PHYSICAL PHARMACEUTICS LABORATORY

LIST OF EXPERIMENTS

S.NO DESCRIPTION PAGE

NUMBER
1 DETERMINATION OF PARTICLE SIZE BY MICROSCOPY

2 STUDY OF PARTICLE SIZE DISTRIBUTION BY MICROSCOPY

3 DETERMINATION OF PARTICLE SIZE BY SIEVING METHOD

4 DETERMINATION OF ANGLE OF REPOSE OF POWDER BY

FUNNEL METHOD
5 EFFECT OF GLIDANTS AND LUBRICANTS ON ANGLE OF
REPOSE

6 PREPARATION OF CALAMINE LOTION

7 EVALUATION OF CALAMINE LOTION

8 PREPARATION OF MULTIPLE EMULSION

9 DETERMINATION OF POROSITY

10 DETERMINATION OF SPECIFIC SURFACE AREA OF A

GIVEN POWDER BY ADSORPTION METHOD
11 DETERMINATION OF VISCOSITY OF LIQUID SAMPLE BY
USING OSTWALD’S VISCOMETER
12 DETERMINATION OF SURFACE TENSION BY DROP
NUMBER METHOD AND DROP WEIGHT METHOD
13 DETERMINATION OF CRITICAL MICELLE
CONCENTRATION

14 DETERMINATION OF REACTION RATE CONSTANT AND

HALF LIFE
 DETERMINATION OF PARTICLE SIZE BY MICROSCOPY

AIM:
To determine the mean particle size of a given sample.

REQUIREMENTS:
Microscope, eye piece micrometer, stage micrometer, glass slide, cover slip,
sample.

PRINCIPLE:
Particle size influences many properties of particulate materials and is a valuable
indicator of quality and performance. This is true for powders, suspensions, emulsions
and aerosols. The size and shape of powders influences flow and compaction properties.
Larger, more spherical particles will typically flow more easily than smaller or high
aspect ratio particles. Smaller particles dissolve more quickly and lead to higher
suspension viscosities than larger ones. Smaller droplet sizes and higher surface charge
(zeta potential) will typically improve suspension and emulsion stability. Powder or
droplets in the range of 2-5μm aerosolize better and will penetrate into lungs deeper than
larger sizes. For these and many other reasons it is important to measure and control the
particle size distribution of many products. There are several methods to determine
particle size.In this experiment,Particle size of given sample is determined by
microscopy.

PROCEDURE:
Calibration of eye piece micrometer:
 1. Align the zero line (beginning) of the stage micrometer with the zero line
(beginning) of the eye piece micrometer. Now, carefully scan over until you see the
lines line up again.
2. Each division of the stage micrometer is 0.01mm or 10 µm.
3. The eyepiece micrometer is divided into 100 units.
4. When the zero marks are lined up, scan across and look for a convenient point
where the lines converge again.

One division of eye piece micrometer = no of division of stage micrometer/no of eye

piece micrometer x 10

Particle size Determination:

Prepare a dilute suspension of the given powder sample with distilled water. Place a drop
of the suspension on a glass slide and observe the particles under the microscope with
calibrated eyepiece micrometer. Determine the average particle size by taking mean of
length and breadth of the particle (Since most of the particles are not spherical).Measure
at least 100 particles to get reliable data.

Determination of particle size

Size range Mean size(d) Number of particle nxd
(n)
0-10
10-20
20-30
30-40
40-50
60-70
 70-80
80-90
90-100

Average particle size =

REPORT
 STUDY OF PARTICLE SIZE DISTRIBUTION BY MICROSCOPY

AIM:
To study the particle size distribution of a given sample by microscopy.

REQUIREMENTS:
Microscope, eye piece micrometer, slide, stage micrometer, cover slip and
sample.
PRINCIPLE:
Any powder is polydisperse (mixture of different sized particles).Hence it is necessary to
know the size of particles and how many particles are present in each size range or what
is the weight of particles present in each size range. Such a distribution of different sized
particles in a powder is called particle size distribution. The particle size distribution of
active ingredients and excipient is an important physical characteristic of the materials
used to create pharmaceutical products. The size, distribution and shape of the particles
can affect bulk properties, product performance, processability, stability and appearance
of the end product.The link between particle size and product performance is well
documented with regards to dissolution, absorption rates and content uniformity.
Reducing particle size can aid the formulation of new chemical entities with poor water
solubility. Particle size analysis is an integral component of the effort to formulate and
manufacture many pharmaceutical dosage forms.Particle size distribution can be
quantified by two ways:Number of particles present in each size range and Weight of
particles present in each size range.In this experiment,Particle size distribution is
analysed by microscopy and various statistical parameters are determined.

