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LABORATORY MANUAL

SECOND YEAR/ THIRD SEMESTER


SUBJECT: UNIT OPERATIONS
SUBJECT CODE: BOP 232P

College of Pharmacy- Agra


Gwalior Road, Rohta ki Nehar, Jakhoda.
Agra

Faculty In-Charge
COLLEGE OF PHARMACY- AGRA
SECOND YEAR/ THIRD SEMESTER
SUBJECT: UNIT OPERATIONS
SUBJECT CODE: BOP 232P

INDEX

S. NO. EXPERIMENTS

1 To determined the surface tension of benzene by using by drop-weight


method by using Stalagomometer.
2 To find out the Viscosity of Ethanol at room temperature.

3 To study the effect of concentration on surface tension using Stalagomometer.

4 To study the effect of concentration on Viscosity by using Ostwald‫ ׳‬s


Viscometer method.
5 To calibrate pH meter and determine pH of given solution using pH meter.

6 To determine the refractive index of a given liquid using Abbe‫ ׳‬s


Refractometer.
7 To determine Partition coefficients of Benzoic acid in Benzene & distill
water.

8 To determine the specific rotation of sugar solution with the help of


polarimeter.

9 To determine the solubility of a given salt (KCl) at different temperature.


Experiment No. 1

Aim: To determined the surface tension of benzene by using by drop-weight method by


using Stalagomometer.
Requirements: Stalagomometer, Stand, Benzene, Distilled water etc.
Reference:
Theory:
Procedure: Wash the Stalagomometer with the distilled water. Fill it by immersing the
lower end into the distilled water and sucking water above the mark A, close the pinch cork.
Allow 10 drops of the liquid to fall into the weighing bottle at the rate of one drop every 4
second. Weigh the Weighing bottle that give the weight of 10 drops of the water, take 3 or 4
reading. Removed it from stand and dry it thoroughly and repeat the procedure as with
water now with benzene and determine density of benzene.

Result:
Experiment No. 2

Aim: To find out the Viscosity of Ethanol at room temperature.


Requirements: Ostwald‫ ׳‬s Viscometer, Stop watch, Specific gravity bottle, 10 ml pipettes,
Ethanol, Distilled water, Thermometer.
Reference:
Theory:
Procedure: 1-Take Oswald’s Viscometer & clean with the help of suitable solvent.
2-Fit the viscometer on the stand.
3-Take about 10 ml of water in large bulb A & suck up to point X.
4-Note down the time to flow of water from X to Y with the help of stop watch.
5-In this manner, take about three reading
6-Same repeat with other solvent (Ethanol) & take readings & then calculate density of
Ethanol with the help of specific gravity bottle.
7-Calculate viscosity of ethanol.

Result:
Experiment No. 3

Aim: To study the effect of concentration on surface tension using Stalagomometer.


Requirements: Stalagomometer, Stand, Sodium carbonate, Distilled water etc.
Reference:
Theory:
Procedure: Wash the Stalagomometer with the distilled water. Fill it by immersing the
lower end into the distilled water and sucking water above the mark A, close the pinch cork.
Allow 10 drops of the liquid to fall into the weighing bottle at the rate of one drop every 4
second. Weigh the Weighing bottle that give the weight of 10 drops of the water, take 3 or 4
reading. Removed it from stand and dry it thoroughly and repeat the procedure as with
water now with given liquid i.e. aqueous solution of sodium carbonate of different
concentration like 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 1.0% and determine density of sodium
carbonate.

Result:
Experiment No. 4

Aim: To study the effect of concentration on Viscosity by using Ostwald‫ ׳‬s Viscometer
method.
Requirements: Ostwald‫ ׳‬s Viscometer, Stop watch, Specific gravity bottle, 10 ml pipettes,
sodium Carbonate, Distilled water.
Reference:
Theory:
Procedure:
1-Take Oswald’s Viscometer & clean with the help of suitable solvent.
2-Fit the viscometer on the stand.
3-Take about 10 ml of water in large bulb A & suck up to point X.
4-Note down the time to flow of water from X to Y with the help of stop watch.
5-In this manner, take about three reading
6-Repeat the procedure as with water now with given liquid i.e. aqueous solution of Sodium
carbonate of different concentration like 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 1.0% and
determine density of sodium carbonate.
7-Calculate viscosity of sodium Carbonate and plot the graph between various
concentration and viscosity.

Result:
Experiment No. 5

Aim: To calibrate pH meter and determine pH of given solution using pH meter.


