4. Thermometers :
 Two thermometers to read the temperature of oil and water are provided.
 The apparatus rests on a tripod stand sufficient space for receiving 50 ml.
flanged volumetric flask beneath the jet.

Procedure :

1. Viscometer is cleaned and leveled using circular spirit level and base screws the
tripod.
2. The ball valve is fixed in position in the oil cup & the oil cup filled up to the level
mark with oil.
3. The water bath is than filled with water nearly up to the point of oil level in the cup.
4. The thermometers are inserted in place provided in water bath and oil cup.
5. Now carefully place the 50 ml. measuring cylinder exactly in the centre below the
jet.
6. Keep the oil and water well stirred and note their temperature.
7. When the temperature of oil and water becomes same & steady at room temperature,
raise the ball valve and suspend it from the thermometer bracket & allow the oil to
flow into the measuring cylinder kept below.
8. Simultaneously start a stop watch or look at your wrist watch when the level of oil
flowing into the measuring cylinder reaches the 50 ml. mark, note the time in
seconds elapsed to collect 50 ml of oil.
9. Replace the ball valve in position to seal the jet to prevent overflow of the oil.
10. Transfer the oil into oil cup from measuring cylinder up to the indicator tip of the
cup.
11. Replace properly clean standard measuring cylinder centrally below the jet.
12. The water bath is then heated which in turn heats the oil.
13. When the oil temperature reaches near to the test temperature, stop heating and bring
down temperature of water equal to the temperature of oil by running out some hot
water through the outlet and adding coldwater from the top with continuous stirring.
14. When temperature of both oil as well as water become steady, again collect 50 ml. of
oil and note the time in seconds required.
15. Now repeat the experiment at 5 elevated temperatures. The temperature difference
between the two observations should not be less than 5 °C and not more than 10 °C.
16. The temperature of oil and water should always be same while recording the
observation.
17. Now plot a graph between temperature and time.

4
Observation table for Viscometer No.1

S. Temperature in °C Time for collecting 50ml.

No of oil ( in seconds )
Water Oil

1.
2.
3.
4.
5.

Calculation:

Absolute kinematic viscosity

( )×
=

Where A and B are constants known as instrument factors t Redwood viscosity and P is
the density of fluid.

Result : Redwood viscosity of the given oil at---°C temperature is -----.

The graph between temperature (base) and time (abscissa) in seconds shows that as the
temperature increases the time decreases means viscosity of the oil decreases with the
increase in temperature.

Precautions:
1. Time should be noted carefully for collecting 50mL of oil.
2. Temperature should be steady and constant while taking observations.
3. Difference in the temperature of water bath & oil should not be more than 2°C while
noting time.

**********

5
 Exercise No. 7

Aim: To determine the viscosity of given sample of lubricating oil with Redwood
viscometer No.2 and to study the viscosity at various temperature.

Articles required: Redwood viscometer, thermometers, oil sample, measuring flask 50 ml.

Significance of determination:

Viscosity is the property of a homogeneous liquid which causes it to offer frictional

resistance to its motion. Viscosity of lubricating oil tells about its suitability for lubricating
purpose.
The function of a lubricant is to reduce the friction between the moving parts and to avoid
the direct metal to metal contact. The moving parts remain a part due to extremely thin
liquid film in between. The frictional resistance therefore is entirely on account of the
shearing of liquid which is in between the metallic surfaces. The viscosity of fluid measures
the amount of this internal resistance of lubricating oil.
The object of this test is to ascertain, whether the lubricating oil is sufficiently viscous to
adhere to the bearings to which it is applied or is so thin that it may be squeezed out of the
bearing due to high pressure & temperature.

Theory/ Principle:

Viscosity is that property of a fluid which is due to the resistance to its flow. It is expressed
in 3 ways.
(a) Absolute dynamic viscosity expressed in C.G.S. unit as poise.
(b) Absolute kinematic viscosity expressed in C.G.S. unit as stoke.
(c) Time taken by the determining instrument in seconds noted by the name of instrument
(Redwood viscosity).

(a) Absolute dynamic viscosity :

It is the tangential force on unit area of either of two parallel layers at unit distance apart
when the space between the planes is filled with the fluid and one of the planes moves
relatively to the other with unit velocity in its own plane.
It is defined as the ratio of the shearing stress to the rate of shearing strain. If F is force
required to keep moving an article of surface area A in contact with the fluid separated from
a stationary surface by thickness d with velocity v then

Shearing stress =
Rate of shearing strain =
Absolute viscosity =
When u is in poise then = 1 dyne, = 1 sq.cm. = 1 cm. = 1 cm. per second.

(b) Absolute kinematic viscosity: It is obtained by dividing Dynamic viscosity by

density. The metric units are stoke and centistokes. Thus if is density, then
kinematic viscosity = stoke.

6
 (c) Redwood Viscosity:: The timing or the rate of flow of given quantity of liquid from
a given height through a calibrated capillary tube under its own weigh
weight may be used
as a means for measuring viscosity and called after the name of the apparatus used
for its determination.

The time in seconds required for 50 ml. of oil to gravitate through the jet Redwood
viscometer at a given temperature is expressed as its
its viscosity in Redwo
Redwood seconds at
that temperature.

Absolute dynamic and kinematic viscosities can also be determined from the Redwood
values by means of the following formula:

( )×
Absolute dynamic viscosity u =
Kinematic viscosity = =

Where A and B are constants known as instrument factors, t is Redwood viscosity and is
the density of fluid. The values of A and B for Redwood viscometer
viscometer No.1 are as follows:-
follows:
A B
Between 34 – 100 seconds 1.79 0.00260
Above 100 seconds 0.50 0.00247

“Water bath must be filled with water before

b starting the experiment.”

Figure:: Redwood Viscometer No. 2 (L. Section view)

7
Difference between Redwood No.1 and No.2:

Redwood viscometer is available in two types, No. 1 and No.2. Redwood No.1 and No.2 are
similar in construction and working except that the jet of No.1 has a diameter of 1.62mm
and length 10 mm. whereas jet of No.2 has a diameter of 3.8mm and length 50mm and
Redwood viscometer No.1 is suitable for oils whose time of flow varies from 30 seconds to
2000 seconds and No.2 is suitable beyond 2000 seconds.

The apparatus consists of the following parts.

1. The oil cup is a silvered copper cylinder which has stout stand. A pointer is fitted
inside the oil cup to indicate the level to which the oil is to be filled. The upper end
of the cup is open while the bottom of the cup is concave internally and cup has a
tapering central hole in which the jet (J) is fitted.

2. The jet, constructed of agate is provided with a concave depression which can be
covered, or uncovered with a ball valve for stopping or starting the flow of oil.

3. Water bath is made of brass and surrounds the oil cup. It is heated electrically. It is
provided with a tap for emptying water. Stirring of the bath is affected by means of
cylinder surrounding the oil cup and is provided with 4 vanes.

4. Thermometers :
 Two thermometers to read the temperature of oil and water are provided.
 The apparatus rests on a tripod stand sufficient space for receiving 50 ml. of
measuring cylinder under the jet.

Procedure:

1. Viscometer is cleaned and leveled using circular spirit level and base screws the
tripod
2. The ball valve is fixed in position in the oil cup & the oil cup filled up to the level
mark with oil.
3. The water bath is than filled with water nearly up to the point of oil level in the cup.
The thermometers are inserted in place provided in water bath and oil cup.
4. Now properly place the 50 ml. measuring cylinder exactly in the centre below the
jet.
5. Keep the oil and water well stirred and note their temperature before heating.
6. When the temperature of oil and water becomes same & steady raise the ball valve
and suspend it from the thermometer bracket &allow the oil to flow into the
measuring cylinder kept below.
7. Simultaneously start a stop watch or look at your wrist watch when the level of oil
flowing into the measuring cylinder reaches the 50 ml. mark, note the time in
seconds elapsed to collect the 50 ml oil at room temperature.
8. Replace the ball valve in position to seal the jet to prevent overflow of the oil.
9. Transfer the oil into oil cup from measuring cylinder up to the indicator tip of the
cup.
10. Properly replace clean standard measuring cylinder centrally below jet.
11. The water bath is then heated which in turn heats the oil.

8
 12. When the temperature of oil reaches near to the test temperature stop heating and
brings down the temperature of water equal to it by running out some hot water
through the outlet and adding coldwater from the top while stirring continuously.
13. When temperature of both oil as well as water become steady and constant, again
collect 50 ml. of oil and note the time in seconds required to collect 50 mL of oil.
14. Now repeat the experiment at 5 elevated temperatures. The temperature difference
between the two observations should not be less than 5 °C and more than 10 °C.
15. The temperature of oil and water should always be same, steady and constant while
recording the each observation.
16. Now plot a graph in between temperature and time.

Observation table: for Viscometer No.2

S. Temperature in °C Time in seconds

No for flow of 50ml.
Water Oil of oil
1.
2.

3.
4.
5.

Calculation:

Absolute kinematic viscosity

( )×
=

Where A and B are constants known as instrument factors of Redwood viscosity and P is the
density of fluid.

