Professional Documents
Culture Documents
Ex. No. :1
Date
:
AIM:
To determine the mean particle size for a given sample through optical microscopy & sieving
technique.
REFERENCES:
Physical pharmacy martin II edition Philadelphia 1983- page no 502.
PRINCIPLE:
The knowledge of particle technology is essential in the formulation of dosage forms such as
powders, capsules, tablets, suspensions, emulsions & aerosols. The size of nature of particles
have direct influence on the drug action. The adequate knowledge of micromeritics is therefore
essential for a Pharmaceutist.
Optical microscopy is widely used to determine particle size in the range of 0.5-100m. A
disadvantage of this method is that the size obtained is only from the two dimensions of the
particles. No estimation of the depth of the particle is available. In addition large number of
particles must be counted for reliable results which makes this technique time consuming &
tedious. However this technique is preferred as the pressure of agglomerates & the heterogenicity
of the sample particles of more than one component may often be detected.
Page 1
Magnification value:
No. of divisions in stage micrometer
=
------------------------------------------------------- X 10
No. of divisions in Eye piece
d=X-A/C
d2
Fd
Fd2
interval
Page 2
PROCEDURE:
A. Optical Microscopy Method:
1. Clean the eye piece micrometer gently with cotton and place it inside the eyepiece of the
optical microscope view the scale of eyepiece micrometer through 10.
2. Place the stage micrometer and focus to view its calibration
3. Observe carefully and identify two points where the eyepiece and stage micrometer
values coincide. Enter these values as x1 y1 and x2-y2.
4. Calculate the magnification value of the eye piece micrometer using formula.
5. Spread a minute quantity of the given sample over a clean microscopic slide focus
through the eye piece.
6. Measure the No. of divisions occupied by the sample particles in the micrometer scale.
7. Change the field and count at least 200 particles in a similar way and enter the values in
the table.
8. Calculate the mean size standard deviation and size range using formula.
9. Submit the result with size distribution curves (histogram).
B. Sieving technique:
1. Arrange British standard sieves namely 20, 40, 60, 80, 100 and 120 in ascending
order.
2. Place 100 gms of given sample on the top sieve and shake for 20 minutes.
3. Remove the sieves and collect the same retain on each sieve.
4. Weigh the individual fractions and calculate the percentage powder retain on each
sieve.
5. Weigh, size, mean particle size using formula.
6. Plot weight under size over size curves and verify the mean particle size by
extrapolating the point of coincidence.
Seive number
Seive
(x) mm
(y) (gm)
powder retained
Powder
(percentage)
S.No
Description
w/w
Individual weight
REPORT:
The mean particle size and standard deviation of the sample was found to be
m.
The particle size range of given sample was found to be ____to ____m.
Page 4
m.
The mean particle size of given sample obtained by graphical approach is ____ m.
Ex. No. :2
Date
:
AIM:
To determine the critical micellar concentration of the given surfactant.
Page 5
REFERENCE:
PRINCIPLE:
Surface active agents are generally used to reduce the interfacial tension and facilitate
emulsification when surfactant molecules are added into a heterogeneous system they get
absorbed at the interface and increases the surface area. As a result the interfacial tension reduces
if the concentration of surfactant is increased, the surface gets saturated and excess goes into the
bulk of solution and forms aggregation or micelles. The micelle formation is useful.
Solubilisation process: The concentration at which micelle formation takes place is formed as
critical micellar concentration sharp changes in some physical properties such as osmotic
pressure, surface tension conductivity of detergency occur at CMC. For intense surface tension
remains constant above CMC due to the saturation of surface area.
MATERIALS/CHEMICALS REQUIRED:
Pipette, Stalagnometer, Specific gravity bottle, Beaker, Surfactant solution.
S.No.
1.
2.
Description
Total weight in gms
Weight of specific gravity bottle
Weight of specific gravity bottle +
3.
water
Weight of specific gravity bottle +
4.
0.05% solution
Weight of specific gravity bottle +
Individual weight
Page 6
5.
0.10% solution
Weight of specific gravity bottle +
6.
0.15% solution
Weight of specific gravity bottle +
7.
0.20% solution.
Weight of specific gravity bottle +
0.30% solution
S. No.
Sample solution
Number of drops
Number of drops
II
Average number
of drops
1.
2.
3.
4.
5.
6.
Procedure:
1.
2.
3.
4.
A&B.
5. Repeat the experiment with 0.05, 0.1, 0.15, 0.2 & 0.3 % w/v surfactant solution & record
the no. of drops.
6. Determine the density of all surfactant solution & calculate their surface tension of water
at 210 C are 0.9956 gm/ml of 71.18 dyn/cm respectively.
7. Plot a graph b/n concentration of surfactant solution (x-axis) and respectively surface
tension on (y-axis). Determine the by CMC extrapolation method.
Page 7
REPORT:
Critical Micellar Concentration was found to be _____ w/v for the given
surfactant.
Density:
Density = Weight of liquid/Weight of water X Density of water.
