PRACTICAL MANUAL BASED ON TABLETS

Ms. TENY SARA THOMAS
MOUNT ZION COLLEGE OF PHARMACEUTICAL
SCIENCES AND RESEARCH, ADOOR, KERALA
ASSISTANT PROFESSOR
B.PHARM FIFTH SEMESTER
FORMULATIVE & INDUSTRIAL PHARMACY

 To carry out preformulation studies of a given
powder.

 Given powder
 Measuring cylinder
 Funnel
 Burette Stand

Preformulation studies are an essential component of drug
development whereas it supports development of formulations, for different
stages of clinical trials. The word preformulation is composed of two words
pre and formulation. Activities done prior to formulation development are
called as preformulation studies. It provides the scientific basis for
formulation development.
Objectives:
 To generate useful data needed in developing stable and safe dosage
forms that can be manufactured on a commercial scale.
 To provide an in-depth knowledge and understanding of the physical
characteristics of a candidate drug molecule prior to dosage form
development.
 To generate useful information on how to design a drug delivery system
with good bioavailability.
Goals of preformulation:
 To establish the physicochemical parameters of a candidate drug
molecule.
 To determine the kinetic rate profile of drug substances.
 To establish the compatibility of a candidate drug molecule with common
excipients.

Preformulation studies involves the study of the various
parameters:-
 Angle of repose : - include the definition from the theory
notes
 Bulk density :- include the definition from the theory notes
 Tapped density :- include the definition from the theory
notes
 Hausners ratio :- include the definition from the theory notes
 Carr’s compressibility index :- include the definition from the
theory notes
Also include the tables of Carr’s compressibility index,
Hausners ratio and its relation to flowability of particles and
table of Angle of repose and type of flow, from the theory
notes.

 BULK DENSITY
An accurately weighed quantity of powder in terms of
mg was transferred to a 100ml measuring cylinder and
the volume occupied by the powder in terms of ml was
recorded.
Bulk Density = weight of powder / volume packed in
ml
 TAPPED DENSITY
Loosely packed powder in the cylinder was tapped
100 times on a plain hard surface and volume occupied
in ml was noted.
Tapped density = weight of powder / tapped volume
in ml

 HAUSNER’S RATIO
Hausner’s ratio is calculated with the following
formula .
Hausner’s Ratio = Tapped density / Bulk density
 CARR’S COMPRESSIBILITY INDEX
Carr’s compressibility index is calculated with the
following formula.
Carr’s compressibility index
= {(Tapped - Bulk) Denisty / Tapped density } * 100

 ANGLE OF REPOSE
A funnel was fixed and secured with its tip at a height
(h) from 2cm above graph paper which was placed on a
horizontal surface. The powder was dropped and the
radius(r) was measured. Angle of repose can be
measured by the following equation:
tanθ = h/r

Preformulation studies of the given powder was conducted
and the following results were observed :-
a) Bulk denisty = ________ gm/ml
b) Tapped density = ________ gm/ml
c) Hausners ratio = _________
d) Carr’s compressibility index = ___________
e) Angle of Repose - __________ ⁰
From the above observations the given powder was
found to have ______________ flow property.

 To prepare and submit granules for the tablets
that contain 500mg paracetamol in each tablet
using wet granulation method.

 Paracetamol powder
 Starch powder
 Starch paste
 Talc
 Stand
 Sieves
 Beaker and stirrer

Wet granulation is the oldest and most widely used method of tablet
preparation. The powdered and mixed tablet ingredients are converted into
moist coherent mass and then into granules before compression into tablets.
The essential steps that are involved during tablet granulation are :-
weighing, sifting, blending, wet screening, drying, dry screening, and
lubrication.
This method is time consuming. The process involves blending and
mixing of the active ingredient, disintegrant, and diluents. The mixed
materials are sifted through a suitable mesh to remove or to break the
lumps. The sifted material are converted into a damp mass using a binder
solution, then forced through appropriate sieves to produce granules. The
wet granules are dried in oven. The particles may agglomerate and form
lumps, so sieving after is often required after drying. To the dried granules,
lubricant is added so as to improve the flow property. The prepared
granules are then used for compression to produce granules.
Paracetamol are commonly used as analgesics and anti-pyretics.
Paracetamol is not susceptible to moisture or heat , so wet granulation is a
best method to prepare granules. Starch can act here both as glidant and
disintegrant.