Result: Redwood viscosity of the given oil at---°C is -------

The graph between temperature (base) and time (abscissa) in seconds shows that as the
temperature increases the time decreases means viscosity of the oil decreases with the
increase in temperature.

Precautions:
1. Time should be noted carefully every time during collection of 50ml. of oil.
2. Temperature should be steady while noting time for flow.
3. Difference in the temperature of water bath & oil should not very even by 1°C while
noting time.

*******************

9
 Exercise No. 2.

Aim : To determine flash point of illuminating or lubricating oil by Abel’s apparatus.

Articles required : Abel’s apparatus, thermometers, oil sample, water and LPG etc..

Definition : Flash point of oil is defined as the minimum temperature at which it gives off
sufficient vapours, which when mixed with air forms an ignitable mixture and gives a
momentary flash of light on the application of a small flame.

Significance of determination : The determination of flash point is of great importance in

case of lubricating and illuminating oils. If the oils are sufficiently volatile at, ordinary
temperatures, the issuing vapors will form an explosive mixture with air and cause fire
hazards. To ensure safety while using oils, certain minimum temperatures are laid down for
illuminating and lubricating purposes, below which it should not give off inflammable
vapors.
The flash point of oil shows the extent of more volatile constituents in the oil. The lower the
flash point the greater is the amount of more volatile constituents.
The flash point is clearly distinguished from fire point, which is the temperature at which
the air space above the oil has sufficient concentration of vapors so that it burns
continuously for about five seconds when brought in contact with the flames.

Part of Apparatus : The Abel’s apparatus is a cylindrical structure consisting of the

following parts :
1. The oil cup : This is a cylindrical vessel, made of brass, open at the top end fitted on the
outside with a flat circular flange. Projecting at right angles, within the cup there is a gauge
consisting of a piece of wire bent upwards and terminating in a point. The oil is filled up to
this point.
2. Cover : This is fitted with a stirrer and thermometer socket made of brass mounted on the
oil cup.
3. Heating Vessel : The heating vessel consists of two flat bottomed cylindrical vessels,
placed coaxially one inside the other and soldered at their tops to a flat copper ring. The
space between the two vessels thus totally enclosed and is used as a water jacket.
In addition to above the working with Abel’s apparatus requires the heating arrangement
and thermometers of appropriate range. It may be heated electrically or with a burner.

Figure: Abel’s Apparatus (L. Section view)

10
Procedure :
1. Fill the oil cup with the oil under test up to the indicator mark. Replace the cover.
2. Fix the oil cup into the apparatus and assemble the paddle stirrer and thermometers
with its bulb dipping into the oil and water at their respective places, provided for in
the apparatus.
3. Fill the water bath with cold water.
4. Close the sliding shutter and light the standard flame and start heating the water bath
with the help of burner.
5. Stir the oil continuously by turning the paddle stirrer. Stirring should be
discontinued only during the introduction of the test flame over the oil surface.
6. At every degree rise of oil temperature open the sliding shutter and introduce the test
flame over the oil surface through the central opening to see whether the oil gives a
flash or not.
7. Record the minimum temperature at which a distinct flash appears as the flash point
of the given oil.
8. Now cool the oil by 5°C and verify the flash point again by every 1°C rise of
temperature.

Observation table No. 1:

S. Temperature (°C ) Observation

No.
1. Room temperature No flash
2.
3.
4.
5.
6.
7.

49
49. Flash
11
 observed

Observation table No. 2: After cooling of 5 °C.

S. Temperature (°C ) Observation

No.
1. No flash
2.
3. 47 Flash observed

1. No flash

3. 47 Flash observed

Result: The flash point of given oil sample is --------- °C

Precautions :
1.
2.
3.
4.
5.

*****************

Exercise No. 6

12
Aim : To determine the flash point of lubricating oil by Pensky Martens apparatus.

Articles required : Pensky Martens apparatus, thermometers, oil sample and LPG etc.

Definition : Flash point of oil is defined as the minimum temperature at which it gives off
sufficient vapors, which when mixed with air forms an ignitable mixture and gives a
momentary flash of light on the application of a small flame.

Significance of determination : The determination of flash point is of great importance in

case of lubricating and illuminating oils. If the oils are sufficiently volatile at ordinary
temperatures, the issuing vapors will form an explosive mixture with air and cause fire
hazards. To ensure safety while using oils, certain minimum temperatures are laid down for
illuminating and lubricating purposes, below which it should not give off inflammable
vapors.
The flash point of oil shows the extent of more volatile constituents in the oil. The lower the
flash point the greater is the amount of more volatile constituents.
The flash point is clearly distinguished from fire point, which is the temperature at which
the air space above the oil has sufficient concentration of vapours so that it burns
continuously for about five seconds when brought in contact with the flames.

Part of Apparatus : The Pensky Martens apparatus consists of the following main parts.

1. The Oil Cup : It is a cylindrical vessel, made of brass with a filling mark grooved
inside near the top. The cup is covered with a lid.

2. Lid : The lid is equipped with the following parts:

(i) Stirrer : The stirring device is carrying two bladed brass propellers mounted
in the centre of the cup.
(ii) Cover Proper : It is made of brass and is provided with four openings one for
thermometer and the rest for the oxygen entry and exposure of vapours to test flame.
(iii) Shutter : It is made of brass and is so shaped and mounted on the lid that when in
one position the holes are completely closed and when in the other these openings are
completely opened so as to test the material for its flash point. It can be worked by
rotating the knob.
(iv) Flame Exposure Device : The lid is provided with a pilot lamp with such a
mechanism that its flame operates simultaneously with the shutter. When the shutter is
in the ‘open’ position the tip of the flame is lowered down
(v) Heating Device : The oil cup is placed in another cup of slightly bigger dimensions.
Air is present between the two cups thus providing an air bath which is heated
electrically.

13
 Figure: Pensky Martens Apparatus (L. Section view)

Procedure :
1. The oil cup and its accessories are cleaned and dried before the test is performed.
2. Fill the oil cup with already dehydrated oil sample to be tested up to the filling mark
(A groove cut inside the oil cup).
cup) Then place
ace the cup in the heating bath.
3. Replace the cover of the oil cup.
4. Insert the thermometer into the thermometer socket, provided on the cover proper.
5. Heat the oil cup from below with burner with constant
constant slow stirring.
6. After every 10°C rise of temperature upto 100 °C and therafter every 5°C rise of
temperature, open the shutter by operating knob and introduce test flame over the oil
surface through the central opening to see whether the oil gives flash
flash or not.
7. When the test flame causes a distinct flash in the interior of the cup, note
temperature which
hich represents the flash point.
8. Place the oil cup in the tray and allow it to cool down by10
by to 15°C C start heating the
sample again and test for the flash
flas point after every 1°CC rise in temperature till flash
observed.
9. Again cooldown the oil cub by 2 to 5 °C then check flash point by every 1°C 1 rise of
temperature till flash observed.
10. Repeat the last step until two consecutive concorrent temperature.

14
 Observation Table No.1 : Every 10 °C rise of temperature.

S.No Temperature (°C ) Observation

.
1. Room temperature No flash
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17. 120 Flash observed

Observation Table No.2 : Every 1°C rise of temperature.

S.No. Temperature (°C ) Observation

1. 115 No flash
2.
3.
4. 118 Flash observed

Observation Table No.3 : Every 1°C rise of temperature.

S.No. Temperature (°C ) Observation

1. 117 No flash
2. 118 Flash observed
3. 117 No flash
4. 118 Flash observed

Result: The flash Point of given oil sample is ……….°C

Precautions :
1.
2.
3.

********************

15
 Exercise No. 3

Aim : Determination of moisture content of coal or coke sample.

Articles required: Clean and dry china dish, chemical balance, hot air oven, pair of tongs,
desiccator weight boxes (major & fractional upto the weight of 10mg ), ridder, forcep,etc.

Coal : It is most import natural solid fuel used for domestic as well as industrial purposes. It
is highly carbonaceous matter containing carbon, hydrogen, nitrogen and oxygen besides
non-combustible inorganic matter.
Quality of coal is ascertained by two types of analyses:

1. Proximate analysis involving determination of :

(a) Moisture
(b) Volatile matter
(c) Ash content and
(d) Fixed carbon

2. Ultimate analysis involving determination of :

(a) Carbon and Hydrogen
(b) Nitrogen
(c) Sulphur and
(d) Ash content

Significance of determination :

(A) Coal samples contain natural moisture and it may increase during
(i) cleaning of coal by gravity or flotation separation
(ii) storage of coal under water to avoid spontaneous ignition causing fire hazards.
Coal are recognised or selected for a particular purpose on the basis of rank or degree of
qualification and transformation from wood to Peat to Lignite toBituminous and finally into
Anthracite. This results in :
1. Increase in carbon content, hardness, calorific value.
2. Decrease in oxygen content, moisture and volatile matter.
Coal with low moisture belongs to a higher rank, possesses higher calorific value and sold /
purchased as a superior grade fuel.

(B) Moisture involves a loss of money paid for it at the rate of coal during purchase and
transportation.