S. No.
Concentration
Density
Page 8
Surface tension:
Surface tensions = No. of drops of water /No. of drops of liquid X Density of liquid/Density of
water X 71.8 dynes
S. No
Ex. No. :3
Date
:
Concentration
Surface tension
AIM:
To determine the effect of lubricant on angle of repose and to compare the flow property of given
sample.
REFERENCE:
PRINCIPLE:
Department of Pharmaceutics, SRM College of Pharmacy
Page 9
Lubricant and glidants are generally known as anti frictional agents need in tablet manufacturing.
In order to improve the flow properties of granules and maintain product uniformity these agents
are used in lower concentration (1-2%).Lubricant (Magnesium stearate) act by giving
intermediate layer between granules and die walls. Glidants eg: Purified talc act by giving a thin
coat over the irregular granules space and lower the interparticulate friction. Above a particular
concentration lubricant and glidants retard the granule flow because of higher interparticulate
friction between these fine particles this effect can be defined by measuring the angle of repose.
MATERIALS /CHEMICALS REQUIRED:
Lactose, microcrystalline cellulose, starch, BSS sieve No 16, funnel, graph sheets, scale and
pencil.
PROCEDURE:
Prepare 200 gms of placebo granules by wet granulation technique. Mix 100gm of lactose &
100 gm of microcrystalline cellulose in a dry mortar. Add sufficient quantity of starch paste
(10%) to make a semisolid consistency. Pass the wet mass through BSS16 and dry at 60 0 C for
30 minutes in a hot air oven. Finally pass the dried granules through BSS20. Divide the granules
S.
Concentration
No.
lubricant
1. Sample
of Height
(cms)
Radius in cm
1st
2nd
h/r
Avg.
Tan-1
h/r
without
lubricant
2. 0.5 % w/w
3. Sample + 1% w/w
4. Sample + 2% w/w
lubricant
Page 10
into four equal portions and lubricate the portions 2,3,4 with 0.5%, 1%, 2% w/w magnesium
stearate. Do not lubricate the portion 1.
Fix a dry and clean funnel on to a burette stand at a particular height (2-3 cms)
Place a graph paper on the flat surface and allow sufficient quantity of the sample to flow slowly
through the funnel to form a heap that touches the tip of the funnel.
Draw the circumference of the heap carefully using a pencil locate the midpoint and
measure the radius. Repeat the experiment in triplicate and calculate the average radius. Carry
out the experiment for all the samples and determine the angle of repose by using the formula.
Compare the influence of lubricant.
REPORT:
Page 11
Formulation
Quantity of calamine
Suspending agent
Final
volume
of
suspension
1.
2.
3.
2.5 gms
2.5 gms
2.5 gms
0.25 gm of acacia
0.25 gm of bentonite
0.25 gm of sod.
Carboxy
4.
5.
6.
2.5 gms
2.5 gms
2.5 gms
methyl
cellulose
0.25 gm of tragacanth
0.25 gm of gelatin
0.25 gm of sod. CMC
+ Bentonite
7.
Control
Page 12
Ex. No. :4
Date
:
AIM:
To determine the effect of various suspending agents on physical stability of suspension.
REFERENCE:
PRINCIPLE:
Suspensions are coarse dispersion in which insoluble solid particles (or) dust are dispersed in
liquid media. The conditions in which the particle remains uniform distributed without
aggregation is called physical stability of suspension. The physical stability of suspension can be
improved by using suspending agent which usually reduces the interfacial tension and contact
angle and there by promote wetting and deflocculation combination of suspending agents
sometimes preferred are they produce excellent suspension.
Sedimentation volume (f) is defined as the ratio of final or ultimate volume of sediment to the
original volume of suspension stability. A suspension is said to be in flocculation equilibrium f=1
or near 1 such suspension are pharmaceutically stable and expectable.
Sedimentation volume = Vu/Vo = Ultimate volume of sedimentation/ Original volume of
suspension.
MATERIALS / CHEMICALS REQUIRED:
Calamine, acacia, bentonite, tragacanth, sodium CMC, bentonite, mortar and pestle and
measuring cylinders.
PROCEDURE:
Page 13
Weigh 2.5gm of calamine with solution and transfer to dry mortar. Triturate with the
suspending agent. All purified water in small amount and triturate until a paste like consistency is
obtained. Add more water and make up to the required volume (50ml). Transfer the suspension
to the measuring cylinder (50ml) and note the total volume of suspension. After 15 mins note the
ultimate volume of sedimentation for 2 hrs. Then calculate the sedimentation volume by the
following formula.
F = Vu/Vo
Vu = ultimate vol. of sedimentation
Vo = original vol. of suspension
Prepare calamine solution by using the above procedure for various suspending agents like
acacia (2%). Bentonite (3%), tragacanth (4%), sodium Carboxy methyl cellulose (1%), PVP
(1%), 0.5, 10, 15, 30, 45, 60, 90 min compare the sedimentation volume for each suspending
agent.
