industrial practicals manual

PRACTICAL NOTEBOOK INDUSTRIAL PHARMACY

COURSE NAME:

INDUSTRIAL LAB

COURSE NO:

PCU 610

SEMESTER:

8th

PROGRAM:

PHARM-D

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LIST OF PRACTICAL PERFORMED

Course: Industrial Pharmacy Laboratory Course No. PCU-610

Course Incharge: Mr. Haroon Rahim Laboratory: Techno Lab

S. NO TITLE OF PRACTICAL PERFORMED

1. Preparation Of Starch Paste

2. To Determine The Angle of Repose of Given Sample

3. Preparation of Simple (White) Ointment

4. Preparation of Sulphur Ointment

5. Preparation of Cold Cream (W/O Emulsion)

6. Preparation of Paracetamol Granules

7. To determine moisture contents in Given Sample

8. Preparation of Paracetamol Tablets

9. Weight Variation Test For Tablets

10. Friability Test For Tablets

11. To determine the Thickness of Tablets

12. To determine the Diameter of Tablets

13. Hardness Test For Tablets

14. Disintegration Test For Uncoated Tablets

15. Disintegration Test For Film coated Tablets

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PRACTICAL NO. 1

PREPARATION OF STARCH PASTE

THEORY:

Starch is a carbohydrate consisting of a large number of glucose units joined by

glycosidic bonds. This polysaccharide is produced by most green plants as an energy store. It is

the most common carbohydrate in human diets and is contained in large amounts in such staple

food as potatoes, wheat, maize (corn) rice cassava.

Pure starch is white, tasteless and odorless powder that is insoluble in cold water or alcohol. It

consists of two types of molecules, the linear and helical amylase and the branched amylopectin.

Depending on plant, starch generally contains 20% to 25% amylase and 75% to 80%

amylopectin by weight.

REQUIREMENTS:

Starch, Purified Water, Weighing Balance, Stirrer, Beakers

FORMULA USED:

Starch--------- 7.0 gm

Cold purified water------ 7.0 ml

Hot purified water------- 50.0 ml

PROCEDURE:

1. Weigh starch 07 gm by weighing balance.

2. Take 07 ml of cold water.

3. Suspend maize/corn starch in pure water with continues stirring till

smooth slurry is obtained.

4. Take 50 ml of pure water in another beaker and heat it to boil.

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5. Add the slurry to the boiling water with stirring and maintaining heat

for some time.

6. Remove the heat and cool the starch paste 40°C with stirrer.

USES:

As tablets binder.

Employed in granulation of powder.

PRECAUTIONS:

Do not store the paste for prolong time as the chances of microbial growth.

Do not store it in refrigerator.

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PRACTICAL NO. 2

TO DETRMINE THE ANGLE OF REPOSE OF GIVEN SAMPLE

THEORY:

Angle of Repose: The angle of repose is the maximum angle of a stable slope determined by

friction, cohesion and the shapes of the particles. When bulk granular materials are poured onto a

horizontal surface, a conical pile will form. The internal angle between the surface of the pile and

the horizontal surface is known as the angle of repose and is related to the density, surface area,

and coefficient of friction of the material.

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Flow property Angle of repose (degrees)

Excellent 25 – 30

Good 31 – 35

Fair-aid not needed 36 – 40

Passable – may hang up 41 – 45

Poor – must agitate,

vibrate

46 – 55

Very poor 56 – 65

Very, very poor >66


REQUIREMENTS:

Funnel, Sample, Weighing balance, Clamp, Calculator

PROCEDURE:

Angle of repose was determined using funnel method. Funnel is adjusted with the help of clamp

to the stand and height of the funnel was adjusted in such a way that the tip of the funnel just

touches the heap of the blends. The angle of repose is the angle formed by the horizontal base of

the bench surface and the edge of a cone-like pile of granules. Funnel used was a stainless steel

funnel and the size of the orifice was 10 mm and the height from the beginning of funnel to end

of orifice was 111 mm. The funnel was fixed in place, 4 cm above the bench surface. After the

cone from 5 g of sample was built, height of the granules forming the cone (h) and the radius (r)

of the base were measured.

Θ= tan-1 (h/r)

Where,

h = Height of pile

r = Radius of pile, and

Θ = Angle of repose

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PRACTICAL NO. 3

PREPARATION OF SIMPLE (WHITE) OINTMENT

FORMULA USED:

Wool Fat --------------------------- 5 grams

Hard Paraffin --------------------- 5 grams

Cetosteryl Alcohol --------------- 5 grams

White Soft Paraffin -------------- 85 grams

PROCEDURE:

1. Weighed accurately all the ingredients using a digital balance.

2. Mix all the ingredients in a beaker.

3. Heat gently with constant stirring until a homogenous mixture formed.

4. Cool the mixture and the ointment is ready for use.

PRECAUTIONS:

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For External use only.