A. PREPARATION OF PARACETAMOL GRANULES
1. Preparation of the granulating medium
10gm starch is weighed and transferred into a
beaker. 50ml of water is added into the beaker and the
slurry is prepared by stirring with a glass rod. 25ml of water
is added and beaker is placed on a wire mesh. The slurry is
heated using a bunsen burner to obtain a paste. Remaining
25ml of water is added and stirred well and heated to form a
translucent starch paste.
2. Weighing and sifting of powders
Desired quantities of paracetamol and starch
powder are weighed as per the working formula. These
powders are passed through sieve #60.

3. Blending of the powders
The sifted powders are mixed thoroughly in a mortar with a
pestle until uniform blend is obtained
4. Wet Granulation
A small quantity of granulating medium is taken into a watch glass
and weighed in gram. From this little quantity of granulating medium are
transferred into the mortar containing the powder and then triturated. This
step is continued until a smooth dough is formed. The end point of addition of
the granulating medium is determined by the following :-
The wet mass is taken
and it is then pressed
with between the
thumb and the
fingers.
The ball crumbles
under the moderate
pressure without the
giving fines
Stop adding the
granulating medium.
The mass is ready for
granulation.
The ball breaks
forming many fines
Continue adding the
granulating medium.
The wet mass is passed through sieve 10# in a tray. This process breaks
the wet mass into wet granules.

5. Drying
The tray containing the granules is placed in a hot air
oven and the temperature is adjusted to 60℃. Drying is continued
until the moisture of the granules is reduced. The oven is switched
off, the granules are allowed to reach room temperature.
6. Dry screening
The total granules are weighed in gms. The dry granules
are passed through sieve 20# and then through sieve 40#. Granules
retained in sieve 20# are called coarse granules and the granules
retained in sieve 40# are called fines. The amount of fines to be
added are then calculated.
7. Dry blending
15% of fines calculated and weighed are added to the
coarse granules. The required quantity of magnesium stearate
(lubricant) and talc (glidant) is added. The ingredients are blended
in order to get uniform distribution of ingredients, so the granules
are ready for compression.

Paracetamol granules IP (500mg) for 40 tablets was
prepared, labelled and submitted.

EXPERIMENT 3 –
PREFORMULATION STUDIES OF
PARACETAMOL GRANULES IP
ASSISTANT PROFESSOR

AIM
□ To evaluate the prepared paracetamol granules
for the tablets that contain 500mg paracetamol
in each tablet.

MATERIALS REQUIRED
□ Prepared paracetamol granules
□ Funnel
□ Burette stand
□ Measuring cylinder

PRINCIPLE
Wet granulation is the oldest and most widely used method of tablet
preparation. The powdered and mixed tablet ingredients are converted
into moist coherent mass and then into granules before compression into
tablets. The essential steps that are involved during tablet granulation are :-
weighing, sifting, blending, wet screening, drying, dry screening, and
lubrication.
This method is time consuming. The process involves blending and
mixing of the active ingredient, disintegrant, and diluents. The mixed
materials are sifted through a suitable mesh to remove or to break the
lumps. The sifted material are converted into a damp mass using a binder
solution, then forced through appropriate sieves to produce granules. The
wet granules are dried in oven. The particles may agglomerate and form
lumps, so sieving after is often required after drying. To the dried granules,
lubricant is added so as to improve the flow property. The prepared
granules are then used for compression to produce granules.
Paracetamol are commonly used as analgesics and anti-pyretics.
Paracetamol is not susceptible to moisture or heat , so wet granulation is a
best method to prepare granules. Starch can act here both as glidant and
disintegrant.