Description :
Chemical balance : It is normally used to weigh accurately to the fourth place of decimal
using a rider.
Air oven : Electrically heated air oven in which temperature can be maintained to the
accuracy of +2°C.
Desiccator : It is a glass container used to dry chemicals or keep them dry. Generally
anhydrous calcium chloride or conc. Sulphuric acid is used as moisture absorbent.

16
Procedure :
Take a clean dried crucible and weigh it accurately to the fourth place of decimal (using a
rider). Now take approximet 1 gm of coal sample in powdered form and weigh again. Using
tongs put the weighed crucible containing coal sample in a desiccator and take the
desiccator to the oven. Transfers the crucible carefully with the help of pair of tongs to the
oven maintained at 115oC and heat the sample for 10 – 15 minutes in the oven. Take out the
crucible containing sample from the oven with tongs and keep it in the desiccator (closed)
for cooling to room temperature for about 2-5 minutes and weigh it to find out the loss of
moisture.

Observation :
1. Weight of the empty crucible = w gm.
2. Weight of the crucible + coal sample = w1 gm.
3. Weight of coal sample taken = (w1 - w) gm.
4. Weight of the crucible + coal = w2 gm. After heating at 115oC.
5. Weight of coal sample after moisture removal = (w2 – w )
6. Loss in weight = (w1 - w ) - (w2 – w )
= (w1 – w2) gm.

Calculation and Result : Percentage of Moisture in the coal sample

(w1 – w2)
= 100 × -------------
(w1 – w)

Conclusion : The moisture content in the sample being

(a) Too high – sample needs drying before use.

(b) Normal – sample can be used as such.
(c) Quite low – sample is very good.

Precautions :
(i) The coal sample should be weighed exactly to the fourth place of decimal.
(ii)The windows of the chemical balance should be kept closed during weighing
operation.
(iii) The crucible should be handled with a pair of tongs.
(iv) The coal sample should be placed in a desiccator for cooling.

*************

17
 Exercise No. 4

Aim : To determine Steam Emulsification Numbers of an oil sample.

Articles required : Thermometers, oil sample, SEN apparatus & LPG.

Definition : The time in seconds elapsed during the separation of 20 mL. of oil from
approximately double of its emulsion with water is reported as steam emulsification
number.

Significance of determination : Certain lubricating oils mix intimately with water and
form emulsion, which then has a tendency to collect dirt, grit particles and other foreign
matters. Thus solid particles are introduced into the lubricated parts and cause abrasion and
wearing out of the machinery.
The tendency of oil to emulsify increases with the time it is used as lubricant. Good
lubricating oil is one which does not form emulsion under lubricating conditions and even if
it forms, it should break off very quickly.
The tendency of emulsion is determined by A.S.T.M. emulsion test. An emulsion of oil and
water is made under standard conditions and then allowed to break. The time in seconds
required for the complete separation of water from emulsion is reported as SEN.
In circulating oiling systems, the high SEN is particularly undesirable because sticky
emulsions and sludge interfere with the circulation of oil. But in certain steam cylinder oils,
the formation of stable emulsion is desirable. In steam turbines, the oils should separate
quickly so that it can be re-circulated for use.
SEN or RE (Rate of emulsion separation) is directly proportional to the emulsification of
tested oil.
To establish a basis for comparison a definite value 100 is assigned to an oil which under
condition of test separates completely from emulsion in one minute. The rate is 33 cc per
second or 20 cc per minute. It was found after experimentation that the results were
pertinent and relative through a wide range of tests. The value assigned is denoted RE or
resistance to emulsion.

The RE of any oil may be found by substituting in following formula

×
RE =

Parts of apparatus:
(i) Steam generator ‘C’ : It is a round bottomed flask heated from below with the
burner.
(ii) Test tube: A 2.5 by 20 cm test tube ‘D’ used as a sample tube graduated (in some)
from zero to 50 ML
(iii) An emulsifying bath ‘B’: It is a glass battery jar of 3 litre capacity.
(iv) Separating Bath ‘F’: It is a glass battery jar of 3 litre capacity.
(v) Delivery Tube ‘D’: Steam from ‘C’ is led into the sample by means of a delivery
tube the other end of which is cut at an angle of 30oC.

18
 Figure:Steam
Figure:Stea Emulsification Apperatus
Procedure:
1. Take approximately 20 ml. of the oil sample in a test tube. Adjust the thread mark on
the test tube up to 40 ml.
2. Place the test tube into the beaker kept in tray (half filled with water).
water)
3. Noww check that steam generator is filled with water (nearly half of its capacity)
capacity).
4. Fill the other beaker 3/4 with water.
5. Now heat this beaker as well as steam generator from below with the help he of burners
separately.
6. perature of water in beaker should be less than 100oC (as soon as some
The temperature
vapours form on the water, stop heating).
heating
7. When a continuous steam is coming out from the delivery tube introduce it is the
test tube containing oil sample (nearly up to the bottom).
bottom)
8. Continue passing steam until the content of the test tube becoms double ( reachs up
to the thread mark).
9. Immediately remove the steam delivery tube and transfer the the test tube
tu into the
beaker (containing hot water) along with the cover.
10. Note down the temperature in seconds required for complete separation of water
and oil as SEN.
11. Now transfer the contents of the test tube into the emulsion bottle kept in the tray.
12. Repeat thiss exercise thrice.

Observation Table:
S.No. SEN
1.
2.
3.
4.
5.

Result: Steam emulsification No. of the given oil is …………..

Precautions:
1. Steaming
teaming rate should be controlled as described.
2. After emulsification the test tube should be transferred rapidly to the separating bath.
*************
19
 Exercise No. 10

Aim : To determine the acid no. of given oil.

Articles required :
Apparatus : Conical flask, Measuring cylinder, Burette, Water Bath,Air Condenser,etc.
Chemicals : Deionized water, Ethanol, oil sample, Phenolphthalein indicator,etc.

Significance of Determination : The value is a measure of the amount of fatty acids, which
have been liberated by hydrolysis from the glycerides due to the action of moisture,
temperature and/or lipase ( lipolytic enzyme) .

Theory/ Principle : The acid value is defined as the number of milligrams of Potassium
hydroxide required to neutralize the free fatty acids present in one gram of fat. It is a
relative measure of rancidity as free fatty acids are normally formed during decomposition
of triglycerides. The value is also expressed as per cent of free fatty acids calculated as oleic
acid, lauric, ricinoleic and palmitic acids. The acid value is determined by directly titrating
the oil/fat in an alcoholic medium against standard alkali solution like potassium
hydroxide/sodium hydroxide solution.

Procedure :
1. Weigh accuretly 5 gms of the cooled oil sample in a 250 mL conical flask.
2. Add 10 mL of distilled water.
3. Add 10 mL of freshly neutralised ethyl alcohol.
4. Add about 1-2 drops of phenolphthalein indicator solution.
5. Heat the mixture for about five minutes in water bath (75-80°C).
6. Titrate carefully while hot against standard alkali solution shaking vigorously till solution
becoms light pink from colorle.

Calculations :
. × ×
Acid value =

Where,
V = Volume in mL of standard potassium hydroxide or sodium hydroxide used.
N = Normality of the alkali solution (potassium hydroxide or Sodium hydroxide solution).
W = Weight in gm of the sample.

Result: Acid no. of given oil is --------------(mg/KOH/g oil)

Precautions:
1. Clamp conical flask proprerly.
2. Keep alcohol and water mixture away from burner.
3. Use water bath for heating.
4. Condenser should fitted tightly.

*************************

20
 Exercise No. 5

Aim : To determine the total solids in water (Dissolved and suspended).

Articles required : Clean and dry china dish, Chemical balance, Hot air oven, Pair of
tongs, Desiccator,etc.

Object and principle : High concentration of dissolved solids in boiler leads to foaming
and priming inside the boiler. Various other difficulties are being encountered in normal and
regular operation of boiler. Removal of solids deposited will necessitate a great number of
boiler blow downs.
The quantitative determination of solids in boiler feed water is very essential. When a
known volume of water sample is evaporated to dryness it gives rise to residue. This residue
constitutes the solids present in the water sample.

Procedure :
Weigh out an evaporating china dish . Take 100 mL of water sample in it. Evaporate water
sample to dryness carefully. When it is almost dried, keep the china dish in an oven at 100-
120oC for 2-5 minutes. See that the residual water is completely removed. Cool the china
dish in a desiccator to room temperature. Find the weight of residue.

Observations :

Volume of water sample = 100 ml.

Weight of empty china dish = x gms.
Weight of residue + china dish = y gms.
Weight of residue = y – x gms.

Calculations : Total solids present in water sample.

= (y - x) gm/100 ml.
= (y - x) x 10 gm/litre
= (y - x) x 10-4 gm/litre
= (y - x) gm/ x 10-4 ppm.

Result : The amount of total solids in the given sample of water is found to be …………
ppm.

*******************

21
 Exercise No. 6

Aim : To determine the Aniline Point of the given oil sample.