PROCEDURE:
Prepare a dilute suspension of the given powder sample with distilled water. Place
a drop of the suspension on a glass slide and observe the particles under the microscope
with calibrated eyepiece micrometer. Determine the average particle size by taking mean
of length and breadth of the particle (Since most of the particles are not
spherical).Measure at least 100 particles to get reliable data. Plot a graph between
%cumulative frequency versus mean size range(d) and %frequency versus d.From the
table values various statistical parameters like length number mean diameter,Surface
number mean diameter and volume number mean diameter are calculated.

S.No Size Mean Number of %Frequency Cumulative nd nd2 nd3

range(µm) size particles(n) =n(100) % frequency
(d)
∑n

Length number mean diameter = ∑nd/ ∑n

Surface number mean diameter = [∑nd2/ ∑n]1/2

Volume number mean diameter = [∑nd3/ ∑n]1/3

REPORT

DETERMINATION OF PARTICLE SIZE BY SIEVING METHOD

AIM:
To determine the average particle size and find out the distribution partition (by sieve
analysis) of the supplied granular sample.

MATERIALS REQUIRED:
Granular sample, Series of sieves, mechanical sieve shaker.

PRINCIPLE:
Sieve is a perforated screen and size of the opening depends on the number of meshes
and the diameter of the wire constituting the mesh. The particles sufficiently small will pass
through and those that are oversize will be retained on the sieve will classify the particles as less
than the dimension of mesh (undersize) and more than the dimension of mesh (oversize).
When a powder sample is passed through a set of around 5 sieves arranged with
descending aperture size. The particle size analysis through sieving is best expressed in the form
of a cumulative over size cumulative undersize or as a histogram.
Unlike microscopy in sieving the distribution is expressed on weight basis (weight
diameter).

PROCEDURE:
About 5 sieves are arranged keeping one above the other in a series when the co arrest
(less no) at the top and the finest at the bottom.
Around 100 gm of pre weighed sample is placed on the top sieve.
The rest of sieves is shaken for about 20 mins preferably in sieve shaker.
The quantity of sample retained on each sieve is weighed.
The average particle size is determined as weight fraction and the distribution is
expressed in a cumulative over size curve.

REPORT:

The average diameter of the particle of given sample was found to be ____________µm
DETERMINATION OF ANGLE OF REPOSE OF POWDER BY FUNNEL
METHOD
AIM:
To determine the angle of repose of a given sample by funnel method.

REQUIREMENTS:
Funnel, scale, Graph paper, stand, sample.

PRINCIPLE:

Angle of repose is the maximum angle possible between the surface of pile of powder
and horizontal plane
tan θ = h/r
= tan-1(h/r)
Where,
h = height of pile of powder
r = radius of pile of powder.

If a powder is allowed to flow on a flat surface, a pile or heap is formed. A material that
flows well spreads out and forms a low heap (Low angle of repose). More cohesive
samples will form high heap and exhibit high angle of repose.Values for angle of repose
≤ 30 usually indicate free flowing and Angle of repose ≥ 40 suggest a poorly flowing
material.Flow properties of powders or granules have great impact during the
manufacturing of solid dosage forms. Poor flowing materials will show many difficulties
such as improper filling, weight variation, poor content uniformity etc.

Flow properties may be improved in one or more following ways

 By decreasing the particle size.
 By producing the particle in spherical form.
 By using additives like glidants
The various approaches used to access the flow property of powder are Angle of repose, Compressibility
index and Hausner ratio. In this experiment, the flow property of given sample was determined by fixed
funnel method.

Flow property Angle of Repose(Degrees)

Excellent 25-30

Good 31-35

Fair 36-40

Passable(may hang up) 41-45

Poor 46-55

Very poor 56-65

PROCEDURE:
1. Dry and clean funnel was fixed on to a burette stand to a particular height of 2.5
cm.
2. The height of the funnel was fixed till the completion of practical.
3. A graph paper was placed on the flat surface.
4. Sufficient quantity of the sample was allowed to flow slowly through the funnel
until the heap touches the tip of the funnel.
5. The circumference of the heap was carefully drawn using a pencil.
6. The radius of the circumference was measured by locating the mid-point.
7. The angle of repose can be calculated by following formula:
Tan θ = h / r
Where, h = height of pile, r = radius of pile
REPORT

EFFECT OF GLIDANTS AND LUBRICANTS ON ANGLE OF REPOSE

AIM: To determine the effect of glidant or lubricant angle of repose.