EVALUATION OF PARACETAMOL GRANULES
 BULK DENSITY
mg was transferred to a 100ml measuring cylinder and the
volume occupied by the powder in terms of ml was
recorded.
ml
 TAPPED DENSITY
100 times on a plain hard surface and volume occupied in
ml was noted.
Tapped density = weight of powder / tapped volume in
ml
PROCEDURE

 ANGLE OF REPOSE
A funnel was fixed and secured with its tip at a height (h)
from 2cm above graph paper which was placed on a horizontal
surface. The powder was dropped and the radius(r) was
measured. Angle of repose can be measured by the following
equation:
tanθ = h/r
The experiment is repeated to get the correct value. In
general, angle of repose decreases with increase in particle size.
Addition of a glidant, here talc, in low concentration decreases
the angle of repose and in higher concentration, increases the
angle of repose.

REPORT
Paracetamol granules were evaluated and the following results were
observed :-
a) Bulk density = ________ gm/ml
b) Tapped density = ________ gm/ml
c) Hausners ratio = _________
d) Carr’s compressibility index = ___________
e) Angle of Repose - __________ ⁰
From the above observations the prepared granules was
found to have ______________ flow property.

 To prepare 40 tablets of paracetamol each
containing 500mg of paracetamol as drug.

 Paracetamol
 Starch powder
 Starch paste
 Talc
 Sieves
 Beaker and stirrer

Pharmaceutical Tablets are solid dosage forms
containing one or more drugs with or without the addition of
excipients. Addictives or excipients are mainly incorporated to
enhance physical appearance, stability, disintegration, or
breakup of tablet after administration. These excipients ensure
that the tabletting operation can run satisfactorily and to ensure
that tablets of specified quantity and quality are prepared.
According to Indian Pharmacopoeia, pharmaceutical
tablets are flat or bi-convex discs manufactured by compressing
a drug or a mixture of rugs with or without suitable excipients.

For increased production, rotary press tablet
compressing machine is used. The tablet compressing
machine comprises of punches and dies revolving
continuously while the tablet granules flow from a
hopper to the die cavity through a feed frame. This
method promotes the uniform filling of die, therefore
an accurate weight of each tablet is achieved.
Compression by the upper and lower punch produces a
slow squeezing effect on the material in the die cavity.
Here, the entrapped air also has a chance to escape
during compression.
Paracetamol tablet is an orally ingested compressed
tablet prepared by wet granulation process. Starch paste
is used as binding agent and starch powder as a
disintegrating agent. Talc is used as an glidant.

Weigh the required amount of paracetamol powder
and talc and transferred into a mortar, which is further
mixed thoroughly. A wet mass of the mixed powder is
prepared by using 10% starch paste as a binding agent.
Pass through sieve no 10 to get uniform granules. Dried
in a hot air oven at 70℃. After drying, pass the granules
again through sieve no 20 and sieve no 40. Weigh out
the total amount of coarse granules and calculate the 15
% of the fine granules required. Mix the calculated
amount of fine granules into the coarse granules. Finally
add 2% talc of the total amount of granules. Mixed well
and compressed in tablet compressing machine to
produce tablets.

40 tablets of paracetamol each containing 500mg of the
drug was prepared, labelled and submitted.

PRACTICAL 5 – EVALUATION OF
PREPARED PARACETAMOL
TABLETS
ASSISTANT PROFESSOR

AIM
□ To perform the quality control tests of the
prepared paracetamol tablets each containing
500mg of paracetamol as the drug.

PRINCIPLE
In Process Quality Control tests are routinely run
to monitor the compression and manufacturing
process.
Quality Control Tests are generally divided
into two :-
1. Official Tests
2. Non - Official Tests
Official tests include :- weight variation tests,
thickness tests, friability tests, hardness tests,
disintegration tests, and tablet dissolution tests.

a) Weight variation tests :- The filling of the die
cavity in the tablet punching machine determines
the weight of the tablet.
AVERAGE WEIGHT PERCENTAGE
80mg or less 10
8-250mg 7.5
250mg or more 5

b) Thickness test :- Thickness of the tablet may be
measured using micrometer, or sliding caliper scale.
Physical dimensions control the weight of the tablet.
c) Friability test :- is done to check the ability of a
tablet to break into smaller pieces under pressure,
mechanical shock, or stress during handling and
transportation. Strength of the tablet plays an
important role in the dissolution and disintegration of
the tablet. After the friability test, tablets are
inspected for breakage and the percentage of tablet
mass lost through chipping.