Articles required : Graduated test tube, Aniline point apparatus, Thermometer, water bath,
and stirrer, etc.

Definition : Aniline point may be defined as the lowest temperature at which the oil is
completely miscible with an equal volume of aniline.

Significance of Determination : Determination of aniline point of fuel oils is very

informative. If petroleum or mineral fuel oils contain a higher percentage of straight chain
hydrocarbons, it produces a rattling noise in the internal combustion engine called
knocking. This knocking is minimum, if the percentage of branched chain hydrocarbons and
or aromatic hydrocarbons is higher. Determination of aniline point gives information about
the type of hydrocarbon content of the fuel oil.
If, the aniline point is lower, the proportion of aromatic hydrocarbons is higher and the oil
will have less or no tendency of knocking in the engine.Aromatic hydrocarbons present in
lubricants have the tendency to dissolve rubber or synthetic rubber packings, sailings etc;
therefore, aniline point of oil gives indication regarding the deterioration, dissolution of
rubber sealing, packing etc. in contact with lubricating oils. For good lubricating oil the
aromatic hydrocarbon content should be low. The higher the aniline point, the lower is the
percentage of aromatic hydrocarbons in the fuel or lubricating oil and is safer to use in
contact with rubber parts. Aniline point gives valuable information about the presence of
type hydrocarbon in the oil.

Parts of apparatus : The aniline point apparatus consists of;

1.Test tube : It is to hold the sample. It is made of heat resistant glass and is approximately
25mm in diameter and 150mm in length. It is fitted with a cork bored to hold the
thermometer centrally and provided with another hole through which stirrer can operate
freely. This tube is suspended in a jacket, made of similar glass material. The test tube along
with jacket is kept immersed in a heating or cooling bath.
2.The stirrer : It is made of metal or glass rod bent at the bottom into a ring about 15mm
in diameter at right angle to the main axis.
3. The thermometer : is suspended in the test tube through a central hole in the cork.

22
Procedure :
1.Equal volume of pure and anhydrous aniline and oil are taken in the test tube (two layers
are observed).
2.Water bath is heated and test tube containing oil and aniline is placed in it.
3.The contents of test tube are stirred (by up and down motion of stirrer) till a homogenous
solution is obtained.
4. Thermometer is placed in the test tube and temperature is recorded.
5. The test tube is then placed in the cooling jacket of the aniline point apparatus.
6. Initially cloudiness appears in the solution and then two layers are obtained.
7.The temperature at which cloudiness appears is noted.
4. The lowest temperature at which cloudiness appears is reported as aniline point.
5. Procedure is repeated thrice, till two concorrent results are obtained.

Observation :

Volume of oil taken = V ml.

Volume of aniline taken = V ml.
(Equal volume )
Observation Table :

Temperature at which cloudiness

S.No. appears in homogeneous solution (°C)

1
2
3

Lowest value = ………..°C

Result and conclusion : The aniline point of the given lubricating oil is ………°C

1. If the aniline point is low, the percentage of aromatic hydrocarbons is higher and the
oil should not be used in contact with rubber.
2. If the aniline point is higher, the percentage of aromatic hydrocarbons is lower and
oil is suitable for use in contact with rubber.

Precautions :
1. Pure aniline should be used.
3. Stirring should be done by up and down motion of stirrer with care. No part of the
mixture should be allowed to splash out.
4. Aniline point should be recorded with care and experiment should be repeated at
least 2 times for consistency

**********************
23
 Exercise No. 10

Aim: Determination of drop point of a grease sample.

Articles required: Drop point apparatus

apparatus, water bath, semi solid lubricant(
lubricant(grease), and
thermometer,etc.

Determination: Drop
Significance of Determination rop point is the temperature at which the grease passes
from semi-solid
solid state to the liquid state. It determines the upper limit of temperature up to
which grease can function as a satisfactory lubricant.

Parts of apparatus:
It consists of a metal cup having an opening of a standard dimension at the bottom. The T cup
is fitted in a glass jar(boiling tube) with a tightly fitting lid. A thermometer is fixed in the
cup that the bulb of the thermometer is just above the surface
surface of the grease sample under
test. The entire assembly is held in position in a glass beaker containing water which is also
provided with a thermometer & a stirrer.

Drop Point Apparatus

Procedure:
1. Place the grease sample in the cup and insert the thermometer in place.
2. Fix the cup along with thermometer into a boiling tube containing cotton. Now place the
boiling tube into the beaker containing water.
3. Heat the beaker from the below with burner slowly. As the temperature increases the
grease sample melts and the first drop emerges out of the opening at the bottom of the
metal cup.

24
4. Record the temperature at which the first drop falls down. This temperature is noted as
drop point.
5. Now remove the burner.
6. Take out small amount of hot water (20 – 25 ml.) and mix cold water.
7. The temperature of water should fall down by 10 °C.
6. Replace the test tube into the beaker and repeat the experiment 2-3 times, till two similar
readings are

Observation table

S.No. Drop Point (°C)

1
2
3

Result : The drop point of given grease sample is …………. °C

Precautions :
1. Pure aniline should be used.
2. Drop point should be recorded with care and experiment repeated at least 2 times for
consistency.

****************************

25
 Exercise No. 11
SYNTHESIS OF POLYMER AND NANOMATERIALS

PART I

Aim : To prepare Phenol formaldehyde (P-F) resin.

Articles required :
Apparatus : Glass rod, beakers, funnel, measuring cylinder, dropper and filter paper.
Chemicals: Phenol, aq. formaldehyde solution or formalin, glacial acetic acid and conc.HCl,
etc.

Significance of preparation: Bakelite is condensation type of thermosetting polymer. This

polymer is applied in many task of our routine life, few uses of this polymer areas follows-
used for making molded articles such as radio and TV parts, combs, fountain pen , barrels,
phonograph records, decorative laminates, wall coverings, electrical goods such as switches,
plugs etc, for impregnating fabrics ,wood and paper, for bonding glue, for laminated
wooden planks, in varnishes and lacquers. Sulphonated phenol-formaldehyde resins are use
as ion-exchange resins.

Theory/ Principle: Phenol formaldehyde resins (PFs) are condensation polymers and are
obtained by condensing phenol with formaldehyde in the presence of an acidic or alkaline
catalyst. They were first prepared by Baekeland, an American Chemist who gave them the
name as Bakelite.

Thermo sets: The polymers which on heating change irreversibly into hard rigid and
infusible materials are called thermosetting polymers. These polymers are usually prepared
by heating relatively low molecular mass, semi fluid polymers, which becomes infusible
and form an insoluble hard mass on heating. The hardening on heating is due to the
formation of extensive cross-linking between different polymeric chains. This leads to the
formation of a 3-dimnesional network of bonds connecting the polymer chains. Since the
3D network structure is rigid and does not soften on heating, the thermosetting polymers
cannot be reprocessed. Some important examples of thermosetting polymers are Urea-
Formaldehyde resin and Melamine-Formaldehyde resins.

Properties:
1. Phenol- formaldehyde resins having low degree of polymerization are soft. They possess
excellent adhesive properties and are usually used as bonding glue for laminated wooden
planks and in varnishes and lockers.
2. Phenol- formaldehyde resins having high degree of polymerization are hard, rigid,
scratch- resistant and infusible. They are resistant to non-oxidizing acids, salts and many
organic solvents. They can withstand very high temperatures. They act as excellent
electrical insulators also.

Procedure:
1. Place 5mL of glacial acetic acid and 2.5mL of 40 % aq. Formaldehyde (formaline)
solution in a100 mL beaker. Add 2g phenol safely.
2. Wrap the beaker with a wet cloth or place it in a 250mL beaker having small amount of
water in it.
3. Add conc. HCl drop wise with vigorous stirring by a glass rod till a pink colored gummy
mass appears.
26
4. Wash the pink residue several times with to make it free from acid.
5. Filter the product and weigh it after drying in folds of a filter or in an oven. Report the
yield of polymer formed.

Scheme: Bakelite synthesis

Observations:
Weight of empty watch glass = W1 g
Weight of watch glass + polymer formed = W2 g
Weight of polymer formed = W2 – W1 g

Result:
Weight of phenol formaldehyde resin =Wg

Precautions:

1. The reaction is sometimes vigorous and it is better to be a few feet away from the beaker
while adding the H2SO4 and until the reaction is complete.
2. The experiment should be preferably carried out in fume chamber.

************************

27
PART II
Aim: To synthesize silver nanoparticls.

Articles required:
Apparatus: Beaker, measuring cylinder, magnetic stirrer, magnetic bar, etc.
Chemicals: Silver nitrate, sodium borohydride, trisodium citrate and distilled water.

Significance of preparation: Silver nanoparticles are important in the field of medicine as

they show strong antibacterial properties.

Theory/ Principle: Silver can be reduced from Ag+ to Ag0 by various reducing agents. One
of the common reducing agents is sodium borohydride (NaBH4) as it is cheap and easily
available. NaBH4 reduces the silver ions to silver atoms which cluster together to form
nanoparticles. The citrate salt acts as capping agent and stabilizes the silver nanoparticles,
thus preventing their aggregation to larger particles.

