This document provides standard operating procedures for qualifying various laboratory equipment used in pharmaceutical quality control testing. It includes procedures for calibrating hardness testers, friability test apparatus, tap density testers, disintegration testers, and dissolution test apparatus. The qualification process involves design qualification, installation qualification, operational qualification, and performance qualification to ensure equipment is properly installed, works correctly, and provides expected results. Calibration procedures are also described to verify equipment meets specifications.

1. QUALIFICATION OF
LABORATORY EQUIPMENTS
Sinhgad Institute of Pharmacy, Narhe
Pune-41
Name of student:
Miss. Pranali Polshettiwar
M. Pharm 1st yr. Sem. II
(Pharmaceutical Quality Assurance)
Name of guide:
Ms. Shubhangee. S. Gaikwad
Assistant Professor M. Pharm
(Pharmaceutical Quality Assurance)
Date of seminar: 24/06/21
Time of seminar: 1:30pm – 2:10pm

2. Contents
Introduction
Qualification of Hardness tester
Qualification of Friability test apparatus
Qualification of Tap density tester
Qualification of Disintegration tester
Qualification of Dissolution test apparatus

3. Validation
A documented objective evidence that provides a high degree
of assurance that a specific process will consistently
produce a product meeting its predetermined specifications.
Qualification
Qualification is part of validation, but the individual qualification steps
alone do not constitute process validation. It is action of proving and
documenting that equipments are properly installed, work correctly,
and lead to expected results.
Calibration
It is the activity of checking, by comparison with a standard, the accuracy of a
measuring instrument of any type.
3

4. Various phases of qualification
1. Design Qualification (DQ)
2. Installation Qualification (IQ)
3. Performance Qualification (PQ)
4. Operational Qualification (OQ)
4

5. A timeline approach to laboratory equipment qualification 5

6. Hardness tester
Hardness (crushing strength)
It is the load required to crush the tablet when placed on its edge.
 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.
 Some of devices used to test tablet hardness are:
1. Monsanto tester
2. Strong-cobb tester
3. Pfizer tester
4. Erwika tester
6
Erwika tester
Strong-cobb tester
Monsanto tester
Pfizer tester

7. Qualification of Hardness tester
Standard Operating procedure
Department : Quality Control Department
Title : Calibration of Hardness Tester
Objective : To provide the procedure for calibration of hardness tester
Scope : Applicable to determination of weight, diameter, hardness and thickness of
a tablet during in process checking.
Responsibility: Quality control chemist
7
Components of hardness tester

8. Procedure:
 Take out the force gauge to be calibrated and hold vertically up.
 Adjust the zero on the force gauge.
 Standard Weights are then applied to the hook of force gauge
and measure the tension of the spring on the force gauge.
 When 1 kg of standard weight is applied, scale on the force
gauge should also show 1 kg tension produced from the
initial point where pointer is adjusted.
 Adjust the zero on the force gauge again.
 Follow the same procedure for other weights.
 The test to be carried out for 1.0 kg, 2.0 kg, 5.0 kg, 10.0 kg,
20.0 kg & 30.0 kg standard weights.
Tolerance: ± 0.25 kg / ± 0.1 kg
Frequency: Once in 6 months.
8
Force gauge and hook

9. Calibration report
9

10. Friability test apparatus
 Friability is the condition of being friable, describes the tendency of a solid substance to break
into smaller pieces under duress or contact, especially by rubbing.
 Friability is defined as the % weight loss by tablets due to mechanical action during the test.
 Minimum weight loss of the tablet should not be NMT 1 %
 Friability is usually measured by use of Roche Friabilator or tumbler test.
 Applicable for compressed uncoated tablet & intended to determine the strength of tablet
during transportation & storage the tablets should retain its shape & size.
https://youtu.be/JZUjnjOjuKg
10
Roche Friabilator

11. Qualification of Friability test apparatus
11
Standard Operating procedure
Department: Quality Control Department
Title : Calibration of Friability test apparatus
Objective : Objective of this report is to provide documented
evidence through the verification of installation,
operation and performance of Tablet Friability
tester to show that the instrument installed, operated
and consistently performed according predetermined
specifications.
Scope : Procedure applicable for calibration of the
friability apparatus.
Responsibility: Quality control chemist

