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Chemistry Lab Manual

EXPERIMENT: 1
Object: To determine the melting point of organic compounds by melting point
apparatus.

Principle: The melting point of a substance is the range of temperature at which


the solid phase changes to liquid completely. Pure substances melt sharply at a
fixed temperature while impurities always lower the melting point.

Fig. 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

Reagents: Solid organic compound.


Apparatus: Melting point apparatus, Capillary tubes, thermometer.
Observations:
Temperature at which the compound starts melting =

Temperature at which the compound gets completely melt =

Results:
Melting point of the given sample = ........................... oC

Precautions:

1. Be careful while handling capillary tube.


Chemistry Lab Manual

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

Fig. Experimental Representation of Sublimation


Substances which have low vapour pressure at their melting points can only
be sublimed under reduced pressures. This is called sublimation under reduced
pressure or vacuum sublimation.
Procedure:
The impure substance (1 g) is taken in a porcelain dish kept in a sand bath
placed on a tripod stand. The dish is covered with a filter paper, which has been
perforated with a number of small holes, made in upward direction. An inverted
glass funnel, with a plug of glass wool in the stem is placed over the filter paper.
The stem of funnel is wrapped with wet filter paper. The dish is slowly heated with
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.

Reagents: Naphthalene mixed with Congo red, ethanol, activated animal


Chemistry Lab Manual

charcoal.

Apparatus: Two beakers 250 cm3, funnel, funnel stand, tripod stand, water bath,
filter paper.

Procedure: Take 1 gm impure sample of naphthalene (mixed with Congo red) in


a beaker and add about 0.05 – 0.06 g of activated animal charcoal to it. Add
minimum quantity of ethanol sufficient to dissolve it and heat the beaker on water
bath for about 10 minutes. Filter the mixture while hot. Collect the filtrate in a
clean beaker. Allow the filtrate to cool by keeping the beaker in cold water. Keep it
for some time (30 minutes) for crystallization. Filter the colourless crystals and dry
them.

Result: ...........
Precautions:
1. Handle the chemicals carefully, should not fall on hands.

2. Keep your face away while taking charcoal.


Chemistry Lab Manual

Experiment 4

Object: Determine the Rf value of methyl orange in Thin Layer Chromatograpy.

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:

Rf = distance travelled by the susbstances from the origin


distance moved by the solvent from the origin
Reagents: silica gel G, methyl orange, methanol, ethyl acetate.
Apparatus: Glass plates, beakers, filter paper, spotting capillaries, for solutions, rulers.
Procedure:
1. Prepare slurry of silica gel G in a beaker and spread it over clean and dry glass plates and
dry it for 5-10minutes.
2. Prepare solution of methyl orange in methanol.
3. Apply the sample over silica gel plate using capillary tube. Allow the plate to dry.
4. Add enough solvent to the bottom of a large beaker so that the entire bottom edge of the
TLC plate will be stirring in solvent (about 1cm in the bottom).
5. The solvent in your beaker can not be above the starting line on your TLC plate. Place a
piece of filter paper along the side of the jar and wet with solvent.
6. Place the TLC plate in the beaker, sample side down. Cover with watch glass.
Chemistry Lab Manual

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

Fig. Pensky Marten’s Apparatus


Pensky-Marten’s apparatus is most commonly used and is a type of closed cup consisting of
following parts:
a) Oil Cup: Material- Brass and is of a standard size having a mark upto which the oil has to be
taken. Lid of the cup is provided with four openings of standard sizes, first opening is for stirrer,
second is for admission of air, third is for thermometer and fourth is for introducing test flame.
b) Heating jacket: The oil is surrounded by a heating jacket containing water/oil. The assembly
is heated in a controlled manner by keeping it on an electrical heater.
c) Shutter: At the top of the cup shutter is provided. By moving the shutter, opening in the lid
opens and flame is dipped in to this opening, bringing the flame over the oil surface. As the test
flame is introduced in the opening, it get extinguished, but when the test flame is returned to its
original position, it is automatically lightened by the pilot burner
Reagents: Given lubricating oil
Apparatus: Pensky-Marten’s flash and fire point apparatus, match box, thermometer, filter
paper
Procedure:
1. Clean and dry all parts of the apparatus to remove any traces of solvent.
2. Fill the oil cup with the test oil up to the mark.
3. Now cover the lid and insert the thermometer, stirrer and flame exposure device
carefully.
4. Heat the apparatus homogenously in a manner that the temperature of oil increases by 5
to 60 oC per minute with continuous stirring.
5. When the temperature is within the range of anticipated flash point, the test flame is
dipped into the oil vapor for about 2 seconds at every degree rise of temperature.
6. Record the flash point at the temperature at which a flash appears in the form of weak
sound and light. This temperature is known as the flash point of that sample.
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.

Results: The flash point of given oil sample = ……….oC.


