A

Report
On

Generation and Validation of Standard

Operating Procedure for Friability
Apparatus.
By

KULDEEP PANDEY
(Roll No. 1509050036)

B. Pharm - 4th Year

2018-19

Submitted to

Department of Pharmacy, IEC Group of Institutions

Knowledge Park-1, Institutional Area, Surajpur Kasna Road,
Greater Noida, Gautam Budh Nagar, Uttar Pradesh-201310, (India)

1
 CONTENTS

 Acknowledgement

 Certification

 Introduction

 Principle

 Instruments

 Procedure

 Validation

 SOP For Operation and Cleaning Friability apparatus

 Friabilator Operation

 Handling of friabilator apparatus

 Conclusion

 Reference

2
 ACKNOWLEDGEMENT

I would like to express my special thanks of gratitude to IEC College of Engineering

And Technology for their able guidance and support in completing my project work.

I respect and thank Ms. [Aparna Datta], for providing me an opportunity to do the
project work on “Generation and Validation of Standard Operating Procedure for
Friability Apparatus”. in IEC college of Engineering and Technology,
“Department of pharmacy” and giving us all support and guidance which made me
complete the project duly.

I am extremely thankful to [Mr. Manoj Kumar Prabhakar ],HOD

“Department of pharmacy” for providing such a nice support and guidance, although
he had busy schedule managing the College programs.

I am thankful to and fortunate enough to get constant encouragement, support and

guidance from all Teaching staffs of “Departmemnt of pharmacy” which helped us in
successfully completing our project work. Also, I would like to extend our sincere
esteems to all staff in laboratory for their timely support.

Kuldeep Pandey Ms. Aparna Datta

3
 CERTIFICATION

To whom it may concern certificate

This is to certify that Mr.Kuldeep Pandey bearing Roll no. “1509050036” is a bonafide
student of UG Bachelor of Pharmacy program the institute IEC College of Engineering
and Technology currently he is a student of 8th semester .

This certificate is issued for the purpose of project work on “Generation and
Validation of Standard Operating Procedure for Friability Apparatus”.

Signature…………….

(HOD-Departmet Of Pharmacy)

4
Introduction to Friability Testing

Friability is the tendency for a tablet to chip, crumble or break following

compression. This tendency is normally confined to uncoated tablets and
surfaces during handling or subsequent storage.

It can be caused by a number of factors including poor tablet design (too sharp
edges), low moisture content, insufficient binder, etc.

For obvious reasons, tablets need to be hard enough such that they do not
break up in the bottle but friable enough that they disintegrate in the
gastrointestinal tract.

Based on an original design by Roche, the friability tester has now become an
accepted standard throughout the pharmaceutical industry for determining the
resistance of uncoated tablets to the abrasion and shock experienced in
manufacturing, packing and shipping operations.

Whilst the basic design remains unchanged, considerable advances have

been made in terms of reliability and ease of usage which have now been
incorporated into current units.

For comprehensive product details, specifications and part numbers, please

request a copy of our brochure “Quality Solutions for the Testing of
Pharmaceuticals”.

5
Friability Testers (Uncoated Tablets)

The basic Friability Tester Model FR 1000/2000 comprises of a single or dual

drums rotated at a fixed speed of 25 rpm. The standard friability drum has an
inside diameter of 287 mm and a depth of 38 mm and is fitted with a curved
baffle which subjects the tablets to be tested to a drop of 156 mm. The
Friability Tester Model FRV 1000/2000 also features either one or two
drums, but allows variable speed between 20 and 60 rpm to be programmed.
Number of turns or test duration can also be programmed into the tester.

The sample (normally 10 tablets) to be tested is first weighed and then placed
into the drum. The drum is then rotated 100 times, any loose dust from the
sample removed and the sample re-weighed. The friability drum features
apertures behind the baffle, such that the tablets can be added and removed
from the drum automatically at the beginning and end of the test.

The Friability of the sample is given in terms of % weight loss (loss in weight
expressed as a percentage of the original sample weight). A maximum weight
loss of not more than 1% is considered acceptable for most tablets.

Abrasion drums for carrying out tests into the attrition of tablets caused by
the product rubbing together during transit are also available on request.

6
For comprehensive product details, specifications and part numbers, please
request a copy of our brochure “Quality Solutions for the Testing of
Pharmaceuticals”.