12.  This testing involves repeatedly dropping a sample of tablets over a fixed time, using a
rotating wheel.
 The result is inspected for broken tablets and the percentage of tablet mass lost through
chipping.
Procedure:
 Switch ON the power.
 The drum will initialize itself to the loading position at the power ON.
 The display will show “start”.
 After the weighing, slide the tablets gently into the drum from the slide slit provided on the
drum:
(A) tablets with a unit mass equal to or less than 650 mg, take sample of whole tablets
corresponding to 6.5 g.
(B) tablets with a unit mass of more than 650 mg, take a sample of whole 10 tablets.
 Select the “TIME MODE” or “REVOLUTION COUNT MODE” as desired by pressing the
TIME/COUNT key respectively.
 The MODE indicator LED will indicate the selected mode. 12

13.  The display will show the previous Time or Count Values.
 Enter the desired value (25 rpm, 4 minutes or described under individual monograph) for the
selected mode and press ENTER KEY to register the value.
 Press RUN/HALT key to start the test .
 The drum will start rotating.
 The display will show elapsed Time or Count on depending on the mode selected.
 When the test is over, the drum rotates in the reverse direction , discharging the tablets into the
tray.
 Take weight after rotation is completed .
 Then drum will initialize itself to loading position and display will show “start” indicating that
the instrument is ready for the next test.
 In case during the test, if the user needs to change the Time/Count value, press RUN/HALT
key.
 Pressing the RUN/HALT key again to continue the test .
 Find out the loss in weight of the tablets(i.e. A-B)
13

14.  Calculate the percentage of loss by following formula :
(A-B)× 100 ÷A
 Find out the percentage loss.
 Make the entry in the usage log book.
 Similarly , operate the instrument and count the revolution for calibration as annexure 1.
Frequency: Monthly and after major maintenance.
14

15. Observations
Qualification shall be executed using following forms:
Annexure- A Installation verification check list
15
Sr.
No
Checks to be performed Acceptance criteria Observation Checked
by/Date
1 Check for the receipt of the
consignment.
It shall be received in good
condition.
2 Check for any scratches on
the machine, body and drums.
It shall not have any scratches
on machine, body and drums.
3 Check for electrical
connection.
It shall not observed a loose
or damage connection.
4 Check for levelling of the
platform.
Air bubble of level indicator
should be at centre.
5 Check both drums are
properly locked with knob on
the shaft.
Both drums should be
properly locked with knob on
the shaft.

16. Annexure- B
Calibration of measuring devices
16
Sr. No Measuring devices Acceptance criteria Observation Checked
by/Date
1 Vernier Calliper It should be calibrated
within calibration
period.
2 Thermometer It should be calibrated
with calibration period.
3 Stopwatch It should be calibrated
within calibration
period.
4 Multimeter It should be calibrated
with calibration period.

17. Annexure- C Site inspection checklist
17
Sr. No Parameter Acceptance criteria Observation Checked
by/Date
1 Room temperature 15 to 30°C
2 Room Humidity 40 to 70%
3 Room environmental checks -away from direct sunlight.
-free from vibration
-no corrosive gases
-free from excess dust
4 Point for electrical connection Single phase of 230 V AC 50 Hz
5 Base / table level Levelled sturdy, with no vibration
6 Earthing Shall be provided
Annexure- D Utility verification checklist
Sr. No Parameter Acceptance criteria Observation Checked by/Date
1 Phase voltage Single phase, 220/230 V AC 50/60 Hz

18. Annexure- E Technical Specification checklist
18
Sr. No Test Acceptance criteria Observation Checked
by/Date
1 Speed 25 revolution per minute (RPM)
2 Speed Accuracy ± 1 RPM
3 Time Range 04 Minutes
4 Count Range 01 to 99999 revolutions
5 Motor DC Stepper Motor of 3.5 KgCm Torque, 6 Volts
6 Type of Drum Electrolab AD Drum and Abrasion Drum
7 Power supply Single Phase, 220/230 V AC 50/60 Hz
8 Fuse Rating T 160 mAmp-(for I/P supply as 220/230 V AC, 50/60
Hz)
9 Dimension 350 mm (L) X 310 mm(W) X 430 (H)
10 Weight 12 Kg. (approx.)
11 No. of Drums 1 or 2 Nos.
12 No. of Discharge 02 Nos.