The fire point of given oil sample = ………oC.
Precautions:
1. The apparatus should be thoroughly dried. There should be no trace of moisture inside
the cup.
2. The thermometer bulb should dip into the oil.
3. Stirring and heating should be stopped at the time of the application of test flame.
4. Fill the sample of the lubricating oil up to the mark. There should be no oil on the outer
part of the cup.
5. Preheating over the surface of the oil should be avoided.

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

Fig. Cloud and pour point apparatus


The cloud point and pour point apparatus consists of the following parts:
i) Test tube: it is made of glass having flat bottom and standard dimensions.
ii) Cooling bath: It consists of an insulated jacket of glass or copper containing cooling
mixture.
iii) Thermometers: In given sample and cooling mixture, there are two thermometers
fitted.

Reagents: lubricating oil, freezing mixtures


Apparatus: Cloud and pour point apparatus
Procedure:
1. Thoroughly dry and clean the flat bottomed glass tube.
2. Fill the oil sample to form a film of 5 cm thickness and fit the cork.
3. Adjust the dipped bulb of thermometer in the oil and in the cooling bath properly.
4. The tube is kept in the freezing mixture.
5. Prepare freezing mixture as mentioned below:

Mixture Composition Temperature range

A Ice + water Upto 10 oC


B Ice + NaCl Upto -10 oC
C Ice + CaCl2 Upto -25 oC
D Solid CO2 + Acetone Upto -60 oC

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

Object: Identification test for aldehyde group.

Principle: The reactions taking place are as follows:

Tollens’ reagent test:

2[Ag(NH3)2]+ + RCHO + H2O 2 Ag (s) + 4 NH3 + RCOOH + 2 H+

Fehling’s solution test:

RCHO + 2 Cu+2 + 5 OH- RCOO- + Cu2O + 3 H2O

Apparatus: Test Tube, Tongs, Spatula, Burner.

Procedure:

Experiment Observation Inference


1. Tollens’ reagent test: To Black silver precipitate. Aldehyde group present.
2 mL of Tollens’ reagent,
add 0.2 g of sample in a test
tube. Shake and warm it.

2. Fehling’s solution test: Deep blue colour Presence of aldehyde group


To 2 mL of Fehling’s disappeared and red confirmed.
solution (A and B). Add 0.5 precipitate appeared.
g of sample and boil for 2-3
minutes.
Chemistry Lab Manual

Result: The given sample contains …………………… group.

Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.

Experiment 8

Object: Identification test for ketones.

Principle: The reactions taking place are as follows:

2, 4 Dinitrophenyl hydrazine Test:

Sodium Nitropruside Test:

R-CO- CH3 + OH- R-CO-CH2- + Na2[Fe(CN)3NO]2-

[Fe(CN)5NOCH2-COCH3]2-

Apparatus: Test tubes, tongs, spatula, burner.

Procedure:

Experiment Observation Inference


1) 2, 4 Dinitrophenyl Yellow/Orange precipitate Ketone group is present.
hydrazine Test: To sample formed.
add 2 mL of reagent
solution.
Chemistry Lab Manual

Shake vigorously. Boil it for


30 seconds
2) Sodium Nitropruside Red-Purple precipitate formed. Ketone group is present.
Test: To original sample add
2 mL of reagent. Add 4-5
drops of NaOH.

Result: The given sample contains …………………… group.

Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.

Experiment 9

Object: Identification test for carbohydrates.

Principle: The reactions taking place are as follows:

Molisch’S test:

Fehling’s test:
Chemistry Lab Manual

Apparatus: Test tubes, tongs, spatula, burner.

Procedure:

Experiment Observation Inference


(1) Molisch’S Test- To 2cm3 of aqueous Violet precipitate is Carbohydrate group
solution of the original substance, add 2 observed. is present.
drops of molisch’s reagent. Carefully
pour about 1cm3 of conc. H2SO4 down
the side of the test tube and allow the
stand for 2 minutes. A red ring changing
to violet red at the junction of the two
layers indicates the presence of
carbohydrates.
(2) Fehling Solution Test- To 2 cm3 of Red precipitate is Carbohydrate group
Fehling solution, add 1cm3 of the obtained in case of is present.
aqueous solution of the original glucose or fructose.
substance and keep the test tube in
boiling water for 1 min. The whole
mixture turns red due to the formation of
Cu2O.

Result: The given sample contains …………………… group.

Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.
3.

Experiment 10
Chemistry Lab Manual

Object: Identification test for phenol group.

Principle: The reaction taking place is as follows:

Ferric Chloride Test:

Liebermann’s Test:

Apparatus: Test Tube, Tongs, Spatula, Burner.

Procedure:

Experiment Observation Inference


1) Ferric Chloride Test: Violet colour is observed. Phenolic group is present.
To 1ml of cold aqueous
solution of substance, add 1
drop of FeCl3 solution.
2) LieberMann’s Test: Black colour is observed. Phenolic group is present.
To 0.5 g of substance, add a
crystal of sodium nitrite.
Chemistry Lab Manual

Heat, cool and add dilute


sulphuric acid.

Dilute with H2O and observe Red colour is observed.


the change in colour again.

Add NaOH and observe the Green colour is observed.


change in colour.