Friability Testers (Granules and Spheroids)

In many cases, such as with hard coated and uncoated tablets, granules and
spheroids, it is impossible to determine the friability of the dosage form using a
conventional tablet friability tester even if the test time is extended simply
because the resistance is such that no measurable attrition is obtained – the
energy imparted by the friability tester is just not sufficient to generate
quantifiable changes in surface mass.

The Friabimat SA-400 is a new instrument specifically designed to address

this particular problem by offering an alternative method of friability
measurement.

For the purpose of the test, the sample is confined within a standard 105 mL
glass bottle horizontally mounted on the end of an oscillating arm. The
abrasive action is generated by the horizontal shaking movement of the
oscillating arm which causes the samples to rub against and collide with each
other and/or the internal surfaces of the sample container.

The intensity of the abrasive action and the duration of the test can be
adjusted via the controls mounted on the front panel between 0 and 400
oscillations per minute and 0 and 9999 seconds respectively.

For comprehensive product details, specifications and part numbers, please

request a copy of our brochure “Quality Solutions for the Testing of
Pharmaceuticals”.

7
PRECENTAGE OF FRIABILITY

Percentage of friability of the tablets of a badge can be find by the following

formula:

Percentage Friability = W1 – W2/W1 × 100

Where, W1 = weight of tablets before testing

W2 = weight of tablets after testing.

LIMIT:

According to B.P = Percentage of friability should be not more than 0.8%.

According to U.S.P = Percentage of friability should be not more than 4%

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Tablet Friability Testing Instruments

Friability testing is used to test the durability of tablets during packing

processes and transit. This involves repeatedly dropping a sample of tablets
over a fixed time, using a rotating drum with a baffle. The result is inspected
for broken tablets, and the percentage of tablet mass lost through chipping. All
Pharma Test friability testers are fully compliant to the current USP, EP and JP
Pharmacopeia and come ready to use with friability („Roche“) drums included
in the standard scope of supply. Abrasion drums as well as friability drums with
anti-static coating are available as options.
Friability is defined as the percentage of weight loss by tablets due to mechanical
action during the test. The tablets are weighed before and after testin. The friability is
expressed as a percentage loss on pre test tablet weight. Friability refers to the ability
of the compressed tablet to avoid fracture and breaking during the transport. It is
related to tablet harness and is designed to evaluate the ability of tablet to withstand
aberration in packing, handling and shipping. It is measured by the use of friablity
tester

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PROCEDURE:-

Start

↓
Connect power cord to an
appropriate electrical outlet

↓
Unscrew locking nut to release drum

↓
Brush any loose dust from tablets

↓
Accurately weigh tablets

↓
Load tablets into drum

↓
Place plastic cover over drum

↓
Hold cover firmly in place and

↓
slide drum onto the shaft

↓
Place locking nut onto the end of the shaft

↓
Tighten locking nut into position

↓
Turn timer to the desired

↓
number of rotations

↓
Wait until drum returns
to stationary position

↓
Remove locking nut

↓
Carefully remove drum from shaft

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 ↓
Remove tablets and brush away
any loose powder

↓
Any cracked, cleaved
or broken tablets

↓
Tablets sample has failed the friability test

↓
Reweigh tablets

↓
Calculate the percentage weight loss using
the following formula:

↓
% Weight Loss = (Initial weight – Final
weight) /

This Standard Operating Procedure (SOP) applies to the staff and students using the Friability Tester in the
laboratories of the Pharmacy Department.

Readings:-

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Validation of an expedited tablet friability method.

The harmonized monograph on tablet friability test in United States

Pharmacopeia (USP), European Pharmacopeia (Pharm. Eur.), and Japanese
Pharmacopeia (JP) is designed to assess adequacy of mechanical strength of
a batch of tablets. Currently, its potential applications in formulation
development have been limited due to the batch requirement that is both labor
and material intensive. To this end, we have developed an expedited tablet
friability test method, using the existing USP test apparatus. The validity of the
expedited friability method is established by showing that the friability data
from the expedited method is not statistically different from those from the
standard pharmacopeia method using materials of very different mechanical
properties, i.e., microcrystalline cellulose and dibasic calcium phosphate
dihydrate. Using the expedited friability method, we have shown that the
relationship between tablet friability and tablet mechanical strength follows a
power law expression. Furthermore, potential applications of this expedited
friability test in facilitating systematic and efficient tablet formulation and tooling
design are demonstrated with examples.

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SOP (Standard Operating Procedure) FOR OPERATION
AND CLEANING

PURPOSE
To provide a written procedure for operation and cleaning of the Automated
Friabilator EF-2 (USP) .