It should be stored at room temperature.

Use within one month.

USES:

Simple ointment is use as Emollient.

It is used as base for medicated ointments.

PRACTICAL NO. 4

PREPARATION OF SULPHUR OINTMENT

FORMULA USED:

Sulphur --------------------------- 10 grams

Mineral oil ------------------------ 10 grams

White Ointment ----------------- 80 grams

PROCEDURE:

1. Weight accurately all the ingredients using a digital balance.

2. Mix Sulphur with mineral oil to form paste.

3. Add the paste to white ointment and mix until homogenous mixture

formed.

PRECAUTIONS:

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It should be stored in well closed container.


USES OF SULPHUR OINTMENT:

It is use for fungal infections.

It is used for skin infections like dermatitis, scabies and eczema.

PRACTICAL NO. 5

PREPARATION OF COLD CREAM (W/O)

THEORY:

Cold cream is a W/O type of emulsion.

INGREDIENTS: Master Formula Formula used

Mineral Oil ---------------------- 500 parts ------------------ 50 grams

Bees Wax ------------------------ 140 parts ------------------ 7 grams

Sodium Borax ------------------- 75 parts ------------------- 37.5 grams

Purified Water ------------------ 35.3 parts ----------------- 17.65 grams

PROCEDURE:

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1. Weighed all the ingredients accurately using a digital balance.

2. Combine the mineral oil and bees wax in a beaker.

3. Heat it at 70˚C and stir the mixture till it melt.

4. Add Sodium borax to purified water and heat it at 75˚C. The borax will be

absorbed in the water.

5. Now put the borax solution slowly into the beeswax mixture. Beat

vigorously till it blends well.

6. Cool the Cream and transfer it to a glass jar. Close the cap tightly.

PRECAUTIONS:



It should be packed in well closed container.


USES OF COLD CREAM:

Cold Cream is use as Emollient.

It is used as base for medicated creams.

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PRACTICAL NO. 6

PREPARATION OF PARACETAMOL GRANULES

THEORY:

Wet Granulation:

The Steps Involve in wet granulation are:

1. Weighing

2. Mixing

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3. Granulation

4. Screening The Damp Mass

5. Drying

REQUIREMENTS:

Weighing balance, Mesh, Mortar, Oven, Paracetamol, Diluent, Magnesium stearate.

FORMUAL USED:

1. Paracetamol (API)--------250 mg

2. PVPK30 (Binder)--- 10% w/w

3. Lactose (Diluent)----(Q.S)

4. Magnesium Stearate (Lubricant) ----------03 mg

PROCEDURE:

The active ingredients of Paracetamol, diluents and disintegrants were mixed. The ingredients

are mixed in stainless steel bowls or mortars. A solution of the binding agents was added to the

mixed powders with stirring. 10 mg of starch was taken in a beaker in 20 ml of hot water was

added and stirred well to make suspension and heated in a boiling water.

The wet granulation is forced through a 16 mesh screen. The moist materials are placed on

large sheets of paper on shallow wire trays and placed in drying cabinets with a circulating air

current in thermostatic heat control. After drying the granulation is reduced the particle size by

passing it through a smaller mesh screen.

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PRACTICAL NO. 7

TO DETERMINE MOISTURE CONTENTS IN GIVEN SAMPLE

PROCEDURE:

1. Switch “ON” the mains.

2. Open the lid cover and put sample on the pan.

3. Spread the sample on the pan evenly with the help of spatula.

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4. When weight is more than 500 mg the instrument symbolically shows that it is ready for

heating.

5. Close the lid cover.

6. Instrument will start heating by itself.

7. When the material start drying, display unit will show automatically loss in weight in

%age.

8. When drying is over the result is displayed in %age on display unit, note the reading.

9. Remove the pan and clean it.

10. Switch “OFF” the instrument when not in use.

PRACTICAL NO. 8

PREPARATION OF PARACETAMOL TABLETS BY WET

GRANUATION METHOD

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1. Paracetamol (API) 250 mg

2. Avicel (Diluent) Q.S

3. Starch (Binder) 10% (W/W)

4. Aerosil (Disintegrant) 3% (W/W)

5. Magnesium stearate (Lubricant) 1 to 1.5 % (W/W)

6. Water Q.S

The steps involved in wet granulation were, Weighing, Mixing, Granulation, Screening the damp

mass, Drying, Dry screening, Lubrication and Compression.

Preparation of Starch solution:

Starch was taken in a beaker in 20 ml of hot water was added and stirred well to make

suspension and heated in a boiling water bath with continues stirring until to translucent paste is

formed.