Procedure:
1. 15mL of 0.002 M sodium borohydride is taken in a beaker in an ice cold water bath. To
this, 5mL of 0.001 M sodium citrate is added and the mixture is stirred using a magnetic
stirrer.
2. Now add 2mL of 0.001 M AgNO3 solution to the above solution in a drop wise manner.
3. Stir the solutions for 15 minutes.

Result: The formation of a yellow colored solution indicates the presence of formation of
silver nanoparticles.

Precautions:
Perform the reaction in an ice cold water bath as the reduction of silver ions by sodium
borohydride is a fast reaction and can lead to generation of larger particles at higher
temperature.

*****************

28
 Exercise No. 12

Aim : To verify Beer - Lambert’s law by UV -Visible spectroscopy.

Articles required :
Apparatus : Beaker, Measuring cylinders, Volumetric flask and Cuvette,etc.
Chemicals : Distilled water and KMnO4,

Significance of determination: To study the dependence of absorbance on the

concentration and path length and confirm the applicability range. Every absorbing species
has a characteristic λmax value which is determined by this method.

Theory:
Absorption spectroscopy can be used to quantify the absorbing species present in a sample.
The greater the quantity of absorbing species present, greater will be the extent of
absorption of incident light through the solution or gasses. When a beam of monochromatic
light falls on a substance, a part of it is absorbed and the rest is transmitted. The intensity of
the transmitted light is decreased.
According to Lambert's law, decrease in intensity (-dI) is proportional to the thickness of the
medium (dl) and intensity of incident light (I). Beer extended this law for solutions and
gases. In such cases decrease in intensity is also proportional to molar concentration (C).

− ∝ . .
− = . . .
Where, = constant
For a solution, the absorbance of the sample ( ) is given by:

= = . .
Where, = intensity of the incident light,
= intensity of the transmitted light,
= molar absorptivity (characteristic of the absorbing species),
c = molar concentration of the absorbing species in the sample,
= distance that the incident radiation travels through the sample.
= Optical density or Absorbance

Since 'ε′ depends on wavelength of the light and nature of the substance so for a given
substance at a given frequency and in a given photochemical cell.
Beer - Lambert’s law states that when l = constant, O.D. = constant *c. then the plot of
O.D. Vs C will be a straight line through origin.
Absorbance has no units. If 'l' is expressed in cm and ' ' in mol/L, then the unit of ' ' will
be Lmol-1cm.-1.
A linear plot of absorbance versus concentration would verify the Beer-Lambert’s Law.

Procedure:
1. 100 ml stock solution of 0.001 M KMnO4 is to be prepared.
2. Know standard solution of 0.0001 M KMnO4 can be prepared by pipeting out 10 ml of
stock solution into 100 ml standard flask and make up upto the mark with distilled water.
3.Record the visible spectrum of 0.0001 M KMnO4 solution in the wavelength range of 350
nm to 800 nm, at the intervals of every 10 nm to get maximum wavelength i.e., λmax. Note
your results in table 1.
29
4. A plot of Absorbance 'A' vs. wavelength in nm gives λmax.
5. From the standard 0.0001 MKMnO4 solution, Prepare 10ml solutions of each proportion
of KMnO4 solution as given in the table 2.
6. Measure the absorbance ‘A’ at λmax for each of the solutions prepared in Step 5 and then
for the unknown solution of KMnO4 also. Note your results in table 2.
7. Plot a graph between Absorbance on y-axis vs. Concentration on x-axis.

Observations :
Room Temp. -----0C

Observation Table No. 1. Determination of λmax for 0.0001 M KMnO4

S. No. Wavelength(nm) Absorbance (A)

Observation Table No. 2. Absorbance of KMnO4 solutions at λmax (.............nm)

S. No. Volume of 0.0001 M Volume of Concentration of Absorbance (A)

KMnO4 (ml) water (ml) KMnO4 (M)
1 10 0
2 7.5 2.5
3 5 5
4 2.5 7.5
5 1 9
6 X Y

Result :
1. λmax for 0.0001 M KMnO4 solution = ........................nm
2. Concentration of Unknown solution = ....................M
3. Comment on the nature of the graph-

****************

30
 Group B
Exercise No. 1

Aim: Determination of total hardness by EDTA method.

Apparatus: Conical flask, pipette, burette, etc.

Solutions required: known water sample, unknown water sample, Eriochrome black – T
indicator, EDTA solution, Buffer solution at pH 10.

Theory: Hardness of water can be determined by complex metric titration. Ethylene-

diaminetetraacetic acid (EDTA) is a well known complexing agent, which is widely used in
analytical work on account of its powerful complexing action and commercial availability.
The EDTA method is based upon the fact that ethylenediamine tetra-acetic acid (EDTA)
forms remarkably stable complex compounds with all metals particularly with di and
polyvalent metals.
Function of EDTA :- For all practical purposes the hydrated disodium salt of the reagent is
used which has the following formula.

Chemical structure of disodium salt of EDTA

This formula may be abbreviated for the sake of simplicity as Na2H2Y and its dissociation at
pH 10 is written as-
⎯⎯ 2 +

+ ⎯⎯ ( − )

+ ⎯⎯ ( − )

EDTA ion reacts with calcium and magnesium forming stable complexes, the calcium–
EDTA complex is more stable then magnesium EDTA which is being more stable then
magnesium indicator complex.

The relative stability of the complexes so far considered is as follows

− > − > −

31
 Chemical structure of Metal
Metal-EDTA complex

Function of indicator: The indicator Eriochrome black-T

black T is a tribasic acid dye
dye, the
abbreviated formula of which is written as H3In and which dissociates producing different
colored
ed ions at various pH as follows:

Chemical structure of eriochrome black

black-T indicator

⇋ ⇋ ⇋

H2In- HIn2- In3-

Red (below pH 6) Blue (pH 7-11) Orange (above pH 12)

The bivalent blue colored

red indicator ion which exists at about pH 10 reacts wi
with magnesium
producing red colored
red magnesium indicator complex:

HIn-- + Mg+ + MgIn- + H+

Free Indicator (blue) Analyte (colorless) Complex (Wine red)

So, if a drop of indicator is added to hard water sample containing Ca2+ & Mg2+ ions at pH
10, the
he magnesium indicator complex will be formed producing wine red color.colo
Now to this solution, if EDTA is gradually added
added, it will remove calciumm ions first because
EDTA complex is more stable. When all Ca2+ ions are used up, excess EDTA
Ca-EDTA EDTA, if added
will snatch Mg2+ ions from Mg M indicator complex because Mg-EDTA complex is more
stable than Mg-indicator
indicator complex leaving bivalent indicator ion free, whichhich being blue in
color will produce blue coloreded solution. Thus,, a change from red to blue colo
color will indicate
the end point.
+ → +
Wine red Blue

Procedure:
1. Pipette out 20 ml of the known water sample into a 100 ml conical flask.
2. Add
dd 2 ml of the buffer solution and 2 drops of Eriochrome Black Black-T indicator. The
solution becomes wine red.

32
3. Titrate it with EDTA solution from the burette until color changes to clear blue at the end
point. Note the burette reading.
4. Repeat the same process, till you get two concordant readings.
5. Now titrate the unknown water sample in the similar manner till two concordant readings
are obtained.

Observation for known solution:

S.No. Volume of Volume of Total Volume of

Known Solution Intermediate Solution (ml) Intermediate
(ml) Solution (ml)
Initial Final
Reading Reading
1.
2.
3.

Observation for Unknown solution:

S.No. Volume of Volume of Total Volume of

Known Solution Intermediate Solution (ml) Intermediate
(ml) Solution (ml)
Initial Final
Reading Reading
1.
2.
3.

Calculations:

= N1 = Normality of known solution

V1 = Volume of known solution
= N2 = Normality of intermediate solution
V2 = Volume of intermediate solution
= N3 = Normality of alloy solution
V3 = Volume of alloy solution
= V2’ = Volume of intermediate solution with
unknown solution

After knowing the normality of unknown solution (N3), we can convert it into strength by
multiplying it with equivalent weight of CaCO3. Equivalent weight of CaCO3 = 50.

N3 x Equivalent weight of CaCO3 = Strength in g/L of CaCO3 Or Hardness of given water

sample g/L.

N3 x Eq. wt. of CaCO3.x 103 = Hardness of given water sample in ppm or mg\L.

Result: The EDTA hardness of the given water sample is……… ppm.

**********************

33
 Exercise No. 2

Aim: Determination of the carbonate, bicarbonate and total alkalinity of given water sample
by neutralization titration.

Apparatus: Conical flask, Pipette, Burette, etc.

Solution required: N/30 Sodium carbonate solution, hydrochloric acid solution,
Phenolphthalein and Methyl orange indicators.

