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EXPERIMENT: 1
Object: To determine the melting point of organic compounds by melting point
apparatus.
Procedure:
1. Take a small amount of compound in the given capillary tube carefully.
2. Put the capillary into one hole of the apparatus and in another thermometer.
3. Note down the temperature, at which the compound melts.
Chemistry Lab Manual
Results:
Melting point of the given sample = ........................... oC
Precautions:
EXPERIMENT: 2
Object: Sublimation of given organic compound.
Principle: Some solids when heated are converted into vapour without coming
into liquid state and these vapours upon cooling from back the solid. This is called
sublimation.
Heat
Solid vapour
Cool
Fig. Sublimation
This process is used for the purification of solids, which sublime on heating.
Camphor, naphthalene, phthalic acid, succinic acid, benzoic acid and quinones are
generally purified by sublimation under normal pressure. This is called simple
sublimation.
Chemistry Lab Manual
the help of burner. Upon heating the pure compound collects on the wall of glass
funnel; heating is stopped when most of the material in the dish has vaporized.
Reagents: Solid organic compounds (which can sublime).
Apparatus: Porcelain dish, Glass funnel, Sand bath, Tripod stand, Filter paper,
Glass wool
Observations:
Result:
Precaution:
Care must be taken that the heating is adjusted so that the funnel does not become
more than Luke warm.
EXPERIMENT: 3
Object: Crystallization and decolourisation of impure naphthalene.
Principle: Sometimes the crude product of an organic reaction may have
coloured impurity, which may not be removed. These coloured impurities can be
removed by boiling the substance in solution with a little decolourising charcoal
powder. The coloured impurities are adsorbed by charcoal and the pure
decolourised substance crystallized out from the filtrate. As the animal charcoal is
insoluble in all the common solvents it can be employed in the solvent used for
recrystallization.
charcoal.
Apparatus: Two beakers 250 cm3, funnel, funnel stand, tripod stand, water bath,
filter paper.
Result: ...........
Precautions:
1. Handle the chemicals carefully, should not fall on hands.
Experiment 4
Principle:
Chromatography is a method of separating the components of a mixture based on their
differential affinity for two chemicals, one of which is immobilized and the other mobile. As the
mobile phase travels across a layer of stationary phase, it will carry with it components of the
mixture. Those components that interact with the mobile phase but poorly with the stationary
phase will travel with the mobile phase; those that interact poorly with the mobile phase but
strongly with the stationary phase will not travel as quickly. As the mobile phase moves, then, it
carries components of the mixture at different rate , when the mobile phase is stopped, different
components will have travelled different distances. Interactions between the components of the
mixture and the stationary and mobile phases may include charge interactions or interactions
between polar substances, including hydrogen bonding interactions.
For instance, a TLC system can be setup with a very polar stationary phase (silica gel or
alumina) and the solvent mixture acts as the mobile phase. In the ideal solvent system the
compounds of the interest are soluble to different degrees. Separation results from the partition
equilibrium of the components in the mixture. Retention factor, Rf, provides better way to
identify substances. Rf is calculated from the following formula:
7. Leave the TLC plate undisturbed in the beaker for around 40 minutes and allow the solvent
to travel up the plates until it has travelled 85% of the way to the top.
8. Remove the TLC plate carefully and immediately draw a thin pencil line at the solvent front.
9. Allow the chromatogram to dry completely.
10. Draw a circle around the outside edge of each spot. Mark the centre of the spot.
11. Measure the distance from the starting line to the top of the solvent line to obtain the distance
travelled by the solvent.
12. Measure the distance from the starting line to the center of each amino acid spot.
13. Calculate Rf values for methyl orange.
Observation: Distance from the starting line to the solvent line- …….. cm
Distance travelled by the methyl orange dye- ……… cm
Result: The Rf value of methyl orange is-……..
EXPERIMENT: 5
Object: To determine flash point and fire point of the given lubricating oil using Pensky
Marten’s apparatus.
Principle:
Flash point is the lowest temperature at which the lubricating oil gives off enough vapors that
ignite for a moment when tiny flame is brought near it.
Fire point is the lowest temperature at which the vapors of the oil burn continuously for at least
five seconds when a tiny flame is brought near it. Fire point is about 5-20 oC higher than the
flash point (depending upon the nature of oil).
Flash and fire points are used to indicate:
Fire hazard of petroleum products and evaporation loses under high temperature loses
It gives us the idea about the maximum temperature below which the oil can be used
It is used as the means of identification of specific lubricating oil
For detection of contamination in the given lubricating oil
The following three standardized forms of apparatus are available for determining the flash and
fire point: (i) Abels’s flash point apparatus (used for the oil flash point below 120 oF) (ii) Pensky-
Marten’s apparatus (used for the oils flash point above 120 oF) (iii) Cleveland’s open cup
apparatus (used for the oil flash point below 175 oF)
Chemistry Lab Manual
7. Allow to cool the oil for some time, heat again and test the flame for a distinct flash.
Repeat 3-4 times the whole process.