Friability test is done using the Roche Friabilator
which consists of a drum or plastic chamber having
diameter 283-291mm and a depth of 36-40mm.
Rotation speed of drum is 25rpm. Tablets are weighed
individually and placed in the plastic chamber and
rotate it for 4 minutes or set 100 number of rotations.
During each revolution, tablets fall from a distance of
about 6 inches. After 100 revolutions or 4 minutes,
remove the tablets from the chamber. Tablets are
dusted and then weighed. Percentage weight loss is
calculated. If there is a loss in weight, this indicates
friability. Loss of 0.5-1% of the weight is considered
acceptable.

d) Hardness test :- Tablets require a certain amount
of strength or hardness during transportation and
handling. Generally, greater compression force is
applied, harder the tablets. Certain tablets such as
lozenges or buccal tablets are intended to dissolve
slowly, so they are made intentionally hard. For
tablets meant for immediate release, they are
intentionally made soft. Tablets should be sufficiently
hard to resist breaking during normal handling and
soft enough to disintegrate properly after swallowing.
Two different types of hardness testers are available :-
□Monsanto Hardness Tester
□Pfizer Hardness Tester

□Monsanto Hardness tester :- This apparatus has a
spring, screw knob, and a graduated scale. The reading
on the graduated scale is adjusted to zero. The tablet to
be tested is placed between the anvil and spindle. The
screw knob moves forward until the tablet breaks. Note
down the reading on the graduated scale, which indicates
the force required to break the tablet. The force is
measured in kilograms.
□Pfizer Hardness Tester :- The tablet to be tested is
placed between the jaws of the apparatus. The reading
on the pressure dial is adjusted to zero. Then the press
the plier like handle with hands. Reading on the pressure
dial is noted which indicates the force required in
kilogram or pound – which is the force required to
break the tablets.

e) Disintegration test :- Generally, when a drug is taken, it should
be readily available to the body. First important step of a tablet to
be readily available :- breakdown of the tablet into smaller
particles or granules – process is called Disintegration. Time
taken for a tablet to disintegrate is measured in a device described
in the USP. Disintegration is mainly used as a guide for the
formulator in preparing an optimum tablet formulation.
The USP device for disintegration comprises – 6 glass
tubes that are 3 inches long, open at the top, and closed at the
bottom with a 10 mesh screen in the basket rack assembly. One
tablet is placed in each tube and a perforated plastic disc is
placed over the tablet. The basket rack is positioned in a 1litre
beaker of water or simulated gastric fluid or intestinal fluid, at
37℃. The assembly moves up and down at a specified rate using
the help of a standard motor driven device. Time taken to
disintegrate the tablets, and all particles must pass through the 10
mesh screen in the standard time.

f) Dissolution test :- the drug dissolution testing is done to predict
the time required for a given amount of drug to release in to the
solution from a solid dosage form under specific conditions. The
test provide in vitro drug release information. There are different
types of dissolution apparatus available but only two of them are
used :- basket types and paddle type apparatus.
The dissolution test apparatus consists of cylindrical
flask with hemispherical bottom made of transparent plastic or
glass having 1000 ml capacity. The flask is partially immersed in a
water bath with a temperature of 37℃. The tablet is placed in a
basket and attached to a rotating shaft in case of basket type
apparatus. The tablet is placed in the bottom of the flask and a
paddle is attached as a stirrer to the rotating shaft. A motor is
attached to the other end of the rotating shaft which is rotated at a
speed of 100rpm. Sample is taken at specific intervals and the
same volume of dissolution medium is replaced , and the
samples are tested to measure the proportion of drug released.