REQUIREMENTS:

Sodium bicarbonate, talc, magnesium stearate, mortar, pestle, funnel, burette stand etc.

PRINCIPLE:

Lubricants are intended to reduce the friction during the ejection of tablet from
wall of die cavity. The most widely used lubricant has been stearic acid and derivatives
such as calcium and magnesium stearate and talc.

Glidants are intended to promote flow property of powder or granules by reducing

friction between particles. Most widely used glidants are silica derivatives.

The frictional force in a loose powder can be measured by the angle of repose.
This is maximum angle possible between the surface of a pile of powder and the
horizontal plane.

The tangent of angle of repose is equal to the co-efficient of friction between

particle i.e. Tanθ = μ.

Values for angle of repose ≤ 30 usually indicate free flowing and

Angle of repose ≥ 40 suggest a poorly flowing material.

PROCEDURE:

1. 50 gm of Sodium bicarbonate was weighed and transferred into a mortar.

2. Required amount of starch paste was added drop wise and triturated.
3. This pasty mass was passed through sieve no. 12 to get granules
4. These granules was dried in an oven at 60˚C and then passed through sieve no.
12/44.
 5. Granules were then weighed.
6. Different concentration of talc (0%, 0.2%, 0.4%, 0.6%, 0.8%, 1.0%) was added
and angle of repose for each concentrate mixture was determined by using
formula.
Tan θ = h/r.

Where,

h = height of pile.

r = radius of pile.

7. Same procedure was repeated for magnesium stearate.

OBSERVATION:

RESULT:
 PREPARATION OF CALAMINE LOTION

AIM:

To prepare and submit 20 ml of Calamine lotion I.P.

MATERIALS REQUIRED:

Calamine, Zinc oxide, Bentonite, Sodium citrate, Liquefied Phenol, Glycerine, Rose
water.

PRINCIPLE:

Lotions are usually liquid preparations or dispersions meant for application to the
skin without friction. Calamine is composed of zinc oxide with small amount of ferric
oxide which imparts characteristic pink colour and is used topically as protective.The
powder is used as an astringent and have weak antimicrobial action due to release of zinc
from zinc oxide which is formed by hydrolysis of acidic skin moisture. Bentonite is a
natural colloidal hydrated aluminium silicate. It is a pale buff coloured powder and is
insoluble in water, swells nearly 12 times of its bulk which imparts desirable rheological
characteristics. Hence it is used as a suspending agent. Sodium citrate acts as a buffering
agent and maintains pH appropriate for skin.It also imparts better consistency to the
product and prevents excessive frothing on shaking.It also prevents discoloration of the
product which occurs due to oxidation of ferric to ferrous oxide. Liquified phenol acts as
an antiseptic, preservative and local anaesthetic. Glycerine is used for its soothing action
and makes the preparation more viscous where as rose water gives pleasant smell to the
product.

PROCEDURE:
1. Triturate Calamine, Zinc oxide and Bentonite in a solution of sodium citrate in about
¾ th quantity of rose water.
2. Add Liquefied Phenol and glycerine to above mixture and mix well.
3. Add sufficient rose water to produce the required volume.
4. Preparation is shaken to ensure uniform distribution. Finally the transfer the
preparation into a bottle, capped, properly labeled and submitted.

Formula:

Ingredients Quantity

Calamine 15 g

Zinc oxide 5.0 g

Bentonite 3.0 g

Sod. Citrate 0.5 g

Liquefied Phenol 0.5 g

Glycerine 5.0 ml

Rose water q.s. 100 ml

REPORT
 EVALUATION OF CALAMINE LOTION

AIM:

To evaluate the physical stability of suspensions prepared using different suspending

agents.

PRINCIPLE:

Physical stability of suspension is evaluated by measuring the sedimentation volume and

redispersibility studies.Sedimentation Volume (F) is the ratio of ultimate volume of
sediment to the total volume of the suspension.