REPORT:
Page 14
Ex. No. :5
Date
:
AIM:
To determine the degree of flocculation induced by a flocculating agent in a suspension.
REFERENCE:
PRINCIPLE:
A suspension is a biphasic system consisting insoluble sparingly solid dispersed in a liquid
dispersion medium. The overall change existing on the suspended particle is zeta potential and is
a measurable indicating of change. Therefore, flocculating and deflocculation may be considered
in terms of zeta potential when zeta potential is high the particles remain dispersed and are said
to be deflocculated. The particles resist collision due to high zeta potential even with the particles
brought close by way or random motion of agitation. Zeta potential can be progressively lower
by the addition of an electrolyte (in which it is oppositely changed to that of the suspended
particle which is preferentially adsorbed at same concentration of electrolyte. The forces of
attraction terminate over the electrical forces of repulsion lightly) under these conditions zeta
potential is sufficiently lowered. The particles when they approach each other forms loose
aggregates commonly called as flocks. Then such a suspension is saw to be flocculated.
Flocculated is more preferred than the deflocculated because of easy redistribution of the
sedimented particles by shaking the container.
Degree of flocculation ():It is the ratio of ultimate sediment volume of flocculated suspension
(f) to the ultimate sediment volume of deflocculated suspension.
= F/F
Page 15
Procedure:
Prepare four separate suspensions each of 100 ml of 5% w/v of zinc oxide in water
containing 0%. Control, 1%, 2%, 3% w/v of Alcl3 as the flocculating agent. Transfer each
suspension separately to 100ml measuring cylinder. Shake well all cylinders keep it aside.
F = Vu/Vo
F = sedimentation volume
Vu = ultimate volume of sediment
Vo= total volume of suspension.
F = Vu/Vo, F = sedimentation vol. of deflocculation
B = F/F
B = Degree of flocculation.
REPORT:
Zinc oxide suspension was prepared. The degree of flocculation after 60 min was found
to be 1% suspension 2% suspension 3% suspension -
Page 16
Ex. No. :6
Date
:
FORMULATION
AND
EVALUATION
OF
IBUPROFEN
AIM:
To prepare and evaluate ibuprofen granules by wet granulation method.
REFERENCE:
PRINCIPLE:
The most widely used general method of tablet preparation is wet granulation. The wet
granulation forms of granules by binding the powder with an adhesive mix of biocompaction.
The steps involved in wet granulation.
1.
2.
3.
4.
5.
6.
Weighing
Mixing
Granulation
Lubrication
Screening
Compression
For small batches the ingredients are mixed and blended in the small mortar or stainless steel
pan. For large batches the sigma blade mixer or a thin shell blender may be used. The wet
granulation employs the solution or suspension or slurry containing a binder which is initially
added to the powder. Due to this liquid bridges or developed between the particles & the tensile
strength of this bond increase as the amount of liquid added increases once the granulating liquid
as been added. It is mixed continuously until the uniform dispersion is obtained. If the
granulation is over wetted the granules will be hard requiring considerable pressure to form the
tablets & the result may have mottled appearance.
Page 17
PROCEDURE:
Preparation of granules:Weigh and powder require ingredients mix thoroughly except a small
amount sodium starch glycolate (10%) talc & magnesium stearate. Grind the powder mass by
moistening with aqueous solution of around 3%. Concentration which is previously prepared,
prepare a damp mass and pass through sieve no 16 or 20. Then prepare granules are dried in the
over at 500 C for 15 min. Then the ginger starch (6%). Talc (2%) and magnesium stearate (1%)
are added to the dry granules then the granules were again subjected to sieving by using # 30.
Evaluation of derive properties of granules:
Tap density:It is defined as a ratio of mass of granules to the tap volume of the granules
procedure for tap density is that a weighed volume of powder is taken in a 100ml graduated
measuring cylinder. Fit a measuring cylinder in a tap density apparatus and let to 100 tappings.
The volume occupied by the powder is noted further another 50 tappings can be continued until
concurrent value is achieved this volume is final tapped volume.
Tapped density is evaluated by
Tapped density = mass of granules/tap volume.
Bulk density:It is defined as the ratio of mass of granules to the bulk volume of granules. A
weighed amount of powder is taken in a 100ml graduated measuring cylinder the initial volume
occupied by the powder is noted which gives the bulk volume of the powder.
Bulk volume = vol. of powder itself + vol. of inter particles + volume of intra particles.
Bulk density is calculated by using the formula
Bulk density = Mass of granules/Bulk volume
Page 18
Hausners ratio:This is also one of the method which is used for the determination of flow
property of the powder. It is determined by the formula
Hausners ratio = Tap density/Bulk density
Hausners ratio
0 -1.2
1.2 1.6
Flow property
Free flowing
Cohesive powder
Compressibility: This compressibility index also denotes the flow property of powder. It is
denoted by I it is given by the formula
I = (I Db/Dt) X 100
Db = Bulk density
Dt = Tapped density
A known amount of granules was taken in measuring cylinder. Measure the initial volume before
& after tapping the measuring cylinder & also measure the volume after 50 tappings. It is also
known as carrs consolidation index.