Theory: The alkalinity of natural water is generally due to the presence of carbonates and
bicarbonates of calcium and magnesium. In industries, hard water is softened by lime soda
process due to which the resulting water contains considerable amount CO3- and OH- which
lead to alkalinity. Highly alkaline water may lead to caustic embrittlement and also may
cause deposition of precipitates and sludge in boiler tubes and pipes.
Depending on the anions that are present in water alkalinity is classified as:-
1. Hydroxides only
2. Carbonates only
3. Bicarbonates only
4. Hydroxides and Carbonates
5. Carbonates and bicarbonates

The possibility of hydroxides and bicarbonates existing together is ruled out because of the
fact that they combine with each other as follows forming carbonates.
+ → +

The type and extent of alkalinity present in a water sample may be conveniently determined
by titrating aliquot of the sample with a standard acid to phenolphthalein end-point, p and
continuing the titration to the methyl orange end-point, m.

The reactions taking place may be represented by the following equations:

+ → (1)
+ → (2)
→ + (3)
The volume of acid run-down up to phenolphthalein end-point (p) corresponds to the
complete neutralization of OH- ions and half neutralization of CO3- ions, while the volume
of acid run after p corresponds to the complete neutralization of HCO3-. The total amount of
acid used from beginning of the experiment corresponds to the total alkalinity present i.e.
those formed from half neutralization of CO32- and those already present in the water
sample.

Procedure:
1. Pipette out 20 mL of the known solution into the conical flask.
2. Now add 2 drops of methyl orange indicator. Titrate the solution against acid solution till
color changes from yellow to pink.
3. Note the volume of acid used.
4. Repeat the same experiment till two concordant readings are obtained.
5. Now pipette out 20 mL of unknown water sample into the conical flask. Add two drops of
phenolphthalein indicator. The solution becomes pink indicating presence of CO32- ions.
6. Titrate the pink solution against acid till solution becomes colorless. Note down the
34
reading of the burette.
7. At this stage add two drops of methyl orange indicator to the same solution. Titrate the
solution against acid till solution becomes pink. Note the burette reading.
8. Repeat the experiment till two concordant readings are obtained.

Observation for known solution:

S.No. Volume of Volume of Total Volume of

Known Solution Intermediate Solution (ml) Intermediate
(ml) Solution (ml)
Initial Final
Reading Reading
1. 20 0.0
2. 20 0.0
3. 20 0.0

Observation for Unknown solution:

S.No. Volume of
unknown Volume of Intermediate Solution (ml)
Solution
(ml)
Initial Final p Initial Final m
Reading Reading Reading Reading
1 0.0
2 0.0
3 0.0

Calculation:

= N1 = Normality of known solution

V1 = Volume of known solution
= N2 = Normality of intermediate solution
V2 = Volume of intermediate solution

Phenolphthalein Titration:

× = × N2 = Normality of intermediate solution

× p = Volume of intermediate solution with
= phenolphthalein indicator
Np = Normality of unknown solution (p)
V3 = Volume of unknown solution

Methyl Orange Titration:

× = × N2 = Normality of intermediate solution

× m = Volume of intermediate solution with
= methyl orange indicator
Nm = Normality of unknown solution (m)
V3 = Volume of unknown solution

35
After knowing the normality of unknown solution (Np, Nm), we can convert it into strength
by multiplying it with equivalent weight of CaCO3.

Phenolphthalein alkalinity, P (in ppm) = Np x eq. weight of CaCO3 x 103

Methyl orange alkalinity, M = Nm x eq. weight of CaCO3 x 103

Result:

Total alkalinity (T) = P+M

Carbonate alkalinity = 2P

Bicarbonate alkalinity = T – 2P

36
 Exercise No. 3

Aim: Determination of the chloride present in given water sample by precipitation titration

Articles required:
Apparatus: Burette, Measuring cylinder, Beaker, Dropper and Stirrer
Chemicals: Potassium chromate indicator and Silver nitrate solution (0.0141 N)

Significance of determination: Chlorides in reasonable concentrations are not harmful to

human. At concentrations above 250 mg/L, they can damage plants when used for
gardening/irrigation and give a salty taste to water, which is objectionable to many people.

Theory/ Principle: (Mohr’s Method)

This method determines the chloride ion concentration of a solution by titration with silver
nitrate. As the silver nitrate solution is slowly added, a precipitate of silver chloride forms.

Ag+ (aq) + Cl-(aq) → AgCl (s)

The end point of the titration occurs when all the chloride ions are precipitated. Then
additional silver ions react with the chromate ions of the indicator, potassium chromate, to
form a red-brown precipitate of silver chromate.

2Ag+ (aq) + CrO42- → Ag2CrO4 (s)

This method can be used to determine the chloride ion concentration of water samples from
many sources such as seawater, stream water, river water and estuary water. The pH of the
sample solutions should be between 6.5 and 10. If the solutions are acidic, the gravimetric
method or Volhard’s method should be used.
The end point of titration cannot be detected visually unless an indicator capable of
demonstrating the presence of excess Ag+ is present. The indicator normally used is
potassium chromate, which supplies chromate ions. As the concentration of Cl- ions
becomes exhausted, the silver ion concentration increases and a reddish brown precipitate
of silver chromate is formed.

2Ag+ + CrO42- → Ag2CrO4 (reddish brown precipitate)

This is taken as evidence that all chloride has been precipitated. Since an excess Ag+ is
needed to produce a visible amount of Ag2CrO4, the indicator error is subtracted from all
titrations. The indicator error or blank varies somewhat with the ability of individuals to
detect a noticeable color change. The usual range is 0.2 to 0.4 mL of titrant.

Procedure:
1. Take 50 mL of the sample in a beaker and add 5 drops (about 1 mL) of potassium
chromate indicator to it.
2. Add standard (0.0141 N) silver nitrate solution to the sample from a burette, a few drops
at a time, with constant stirring until the first permanent reddish color appears. This can be
determined by comparison with distilled water blank. Record the volume of silver nitrate
used.
3. If more than 7 or 8 mL of silver nitrate solution is required, the entire procedure should
be repeated using a smaller sample diluted to 50 ml with distilled water.

37
Observation for Unknown solution:

S.No. Volume of Volume of Total Volume of

Known Solution silver nitrate solution(ml) Silver nitrate
(ml) solution (ml)
Initial Final
Reading Reading
1.
2.
3.

Calculations:
Chloride, Cl- (mg/L)

= (mL of AgNO3used - "error" or "blank") x Multiplying Factor (M.F.)

Where,

Result: The concentration of chloride ion in the the given water sample is……… mg/L.

38
 Exercise No.4

Aim: To determine percentage purity of Iron alloy by internal indicator method.

Apparatus: Conical flask, Pipette, Burette, etc.

Solutions required: N/40 ferrous ammonium sulphate solution, diphenylamine as an
internal indicator, potassium dichromate solution, a mixture of H2SO4 & H3PO4, alloy
solution (concentration 4 g/L).

Theory:
K2Cr2O7 contains oxygen available for oxidation which it loses in presence of a substance
capable for receiving it, and in presence of an excess of sulphuric or hydrochloric acid. Thus
a ferrous salt in an acidified solution is readily oxidized to ferric salt by the addition of a
solution of potassium dichromate.

FeSO4 (NH4)2SO4.6H2O → FeSO4 + (NH4)2SO4 + 6H2O

6FeSO4 + K2Cr2O7 + 7H2SO4 → 3Fe2(SO4)3 + Cr2(SO4)3 + K2SO4 + 7H2O

At the beginning of titration there are only ferrous ions, as the titration proceeds these ions
are converted into ferric ions. At the end point all the ferrous ions are converted into ferric
ions. Gram equivalent weight of the K2Cr2O7 used upto the end point will correspond to the
gram equivalent of ferrous ions present in the solution of alloy.

The end point of the reaction can be detected using diphenylamine as an indicator, 1%
solution of diphenylamine in concentrated sulphuric acid is used for the titration of iron (II)
with potassium dichromate solution. Diphenylamine is first as oxidized in to biphenyl
benzidine (colorless) which is the real indicator. It is reversibly oxidized to its quinonoid
form (violet color). As it shows different colors in reduced & oxidized form, it acts as a
redox indicator.

39
During the titration, oxidation of two species takes place. The first one is the oxidation of
ferrous into ferric ions and another one is the oxidation of diphenylamine into
diphenylbenzidine.
The oxidation potential of the two systems is given by the Nernst’s equation:

[ .]
= + ln
[ .]

And the formal potential of system:

→ is 0.68 V.

Similarly, formal potential of indicator system is 0.76 V. The system having low oxidation
potential will oxidize first. Due to oxidation of Fe2+ into Fe3+, concentration of Fe3+
increases. It results in the increase in the potential of the system. If the potential of the
system exceeds 0.76 V, it results in the oxidation of indicator even before the actual end
point. So phosphoric acid is added to reduce the formal potential of ferrous-ferric ion
system.
Excess of Fe3+ ions are removed by phosphoric acid which forms stable green colored
complex with Fe3+:
H3PO4 + Fe3+ → (FeHPO4)+ + 2H+
Green Colored Complex

Due to the formation of this complex the potential of the system remain below 0.76 V till
the end point. At end point, one drop of K2Cr2O7 will oxidize the indicator and color of the
solution changes to blue violet.