F=Vu/Vo

Sedimentation volume is normally less than 1.when F=1 then such suspensions are
pharmaceutically acceptable.When F>1,it indicates that the network of flocs formed in
the suspension is loose and fluffy that it encompasses a volume greater than the original
volume of the suspension.Redispersibility is one of the major considerations in assessing
the acceptability of the suspension.Since the sediment formed should be easily dispersed
by moderate shaking,measurement of sedimentation volume and its ease of redispersion
are common procedures for evaluation.

PROCEDURE:

1. Prepare four different formulations of suspension using Bentonite,Guar

gum,Hydroxy Propyl methyl cellulose and Ethyl cellulose.
2. Pour the formulation into measuring cylinder and keep aside undisturbed.
3. Calculate the F value for all the formulations for one hour(every 10 mins) and 24 th
hour
 4. Carry out redispersibility studies after 24hours
5. Conclude the most stable suspension based on F value and its ease of redispersion.

REPORT
 PREPARATION OF MULTIPLE EMULSION

AIM: To formulate Aspirin multiple emulsion.

REQUIREMENTS:

Aspirin, Tween-80, arachis oil, Acacia and Distilled water

PRINCIPLE:

Multiple emulsions are complex and poly dispersed in nature where both w/o and o/w
emulsion exists simultaneously in a single system. Lipophilic and hydrophilic surfactants
are used for stabilizing these two emulsions respectively. The droplets of the dispersed
phase contain even smaller dispersed droplets themselves, therefore also called as
"emulsions of emulsions”. There are two major types of multiple emulsions are the water-
oil-water (w/o/w) and oil-water-oil (o/w/o) double emulsions. The most common
multiple emulsions are of W/O/W type, although some specific applications O/W/O
emulsions can also be prepared. Multiple emulsions are used for taste masking and for
slow or controlled delivery of drugs.

PROCEDURE:

Preparation of Multiple Emulsions (w/o/w) (100ml):

 The emulsion was prepared by w/o/w method.

 First Step: Prepare W/O emulsion by following method
1) Take 4g Gum acacia in mortar, add 150mg of drug, 10ml of water and
triturate to form mucilage.
2) Add 0.3ml of span 80(lipophilic surfactant) and required quantity of oil
(20ml) in small portions with rapid trituration to produce W/O emulsion
 Second Step:
1) 1ml of Hydrophilic surfactant Tween 80 dissolved in 60 ml water.
 2) The first step emulsion was added in to second step with continuous stirring
for 15mins to form a multiple emulsion

REPORT
 DETERMINATION OF POROSITY

AIM:
To determine the Porosity of the given powder sample.

REQUIREMENTS:
Measuring cylinder, Specific gravity bottle, purified water, weighing balance and
powder sample.

THEORY:

Porosity is the ratio of void volume to bulk volume. It is normally expressed in

percentages. Porosity not only affects compatibility but also density. It can be estimated
from bulk and true density. It is an important attribute of pharmaceutical granules. Low
porous granules will be harder to compress than the granules with high porosity. It may
also affect product dissolution rate. It is believed that porous granules dissolve faster than
dense granules since the pores allow water to penetrate granules more readily. Processing
conditions can have a strong influence on the porosity of a powder. Thus porosity play an
important role in compressibility and dissolution characteristics of powder. In this
experiment, Porosity is determined by using true density and bulk density values.

Porosity = Void volume / Bulk volume *100

= 1-(Bulk density / True density) *100

PROCEDURE:
1. Determination of True density:
The empty specific gravity bottle accurately weight .It was filled with given
sample and weight was determined. The Purified water was added till water displaces
voids of the powder. The weight of the specific gravity bottle containing purified water
and given sample was also found out. Then remove the powder sample and liquid, filled
up the bottle with purified water upto the mark. Finally the true density of the given
sample was calculated by using following formula.

True Density = Weight of the powder / True volume of powder

2. Determination of bulk density:

Weight accurately about 10-20g of the givensample. Carefully introduced the
sample into a graduated measuring cylinder. The cylinder was tapped at 2 seconds
intervals on to a hard surface 3 times from a height of 1 inch and note the volume of
powder. The bulk density of the given sample was calculated by using following formula.

Bulk density = Mass of powder / Bulk volume of powder.