Carrs index
5 12
12 16
18 21
23 - 25
33 38
>40
Flow property
Free flowing
Good
Fair
Poor
Very poor
Extremely poor
Porosity:
W1 = weight of empty bottle =
W2 = weight of bottle + 1/4th of granules =
W3 = weight of bottle + 1/4th of granules+ H2o =
W4 = weight of bottle + H2O =
True volume:
Department of Pharmaceutics, SRM College of Pharmacy
Page 19
flow property
Excellent
Good
35-40
Possible
>40
very poor
Porosity: The granules will determine the flow property. It is defined as the ratio of the void
volume to the bulk volume of granule
Porosity = void volume/Bulk volume
= Bulk volume true volume/Bulk volume
Void volume = Bulk volume/true volume
True volume = volume of granule itself
% porosity = (1 Vp/Vb) X 100.
REPORT:
Ibuprofen granules were prepared and evaluated.
Page 20
gm/cc.
mg/ml.
Page 21
THE
ON THE
FORMULATION AND
Page 22
Procedure:
The weighed quantity of drug & excipients are uniformly mixed with the help of mortar
& pestle & passed through sieve no: 16 to get uniform size of particles. Wet granulation
technique is employed so the prepared different binding agents were added to the above mixture
& a collusive mass was prepared pass the mass through sieve no: 14 to get granules. Dry the
granules through sat 60 degree C for 15 min. After drying pass the granules through set of sieves
18 & 44 to get the uniform size granules. Add 15% of fines to the above obtained granules. Add
the manufacturing granules & mix thoroughly then compress the granules to tablets.
Weight variation test:
Above 20 tables are weighed & average wt is calculated. The tablets having highest &
lowest weight are to e formed in above 20 tables. The maximum deviation is to be calculated.
The no. of tablets deviating from the specification is the monograph is to e noted down.
S. No.
1.
% deviation
+
Report:
Page 23
Ex: 8
Formulation and evaluation of ferrous sulphate capsules
Aim:
To prepare and submit 10 capsules of ferrous sulphate capsules.
Principle:
Capsules represent the unit dosage forms in which the one usual dose of the drug has been
accurately placed within the capsule. Capsules have been used as popular dose forms because
they provide a smooth slippery, easily swallowed, tasteless shell for drugs and is practically
beneficial for drugs having an unpleasant taste or odour.capsules are made principlyof gelatin
blends and may contain small amount certified dies,opacifying agents, plasticizers and
preservatives.
Capsules have been made with methyl cellulose, PVA and denatured gelatin to
modify their solubility produced an enteric effect.Geltin is an heterogeneous product derived by
irreversible hydrolytic extraction.Two types of capsules
1.Hard gelatin capsules.
2Soft gelatin capsules.
Page 24
S.NO
Ingredients
Ferrous sulphate
Starch
Lactose
Talc
Magnesium stearate
For 1 Tablet
For 10 Tablets
PROCEDURE:
Mix ferrous sulphate with starch and lactose,moistuned with sugar
syrup(20%) and granulate through sieve no:12.Dry the granules at 500 c for 20 min in hot air
oven. Add talc and magnesium stearate to the dried granules. Then pack it in empty capsule shell.
EVALUTION of capsules:
Capsule size determination:
The average weight of 20 empty capsules was determined.
Capsule size
Department of Pharmaceutics, SRM College of Pharmacy
Capsule weight
Page 25
UNIFORMITY TEST:
Weigh 20 capsules. Remove the contents of capsule of means of cotton
swab. Then take the tare wt of empty capsules which gives the net wt of empty capsules.
S.NO
Weight
SPECIFICATION:
Page 26
Not more than one individual weight should not be deviated by more than 1% with that of
average weight.
DISINTEGRATION TEST:
By taking 6 capsules being used for the determination as per monograph
of ferrous sulphate capsules. Not more than one capsule should exceed from I.P limit. If it is
failed, repeat with another 6 capsules and determine the time
IDENTIFICATION TEST:
Boil one capsule shell with 20 ml of water. Allow it to cool and centrifuge.
To 5ml of supersaturated liquid, add 1ml of picric acid solution. To another 5ml add 1ml of
tannic acid. A ppt should be formed in each case.
DISSOLUTION TEST:
Carry out dissolution test for ferrous sulphate capsules with 900 ml of 0.1
Hcl at 50 rpm wit paddle method for 90 min at37 020c.A periodic time interval withdraw 5ml of
sample and filter promptly through membrane filter. Reject first few drops and dilute for
necessary concentration& measure the absorbance at 248 nm.
DILUTION
TIME
ABSOBANCE
COCENTRATION
FACTOR
AMOUNT
AMOUNT
IN
IN
5 ML
900 ML
CDR
CD
Page 27
Concentration(x ) = y-m
c
Label claim= Amount of tablet
* 100
L.C
REPORT:
Formulation and evaluation of ferrous sulphate capsules were done.