Procedure:
1. Pipette out 20 ml of the known solution into the conical flask. Add about 2 ml of acid
mixture and 2 drops of diphenylamine indicator into it.
2. Now titrate it against K2Cr2O7 solution till solution becomes blue. Note down the reading
and repeat the experiment for two concordant observations.
3. Similarly, repeat the experiment with unknown alloy solution.

Observation for known solution:

S.No. Volume of Volume of Total Volume of

Known Solution K2Cr2O7 Solution K2Cr2O7 Solution
(ml) (ml) used (ml)
Initial Final
Reading Reading
1. 20 0.0
2. 20
3. 20

40
Observation for unknown solution:

S.No. Volume of Volume of Total Volume of

Known Solution K2Cr2O7 Solution K2Cr2O7 Solution
(ml) (ml) used (ml)
Initial Final
Reading Reading
1. 20 0.0
2. 20
3. 20

Calculations:

= N1 = Normality of known solution

V1 = Volume of known solution
= N2 = Normality of intermediate solution
V2 = Volume of intermediate solution
= N3 = Normality of alloy solution
V3 = Volume of alloy solution
= V2’ = Volume of intermediate solution with
alloy solution

Strength in g/L = Normality x equivalent weight of Iron

% of Iron in given alloy solution = Strength in g/L x 55.8 x 100/4

Result: The percentage of iron in the given alloy sample is……….

41
 Exercise No.5

Aim: To determine percentage purity of iron alloy by external indicator method.

Apparatus: Conical flask, Pipette, Burette, etc.

Solutions required: N/40 ferrous ammonium sulphate solution, potassium ferricyanide as
an external indicator, potassium dichromate solution, dilute H2SO4 solution, alloy solution
(concentration 4 g/L).

Theory: K2Cr2O7 contains oxygen available for oxidation which it loses in presence of a
substance capable for receiving it, and in presence of an excess of sulphuric or hydrochloric
acid. Thus a ferrous salt in an acidified solution is readily oxidized to ferric salt by the
addition of a solution of potassium dichromate.

FeSO4 (NH4)2SO4.6H2O → FeSO4 + (NH4)2SO4 + 6H2O

6FeSO4 + K2Cr2O7 + 7H2SO4 → 3Fe2(SO4)3 + Cr2(SO4)3 + K2SO4 + 7H2O

At the beginning of titration there are only ferrous ions, as the titration proceeds these ions
are converted into ferric ions. At the end point all the ferrous ions are converted into ferric
ions. Gram equivalent weight of the K2Cr2O7 used up to the end point will correspond to the
gram equivalent of ferrous ions present in the solution of alloy.
Conversion of whole of the ferrous ion to ferric ion is determined by using potassium
ferricyanide as an external indicator. Ferrous ions but not ferric ions give a blue precipitate
with this indicator. The dichromate solution is accordingly added to acidified iron solution,
until a drop of the liquid ceases to give a blue coloration when it is brought into the contact
of a drop of potassium ferricyanide solution placed on a glazed white tile.
The formation of blue precipitates occurs due to the following reaction:

K3[Fe3+(CN)6] + Fe2+SO4 → KFe2+[Fe3+(CN)6] + K2SO4

Potassium ferro-ferricyanide
(Prussian blue)

Procedure:
1. Five separate drops of the potassium ferricyanide indicator are placed on a clean and dry
white glazed tile in an orderly row.
2. Pipette out 20 ml of known solution into the conical flask and acidify it by adding dilute
acid (about half test tube).
3. Fill the burette with intermediate K2Cr2O7 solution with the help of funnel. Remove
funnel from top and the air bubble, if any, from the nozzle of the burette.
4. Now add 5 ml of the dichromate solution in the acidified known solution from a burette
with constant stirring.
5. Withdraw a drop of this solution with a glass rod and mix it with one of the drops of
indicator solution on the tile. If a blue color or precipitate is seen, an additional 5 ml of
dichromate solution should be added from the burette and tested again, and so on, adding
the dichromate solution in volumes of 5 ml at a time until only a greenish yellow color is
seen on the tile.
In this way the end point is ‘bracketed’ first within the limit of 5 ml . Suppose the end point
is found to be between 15 ml and 20 ml.
6. Now, fresh 20 ml of known solution is taken, acidified and then 15 ml of K2Cr2O7
42
solution is added directly without testing. The end point is tested by adding 1 ml of
intermediate solution, every time and so on, until a new ‘bracket’ of one ml is found. Let it
be 16-17 ml.
7. A third volume of known solution is taken, acidified and 16 ml of dichromate solution is
added to conical flask directly. The end point is tested by adding 0.1 ml of intermediate at a
time until the disappearance of the blue color on the tile is obtained. The last result is
checked by the fourth volume of the known solution.
8. The unknown alloy solution is now, titrated with a standard dichromate solution by
repeating the above steps.

Observation for known solution:

S.No Volume of Volume of Total Volume of Color observed

. Known Solution K2Cr2O7 Solution K2Cr2O7 Solution
(ml) (ml) used (ml)
Initial Final
Reading Reading
1 20 0.0 5.0 5.0 Blue
2 10.0 10.0 Blue
3 15.0 15.0 Blue
4 20.0 20.0 Greenish yellow
1 20 0.0 15.0 15.0 Blue
2 16.0 16.0 Blue
3 17.0 17.0 Greenish yellow
1 20 0.0 16.1 16.1 Blue
2 16.2 16.2 Blue
3 16.3 16.3 Greenish yellow
1 20 0.0 16.1 16.1 Blue
2 16.2 16.2 Blue
3 16.3 16.3 Greenish yellow

Observation for unknown solution:

S.No Volume of Volume of Total Volume of Color observed

. Known Solution K2Cr2O7 Solution K2Cr2O7 Solution
(ml) (ml) used (ml)
Initial Final
Reading Reading
1 20 0.0 5.0 5.0 Blue
2 10.0 10.0 Blue
3 15.0 15.0 Greenish
yellow
1 20 0.0 10.0 10.0 Blue
2 11.0 11.0 Blue
3 12.0 12.0 Greenish
yellow
1 20 0.0 11.1 11.1 Blue
2 11.2 11.2 Greenish
yellow
1 20 0.0 11.1 11.1 Blue
2 11.2 11.2 Greenish
43
 yellow

Calculations:

= N1 = Normality of known solution

V1 = Volume of known solution
= N2 = Normality of intermediate solution
V2 = Volume of intermediate solution
= N3 = Normality of alloy solution
V3 = Volume of alloy solution
= V2’ = Volume of intermediate solution with
alloy solution

Strength in g/L = Normality x equivalent weight of Iron

% of Iron in given alloy solution = Strength in g/L x 55.8 x 100/4

Result: The percentage of iron in the given alloy sample is……….

44
 Exercise No. 12

Aim: To study the Chemical oscillations of Iodine clock reaction.

Articles required:
(a) Apparatus: Beakers, Graduated cylinder, and Stir plate or stir bar
(b) Chemicals: H2O2, KIO3, H2SO4, MnSO4·H2O, Malonic acid, Soluble starch, and
Deionized water.
Significance: Study of oscillatory reaction completed. Demonstration of two reactions which
can switch back and forth in which the product of one reaction will be the reactant for the
other.

Theory/ Principle:
Briggs-Rauscher Reaction –It is Oscillation time (switch time) in which solution turns
from yellow to blue color as per following reactions.

IO3ˉ+ 2 H2O2 + CH2(CO2H)2 + H+ = ICH(CO2H)2 + 2 O2 + 3 H2O

The BR reaction can be summarized by two chemical reactions:

IO3ˉ + 2 H2O2 + H+= HOI + 2 O2 + 2 H2O -----> (A)

HOI + CH2(CO2H)2 = ICH(CO2H)2 + H2O -----> (B)

When the reaction begins, the solution becomes yellow a I-( generated from reaction of HOI
with H2O2, not shown) reacts with HOI under acidic conditions to produce I2. The solution
suddenly changes to dark blue as a buildup of Iˉ reacts with I2 in the presence of starch to
generate the pentaiodide ion (I5ˉ) which is encased in the amylose present in solution. The
reaction proceeds by consuming I2 at a rate greater than it is being produced thus removing
the presence of I5ˉand increasing the concentration of Iˉ(colorless). The oscillations
continue until malonic acid or IO3ˉis completely consumed.

Solution Prepration

1. Solution A: Prepare 100 mL by diluting 30 mL of 30% H2O2 with 70 mL of deionized

H2O.
2. Solution B: Prepare solution by adding 10 mL of 1.0 M H2SO4 to 80 mL of deionized
water. Dissolve 4.3 g KIO3 in this solution and dilute to 100 mL.
3. Solution C: Prepare starch solution by dissolving 0.1 g of soluble starch in 90 mL of
boiling deionized water. When cool, add 1.5 g malonic acid, 0.4 g MnSO4·H2O, stir and
dilute to 100 mL.