Result: The given sample contains …………………… group.

Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.

Experiments 11

Object: Identification test for alcoholic group.

Principle: The reaction taking place is as follows:

Ester test:

CH3COONa + H2SO4 CH3COOH + Na2SO4

RCH2OH + CH3COOH RCH2COOCH3 + H2O

Apparatus: Test Tube, Tongs, Spatula, Burner.

Procedure:

Experiment Observation Inference


1. Ester test: To 0.5 g Pleasant fruity smell Alcohol is present.
substance add 0.5 g of on obtained.
anhydrous sodium acetate,
then add 4 to 5 drops of
concentrated sulphuric acid
and warm gently.
Chemistry Lab Manual

Result: The given sample contains …………………… group.

Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.

Experiment 12

Object: Identification test for ester group.

Principle: The reaction taking place is as follows:

Phenolphthalein test:

CH3COO-R + H2O CH3COOH + R-OH

Apparatus: Test Tube, Tongs, Spatula, Burner.

Procedure:

Experiment Observation Inference


1. Phenolphthalein test: To Pink colour appears.
sample, add one drop of
phenolphthalein. To this add
dilute NaOH, dropwise.
Heat the sample.

2. Heat the sample. Pink colour disappears. Presence of ester confirmed

Result: The given sample contains …………………… group.

Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.

Experiment 13
Chemistry Lab Manual

Object: Identification test for nitro group.

Principle: The reactions taking place are as follows:

Mulliken Barker test:

R-NO2 + 4 [H] + Zn + NH4Cl R-NHOH + H2O

R-NHOH + 2Ag(NH3)2OH + RCHO + H2O RNO + 2 H2O + 2 Ag (s) + 4 NH3

Apparatus: Test Tube, Tongs, Spatula, Burner.

Procedure

Experiment Observation Inference


1. Mulliken Barker test: Black silver precipitate Nitro group present.
Take 0.1 g of sample and formed.
add 2 mL alcohol to it in a
test tube. Add a few drops
10% NH4Cl solution and a
pinch of Zn dust. Heat the
solution for 5 minutes and
cool it. Filter it and add 2
mL of Tollens’ reagent to
the filtrate.

Result: The given sample contains …………………… group.

Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.

Experiment 14
Chemistry Lab Manual

Object: Identification test for amino group.

Principle: The reaction taking place is as follows:

Amino Group Test:


RNH2 + HCl + NaNO2 ROH + N2 + NaCl + H2O

Apparatus: Test Tube, Tongs, Spatula, Burner.

Procedure:

Experiment Observation Inference


1. Amino Group Test: Brisk effervescences are Aliphatic primary ammine is
To 0.5 g substance add 2 to observed. present.
3 mL of dilute HCl, heat it,
cool it, add sodium nitrate
(NaNO3) solution drop wise.

Result: The given sample contains …………………… group.

Precautions:
1. Handle sample and reagents using gloves.
2. Make sure the glassware is washed properly before use.

Experiment 15

Object: Preparation of p-Nitroacetanilide

Chemicals Required:

(i) 8 g Acetanilide
Chemistry Lab Manual

(ii) 8 mL Glacial Acetic acid

(iii) 4 mL Conc. HNO3

(iv) 20 mL Conc. H2SO4

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

Object: Preparation of Iodoform (Haloform Reaction).

Principle: The reaction is as follows-

NaCl + H2O + 2KI NaOH + KOH + I2 + KCl

CH3COCH3 + I2 + 4NaOH CHI3 + CH3COONa + 3NaI + 3H2O

Chemicals Required:
Potassium Iodide= 6 g

Acetone= 2 mL

5% sol. of Sodium Hypochlorate= 70 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

Description of the Redwood viscometer


It is divided in to three parts
1. Oil Cup: Material- Silver plated brass. It holds the test sample of lubricating oil. The bottom of
the cup is fitted with polished-agate discharge tube containing an orifice of specified dimension
2. Water Bath: Oil cup is surrounded by water bath for adjusting the temperature
3. Kohlrausch Flask: It receives the oil from polished-agate discharge tube
Reagents and apparatus: Redwood Viscometer, Thermometer 0-100°c (2 Nos), Stop
watch, 50 ml standard narrow necked flask, Given Sample of oil.

Procedure:
1. Select the Redwood viscometer according to the nature of oil (RW 1 for light oil and RW2
for heavy oil).

2. Level the viscometer by leveling screws.

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

where ν = Kinematic viscocity (in centistokes, cst)


t = time of flow in sec.
A and B are instrument constants
A = 0.264 and B = 190 for t = 40-85 seconds
A = 0.247 and B = 65 for t = 85-2000 seconds
Note: 100 cst = 1 stoke
And 1 poise = stoke × density

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.

2. The temperature of bath and oil cup should be the same.

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

Object: Preparation of phenol formaldehyde resin (Bakelite).

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

Glacial acetic acid = 5 mL

40% formaldehyde solution= 3 mL

Conc. HCl= Few drops

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 ………. %

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