PROCEDURE
a) Weight variation test :- Weight variation test was done by
weighing 20 tablets individually. From this total weight
and average weight of 20 tablets are calculated. IP/BP &
USP limits for tablet weight variation are given below.
Percentage weight variation is calculated by using following
formula.
% weight variation = {(actual weight – average weight) /
average weight } * 100

b) Thickness test :- 10 tablets are selected and thickness is
measured by using screw gauge.
c) Hardness test :- 10 tablets are selected and hardness test is
done using monsanto and pfizer apparatus. The pressure
is applied until the tablet breaks and the reading on the
dial is moted.
d) Friability test :- 10 tablets are taken and weighed
individually. Place in the chamber and rotated in the
roche friabilator for 100 rotations. Take the tablets, dust
and reweigh. The percentage of weight loss is calculated
using the following formula :-
% friability = {(initial – final weight)/ initial weight} * 100

e) Disintegration test :- 6 tablets are placed in each tube of
the basket assembly of the disintegration apparatus.
Placed the perforated disk over each tablet in the tube
and the whole basket assembly is placed in a beaker
containing 900ml of the disintegration medium. The
experiment is done until all the tablets disintegrate and
pass through the pores, and the disintegration time is
noted.
f) Dissolution test :- the water bath is filled with water and the
temperature is set to 37℃. Then the cylindrical flask is
filled with 900 ml of the dissolution medium. The
prepared tablet is placed in the basket and closed with a
lid. RPM is adjusted and the apparatus is switched on.
2ml samples are taken at 5, 10, 15, 20, 25, 30 minutes
and 2ml of the dissolution medium is replaced. Calculate
the release of the drug.

REPORT
Quality control tests of the prepared tablets were conducted
and the results were calculated.
□ 1) Average hardness of tablet = …………….. Kg/cm2
□ 2) Average weight of tablet = ……………..
□ 3) Friability percentage = ……………..%
□ 4) Disintegration time =…………min
□ 5) Percentage drug release after 30 minutes =…………..%

PRACTICAL 6 – PREPARATION OF
ASPIRIN GRANULES IP
ASSISTANT PROFESSOR

AIM
□ To prepare and submit granules for tablets that
contain 300mg aspirin in each tablet using
direct compression technique.

MATERIALS REQUIRED
□ Aspirin (acetyl salicylic acid)
□ Starch
□ Talc

PRINCIPLE
Direct compression is a dry process where in the
powdered material is compressed directly into the tablets
without the physical nature of the powder being modified.
This method is of special interest in preparing
granules when the substances consist of small crystalline
groups having all the physical characteristics that enable
them to be directly compressed into tablets without an
intermediate granulating step. Eg. potassium salts,
ammonium chloride, and methanamine.
The processing of drug with excipients can be
achieved without any need of granulation and related unit
operations. By simply mixing in a blender, formulation
ingredients can be processed and compressed into tablets
without any of the ingredients having to be changed.

□Advantages – minimum material handling, fewer processing
steps, less equipment, less expensive, no involvement of
moisture and heat, faster dissolution rate, chance of transfer
losses, and lesser equipment contamination.
□Disadvantages – only few crystalline drugs can be
formulated, selection of excipients is highly restricted due to
less inherent binding property in most of the excipients, low
dose of drugs will not be uniformly mixed, excipients for
direct compression are expensive and they also have a
problem of interaction with drug substances.
Aspirin or acetyl salicylic acid, a non – steroidal anti –
inflammatory drug, is highly unstable and may undergo
hydrolysis reaction. Hence, wet granulation cannot be used.
When aspirin is available as a granular material, direct
compression is used to prepare granules. Starch is used as a
disintegrant and talc as a lubricant.

PROCEDURE
a) Weighing :- acetyl salicylic acid and other ingredients are
weighed approximately.
b) Screening :- weighed aspirin is passed through 36/44
mesh sieve. The powder retained on sieve 44 is
collected. This is called the coarse granules. Then 15%
fines, 5% starch powder and 2% talc was calculated,
weighed and added.
c) Blending :- coarse granules, fine powder, starch and talc
are blended thoroughly to get a uniform distribution of
ingredients.
d) Now the granules are ready for direct compression.
e) Store the prepared granules in a well closed and labelled
container.

REPORT
Aspirin granules IP for tablets that each contain
300mg aspirin is prepared, labelled and submitted.

EXPERIMENT 7 –
PREFORMULATION STUDIES OF
ASPIRIN GRANULES IP
Ms. TENY SARATHOMAS
SCIENCES AND RESEARCH, ADOOR,KERALA
ASSISTANT PROFESSOR
FORMULATIVE & INDUSTRIALPHARMACY

AIM
□ To evaluate the prepared aspirin granules for
the tablets that contain 300mg aspirin in each
tablet.