Procedure:

Add 50 mL of 9.0 % H2O2 Solution to a clean beaker fitted with a stir bar. Then add 50 mL
of an acidified 0.2 M KIO3 Solution, mix thoroughly then add 50 mL of 0.9 % Starch and
stir it. Upon addition of the final solution, bubbles should appear. Initially solution turns
45
yellow then blue and finally colorless. This reaction will oscillate for 5-10 minutes.Take
atleast 10 observations

Observations:
Room Temp. -----°C

Observation Table-

S. No. Oscillation time (minutes) Average Oscillation

(Yellow to Blue color switch time) Time(minutes)
1
2
3

Oscillation time (Yellow to Blue color switch time) ----------------minutes

Result:

The three colors observed are a result of an increase in the concentrations of I2 (yellow),
starch-iodine complex (blue), and Iˉ (colorless) in order of appearance during the
demonstrat and demonstrated in Lab.

Precautions:

1. Wear proper protective equipment including gloves and safety glasses when preparing
and performing this demonstration. Concentrated hydrogen peroxide can cause burns. KIO3
is an oxidizer. Sulfuric acid is severely, corrosive to eyes, skin and other tissue. Malonic
acid solution is moderately toxic and corrosive to eyes, skin and respiratory tract. The
reaction produces iodine which is toxic by inhalation and irritating to eyes, skin, and
respiratory tract.
2. Perform the demonstration in a well-ventilated room.
3. Disposal of final solution should be in an appropriate aqueous waste container.

Exercise No. 13

Aim: To determine the amount of ferrous ammonium sulphate (FAS) present in the given
solution using standard K2Cr2O7

Articles required:

Apparatus: potentiometer (pH meter) measuring cylinder. Beakers, Burette.etc

46
Chemicals: Ferrous Ammonium Sulphate, Potassium Dichromate, H2SO4, Deionized water.

Principle: The titrations involving the determination of end point of redox system by the
measurement of e.m.f. of the cell are called potentiometric titrations. In the case of
oxidation-reduction titration of FAS using standard dichromate solution, a standard calomel
electrode (SCE) is used as the reference electrode, whose E0 remains constant.

→ +
From Nernst’s equation we have:

[ ]
= + ln
[ ]

As the oxidation of Fe2+ progress, ΔE value increases slowly in the beginning and then
sharply changes near the equivalence point.

Procedure:

1. Pipette out exactly 25 mL of given FAS solution in a clean 100 mL beaker and add 1
test tube full of dil. H2SO4 to maintain acidic media.

2. Rinse the standard calomel electrode and bright platinum electrode assembly of pH
meter with ion exchange water and immerse them in the reaction mixture. Connect
the electrode assembly to the (in mV mode). Switch on the potentiometer and record
the potential.

3. Add standard K2Cr2O7 from the burette in 0.5mL quantity at a time and stir the
solution using a glass rod for uniform mixing. Record the potential value (E) after
each addition of K2Cr2O7.

4. Continue the procedure till the potential increases more rapidly near the equivalence
point. Once equivalence is past there will be only a slight increase in the potential
for the successive addition of K2Cr2O7 solution.

5. Plot a graph of ΔE/ ΔV values (along y-axis) versus volume of K2Cr2O7 (along x-
axis). From the graph find out the volume of K2Cr2O7 solution required for complete
oxidation (peak value of sharp curve). Finally, calculate the normality of FAS and
amount of ion present in the given solution.

Calculations: Calculate the amount of present in the given solution using following
formula

Where,

47
N1 = Normality of K2Cr2O7 solution (given)
V1 = Volume of K2Cr2O7 used
(cm3 of K2Cr2O7 solution corresponding to the equivalence point from graph)

V2 = Volume of FAS solution

N2 = Normality of FAS solution

Then

Weight of ferrous ammonium sulphate present in one liter of its solution

= N2 x equivalent weight of FAS
= N2 x 392.14 g/L

Volume of K2Cr2O7 EMF in mV ΔE ΔE/ΔV

0.0
0.5
1.0
1.5

Result:
1. The volume of K2Cr2O7 solution corresponding to the equivalence point =
……………….. mL
2) Normality of given FAS solution (N2) = ………………. mL
3) Amount of FAS present in litre =…………… g/L

Precautions

48
 Exercise No. 14

Aim: (i) To determine the distribution coefficient of iodine between CCl4 and water at room
temperature.
(ii) To find the equilibrium constant of above distribution.
(iii) To find the concentration of given KI solution.

Articles required:

Apparatus: Stoppered bottles, mechanical shaker, separating funnel, conical flask, beaker
and titration tiles etc.
Chemicals: Iodine, KI, CCl4, sodium thiosulphate solution (hypo), starch and distilled
water,

Theory/ Principle: According to Nernst distribution law, when a solute distributes

between two immiscible solvents in contact with each other, there exists, for similar
molecular species, at a given temperature, a constant ration of distribution between the two
solvents irrespective of the total amount of the solute and any other molecular species which
may be present. In other words,

C1/C2 = KD

Where KD is termed as the distribution coefficient, and, the terms C1 and C2 refer to the
concentrations of similar molecular species in the two liquids at a constant temperature.
Here we are considering a system of distribution of iodine between aqueous and CCl4 layer
in the presence of KI in aqueous layer. Equilibrium between KI and I2 will be attained in the
aqueous layer. The equilibrium attained is

KI + I2 → KI3ˉ

The equilibrium constant

Kequ. = [KI3ˉ]/ [KI]·[I2]

Procedure:

1. Serially labelled three bottles are taken and mixtures are made in each bottle as
follows:

Bottle No. Contents

I 20 ml of I2 in CCl4 + 40 ml of water
II 20 ml of I2 in CCl4 + 40 ml of known KI
III 20 ml of I2 in CCl4 + 40 ml of unknown KI

2. These bottles are stoppered well and shaken in a mechanical shaker for about an hour.
49
After shaking, they are set aside for about 20 minutes in a water trough so that it will attain
equilibrium.

3. Exactly 2 ml of the CCl4 layer from bottle I is pipetted out into a conical flask and
approximately 20 ml of distilled water is added this biphasic solution is titrated against
previously standardized thio solution using starch as indicator. The end point is the
disappearance of blue color.

4. The experiments are repeated to get concordant values.

5. From bottle I, about 10 ml of the aqueous layer is pipetted out and the amount of I2 is
estimated as done with CCl4 layer. The above procedure is repeated for bottles II and III.

Observations:
Room Temp. -----°C
Observation Table No. (1)

Bottle No. Volume of Volume of Thio used by Burette Concordant

CCl4 Value (ml)
layer(ml)
Initial Final Difference
2.0
I 2.0
2.0
II 2.0
2.0
III 2.0
Bottle No. Volume of Volume of Thio used by Burette Concordant
water Initial Final Difference Value (ml)
layer(ml)
10.0
I 10.0
10.0
II 10.0
10.0
III 10.0

Observation Table No. (2)

Strength
Bottle No Layer Volume of Thio (ml) of Iodine KD = C1/C2
CCl4
I Aqueous

50
 CCl4
II Aqueous
CCl4
III Aqueous

Result:
(i) The distribution coefficient of iodine between CCl4 and water is found to be _________
(ii) The equilibrium constant, Keq, for above equilibrium is found to be ____M-1.
(iii) The concentration of given KI solution is found to be _________ M.

Precautions: Wear proper protective equipment including gloves and safety glasses when
preparing and performing this demonstration. Iodine is corrosive to eyes, skin and other
tissue. The reaction uses CCl4which is toxic by inhalation.

51
 Group A

1. Determination of viscosity of lubrication oil by Redwood viscometer no. 1

(At five different temperatures).
2. Determination of percentage of moisture in a coal sample
3. Determination of flash point of a given oil by Abel’s apparatus
4. Determination of flash point of a given oil by Pensky Martin’s apparatus
5. Determination of total solids in a water sample
6. Determination of aniline point of a given oil sample
7. Determination of Drop point of a semi-solid lubricant
8. Determination of acid value of an oil sample
9. Determination of viscosity of lubrication oil by Redwood viscometer no. 2.
(at five different temperatures)
10.Determination of Steam emulsification number (SEN) of a given lubricating oil sample
11. To study the Chemical oscillations (Iodine clock reaction )
12. Potentiometric estimation of Ferrous Ammonium Sulphate using standard Potassium
Dichromate Solution
13. Determination of the partition coefficient of a substance between two immiscible liquids.
14 Synthesis of polymer and nanomaterials
15 Verification of Beer- Lambert’s law by visible spectroscopy

52
 Group B

1 Determination of hardness of water by EDTA method

2 Determination of carbonates, bicarbonates and total alkalinity of a water sample
3 Determination of chloride content of water
4 Determination of percentage purity of iron alloy by internal indicator method
5 Determination of percentage purity of iron alloy by external indicator method

Course Outcomes: This course will illustrate the principles of chemistry relevant to the
study of science and engineering.The students will learn to Properties,prectical applications,
analysis and determination of engineering materials like

 Lubricants (liquids and semisolid )

 Fuel oil & Coal samples,
 Water in terms of hardness, chloride content and alkalinity
 Polymers
 Application of spectroscopic techniques for

53