19. Annexure- F
Drums Specification checklist
19
Name Acceptance criteria (as per USP
general chapter- 1216)
Observatio
n
Checked
by/Date
Drums One side removable
Material Transparent synthetic polymer with
polished internal surfaces
Inside radius of curved
projection
80.5 ± 5.0 mm
Diameter of central hole 10.0 ± 0.1 mm
Diameter of central ring 25.0 ± 0.5 mm
Inside diameter of drum 287.0 ± 4.0 mm
Outside diameter of
drum
302.5 ± 4.0 mm
Depth of drum 38.0 ± 2.0 mm
Tablet dropping height 156.0 ± 2.0 mm
Drums

20. Annexure- G Operational verification checklist
20
Sr.
No.
Operation Acceptance criteria Observation Checked
by/Date
1 Switch ON the power
switch
Drum shall initialize itself to loading position & display shall
now show START
2 a) Press TIME key to
select the TIME MODE.
The MODE indicator LED shall indicate the TIME MODE.
The display shall show the previous time values.
b) Enter desired value by
using numerical keys.
Press ENTER key to
register value.
The display shall show 00
c) Press RUN/HALT key. The drum shall start rotating in forward direction. The display
shall show elapsed time. When the test is over the drum shall
rotate in reverse direction for discharging the tablets into the
tray. Indication of test over shall show by an audible beep.
The display shall show END.
d) Press RESET key Instrument shall initialize and will stop at loading position.

21. Annexure- I Power failure challenge study
21
Sr.
No
Test procedure Acceptance criteria Observation Checked
by/Date
1 Start the instrument. Instrument shall run.
2 Turn main power to the
instrument OFF.
The instrument shall get OFF.
3 Turn power ON. Instrument should not start spontaneously.
4 Start the instrument. Instrument should resume from the stop condition with
all the parameters found as before POWEROFF.
Annexure- J Performance of Instrument
Performance of instrument is checked by taking different size or shape of tablets (different size and shape
causes a regular and irregular tumbling). Initially weighed tablets are transferred gently into the drum from
the side slit provided on the drums. The TIME mode is set for 4 min. i.e., 100 rotations. Calculated the
friability and result is recorded.

22. Tap density tester
Tapped density
 The tapped density is an increased bulk density attained after mechanically tapping a container
(graduated measuring cylinder) containing the powder sample.
 It is used to predict both flow properties and its compressibility.
https://youtu.be/gDvEbkuhuvc
22
Tap density tester

23. Qualification of Tap density tester
Standard Operating procedure
Department: Quality Control Department
Title : Calibration of Tap density tester
Objective : To describe the operation and calibration procedure of Tap density apparatus.
Scope : This SOP is applicable to the operation and calibration procedure of
Tap density apparatus
Responsibility: Officer / Executive - Quality control
23

24. Procedure:
 Ensure that working area is clean and all the connections of instruments are proper.
 Weigh the sample and fill in a measuring cylinder of tapped density tester.
 If sample weight is about 100g or above, use 250 ml measuring cylinder otherwise use100 ml
measuring cylinder.
 Fix the measuring cylinder into the holder provided for holding the measuring cylinder on the
instrument.
 Power ON the instrument.
 The system will initialize itself and the display will flash and show the startup screen.
 The system is now ready for setting of the test parameter and to run the test.
 Set the mode of operation as USER.
24

25.  Press the SET key to set the test parameter. The taps are programmable from 1 to 9999 taps.
 By using the arrow SET THE TAP VALUE.
 After setting the tap value, press the START key to start the test.
 After tapping is complete, check the volume, set the similar number of taps again and run the
test once more.
 Check the volume after second tapping cycle and calculate the difference between the two
volumes observed after tapping.
 If this difference is not less than 2% continue the tapping for one more cycle and this activity
shall be repeated until the difference between succeeding measurement is less than 2%.
Frequency : Monthly
25

26. URS for tap density apparatus
 Operating criteria must be adequate.
 Easy maintenance.
 Equipment should not disseminate dust.
 Low cost.
 Non reactive surface.
 Capacity (100 ml, 250 ml)
Design Qualification (DQ)
The following are the key considerations for DQ:
 Physical dimensions of the equipment and accessories.
 Suitable operating environment of the instrument.
 Health and safety requirement.
26

27. Installation Qualification (IQ)
Details of the equipment:
 Equipment name, made by & model no. shall be noted down.
 Location for the installation equipment shall be checked.
 Utilities required shall be listed down.
 Any deviation observed during above procedures should be informed for corrective action.
Installation procedure:
 After checking all the specifications as mentioned in the selection criteria, service engineer
shall commission the equipment.
 Authorized validation team shall carry out installation qualification.
27