DETERMINATION OF TRUE DENSITY

Weight of the empty specific gravity bottle (W1) =________g

Weight of the specific gravity bottle + sample (W2) =________g
Weight of the specific gravity bottle + sample + liquid (W3) =________g
Weight of the specific gravity bottle + liquid (W4) =________g

Weight of the powder = W2-W1

=________g

Weight of the liquid = W4-W1

=________g

Weight of liquid displaced = W3-W2

=________g

Density of liquid = Weight of the liquid/ Volume

=________g/ml

True Density = Weight of the powder / True volume of powder

= ________g/ml
Bulk Volume = True Volume+ Void Volume
True Volume = Bulk Volume – Void Volume

True density = Mass/True Volume

Bulk Density:
S.No Weight of Volume of sample after Bulk
sample(g) tapping (ml) density(g/ml)
1
2
3

Trial 1:
Bulk density = M/V =
=______g/ml
Trial 2:
Bulk density = M/V =
=______g/ml
Trial 3:
Bulk density = M/V =
=______g/ml
Average =

Porosity = 1-(Bulk density / True density) x100

REPORT
DETERMINATION OF SPECIFIC SURFACE AREA OF A GIVEN POWDER BY
ADSORPTION METHOD

AIM:
To determine the specific surface area of a given powder sample by adsorption
method.

REQUIREMENTS:
Methanolic stearic acid, sodium hydroxide, conical flask, oxalic acid, pipette and
phenolphthalein indicator.

THEORY:
The surface area of a powder can be derived indirectly from the size and size distribution
obtained by methods like microscopy, sedimentation etc.Direct calculation of surface
area can be done by adsorption and air permeability methods. In adsorption method, the
amount of liquid solute or a gas that is adsorbed onto a powder sample to form a
monolayer is found out and from this data, surface area of the powder may be
determined. In this experiment, surface area of magnesium oxide is determined by liquid
adsorption using methanolic solution of stearic acid.Stearic acid being a linear molecule;
the molecules get adsorbed on solid surface as a monolayer. This method is applicable to
powders insoluble in methanol.

PROCEDURE:
Preparation of 0.02 N NaOH solution

Weigh 0.4 g of NaOH pellets in a clean, preweighed 100-mL beaker on a balance. Put
250 mL of distilled water into a clean 500 mL volumetric flask. Add the NaOH pellets
completely. When the NaOH has dissolved completely add another 250 mL of distilled
water up to the marking. Mix thoroughly.

Standardization of NaOH solution using diprotic acid (oxalic acid)

Place the standard oxalic acid solution 0.025 M in the burette. Transfer 10 mL of the
NaOH solution into a 125 mL conical flask with the aid of a pipette, add 1-2 drops of
phenolphthalein indicator and titrate with the standard oxalic acid. Repeat the titration
until duplicate determinations agree within 0.05mL of each other. (If three titrations do
not result in the desired precision, it will be necessary to conduct additional titration.)

Determination of Surface area:

2.5gm of sample was accurately weighed and taken in a stoppered conical flask.
To this added 25ml of 0.5% stearic acid solution in methanol, the contents are stirred well
and kept aside for 1 hour for adsorption to attain equilibrium and filtered. The filtrate
contains unadsorbed stearic acid. 10ml of filtrate was pipette out and titrated with N/50
sodium hydroxide solution using phenolphthalein as an indicator. A blank of titration was
performed to find out the amount of stearic acid originally present in the solution.
The amount of stearic acid adsorbed in 25ml of solution was calculated by using
the following formula.
(B-A) x Normality of sodium hydroxide
X= --------------------------------------------------------
Required normality x Equivalent weight factor

1ml of 0.02N sodium hydroxide ≡ 0.00568 gm of stearic acid.

The amount of stearic acid adsorbed

Y= -----------------------------------------------------
Weight of sample
 284 gms of stearic acid contains 6.023 x 10 23 moles are stearic acid ‘Y’ gm of
stearic acid contains ‘Z’ moles of stearic acid.One molecule of stearic acid occupies an
area about 20.5 x 10-16cm2
Y x 6.023 x 1023
Z= --------------------
284

Specific surface area =number of molecules adsorbed x Surface area of one molecule of
solute

REPORT

The specific surface area of the given sample was found to be _______________
 DETERMINATION OF VISCOSITY OF LIQUID SAMPLE BY USING
OSTWALD’S VISCOMETER

AIM:
To determine the viscosity of the given liquid sample using Ostwald’s viscometer.

THEORY:

The internal property of a fluid for its resistance to flow is known as viscosity. In 1844
Hagen–Poiseuille did their work concerning the interpretation that liquid flow through
tubes and he proposed an equation for viscosity of liquids. This equation is called
Poiseuille’s equation.

