VALIDATION OF PULVERISATION MACHINESM.SRINIVASM.PHARM. II SEM.VAAGESWARI COLLEGE OF PHARMACY

CONTENTS

•DEFINITION•PRINCIPLE•CONSTRUCTION •WORKING•APPLICATIONS•VALIDATION•CONCLUSION

PULVERISATION:

pulverization is process to make a fine particle (powder)form of any solid substance by hammering ,attrition or any other

compression methods

VALIDATION:

Validation is defined as a documentary evidence which provides a high degree of assurance that a

specific process /equipment will consistently produce a product meeting its predetermined

specifications and quality attributes.

WHY TO VALIDATE?

To ensure that the products intended for human administration are manufactured under state

of control.

Principle:The size reduction is effected due to shears when the material is placed between the narrow gap of milling surfaces of rotor & stator.

construction:colloidal mill consists of a rotor & a stator, the rotor rotates at a speed of 3000 to 20,000rpm.The stator have conical milling surface between which there is an adjustable clearance between 0.002 to 0.3 .

working:The material Eg:- emulsion & suspension is placed into the hopper of the mill. It is then passed through the narrow gap between the rotor & stator & thus reduced to fine particle size.

APPLICATIONS:

colloid mill is used for preparing suspensions, emulsions and ointments.

capable of producing pharmaceutical products with reduced particle size <1 μ.

Colloidal mill can be sterilized so it can be used in the production of sterile products

COLLOIDAL MILL

VALIDATION

VALIDATION

DESIGN QUALIFICATION

INSTALLATION QUALIFICATION

OPERATIONAL QUALIFICATION

PERFORMANCE QUALIFICATIO

N

1)DESIGN QUALIFICATION:

There is no legal requirement to perform a design qualification and to check the design documents of a technical system to ensure that they fulfill the user requirements.

2)INSTALLATION QUALIFICATION:

An IQ evaluation establishes confidence that the equipment is

properly installed .

The installation must meet the manufacturers specified

guidelines along with design changes at installation, also the

supporting electrical utilities must meet all electrical codes.

EQUIPMENT QUALIFICAT

ION

REQUIRED

DOCUMENTS

UTILITIES

MAJOR COMPONENT

S

COMPONENT MATERIAL

LUBRICANTS

EQUIPMENT SAFETY FEATURES

MANNUAL DRAWINGS

SOPS

VOLTS(460)

AMPS(20)

DRIVE&

AUGERMOTORS

IQ ELEMENTS OF A COLLOID MILL

EQUIPMENT IDENTIFICATION:Record the equipment identification numbers along with the following order

REQUIRED INFORMATION:

Purchase order 009235 Model number DAS60Serial number 78801Equipment number 6492Location Room 270(this equipment is portable)

• REQUIRED DOCUMMENTS:• Record the equipment manufacturers operation

and maintenance manual and maintenance manual and draw a table.

• Record the SOPs that cover the setup operation cleaning of the mill.

• EQUIPMENT UTILITY REQUIREMENTS:

utility specified

Measured result

acceptable

Volts Drive motor

460±10%

A-B455;A-C457

Yes

amperes Drive motorAuger motor

11

1.17

B-C456

20 circuit rotations

yes

MAJOR COMPONENTS:The component specifications of the protocol verifies that the mill components purchased were delivered and installed.Record the major components:

MAJOR COMPONENTS

AS FOUND CONDITIONS

Drive motor Manufacturer

Model number-A51QA

Volts-460

Ampers-11

Rpm-3000 to 20,000

Material-stainless steel

Type-conical

Size-2-7/8 in diameter

Phases-3

Clearance between 0.002

To 0.03 inches

COMPONENT MATERIAL:mainly high strength, low corrosion materials are used for construction of colloid mill

Component material

Mill chambers 316 stainless steel

Rotor 316 stainless steel

Auger feed Stainless steel

stator 316 stainless steel

EQUIPMENT OPERATION:The objective of the rotation direction test is to verify that the rotor blades and the auger feed rotate in the proper direction.The following tests will be performed with the colloidal mill empty.Record the results in the table.