Weight variation of capsule were found to be
Positive deviation=
Negative deviation=
The disintegration time for prepared capsules was found to be=
The %cumulative amount of drug release was found to be=
The net uniformity content was found to
Department of Pharmaceutics, SRM College of Pharmacy
Page 28
EXP:01
EVALUATION OF PRIMARY PACKAGING MATERIAL
Aim:
To evaluate and report the given primary packaging materials
Materials required:
Blister packs, strip pack, glass bottles, polyethylene bags, electronic balance, screw guage,
vernier calliper, label, centimetre scale
Reference:
Indian pharmacopoeia 1996 vol-II
Discussion:
In the pharmaceutical industry it is vital that the package selected adequately pressure the
integrity of the product. The material selected must have the following characteristics.
Page 29
Utmost care should be taken while selecting the packaging materials were patient acceptance is
also a major criteria. Stability aspects should also be considered
Evaluation of unit dose materials: The primary packaging materials are evaluated for length,
breadth, thickness and GSM (g/m2).particularly for aluminium foil, paper foil, pvc foil, glass
bottle. Apart from this for glass bottles over flow capacity (ofc), internal &external diameter is
measured.
All this tests will give strength, purity of materials of package material which
should be compared with standard specifications.
Blister pack: They are used for packing unit dose of tablets, capsule etc. To the medicament it
act as a compartment in a base material to made of paper, plastic and materials of floor a
combination of them. The protection depends on the design and method used to pack
Types: 1) PVC with AL
2) PVC with Paper
Strip Packing:
In this 2 webs of materials will be sent with various types of the medicament such as
tablets and capsules. Aluminium foil is commonly used to manufacture strip pack and provide
good barrier against moisture penentration.these are the most widely used for packing of tablets
and capsule. The can be evaluated for 4 parameters
o
o
o
o
Length
Breadth
Thickness
GSM(g/m)
Text Matter: This gives information about the product to the patients, doctors and retailers. The
test matter should be legible and should be represented in a clean manner such as shake well
before use
GSM (g/m):
Page 30
It is a parameter which is calculated to give the information about the quantity of the packing
material and to see whether it is within the required specification. Indirectly the mechanical
strength of the packaging material can be calculated by taking a 1cm X 1cm (lxb) on electronic
balance and the volume obtained is in (g/m).
Thickness:
The thickness of the given material is checked or evaluated using a screw gauge. The length and
breadth is measured using a scale.
Bottles:
They may be, made of either glass or plastic. They are evaluated for the following parameters.
Over Flow Capacity [OFC]:
The bottle taken for the test is washed properly. Then it was filled with water up to the
brim fill it till it over flows and then volume of the water is measured by placing the
volume in a measured cylinder. This gives information about the capacity of the bottle.
Expressed in millilitres [ml]
Other parameters: Other parameters such as total height, diameter of cap, diameter of border
are measured using vernier calipers.
Polyethylene bags or covers:
These are also evaluated for the above parameters such
Length
Breadth
Thickness
GSM(g/m)
Parameter
Bottle-I
Bottle-II
Page 31
Description
Total Height
Cylindrical diameter
Diameter of neck
Diameter of base
Diameter of Cap
REPORT:
The given primary packaging material are evaluated and the results are as follows
Parameters
Al-Al
Paper-Paper
Length
Breadth
Department of Pharmaceutics, SRM College of Pharmacy
Thickness
GSM
Page 32
Parameters
PVC-Al
PVC-Paper
Length
Breadth
Thickness
GSM
EXP: 02
EVALUATION OF SECONDARY PACKAGING MATERIAL
Aim: To evaluate and report the given secondary packaging materials.
Materials required:
Electronic balance, screw gauge, vernier caliper, scale, labels catch covers, shippers.
Discussion:
Secondary packaging materials are those materials which dont come in direct contact
with the product. These are to improve the mechanical strength and tensile strength of the
product during handling. They include cartons, shippers and labels
The labels are mainly put up to provide information to the patient and help in
medication of the product. The label should be sticked on the container completely. There should
be a provision to see the contents.
Page 33
The label should make proportional to the size of the container. The secondary packaging
materials are evaluated for test matters, length, breadth thickness and GSM.
EVALUATION:
Text Matter:
This gives information about the product to the patients, doctors and retailers. The text
matter is printed on label and shipper also.
Thickness:
The thickness of the given material is checked or evaluated using a screw gauge. The
length and breadth is measured using a scale. The thickness of cartons plays a major role since
they have enough resistance to with stand any damage during transportation.
GSM (g/m):
It is a parameter which is calculated to give the information about the quantity of the
packing material and to see whether it is within the required specification. Indirectly the
mechanical strength of the packaging material can be calculated by taking a 1cm X 1cm (lxb) on
electronic balance and the volume obtained is in (g/m).