8. Further heat the oil at the rate of 10 oC/ min. and continue applying the test flame as
before.
9. The temperature at which the vapors of the oil give a clear and distinct blue flash for five
seconds is recorded as the fire point of the oil.
EXPERIMENT: 6
Object: To determine cloud and pour point of a given sample of lubricating oil using cloud and
pour point apparatus.
Principle: Cloud point and pour point are important physical properties of any liquid. Cloud
point, as the name suggests is the temperature at which a cloud of wax crystals first appear in a
liquid fuel when it is cooled under special testing conditions. The cloud point of any petroleum
product is an indicator of how well the fuel will perform under cold weather conditions. Pour
point is just the opposite of cloud point as it refers to the lowest temperature at which movement
of oil is observed and the fuel can be pumped easily.
Chemistry Lab Manual
6. The temperature of oil falls on cooling (when cooling bath filled with freezing mixture).
7. Take out the tube after every 1 oC fall in temperature and inspect for a moment. It may
restore if the cloudiness has not formed. This step should be completed in 3 Seconds.
8. For cloud point, note the temperature for hazy appearance.
9. And for pour point, continue the cooling process. After every 3 oC fall, the tube is
withdrawn and tilted to horizontal position for about 5-10 seconds. When oil stops
flowing out of the jar, note the temperature. It is the pour point for the given sample of
lubricating oil.
Result: The cloud point of the given sample is ………..oC and pour point is ……oC.
Precautions:
i. The observation of tube should be completed within 3 to 5 seconds.
ii. According to the pour point of oil, suitable freezing mixture should be chosen.
iii. The test oil should not be disturbed during the process which may delay the
observation.
Chemistry Lab Manual
iv. Temperature of the cooling bath and the jacket should be maintained in equilibrium.
Experiment 7
Procedure:
Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.
Experiment 8
[Fe(CN)5NOCH2-COCH3]2-
Procedure:
Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.
Experiment 9
Molisch’S test:
Fehling’s test:
Chemistry Lab Manual
Procedure:
Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.
3.
Experiment 10
Chemistry Lab Manual
Liebermann’s Test:
Procedure:
Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.
Experiments 11
Ester test:
Procedure:
Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.
Experiment 12
Phenolphthalein test:
Procedure:
Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.
Experiment 13
Chemistry Lab Manual
Procedure
Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.
Experiment 14
Chemistry Lab Manual
Procedure:
Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.
Experiment 15
Chemicals Required:
(i) 8 g Acetanilide
Chemistry Lab Manual
Procedure: Place 8 g acetanilide in a 250 mL round Bottom flask and add to it 8 mL glacial
acetic acid and 16 mL conc. H2SO4. Cool the flask in an ice bath. Meanwhile mix 4 mL each of
conc. HNO3 and H2SO4 in a test tube and cool the mixture. Add this nitrating mixture to the
solution of acetanilide in acid drop by drop with stirring and keeping the temperature below 10
0
C. after complete addition of acids remove the flask from ice bath and allow it to stay for 1 hour.
Then pour the reaction mixture on to 200mL water, containing pieces of crushed ice. When
crude p-nitroacetanilide seperates out, allow it to stay for 15 minutes., filter in a Buchner funnel
with suction, wash with cold water and dry in an oven at 100 0C . Recrystallize from rectified
spirit. 6 g pure yellow crystals of p-nitroacetanilide melting point 2140C is obtained.
Experiment 16
Chemicals Required:
Potassium Iodide= 6 g
Acetone= 2 mL
Procedure:
1. Place 2 mL acetone, 6g potassium iodide and 100 mL of water in a flat bottom flask.
2. To this add slowly 70 mL of 5% NaOCl solution with constant stirring .
3. Idoform separates as yellow crystals. Continuous addition of NaOCl till the precipitate of
iodoform separates.
Chemistry Lab Manual
4. Allow the mixture to stand for 15 minutes & then filter it and dry.
Result:
Weight of the product is ……….. g
Yield of product is ………. %
EXPERIMENT: 17
Object: To determine the viscosity of a given lubricating oil at various temperatures using
Redwood Viscometer No. 1 or No. 2.
Principle: Viscosity is a measure of the internal resistance to the motion of a fluid and is
mainly due to the forces of cohesion between the fluid molecules.
Absolute Viscosity may be defined as “the tangential force per unit area required to maintain
unit velocity gradient between two parallel planes in the fluid at a unit distance apart. It is
denoted by η(eta). Its Unit in CGS system is poise. Poise is equal in one dyne/second/cm 2
(Dimensions of absolute viscosity are ML–1T-1).