Where η is called the viscosity coefficient, t is the time of flow of liquid, V is the volume
of the liquid, P is the hydrostatic pressure, and L is the distance travelled by the liquid
during time t. In the honour of Hagen–Poiseuille the unit of viscosity is called the Poise
(P). The official SI unit for absolute viscosity is kg/m s (or Pascal-seconds, Pa
s).Viscosity can be measured using a viscometer. The different types of viscometer are as
follows: Ostwald viscometer, Falling sphere viscometer, Falling piston viscometer,
Oscillating piston viscometer, Vibrational viscometers, Rotational viscometers and
Bubble viscometer

Ostwald viscometer, also known as U-tube viscometer or capillary viscometer is a device

used to measure the viscosity of the liquid with a known density. The method of
determining viscosity with this instrument consists of measuring the time for a known
volume of the liquid (the volume contained between the marks A and B to flow through
the capillary under the influence of gravity. Ostwald viscometers named after the German
chemist Wilhelm Ostwald (1853-1932).The instrument must first be calibrated with
materials of known viscosity such as pure (deionized) water. Knowing the value of
viscosity of one liquid, one can calculate the viscosity of other liquid.

where η1 and η2 are viscosity coefficients of the liquid and water, and ρ 1 and ρ2 are the
densities of liquid and water, respectively.

PROCEDURE:
1. Clamp the clean and dry Ostwald viscometer in a vertical position.
2. With the help of a pipette take 20ml of distilled water ad suck the liquid into the
bulb just above the mark.
3. Determine the time of flow of liquid (i.e) time required for the liquid level to fall
from one mark to another mark. Use stop watch to determine the time t1
4. Using the same clean and dry viscometer determine the time of flow t 2 of given
liquid.
5. Determine the density of liquid (ρ2) by using specific gravity bottle if not given.
6. Calculate absolute viscosity, relative viscosity and kinematic viscosity of the given
liquid.

REPORT:
Absolute viscosity of liquid was found to be ________
Relative viscosity of liquid was found to be_________
Kinematic viscosity of liquid was found to be ________
 DETERMINATION OF VISCOSITY OF LIQUID SAMPLE BY USING
OSTWALD’S VISCOMETER

CALCULATION:
Weight of the empty specific gravity bottle (W1) =________g
Weight of the specific gravity bottle + water (W2) =________g
Weight of the specific gravity bottle + sample (W3) =________g
Mass of water = W2-W1

=___________ g

Mass of liquid = W3-W1

=___________ g

Density of liquid = mass of liquid/mass of water x Density of water

= W3-W1 * 0.9998
W2-W1

=____________g/ml.

CALCULATION:

Time in seconds for Water

Sample Time of flow of water in Concordant value
seconds
 Water

Time in seconds for sample

Sample Time of flow of water in Concordant value
seconds

Liquid

CALCULATION:

Density of liquid = _________g/ml

Density of water =_________g/ml
Viscosity of water = _________poise
Viscosity of liquid = _________poise
Time in seconds of liquid =
Time in seconds of water =

Absolute viscosity=

Relative viscosity = Viscosity of liquid

Viscosity of water.
Kinematic viscosity = Absolute viscosity
Density of liquid
 DETERMINATION OF SURFACE TENSION BY DROP NUMBER METHOD
AND DROP WEIGHT METHOD

AIM:
To determine the surface tension of given sample using stalagmometer by drop
number method and drop weight method.

THEORY:
Molecules of the liquid at the surface are in a different situation than those in the
interior of the liquid. A molecule lying inside the liquid is surrounded by other molecules
and so is attracted equally in all directions. Hence the net force of attraction acting on the
molecule is zero. But a molecule lying at the surface is attracted downwards by the
molecules lying in the bulk of liquid. Thus a molecule lying at the surface experiences a
net inward attraction. As a result of this inward pull on all molecules lying at the surface,
the surface behaves as if it were under tension. This property of liquids is called surface
tension.
The surface tension of a liquid is defined as the force acting at right angles to the
surface along one centimeter length of the surface. Thus the units of surface tension are
dynes per centimeter or Newton per meter. There are several methods of surface tension
measurements: Capillary rise method, Stalagmometer method, Wilhelm plate or ring
method, Maximum bulk pressure method and Dynamic methods. In this experiment
surface tension is determined by drop number and drop weight methods using
stalagmometer.