Requirements: pH meter, Buffer Solution, solution of pH 4 and 9.2.
Reference:
Theory:
Procedure: 1-Switch on the pH meter and allow instrument to warm up for at least 5
minute.
2-Prepare buffer solution of ph 4 and 9.2 by dissolving one appropriate tablet or capsule in
specified volume of distilled water (100ml).
3-Insert the electrode in small beaker containing standard solution of pH 4.
4-Push read pH switch to know pH solution.
5-Adjust the set buffer on calibrate knob until reading agree with known ph of buffer
solution.
6-Remove the electrode from this solution and rinse with distilled water.
7- Place the electrode in second buffer solution of pH 9.2.
8-Adjust calibrate if meter reading dose not show exactly known pH.Untill the required pH
is obtained.
9-Remove the electrode and rinse with distill water and then place in first buffer solution
and conform that correct pH reading is shown on pH.
10-If calibration is satisfactory then rinse the electrode with the distill water and place it test
solution of unknown ph in small beaker.
11-Read pH of given solution and calculate the mean of three reading is performed.
Result:
Experiment No. 6

Aim: To determine the refractive index of a given liquid using Abbe‫ ׳‬s Refractometer.
Requirements: Abbe‫ ׳‬s Refractometer, water, ethanol.
Reference:
Theory:
Procedure: 1-Placed the apparatus in front of proper light source.
2-Clean the apparatus using soft cloth and wipe the prism with tissue paper moistened with
alcohol and then acetone.
3-Place a drop of distilled water on the lower surface of prism and then close the prism box.
4-focus the telescope eye piece on the lens section of the instrument.
5-Rotate the index arm with a screw until a colored band or fringe is seen, through the
telescope.
6-Adjust the eye piece on the movable arm to give sharp focus on the scale.
7- Record the refractive index to the formula place of decimal using reading lens.
8-Take at least 3 reading of each sample and then determine its mean value for the result.
9-Clean the prism and clean the face of the prism. Put a few drops of test solution on the
lower prism and then close properly.
9-Take three readings of sample solution & determine the mean value for result.

Result:
Experiment No. 7

Aim: To determine Partition coefficients of Benzoic acid in Benzene & distill water.
Requirements: Benzoic acid, Benzene, 0.05M NaOH, Separating funnel, conical flask,
Burette, pipette, Reagent bottle.
Reference:
Theory:
Procedure: 1-Take five reagents bottle and clean them using reagent and distilled water.
2-Prepare the composition of solution as shown below;-
I-1g of benzoic acid + 50 ml of water + 50ml of Benzene.
II-1.5g. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . .
III-2 g. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . .
IV-3 g. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . .
V-4 g. . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . .
3-Transfer these solutions in clean and dry reagent bottle and level them as 1, 2, 3, 4, and 5.
4-place the stopper on each bottle and it for thirty minute
5-take these mixtures in separating funnel and keep aside for 30 minute.
6-Separate aqueous and organic layer into conical flask.
7-Intermediate liquid should not be collected because it contains both the liquid.
8- Pipette out 10 ml aqueous layer and transfer it into another conical flask.
9-Add 2-3 ml of phenolphthalein as indicator and in with 0.05M sod. Hydroxide and repeat
it for three times.
10-Withdraw 10 ml of organic layer in another conical flask and proceeds as for aqueous
layer.

Result:
Experiment No. 8

Aim: To determine the specific rotation of sugar solution with the help of polarimeter.
Requirements: polarimeter, sugar solution, test tube.
Reference:
Theory:
Procedure: 1-Take the polarimeter tube and fill it with pure water, these should be no air
bubble in the polarimeter tube, place the polarimeter tube in the polarimeter.
2-If the polarimerter employing a half shade device a monochromatic source should be used
and if biquartz device is used than white light can be used.
3-See through the eye piece to half unequal intensity rotate the analyzer in clockwise
direction until the intensity of two half appear the main scale as well as vernies’s scale and
find out the total reading and rotate the screw in anti-clockwise direction until the intensity
of two half appear the same. Note down the total reading main scale and vernies’s scale.
4-Prepare a sugar solution of known strength are fill it polarimeter tube& place it in
polarimeter.
5-Rotate the analyzer to obtain the equal intensity position first in clockwise direction and
then in anti clockwise direction. Repeat the experiment with the sugar solution of defrent
concentration.
6-Measure the length of tube.

Result
Experiment No. 9

Aim: To determine the solubility of a given salt (KCl) at different temperature.


Requirements: Thermostat, Heater, Thermometer etc
Reference:
Theory:
Procedure: 1-Take about 1ml distill water in a beaker and to it some amount of the given
salt (KCl) and stir contents.
2-Heat the solution to about 85-90ºC and go on adding further amount of salt.
3-Note that the salt should be in excess at 85-90ºC.
4-Now cool the solution and as the temperature falls to say 80ºC pipette about 4-5ml of
surfactant liquid quickly and transfer it to a previously weighed beaker or water glass.
5-Again pipette–out about 4-5ml of surfactant liquid when the temperature falls 60ºC and
transfer it to a previously weighed beaker or water glass.
6-Repeat the above process at temp. 40ºC & 25ºC.
7-Dry the solution in a electric oven at 120ºC or on a water bath still whole of water
evaporates and weigh the dry residue of the solid.

Result

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