Other parameters:
Other parameters such as length and breadth were calculated by scale. In case of shippers
no of ply present in it are to be determined. The number of ply present determines the strength of
the product.
e.g.: 3 ply, 5 ply, 7 ply shippers are available. The more the number of plys the more the
strength of the shipper. (i.e. the strength of shipper is directly proportional to the number of
plys).
REPORT:
The given secondary packaging material was evaluated and the result are as follows
Parameters
Small
Medium
Large
Cartons
Length
Breadth
Thickness
Department of Pharmaceutics, SRM College of Pharmacy
Page 34
Parameters
1PLY
2PLY
3PLY
Shippers
Length
Breadth
Thickness
GSM
EXP: 03
EVALUATION OF SECONDARY PACKAGING MATERIAL
Aim:
To carry out the evaluation test for the given glass containers
Materials Required:
Powdered glasses, whole container, sieve no-20, Distilled water, 0.02 N HSO and
methyl red.
Reference:
I.P 1996, Theory and Practice of industrial pharmacy By LACHMAN.
Powdered Glass Test:
Preparation of glass powder specimen: Rinse thoroughly the ampoules with purified
water, dry with steam. Take the ampoule and place it in a mortar pestle and grind it to fine
powder. Inside the pestle a hole is made through a butter paper and places it in a mortar for
preventing the glass from striking the eyes and face. Pass the powder through sieve no-20 and
collect the powder and use it as specimen.
Washing Of Specimen:
Transfer the specimen i.e. 10 g to a 250 ml conical flask and wash it with about 30 ml of
acetone. Repeat the washing by acetone. Repeat the washing and carefully decant the acetone.
After washing the specimen should be free from agglomerates of glass powder. Use this
specimen within 48 hr.
Department of Pharmaceutics, SRM College of Pharmacy
Page 35
Method:
Transfer 10 gm of accurately weighed specimen to a 250 ml conical flask. Add 50 ml of
high purity water to the flask and seal. Place in the auto clave and close it securely. Adjust the
temp to 1202 c and maintain for 30 min. reduce the heat to atmosphere condition cool the
flask. Decant the solution into another conical flask. Wash the residual. Powders with 15ml of
high purity water and again wash the residual. Powder with 15ml of high purity water and again
decant into conical flask. Titrate immediately with 0.02N HSO by using methyl red as
indicator. Record the volume of 0.02N HSO used. The volume doesnt exceed the indicated
limits for the type of glass container.
WATER ATTACK TEST:
Rinse thoroughly the test container with high purity water. Fill each container to 90% of
overflow capacity with high purity water. Cap the container and place them in the autoclave.
Adjust the temp to 121c and maintain for 30 mins, reduce the heat to bring it to atmospheric
temperature. Empty the contents from the container in to a 100 ml graduated cylinder. The
content should be washed to get a volume of 100 ml. Transfer the solution to 250 ml conical
flask and titrate with 0.02m solution. Repeat it with blank. The sample reading is subtracted from
the blank and the volume is reported. The volume doesnt exceed the limit indicated in the table.
Report whether the glass container passes the test or fails the test.
Test
Containers
Limits(0.02N HSo)
Type-I
1ml
Type-II
8.5ml
N.P
15ml
Type-I(100 ml or less)
0.7
0.2
Page 36
Sample
Contents
Burette reading
Initial
Sample
Sample+50
Sample+50
ml
water+indicator
Contents
water+
Autoclaved
water+indicator
indicator
point
methyl
colourles
red
s to pink
0 ml
Initial
water+indicator
Blank:
value
Final
Burette reading
indicator
End
0 ml
water+indicator
Blank:
Indicato
ml
Autoclaved
A
Titer
water+
Titer
Indicato
End
value
point
methyl
colourles
red
s to pink
methyl
colourles
red
s to pink
Final
0 ml
0 ml
0 ml
0 ml
REPORT:
EXP: 04
PREPARATION AND EVALUATION OF SODIUM CITRATE INJECTION
Department of Pharmaceutics, SRM College of Pharmacy
Page 37
Page 38
EXP: 05
ACCELERATED STABILITY STUDIES OF ASPIRIN
Aim: To determine shelf life of aspirin solution in 0.1 N Hcl by using accelerated stability
studies.
Reference: Physical Pharmacy by Alfred Martin- 4th edition.
Requirements:
Equipment
volumetric flask
conical flask
Pipette
test tubes
Burette
Thermostat
water bath
Colorimeter
250 ml
250 ml
10
ml,
5ml
20 ml
50 ml
Page 39
Spectrophotometer
Chemicals
Salicylic acid
Ferric nitrate
Hcl solution
1g
100ml
100ml
(0.1 N)
Aspirin
Alcohol
1g
2 ml
Principle:
Accelerated stability studies are an experimental design to evaluate stability of product by
accelerating rate of reaction. In general, the rate of reaction increases with decreased in
temperature. A quantitative relationship between temperature and rate of reaction was reported
by Arrhenius equation.
The equation is
k =AeEa / RT
Where
Ea
2.303 RT
Page 40
According to this equation: A plot can be drawn by taking log K on Y-axis and 1/T on X-axis.
