validation of colloidal mill

1. VALIDATION OF PULVERISATION
MACHINES
M.SRINIVAS
M.PHARM. II SEM.
VAAGESWARI COLLEGE OF PHARMACY

2. CONTENTS
• DEFINITION
• PRINCIPLE
• CONSTRUCTION
• WORKING
• APPLICATIONS
• VALIDATION
• CONCLUSION

3. 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.

4. 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.

5.  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

6. COLLOIDAL MILL

7. VALIDATION
VALIDATION
PERFORMANCE
DESIGN INSTALLATION OPERATIONAL
QUALIFICATIO
QUALIFICATION QUALIFICATION QUALIFICATION N

8. 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.

9. 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.

10. IQ ELEMENTS OF A COLLOID MILL
EQUIPMENT REQUIRED COMPONENT EQUIPMENT
MAJOR
QUALIFICATI DOCUMEN UTILITIES MATERIAL LUBRICANTS SAFETY
COMPONENTS
ON TS FEATURES
DRIVE
MANNUAL
VOLTS(460) &
DRAWINGS
AMPS(20) AUGER
SOPS
MOTORS

11. EQUIPMENT IDENTIFICATION:
Record the equipment identification numbers along with the
following order
REQUIRED INFORMATION:
Purchase order 009235
Model number DAS60
Serial number 78801
Equipment number 6492
Location Room 270(this equipment is
portable)

12. • 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 Measure acceptab
d result le
Volts Drive 460±10% A-B455;A- Yes
motor C457
amperes Drive 11 B-C456
motor
Auger
motor 1.17 20 circuit
rotations yes

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

14. 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.

15. 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 type manufacture Product
used rs contact
Gear box Amolitb#2 oil No
Pillow block Lubriplate 630- No
bearing and 2 grease
casters

16. Safety features test procedure
Test function Expected results Acceptable
Safety interlock switch When the mill and Yes
operations 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 yes
removed

17. 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 ACCEPTAB
LE
Mill start push button The mill motor starts and the green Yes
operation light goes on
Mill stop push button The mill motor stops and the green Yes
operation light
goes off
Auger feed start push Auger feed motor starts and the green Yes
button operation light goes on
Auger feed stop push Auger feed motor stops and the green Yes
button operation light goes off
Auger feed control dial Rotated from 0 to 6 & 6to0 ,the auger Yes
operation speed increases & decreases
Disconnect handle Yes
operation

18. O.Q elements in a colloidal mill
Colloid mill
Calibration Equipment Equipment
requirements control functions operations
Switches and push Equipment Motor fixed speed
buttons rotation directions mill empty
Rotor blades
Auger feed Auger feed
Motor direction 1000 rpm., Rotor blades
direction 21 rpm,208rpm
2450 &4600 rpm

19. 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
There was no calibrated instruments on the blender non
calibrated instruments as found conditions
Identification no. AM-1463
Type AMMETER
Manufacturer Any gauge co.
Model no. 5449
Serial no. Not specified
Range 0-20AA
Scale division 0.5A
Location Mounted on the control
Use panel
Calibration due date Monitors the drive motor
Critical or non critical Calibration not required
Not critical to be operation
of the mill

20. Rotor and auger rotation test procedure
element Expected Result Acceptable
result
Rotor direction The rotor The rotor rotate Yes
should rotate in in the same
the same direction
direction as the
incoming
product from
the auger feed
and the mill
direction arrow
Auger Feed The auger feed The auger feed yes
direction should rotate in rotating in the
the same same direction
direction as the
mill direction
arrows

21. Rotor blade test results
Specificati Rotor fly Drive Measured Acceptable
on(rpm±1 wheel motor speed(rpm
0%) pulley pulley )
setting settings
1000 Large Small 1028 Yes
2450 small Medium 2580 Yes
4600 Small large 4747 yes
Auger feed test results
Auger feed Speed Measure acceptable
speed specializati speed(rpm
control on )
dial (rpm±10%)
settings
0 21 21 Yes
6 208 211 yes

22. Instrument used
Test instrument Identification no. Calibration due
date
Tachometer 64020

23. PQ ELEMENTS OF A COLLOIDAL MILL
Rotor blades(1000
rpm,2450
rpm,4600 rpm)
Motors fixed speed
Auger feed(21
Colloidal mill rpm,208 rpm)
operation
Reduce granulation Milling medium
size sieve no

24. 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 Granulatin Granulatio Acceptable
g weight n and
before weight
milling after
milling
Sieve 262g 0g Yes
pan 738g 1000g Yes

25. • 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)

26. Instruments used
Test instrument Identification Calibration due date
number
1)Scale PE600
2)Stopwatch 54039
3)Tachometer 64020

27. 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