The active ingredients of paracetamol, diluents and disintegrants are mixed. For small batch the

ingredients may be mixed in stainless steel bowls or mortars. A solution of binding agents was

added to mixed powder with stirring. The Powder mass is wetted with the binding solution until

the mass has consistency of the damp snow. If the granulation is over-wetted the granules will be

hard, requiring considerable pressure to form the tablets. If the powder mixing is wetted

sufficiently the resulting granules will be too soft, breaking down during lubrication and causing

difficulty during compression.

The wet granulation is forced through a 16 mesh screen. The moist materials are placed on large

sheets of paper on shallow wire trays and placed in drying cabinets with a circulating air current

in thermostatic heat control. Particle size distribution can be controlled by varying the speed of

rotation and drying temperature. After drying the granulation is reduced the particle size by

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passing it through a smaller mesh screen. After drying granulation the lubricants is such as

Magnesium Stearate was added. Then the lubricated were compressed by using the single punch

machine.

RESULT:

After passing through mesh No.16 and Drying we obtained Fine granules of paracetamol for

tableting.

PRACTICAL NO. 9

WEIGHT VARIATION TEST FOR TABLETS

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THEORY:

Weight variation or uniformity of weight is an official test in all current pharmacopoeias.

Weight variation test is one of the In-Process tests during production of tablets in any

pharmaceutical industry. Any variation in weight of tablets ultimately leads to variation in

doses.

REQUIREMENTS:

Tablets

Analytical balance

PROCEDURE:

1. Select 10 tablets randomly and weighed them all using a digital balance.

2. Determine the average weight of tablets.

3. Now each tablet is weighed individually (prescribes limits already calculated)

4. Not more than two tablets should be deviated from the allowed limits.

5. None of the tablets should deviate from twice the percentage limits.

USP Weight variation Tolerances for Uncoated Tablets

S. No Average wt. of tablet(mg) Max. % difference allowed

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1 130 or Less 10%

2 130-324 7.5%

3 More than 324 5%

B.P (British Pharmacopeia) Weight variation Tolerances for Uncoated Tablets

Average weight of tablet

(x)

Deviation allowed from average weight

80 or <80 mg10%

80-250 mg7.5%

>250mg5%

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PRACTICAL NO. 10

FRIABILITY TEST FOR TABLETS

(OFFICIAL TEST)

THEORY:

It is physical parameter which indicates resistance of tablets against mechanical shock during

packaging, transport or stripping.

REQUIREMENTS:

Friabilator, Analytical balance, Tablets, Calculator

PROCEDURE:

1. For tablets having weight equal or less than 650mg, take sample of 20 tablets.

2. For tablets having weight more than 650mg, take sample of 10 tablets.

3. De-dust the tablets with addition of air pressure or soft brush.

4. Accurately weighed the tablets and placed in the drum of the Friabilator.

5. Operate the Friabilator for 4 minutes at 25 rpm to complete 100 rotations.

6. Collect, de-dust and weighed the tablets again.

7. The percentage friability can be determined by using following formula:

% age Friability = W1 – W2 / W1

Where, W1 = initial weight and W2 = final weight

Limits:

U.S.P = not more than 1%

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B.P = not more than 0.8%.

PRACTICAL NO. 11

TO DETERMINE THICKNESS OF TABLETS

THEORY:

Tablet thickness is an important quality control test for tablet packaging. The thickness of tablet

can affect the therapeutic effectiveness of tablets. Very thick tablet affects packaging either in

blister or plastic container. Tablet thickness is determined by the die of the tableting machine and

is generally controlled to minimize appearance problems.

Thickness is an unofficial test.

It can be dimensionally described & controlled. The thickness of a tablet is only variable. Tablet

thickness can be measured by Vernier caliper or by other device. Tablet thickness should be

controlled within a ±5% variation of standard value as per U.S.P specifications.

Thickness of the tablet is inversely proportional to hardness i.e. increase in hardness

decrease the thickness & vice versa.

Thickness of tablet is measured by Vernier caliper Digital tester.

It is determined for 10 tablets.

REQUIREMENTS:

Tablets, Vernier caliper or Digital Tester

PROCEDURE:

1. Turn on the Instrument. 10 tablets are selected and then the test for thickness is

carried out by using the Digital Tablet Testing Instrument HT-0607 by clicking Mode

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button and adjusting operating mode to thickness. Turn ON the hardness tester and set

its mode to the specifications as required.

2. Place the tablet between its jaws and start the apparatus.

3. The jaws will apply force on the tablet till it breaks.

4. The force will be displayed on the screen of tester, note that value along with its unit.

5. Repeat the same procedure for 10 tablets and note their readings and then average

was calculated.

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PRACTICAL NO. 12

TO DETERMINE DIAMETER OF TABLETS

THEORY:

REQUIREMENTS:

1. Turn on the Instrument HT-0607. 10 tablets are selected and then the test for diameter

is carried out by using the Digital Tablet Testing Instrument HT-0607 by clicking

Mode button and adjusting operating mode to diameter.