28. Operational Qualification (OQ)
 Check the OQ parameters against their specifications.
 Document the deviation details. The quality head and the department head shall decide whether
deviation is acceptable or not.
 It should support USP I (300 taps/min) and USP II (250 taps/min).
 It should have simultaneous rotating and tapping motion assures an evenly packed surface.
 Calculation of test results like tapped density, compressibility index and hausner ratio.
 It should have printer port for documenting test results as per GMP/GLP standards.
 The acoustic cabinet reduces the sound level to 71 dB to meet laboratory standards.
28

29. Performance qualification (PQ)
 It is determined by placing a graduated cylinder containing known mass or volume of drug or
formulation on a mechanical tapper apparatus, which is operated for a fixed no. of taps until
the power bed volume has reached a minimum.
 Count and check RPM as per international standards.
 Other procedures specified by relevant international standards. Such as in pharmaceutical test,
weigh the tapping assembly including the cylinder and cylinder holder and check if weight is
in the right range.
29

30. Disintegration apparatus
 For a drug to be readily available to the body, it must be soluble and form solution.
 For most tablets, the first important step toward solution is break down of the tablet into
smaller particles or granules, a process called disintegration.
 Disintegration Tester is designed for the accurate estimation of disintegration time of tablets as
per IP/USP standards. The instrument is designed to test two batches of six tablets,
simultaneously. https://youtu.be/KqtOdo8Kxvk
30
Disintegration apparatus

31. Qualification of Disintegration tester
31
Standard Operating procedure
Department: Quality Control Department
Title : Calibration procedure for Disintegration
apparatus
Objective : To calibrate disintegration apparatus
Scope : This SOP applies to the disintegration test
apparatus in the quality control department
Responsibility: Quality control chemist

32. A. Calibration for Number of Oscillations per minute
 Take a pre-calibrated stopwatch. Operate the apparatus as per SOP. Start the apparatus and
stopwatch simultaneously and count the number of oscillations per minute.
 Repeat the same for five times and note down the number of oscillations per minute for each
time.
 The oscillations per minute shall be within the limit of 29 to 32 through a distance of 53 to 57
mm throughout the period of operation. Record the observation.
B. Calibration for Temperature:
 Switch on apparatus and turn on the heater by pressing ‘ON’ key.
 Set the bath temperature by pressing scroll keys.
 Wait till the temperature of beaker A and beaker B attain the set value.
 Screen shall show the set temperature of bath and the temperature of beaker A and beaker B.
 Take a pre-calibrated thermometer and check the temperature of beaker A and beaker B.
 Record the observation.
32

33. C. Timer Calibration
 Set the timer for 30 minutes. Start the equipment and stop watch simultaneously. Note the stop
watch reading immediately when equipment stops and note down the observation.
 Observed time should not deviate by ‘± 1 min’ of set time.
D. Sieve Integrity Test
Check the ‘integrity’ of woven stainless steel cloth (sieve) attached to the base plate of each
basket with a pre-calibrated vernier calliper. The sieve has weaven squares of aperture of 1.8 –
2.2 mm and wire diameter of 0.57 to 0.66 mm.
Note the observations.
 Affix the ‘CALIBRATION STATUS’ tag duly filled and signed on the equipment after
completion of calibration.
 If the instrument is out of calibration then affix ‘UNDER MAINTENANCE’ tag and inform to
maintenance department.
Frequency: Once in a month or after each maintenance.
33

34. URS for Disintegration test apparatus
 Operating criteria must be adequate.
 Easy maintenance.
 Equipment should not disseminate dust.
 Low cost.
 Spares should be easily available.
 Non reactive surface.
 Audio visual indicators for system status.
 Printer attachment facility.
Operational Qualification (OQ)
 Check the OQ parameters carefully.
 Document the deviation details. The quality head and the department head shall decide whether
deviation is acceptable or not. 34

35. Disintegration apparatus Model 901
System Digital Tablet Disintegration Apparatus
Up and Down speed 30 RPM ± 2 RPM
Accuracy 2 %
Operating temp. range 0 – 100 °C
Power 230 ± 10 %, 50 Hz AC
Dimensions 450 mm (H) X 300 mm (W) X 320 mm (L) (approx.)
Weight 8 ltrs. (approx.)
Performance Qualification (PQ)
 Ensure the apparatus is properly connected to the power supply.
 When the power is switched on , the timer and temp. shows digital value.
 Fill the beaker of apparatus with purified water and adjust the temp. between 37 ± 2°C.
35