LUBRICANTS:Lubricants are used to increase the smoothness of the mill and to increase the life span of colloid mill.Mainly oil ,grease type of lubricants are used

Where to be used

type manufacturers

Product contact

Gear box Amolitb#2 oil No

Pillow block bearing and casters

Lubriplate 630-2 grease

No

Safety features test procedureTest function Expected results Acceptable

Safety interlock switch operations

When the mill and auger feed push buttons are pressed ,the miller and auger motors will not start with the throat removal

When the mill and auger feed push buttons are pressed , the mill and auger motors will not start with the safety guide removed

Yes

yes

EQUIPMENT CONTROL FUNCTIONS:The objective of testing equipment control functions in verify that the switches and push buttons on the mill operate as per the manufacturer specifications.

TEST FUNCTIONS EXPECTED RESULTS ACCEPTABLE

Mill start push button operation

The mill motor starts and the green light goes on

Yes

Mill stop push button operation

The mill motor stops and the green light goes off

Yes

Auger feed start push button operation

Auger feed motor starts and the green light goes on

Yes

Auger feed stop push button operation

Auger feed motor stops and the green light goes off

Yes

Auger feed control dial operation

Rotated from 0 to 6 & 6to0 ,the auger speed increases & decreases

Yes

Disconnect handle operation

Yes

O.Q elements in a colloidal mill

Colloid mill

Calibration requirements

Equipment control functions

Switches and push buttons

Equipment operations

Equipment rotation

directions

Motor directio

n

Auger feed

direction

Rotor blades1000 rpm.,2450 &4600

rpm

Motor fixed speed mill empty

Rotor blades

Auger feed21

rpm,208rpm

CALIBRATION REQUIREMENTS:Verify that all critical instruments on the equipment have been logged into the calibration system,record all information for the calibrated instruments used to control the mill in table

Calibrated and non calibrated instruments

Identification no.TypeManufacturerModel no.Serial no.RangeScale divisionLocationUseCalibration due dateCritical or non critical

AM-1463AMMETERAny gauge co.5449Not specified0-20AA0.5AMounted on the control panelMonitors the drive motorCalibration not required Not critical to be operation of the mill

There was no calibrated instruments on the blender non calibrated instruments as found conditions

Rotor and auger rotation test procedure

element Expected result

Result Acceptable

Rotor direction

The rotor should rotate in the same direction as the incoming product from the auger feed and the mill direction arrow

The rotor rotate in the same direction

Yes

Auger Feed direction

The auger feed should rotate in the same direction as the mill direction arrows

The auger feed rotating in the same direction

yes

Rotor blade test resultsSpecification(rpm±10%)

Rotor fly wheel pulley setting

Drive motor pulley settings

Measured speed(rpm)

Acceptable

100024504600

LargesmallSmall

SmallMediumlarge

102825804747

YesYesyes

Auger feed test resultsAuger feed speed control dial settings

Speed specialization (rpm±10%)

Measure speed(rpm)

acceptable

06

21208

21211

Yesyes

Instrument used

Test instrument Identification no. Calibration due date

Tachometer 64020

Colloidal mill operation

Motors fixed speed

Rotor blades(1000 rpm,2450 rpm,4600 rpm)

Auger feed(21 rpm,208 rpm)

Reduce granulation size

Milling medium sieve no

PQ ELEMENTS OF A COLLOIDAL MILL

Mill operation:The mill operation test is designed to document the performance of the colloidal mill using placebo granulation.The placebo is used for maximum loading conditions, this test is also design to verify the colloid mill can reduce the size of granules.The materials & instruments required for this test are a placebo , sieve , pan, scale & tachometer.Weigh the granulation in the sieve & pan before & after milling to verify the reduction in particle size.MILL PERFORMANCE TEST PROCEDURE:

Equipment

Granulating weight before milling

Granulation and weight after milling

Acceptable

Sieve 262g 0g Yes

pan 738g 1000g Yes

•Test materials & conditions:

item Specifications

Lactose hydrate 1kg

sieve 80 mesh size

Measure the speed of the rotor with a tachometer

Rotor speed specification=1000rpm±10%(±100)

Rotor speed specifications=2450±10%(±460)

Auger feed speed specifications =21rpm±10%(±2.1)

Auger feed speed specifications=208rpm±10%(±20.8)

Instruments usedTest instrument Identification

numberCalibration due date

1)Scale PE600

2)Stopwatch 54039

3)Tachometer 64020

conclusion

•Validation of equipments is done for the safety of the operators ,to minimize the errors in manufacturing products

•All this protocol of validation is to design by the quality control dept. in the industry

THANK YOU