PROCEDURE:
Drop weight method:
This method is based upon the principle that the weight of drop falling slowly out of a
capillary held vertically is directly proportional to its surface tension. The procedure
consists of following steps:
1. Stalagmometer is clamped vertically on a stand and a rubber tube with a pinch cock
is attached to the upper portion.
2. Distilled water is sucked into the apparatus and then the pressure is adjusted with
the help of pinch cock so that the rate of fall of drops is about 15-20drops per
minute.
3. 10 drops of water are allowed to fall into a clean weighing bottle which has already
been weighed when empty. The weight of the weighing bottle along with the drops
is taken.
4. The apparatus is now rinsed with acetone and then allowed to dry.
5. Now the experimental liquid is sucked into the stalagmometer, the rate of fall of
drops adjusted as before and 10drops of the liquid taken into the empty weighing
bottle and the bottle weighed.

Drop number method:

In this procedure, the apparatus is cleaned and clamped vertically. Distilled water is first
sucked into the apparatus upto upper mark. The number of drops while water flows from
upper mark to lower mark is noted. The apparatus is rinsed with acetone and dried. The
experimental liquid is now sucked and the number of drops while the liquid flows from
upper mark to lower mark is counted. The result is calculated using the given formula.

REPORT:
DETERMINATION OF SURFACE TENSION BY DROP WEIGHT METHOD

CALCULATION:
Weight of the empty specific gravity bottle (A) =_________g
Weight of the bottle +20 drops of water (B) =_________g
Weight of 20 drops of water (W1) = B-A
=_______g
Weight of 20 drops of sample + bottle (C) =
Weight of 20 drops of sample (W2) = C-A
=_______g

Surface tension of water (∂1) = __________dynes/cm

∂2 = W2/W1 X ∂1
=
=_________dynes/cm
DETERMINATION OF SURFACE TENSION BY DROP NUMBER METHOD

CALCULATION:
Weight of the empty specific gravity bottle (W1) =________g
Weight of the specific gravity bottle + water (W2) =________g
Weight of water taken = W2-W1
=_______ g

Weight of the specific gravity bottle + sample (W3) =________g

Weight of sample = W3-W1
=_________g
Density of sample = W3-W1/ W2-W1 x Density of water
=_____________g/ml
Tabulation
To calculate the number of drops.

S.No Number of drops of water (ηl) Number of drops of sample(η2)

1
2
3

∂2 = surface tension of sample =

∂1 = surface tension of water =
ηl = number of drops of water =
η2 = number of drops of sample =
p1 = density of water =
p2 = density of sample =
∂2 = ηl p2/η2 p1 x ∂1
=
=__________
 DETERMINATION OF CRITICAL MICELLE CONCENTRATION

AIM:
To determine the critical micelle concentration of given surfactant using
stalagmometer.

REQUIREMENTS:
Stalagmometer, specific gravity bottle, volumetric flask, pipette and surfactant.

THEORY:
Surfactants may be described as materials which have a tendency to preferentially
get adsorbed at the interface between two phases. Their molecules consist of a polar and
non polar part. When they placed in two phases of different polarities, the non polar part
sets oriented towards the phase of low polarity while polar towards high polarity phase.

When a surfactant is placed in a solvent, the molecule of surfactant present in a

large numbers at the interface than in bulk of solution. Preferential adsorption continues
until all the available space at the surface is occupied.

There after the surfactant molecule descent down in to bulk of solution in the form
of micelles. The concentration of the surfactant at which it forms micelle is known as
critical micelle concentration.

PROCEDURE:

Preparation of different concentration of surfactants:

1. 2%w/v stock solution was prepared by dissolving 2g of sodium lauryl sulfate in

100ml of distilled water.
 2. 0%, 0.02%, 0.04%, 0.06%, 0.08%, 0.1%, 0.2% and 0.3%w/v were obtained by
taking 0, 1, 2, 3, 4, 5, 10 and 15ml of stock solution and making it upto100ml in
standard flask.
3. The surface tension of each solution was determined using stalagmometer.

Determination of surface tension:

1. Stalagmometer was cleaned thoroughly with distilled water and then rinsed with
small amount of acetone and dried.
2. The flattened end of stalagmometer was dipped in a reference liquid and was
placed in a clean beaker.
3. Liquid was sucked until the level rises above mark A.
4. The liquid was allowed to run down slowly.
5. Weight of bottle along with 10drops was taken.
6. The determination was repeated at least twice and its surface tension was
calculated.
7. A graph was plotted between concentration of surfactant on X-axis and surface
tension on Y-axis.