The slope gives energy of activation.
ta=( slope )(2.303 ) ( R)
Where R= 8.314 j/m.k
Under acidic conditions, the degradation of aspirin follows pseudo first order kinetics
Procedure:
Salicylic acid stock solution (1 mg/ml): weigh 100 mg salicylic acid & transfer in to 100 ml
volumetric flask & make up to 100 ml.
Ferric Nitrate solution (4%): weigh 4 g of FeNo & transform in to 100 ml volumetric flask &
make up volume to 100 ml.
Standard graph of Salicylic acid:
Prepare various dilutions from stock solution (as shown in table) in 20 ml test tube.
Add 5 ml FeNo solution to each test tube for development of colour.
Measure absorbance of above solution at 547 nm in colorimeter & report readings in
same table.
Plot the graph by taking conc. on X- axis & absorbance on Y-axis.
Accelerated stability study:
Decomposition at 40C:
Page 41
Process the data according to table & plot a graph of log % aspirin on X-axis &
Decomposition on Y-axis
Determine the slope of curve using equation (4)
Calculate the rate constant K using equation (5)
Report the data in table
Repeat the procedure at 60C & 80C.
Report:
The activation energy of aspirin by accelerated stability studies was found to be
The shelf life of aspirin solution in 0.1N Hcl solution using accelerated stability studies
was found to be
EXP: 6
FORMULATIONS AND EVALUATION OF SHAMPOO
AIM: To prepare and evaluate 50gm of shampoo
Principle: Shampoo cleanses the hair of accumulated sebum, scalp debris and residue of hair
grooming preparation by involving as under of complex physical phenomenon like wetting
,combing, emulsifying it by lowering the interfacial tension to such are extent that it always
allows the dirt or oil particles to be displaced.
Procedure: Sodium lauryl sulphate ,coconut oil, anhydrous lanolin, and Nacl are dissolved in
water .dissolve NaOH in water add it to the above solution and heat it at 70 0c stirring as it was
heated separately and added to the above at the same temperature with agitation cool the mixture
and add the perfume, preservative, colour and finally the volume was adjusted to required
quantity with distilled water.
Evaluation: The shampoo can be evaluated for
Department of Pharmaceutics, SRM College of Pharmacy
Page 42
Evaluation test:
Test for foam stability: 2gm of sample was taken and shaken with 50ml of distilled water and
foam height was measured using measuring cylinder for a time period of 90mins
Test for detergency and colour reaction: place 5gmof wool yarn in gauze soak it in 2oml of
water continue raising 1gm of shampoo in a flask placed the general wool yarn. The temperature
of water should be 35c .shake the flask for 4 mins at the rate of 50times/min. Remove the
solution and dry the sample and weigh it .calculate the amount of soil removed under
experimental conditions.
Test for volatile matter: 5gm of shampoo was dried on a Petri dish and heated on a water bath
until most of volatile matter escapes. Heating was continued at 1050c for 2hours in an oven the
cool and desiccators it. The residue was weighed
residue weig ht
X 100
sample weig h t
Test for inorganic salts: 2gm of sample was weighed in a facial crucible and ignited and heated
at 450oc to destroy the organic matter and cool and desiccate it. few drops of hydrochloride was
added and heated again to dryers and cool . The final residue was weighed.
Test for surface activity and drop count method: stalagnometer was cleaned thoroughly and
rinsed with distilled water and dried with acetone. A clean rubber tube is attached with a screw
clip at the top of stalagnometer to regulate the flow of liquid. The flattened stalagnometer is
dipped in reference liquid which is placed in clean beaker. Liquid is sucked with the rubber
tubing until rinses is above.
Page 43
The screw tip is closed tightly because that the liquid meniscus does not fall. The
stalagnometer is fixed in the stand and screw tip is loosened carefully to allow the liquid to run
slowly. The cubes of drops formed are counted from the liquid between A and b. The counting is
repeated at least twice the stalagnometer is the filled with test liquid and number of drop formed
is determined.
Determination of PH: 3gm of sample is dissolved in 27ml of water and stirred well and P H meter
(liquid3-9)
Report: The shampoo was prepared and evaluated. The evaluation parameter as follows.
S. No
PARAMETERS
MARKETED PRODUCT
Retention time;90min
2.
73%
3.
14.8
4.
20.2 dyne/cm
5.
pH
5.6
FORMULATED PRODUT
Page 44
Exp: 7
FORMULATION AND EVALUATION OF FACE POWDERS
Aim: To Formulate and evaluate 10g of face powder.
THEORY:
The quantity of face powder should be fine and good enough. The ingredients must be
finely distributed and adhere to the skin and must be dissipated within few minutes. It must show
good absorption and transparency.
PROCEDURE: All the ingredients are mixed and sieved. The colour and binder are added. The
mixture is sieved and hot dried in air.
s. no
Ingredients
For 100gm
1.
Kaolin
3g
2.
Talc
74g
3.