SCOPE:
Applicable to determine Friability of tablets in Manufacturing.

RESPONSIBILITY:
Executive Manufacturing,Executive QA and Assistant Manager QA.

DEFINITIONS:

Tablet friability can be used to measure efficiency of tabletting equipment or as

an indicator of formulation suitability as well as routine QC functions. It can
also be thought of as measuring “dusting”. Tablets are rotated in a plastic
drum for a specified period of time. A gravimetric determination is then made
to quantitate the amount of surface material that has worn off.
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FRIABILATOR OPERATION:

 Check cleanliness of the equipment.

 Switch ON the instrument, drum will initialize itself to the loading
position, the display will now show START.
 Weigh and record the weight of the tablets.
 For the tablets having individual weight up to 0.650 g take 20 tablets.
B. For the tablets having individual weight above 0.650 g take 10 tablets.
 Adjust the counts to 100 by pressing the COUNT key followed by ‘1’, ‘0’,
‘0’ keys. (Count range 1 to 99999).
 Press ENTER to confirm the reading.
 To see and confirm the number of counts press COUNT key.
 On confirming the number of counts press RUN/HALT key to start, the
display shows the elapsed count.
 NOTE: Test can be performed by adjusting ‘TIME’ similarly as ‘COUNT’.
 When test is over drum rotates in reverse direction discharging the
tablets in the tray.
 The test over is indicated by an audible beep and display shows END
 The drum initializes itself to loading position and display shows START
indicating the instrument is ready for the next run.
 Remove the tablets from the tray.
 De- dust and weigh the tablets and note down the weight of the tablets.
 Calculate the percentage loss in the weight by using the formula
 Percentage Loss =Initial Wt – Final Wt/Initial Wt X 100

Notes :

• Do not hold the drums while rotating.

• After testing destroy the tablets
.

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CLEANING: Friabilator

 Remove the knob on the shaft by pressing the button.

 Pull the outside drum out from the shaft carefully. Similarly remove the

inside drum by pulling it outside.

 Remove the detachable disc from the drum by pulling it outside of both

the drums.

 Clean both the drums with clean cloth.

 Remove both the trays.

 Clean the trays with clean cloth.

 After cleaning, put the drums and trays back on its position.

Handling of friabilator apparatus Precautions

 Do not open the electical compartment due to the risk of shock and allow
only trained personnel to do so.
 When tightening the locking nut, ensure that it is not overtightened since
this can cause damage to the drum.
 Do not use cleaning compounds containing ammonia or abrasive
cleaners to clean the plastic drum since such compounds may damage
plastic, causing it to crack and fracture.

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  For tablets with a unit mass equal to or less than 650mg, a sample of
tablets corresponding as near as possible to 6.5g is to be used whilst for
tablets with a unit mass greater than 650mg, a sample of 10 whole
tablets is to be used.
 According to the British Pharmacopoeia, 100 rotations are considered to
be the standard number of rotations to be used for each test.
 According to the British Pharmacopoeia, a maximum loss of mass not
greater than 1.0 per cent is considered acceptable for most types of
tablets.

ABBREVIATION:

Tablet friability can be used to measure efficiency of tabletting equipment or as

an indicator of formulation suitability as well as routine QC functions. It can
also be thought of as measuring “dusting”. Tablets are rotated in a plastic
drum for a specified period of time. A gravimetric determination is then made
to quantitate the amount of surface material that has worn off.

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 Conclusion

As a conclusion, the weight difference between before and after the tablet friability
operation is 6.8212 g – 6.6935 = 0.1277 g. The percentage loss of weight is 1.87% and
it is more than 1% of it should be. This may happened because of the expiry date of
the tablets.

Example:-

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 REFERENCES

 British Pharmacopoeia 2009 Vol 4. London: The Stationary Office; 2009.

P. A438-A439.

 Chourasia A, Mishra BJ, Mishra R, Kannojia P. Comparative in vitro

Evaluation of Government Hospital Supplied and Commercial Brands of
Paracetamol Tablets. The Pharmacist 2007; 2 (2): 37-39.

 Huynh-Ba K, editor. Handbook of Stability Testing in Pharmaceutical

Development. New York: Springer; 2009. p. 215-216.

 Salman AD, Ghadiri M, Hounslow MJ editors. Volume 12 Paul Breakage.

 The Netherlands: Elsevier; 2007. p. 960-962.Varian. Friability Tester

Operator’s Manual. No

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