3. The diameter will displayed on screen of tester, note that value along with its unit.

4. Repeat the same procedure for 10 tablets and note their readings and then average

was calculated.

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PRACTICAL NO. 13

HARDNESS TEST FOR TABLETS

(NON-OFFICIAL Test)

THEORY:

Hardness (crushing strength): It is the load required to crush the tablet when placed on its

edge.

Hardness is measured:

To determine the need for pressure adjustments on the tableting machine.

Hardness can affect the disintegration. So if the tablet is too hard, it may not disintegrate

in the required period of time. And if the tablet is too soft, it will not withstand the

handling during subsequent processing such as coating or packaging.

In general, if the tablet hardness is too high, we first check its disintegration before

rejecting the batch.

If the disintegration is within limit, we accept the batch.

If Hardness is high + disintegration is within a time accept the batch.

Factors Affecting the Hardness:

• Compression of the tablet and compressive force.

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• Amount of binder (More binder à more hardness).

• Method of granulation in preparing the tablet (wet method gives more hardness than

direct method, Slugging method gives the best hardness).

LIMITS: 5 kilograms minimum and 10 kilograms maximum.

Make hardness test on 5 tablets and then take the average hardness.

REQUIREMENTS:

Sample ---- 10 tablets

Hardness tester (Digital Hardness Tester)

PROCEDURE:

1. Turn ON the hardness tester and set its mode to the specifications as required.


3. The jaws will apply force on the tablet till it breaks.

4. The force will be displayed on the screen of tester, note that value along with its unit.

5. Repeat the same procedure for 10 tablets and note their readings.

NORMAL LIMITS:

Minimum limit ---------- 5 kg

Maximum limit -------- 10 kg.

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PRACTICAL NO. 14

DISINTEGRATION TEST FOR UNCAOTED TABLETS

THEORY:

It is the time required for the tablet to break into particles, the disintegration test is a measure

only of the time required under a given set of conditions for a group of tablets to disintegrate

into particles. Disintegration test is an official test.

It is performed to identify the disintegration of tablet in particular time period.

Disintegration test is not performed for controlled & sustained release tablets.

APPARATUS USED:

Disintegration apparatus consists of Basket rack assembly supporting six cylindrical glass

tubes. The assembly is attached with a device for lowering and raising the assembly in the

medium placed in a cylindrical vessel having 1000 ml capacity. This whole apparatus is placed

in a water bath for maintaining the desired temperature of 37˚C ± 1 ˚C.

REQUIREMENTS:

Sample ------- 6 tablets

Disintegration apparatus

PROCEDURE:

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1. Turn ON the apparatus and maintain the temperature at 37˚C ± 1 ˚C.

2. Remove the Basket-rack assembly from the water.

3. Select six tablets randomly from the sample and place one in each of the tubes of the

Basket-rack assembly.

4. Now reset the assembly in the apparatus and set the machine in motion.

5. Note the disintegration time and compared it with that of prescribe time. The tablets must

disintegrate within the prescribed time.

6. Repeat the same procedure for coated and effervescent tablets.

According to the test the tablet must disintegrate and all particles must pass through the

10 mesh screen in the time specified. If any residue remains, it must have a soft mass.

Liquids used in disintegration Water, Simulated gastric fluid (pH = 1.2 HCl), or

Simulated intestinal fluid (pH = 7.5, KH2PO4 (phosphate buffer) + pancreatic enzyme +

NaOH).

U.S.P. method for uncoated tablets:

Start the disintegration test on 6 tablets.

If one or two tablets from the 6 tablets fail disintegrate completely within 30min repeat

the same test on another 12 tablet. (i.e. the whole test will consume 18 tablets).

Not less than 16 tablets disintegrate completely within the time

if more than two tablets (from the 18) fail to disintegrate, the batch must be rejected.

TABLETS DISINTEGRATION TIME

Soluble tablets 3 minutes

Uncoated tablets 3-15 minutes

Film coated tablets 30 minutes

Sugar coated tablets 1 hour

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Enteric coated tablets 2-3 hours

PRACTICAL NO. 15

DISINTEGRATION TEST FOR FILM CAOTED

TABLETS

REQUIREMENTS:

Tablets, Water, Disintegration Test Apparatus.

PROCEDURE:

Start the disintegration test apparatus on 6 tablets.

If one or two tablets from the 6 tablets fail disintegrate completely within 30 min repeat

the same test on another 12 tablet. (i.e. the whole test will consume 18 tablets).

Not less than 16 tablets disintegrate completely within the time, if more than two tablets

(from the 18) fail to disintegrate, the batch must be rejected.

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industrial practicals manual

Documents

tablets practical

pure starch

cold water

maizecorn starch

pure water

tablets binder

uncoated tablets

thickness of tablets