REPORT
The critical micelle concentration of given sample was found to be
_____________.
DETERMINATION OF CRITICAL MICELLE CONCENTRATION

CALCULATION:
Weight of empty specific gravity bottle = ____________ gm.
Weight of bottle +10 drops of water = ____________ gm.
Weight of bottle +10 drops of 0.02% of surfactant = ____________ gm.
Weight of bottle +10 drops of 0.04% of surfactant = ____________ gm.
Weight of bottle +10 drops of 0.06% of surfactant = ____________ gm.
Weight of bottle +10 drops of 0.08% of surfactant = ____________ gm.
Weight of bottle +10 drops of 0.1% of surfactant = ____________ gm.
Weight of bottle +10 drops of 0.2% of surfactant = ____________ gm.
Weight of bottle +10 drops of 0.3% of surfactant = ____________ gm.

Surface tension of water (∂1 ) =____________dynes/cm.

Weight of 10 drops of water =____________gm.

Weight of 10 drops of 0.02% surfactant =____________gm.
Weight of 10 drops of 0.04% surfactant =____________gm
Weight of 10 drops of 0.06% surfactant =____________gm
Weight of 10 drops of 0.08% surfactant =____________gm
Weight of 10 drops of 0.1% surfactant =____________gm
Weight of 10 drops of 0.2% surfactant =____________gm
Weight of 10 drops of 0.3% surfactant =____________gm

S.No Concentration Weight of Weight of Surface tension

%w/v sample(w2) water (w1) (dynes/cm)
1
2
3
4
5
6

Surface tension of water (∂2 ) = w2/w1 x ∂1

0.02% =
0.04% =
0.06% =
0.08% =
0.1% =
0.2% =
0.3% =
 DETERMINATION OF REACTION RATE CONSTANT AND HALF LIFE

AIM

To determine the reaction rate constant and half-life of ester subjected to acid hydrolysis.

REQUIREMENTS:
Conical flask, pipette, water bath, burette, cold water, Sodium hydroxide hydrochloric
acid, ethyl acetate and phenolphthalein indicator.

THEORY:

The reaction rate for a reactant or product in a particular reaction is intuitively defined as
how fast a reaction takes place. The rate of reaction is defined as the change in the
number of molecules of reacting species per unit volume per unit time. It is also defined
to be proportional to the concentration of reacting species raised to a certain power called
the order of reaction. It is usually taken as the rate at which the reactant disappear or the
rate at which the product is formed. The rate at which the reactant ‘a’ is disappearing is
proportional to its concentration at any instance,

Rate (r) = k (a - x)

Where k = rate constant

Hydrolysis is a chemical decomposition involving breaking of a bond and the addition of

elements of water. In this hydrolysis of ester (ethyl acetate) with an alkali (sodium
hydroxide), HCl was used as catalyst to accelerate it. The fact that this is a first order
reaction is established by substituting the results in the first order rate expression;
The hydrolysis of an ester such as ethyl acetate in the presence of a mineral acid gives
acetic acid and ethyl alcohol.

The value of rate constant, K

Where, Vo = initial titre value

Vα= final titre value at the end of the experiment and

Vt = titre value at the various time intervals chosen

As the hydrolysis proceeds, there will be proportional increase in the concentration of

acetic acid formed. This experiment involves determination of specific rate constant and
half-life of a reaction undergoing at different temperatures.

PROCEDURE:

Mix 5ml of ethyl acetate with 100ml of 0.1Nhydrochloric acid taken in a conical flask
and maintain at a temperature of 40°C.Withdraw 10ml of aliquot of the reaction mixture
at regular intervals (0, 15, 30, 45,60,75,90,105 and 120mins).Transfer each reaction
mixture into 30ml of ice cold water and titrate against 0.1N Sodium hydroxide using
phenolphthalein as indicator. Titrate each reaction mixture immediately after transferring
into the ice cold water and mixing with the indicator. Repeat the experiment in the same
way but maintaining the temperature at 50 °C, 60°C and 70°C.Calculate the k values from
the data obtained at each of the above temperatures and determine its corresponding half-
life.

t1/2 = 0.693/K

REPORT
Determination of rate constant and half life:

S.No Time in Volume of Volume of V∞ - K

mins NaOH(ml) NaOH(ml) Vt
Initial Final

t1/2 = 0.693/K