The ratio of absolute viscosity to density for any fluid is known as its absolute kinematic
viscosity.
η Absolute viscosity
Absolute kinematic viscosity ν = =
ρ density of the fluid
Viscosity Index: Viscosity generally decreases with increase in temperature. The maintenance of
viscosity over the range of temperature is called the viscosity Index (V.I). A relatively small
change/no change in viscosity with temperature is indicated by high viscosity index whereas low
viscosity index shows relatively large change in viscosity with temperature.
The instrument used for measuring the viscosity is known as viscometers. Different types of
viscometers are: Saybolt Viscometer, Angler’s Viscometer, Ostwald Viscometer, Kinematic
Viscometer, Redwood Viscometer.
Redwood Viscometer: It is of two types
a) Redwood viscometer No.1 b) Redwood viscometer No.2
Both the above viscometers are identical in principle, shape and mode of testing. The essential
differences between the two are:
Redwood viscometer No.1 Redwood viscometer No.2
Dimensions of orifice Length-10mm, Dia-1,62mm Length-50mm, Dia-3.8mm
Kohlrausch flask Smaller mouth Wider mouth
Useful for Low viscous oil having flow Higher viscous oils having
time flow
between 30s-2000s time greater than 2000s
Chemistry Lab Manual
e.g. Kerosine oil and mustard oil e.g. Fuel oil, mobile oil
Procedure:
1. Select the Redwood viscometer according to the nature of oil (RW 1 for light oil and RW2
for heavy oil).
3. Clean the cylindrical oil cup and ensure the orifice tube is free from dirt.
Chemistry Lab Manual
4. Seal the orifice by means of the brass ball and put the receiver (Kohlraush’s flask-50 ml)
below the jet.
5. Fill the bath with water or oil according to the temperature of the experiment.
6. Maintain the desired temperature and stirr the water and oil in bath and cup respectively.
7. At particular temperature lift the ball and simultaneously start the stopwatch.
8. Collect the oil in the 50 ml flask and note the time taken in seconds for the collecting 50
ml of oil.
9. Repeat the whole process at five different temperature and note respective times.
Observations:
S. No. Temperature Time t (sec) Viscosity
(mean)
(oC) Trial 1 Trial 2 Trial 3
Chemistry Lab Manual
Calculations:
The ratio of absolute viscocity to density for any fluid is known as its absolute kinematic
viscocity. Because the instruments used sre of standard dimensions, the kinematic viscocity
of the oil in centistokes can be calculated from the time taken by the oil to flow through the
standard orifice of the instrument with the help of the following equation.
The viscocity of the given oil sample with the help of the redwood viscometer at t oC =
………………Redwood seconds.
B
ν = At –
t
Result: The kinematic viscosity of given oil at different temperatures were determined.
Precautions:
1. The cup and receiver should be properly washed with appropriate solvent.
3. The oil should be filtered thoroughly to remove solid particles that may clog the jet.
4. The receiving flask should be placed in such a manner that the oil stream from jet strikes
the neck of receiving flask and do not cause any foaming.
5. After each reading the oil should be completely drained out of receiving flask.
Chemistry Lab Manual
Experiment 18
Principle:
Phenol-formaldehyde polymers (also called Bakelite) are the oldest synthetic polymers.
These are obtained by the condensation reaction of phenol with formaldehyde in the presence of
either an acid or a base catalyst. In the presence of acid catalyst, the reaction starts with the initial
formation of o-and/or p-hydroxymethylphenol derivatives, which further react with phenol to
form compounds having rings joined to each other through –CH2 groups. The initial product
could be a linear product – Novolac used in paints.
Novolac on heating with formaldehyde undergoes cross linking to form infusible solid
mass called Bakelite. It is used for making combs, phonograph records, electrical switches and
handles of various utensils. The phenol formaldehyde resin (Bakelite) is prepared by
condensation polymerization of phenol with formaldehyde in presence of acidic/alkaline
catalysts.
Chemistry Lab Manual
Chemicals Required:
Phenol= 2 g
Apparatus: Beaker (250 mL), measuring cylinder, glass rod, funnel, filter paper.
Procedure:
1. Place 5 mL of glacial acetic acid and 3 mL of 40% formaldehyde solution in a beaker
and add 2 g of phenol.
2. Add few drops of conc. hydrochloric acid in to the mixture carefully.
3. Within 5 minutes a large mass of pink plastic is formed.
Chemistry Lab Manual
4. The residue obtained is washed several times with distilled water, and filtered.
Result:
Weight of the product is ……….. g
Yield of product is ………. %