36.  Fix the beaker in its position and adjust the level of water.
 Start the basket- rack assembly and timer simultaneously.
 Place the standardized calibrated thermometer to record the actual temp. against the temp.
displayed.
 Note the temp. of water in the beaker and oscillation per minute of the basket- rack assembly.
 Switch OFF the apparatus and record the observation in the calibration record.
Acceptance criteria
 The temp. shall be between 37 ± 2°C.
 The frequency of basket rack shall be between 29 to 32 cycles per minute.
36

37. Dissolution apparatus
Dissolution
 The process by which a known amount of drug substance goes into solution per unit of time
under standardized conditions.
 Dissolution testing is used as a quantitative tool to provide measurements of the bioavailability
of a drug as well as to demonstrate bioequivalence from batch-to-batch.
https://youtu.be/hhb2I-fIwB4
Types of dissolution apparatus
 IP : Paddle, Basket
 BP : Basket, Paddle,
Flow through cell
 USP: Basket, Paddle,
Reciprocating cylinder,
Flow through cell,
Paddle over disc,
Rotating cylinder,
Reciprocating disc.
37

38. Qualification of Dissolution Apparatus
Standard Operating procedure
Department: Quality Control Department
Title : Calibration procedure for Dissolution test
apparatus
Objective : To provide a procedure for the calibration and
validation of dissolution test apparatus.
Scope : Procedure describes how to validate the centering of paddle and basket rod
with that of jar, validate wobbling of paddle/basket rod, temperature of
test medium throughout the test revolution per minutes of paddle or basket
shaft as well as the distance between paddle and jar bottom.
Responsibility: Quality control chemist
38

39. The instrument shall be calibrated for RPM and Temperature.
For Temperature Calibration:
 Measure the temperature of the water bath and of each jar with a calibrated thermometer and
compare the result against the digital display on the apparatus.
 Acceptance Criteria: 37°C ± 0.5°C
For RPM Calibration:
 Calibrate the apparatus at 50 and 100 RPM.
 Compare the RPM shown on the digital display
of the apparatus with the RPM measured with a
stopwatch or Tacometer.
Acceptable criteria: ± 1 RPM – for 50 RPM
± 2 RPM – for 100 RPM
Frequency: Monthly 39
Stopwatch measuring RPM

40. Installation Qualification
Details of the equipment
 Supplier or manufacturer name and address
 Equipment name and model no
 In-house equipment code no.
 Location
 Utilities
Procedure
 Site inspection, environmental conditions and prerequisite
 Parts identification list
 Validation of physical parameter
 SOPs
 Computerized system 40

41. Operational Qualification
Procedure
 Power ON check
 Lift movement check
 Temperature accuracy
 Accuracy of shaft rotation
 Control of paddle wobbling
 Control of paddle centering
 Control of distance of shaft to side vessel
 For automated dissolution system
 Software/hardware communication
 Operator interface functions
 Stress/boundary/challenge testing
41

42. Performance Qualification
Procedure
 Test must be conducted for each of the combinations of vessels and apparatus.
 USP calibrator tablets are used: Disintegrating Tablets (Prednisone)
Non- disintegrating Tablets (Salicylic acid)
 Effectiveness of dissolution will be qualified by determining drug content in the solution.
 For the comparison, solution of known concentration of USP reference standards is used.
 Document the deviation details.
Maintenance Schedule:
42
Frequency Procedure/Parameter
After each test Clean up the system
weekly Inspect: Circulating water pump
Bath water
monthly Replace bath water
Every 6 months Check temperature calibration
Calibration of the system
Inspect- guide rods & spindle bearings
annually Inspect: belts & idler pulleys
Every 2 years Replace the belts

43. � Key References
1. Jain, K. and Bharkatiya, M., 2018. Qualification of Equipments: A Systematic
Approach. International Journal of Pharmaceutical Erudition, 8(1), pp.7-14.
2. Kapoor, D., Vyas, R.B. & Dadrwal, D., 2018. An Overview of Analytical Instrument
Qualification with Reference of Pharmaceutical Industry. Journal of Drug Delivery and
Therapeutics, 8(5), pp.99–103.
3. Frost, S.M.A., 2004. Introduction to the Validation of a Dissolution Apparatus. Dissolution
Technologies, 11(1), pp.19–21.
4. Bansal, S.K. et al., 2004. Qualification of analytical instruments for use in the pharmaceutical
industry: A scientific approach. AAPS PharmSciTech, 5(1), pp.151–158.
5. Potdar, M. and Dubey, R., 2018. cGMP: Current Good Manufacturing Practices for
Pharmaceutical. 2nd ed. Pharmamed press, pp.444–446.