Magnesium sterate
1.5g
4.
Magnesium carbonate
0.5g
5.
Zinc oxide
15g
6.
Perfume
Q.s
For 10gm
DISCUSSION:
EVALUATION: The evaluation and assessment of various powdered products are essential to
justify the quality of formulated product.
Department of Pharmaceutics, SRM College of Pharmacy
Page 45
Angle of Repose:
The flow property can be studied by measuring the angle of repose by allowing the powder to
fall on the plate from funnel and measuring the height and radius formed.
Angle of Repose can be calculated by:
tan=
h
r
Particle size:
The powder is allowed to pass through sieve number.
Microscopy:
The powder is diluted with little amount of glycerine and is kept on the slide viewed under the
microscope and particle size is measured with eye piece micrometer which is pre calibrated with
the stage micrometer.
Bulk Density: Weigh 10g of powder and place it in measuring cylinder and note the bulk
volume.
Bulk Density=
M ass
Bulk Volume
Tapped density: Weigh 10g of powder and place it in measuring cylinder. Tap 100 times and
note the tapped volume.
Tapped Density=
Mass
Tapped volume
REPORT:
10 gm of face powder was prepared and submitted and following parameter was evaluated.
s.no
Parameter
Marketed product
Formulated product
Page 46
1.
Bulk density
0.390
2.
Tapped density
0.512
3.
Angle of repose
31 082I
4.
Particle size
24.56m
Exp-8
PREPARATION AND EVALUATION OF TOOTH PASTE
AIM:
To prepare and evaluate 20gm of tooth paste
Theory:
Tooth paste is categorised under synthetic detergent containing agent that as a bactericidal
bacteriostatic enzyme inhibiting or acid neutralizing qualities. Thus it reduces dental diseases and
removes mouth odour.
Department of Pharmaceutics, SRM College of Pharmacy
Page 47
Procedure: The gum or binder or soap or soap less detergents are mixed well and with glycerine
and water mixture then gum tragacanth , mucilage, blended solids are mixed. Flavours were
incorporated towards the end.
Discussion:
Evaluation test:
Foam character: This test is especially required for foaming tooth paste. 1gm of the product is
mixed with 50ml of water taken in a measuring cylinder and shaken. The foam thus taken found
was studied natural stability and solubility.
pH: the pH of the dispersion of 10% of the product was determined by pH meter.
Particle size: the particle size was determined using microscopic technique.
Report:
20gm of tooth paste was prepared and submitted the following parameters was evaluated
S.N
Evaluation parameter
Marketed product
o
1.
Foam character
3.33
2.
pH
3.
particle size
14.98-42.45
Prepared product
Page 48
Exp:-9
PREPARATION AND EVALUATION OF LIPSTICK
Aim: to formulate and evaluate 10g of lipstick
Theory:
A good quality of lipstick should have the following ideal qualities. A lipstick basically consists
of an oily wax fit enough to form dispersed in oily or red pigment .suspended drug with a
suitable perfume. The softening point of lipstick should be sufficiently high to that the lipstick
can with stand high temperature. Indian standards 1975 prescribe that the particle size of
undispersed pigments should not be more than 40 .
In this experiment bees wax was poured in to the stick which keeps it solid even in warm
climates castor oil is used in unique along with vegetable oil, high quality of oil is used in
delaying the shining from the molten lipstick mass of lightening the tendency of lipstick
Lanolin is used as plasticizer agent cetyl alcohol is used for its thyrotrophic properly .perfume
was added to overcome the fatty odour of the base
Page 49
S.NO
1.
INGREDIENTS
Hard paraffin
FOR 100g
10gm
2.
Bees wax
15gm
3.
Lanolin
5gm
4.
Cetyl alcohol
5gm
5.
Castor oil
65gm
6.
Eosin
1%
7.
perfume
Q.s
FOR 10g
PROCEDURE:
The bases are melted first then the acid erosion is dissolved in alcohol with the help of gentle
heat. The base is then added to erosion .The pigments are then added. Finally the lip sticks are
passed in to lipstick moulds.
Discussion:
Department of Pharmaceutics, SRM College of Pharmacy
Page 50
Bees wax
used as base
Hard paraffin
Lanolin
Cetyl alcohol
thyrotrophic property
Eosin
colouring agent
Perfume
Evaluation test:
Breaking point: lipstick is held horizontally in a socket fitting over about inch of it base and
weight is applied at measured distance from the edge of support. The weight is increased by
applying predetermined increase of weight for every 30sec until lipstick breaks.
Texture: Appearance of product is observed
Colour match test: The prepared lipstick was subjected for colour match test also for colour
comparison and colour match the skin
Stability: Determined by keeping the product at 400c in hot air oven for half an hour .if it melts
the test fails.
Particle size analysis: Particle size is determined by microscopic technique
REPORT:
10gm of lipstick was prepared and submitted.
S.no
Evaluation parameters
Marketed
Formulated
Page 51
1.
2.
Particle size
3.
Stability
4.
Texture
Page 52