MATERIALS REQUIRED
□ Prepared aspirin granules
□ Funnel
□ Burette stand
□ Measuring cylinder

PRINCIPLE
Direct compression is a dry process where in the powdered
material is compressed directly into the tablets without the physical
nature of the powder being modified.
This method is of special interest in preparing granules when
the substances consist of small crystalline groups having all the physical
characteristics that enable them to be directly compressed into tablets
without an intermediate granulating step. Eg. potassium salts,
ammonium chloride, and methanamine.
The processing of drug with excipients can be achieved
without any need of granulation and related unit operations. By simply
mixing in a blender, formulation ingredients can be processed and
compressed into tablets without any of the ingredients having to be
changed.
Aspirin or acetyl salicylic acid, a non – steroidal anti –
inflammatory drug, is highly unstable and may undergo hydrolysis
reaction. Hence, wet granulation cannot be used. When aspirin is
available as a granular material, direct compression is used to prepare
granules. Starch is used as a disintegrant and talc as a lubricant.

EVALUATION OF ASPIRIN GRANULES
 BULK DENSITY
mg was transferred to a 100ml measuring cylinder and the
volume occupied by the powder in terms of ml was
recorded.
ml
 TAPPED DENSITY
100 times on a plain hard surface and volume occupied in
ml was noted.
Tapped density = weight of powder / tapped volume in
ml
PROCEDURE

REPORT
Aspirin granules were evaluated and the following results were
observed :-
a) Bulk density = gm/ml
b) Tapped density = gm/ml
c) Hausners ratio =
d) Carr’s compressibility index =
e) Angle of Repose - ⁰
From the above observations the prepared granules was
found to have flow property.

 To prepare 40 tablets of aspirin each containing
300mg of paracetamol as drug.

 Aspirin
 Starch
 Talc

According to Indian Pharmacopoeia, pharmaceutical tablets
are flat or bi-convex discs manufactured by compressing a drug or
a mixture of rugs with or without suitable excipients.
For increased production, rotary press tablet compressing
machine is used. The tablet compressing machine comprises of
punches and dies revolving continuously while the tablet granules
flow from a hopper to the die cavity through a feed frame. This
method promotes the uniform filling of die, therefore an accurate
weight of each tablet is achieved. Compression by the upper and
lower punch produces a slow squeezing effect on the material in
the die cavity. Here, the entrapped air also has a chance to escape
during compression.
Aspirin tablet is an orally ingested compressed tablet prepared
by dry granulation process. Starch powder as a disintegrating agent
and talc is used as an glidant.

Weigh the required amount of aspirin powders and
passed through 36/44 mesh sieve. Material retained on
44 mesh sieve is collected and is termed as coarse
granules. Then 15% of fine powder required and 5%
starch powder is calculated and weighed out. The
powder is then blended to get uniform distribution of
ingredients and compressed by using the tablet punching
machine.

40 tablets of aspirin each containing 300mg of the
drug was prepared, labelled and submitted.

PRACTICAL 9 – EVALUATION OF
PREPARED ASPIRIN TABLETS
ASSISTANT PROFESSOR

AIM
□ To perform the quality control tests of the
prepared aspirin tablets each containing 300mg
of aspirin as the drug.

PRINCIPLE
In Process Quality Control tests are
routinely run to monitor the compression and
manufacturing process.
Quality Control Tests are generally divided
into two :-
1. Official Tests
2. Non - Official Tests
Official tests include :- weight variation tests,
thickness tests, friability tests, hardness tests,
disintegration tests, and tablet dissolution tests.

REPORT
Quality control tests of the prepared aspirin tablets were
conducted and the results were calculated.
□ 1) Average hardness of tablet = …………….. Kg/cm2
□ 2) Average weight of tablet = ……………..
□ 3) Friability percentage = ……………..%
□ 4) Disintegration time =…………min
□ 5) Percentage drug release after 30 minutes =…………..%

PRACTICAL MANUAL BASED ON TABLETS

More Related Content

What's hot

Similar to PRACTICAL MANUAL BASED ON TABLETS

More from Teny Thomas

Recently uploaded

PRACTICAL MANUAL BASED ON TABLETS