1.0   OBJECTIVE:

1.1 Objective is to record the findings of qualification study executed as per pre-approved protocol and to show that the digital weighing balance stands qualified for routine use.

2.0  SCOPE:

2.1 The scope of this report is limited to Digital Weighing Balance having Id No. XYZ

3.0 RESPONSIBILITIES:

Maintenance Officer/Executive: To prepare qualification protocol, report and co-ordinate the entire qualification activity.

Quality Assurance Officer/Executive: To witness the qualification study and ascertain that the study is conducted as per the protocol.

Production Officer/Executive: To execute qualification study in co-ordination with other departments.

Head Maintenance: To review the qualification documents.

Head Quality Assurance: To approve the qualification documents.

4.0 BALANCE DESCRIPTION:

Sr. No.	ID. No.	Capacity	Least   count	Location	Make	Model No.	Serial No.
1	XYZ	Max. : 50.00 Kg Min. : 0.50 Kg	0.01 Kg	Packing Hall	Mettler Toledo	NA	Example: ABCD

5.0 ACCEPTANCE CRITERIA:

Qualification of the equipment should meet the acceptance criteria outlined in the following steps.

5.1 Installation Verification Report

Sr. No.	Check points	Acceptance criteria	Observations	Checked by sign/date
1	Check the levelling of the equipment on level indicator.	Air bubble shall be at centre position of level indicator.
2	Placing location	1. Bench top or floor shall be steady and even surface. 2. Location shall be free from heat, vibration and moisture.

5.2 Multimeter Calibration Verification Report

Sr. No.	Measuring Device	Acceptance Criteria	ID. No.	Calibration  done On & due on	Observation	Checked by Sign/ Date
	Multimeter	It shall be calibrated for its performance.

5.3 Calibration Status of Standard Weights

Sr. No.	Standard Weights	Acceptance criteria	Observation	Checked by sign/date
1	Check the calibration of standard weights.	Standard weights should be calibrated for its performance.

5.4 Operational Verification Report

Sr. No.	Check points	Acceptance criteria	Observations	Checked by sign/date
1	Press ‘Φ’ button.	Balance should turn ON.
2	Press ‘T’ button.	Balance should tare (zero – setting).
3	Press ‘Φ’ button.	Balance should turn OFF.

5.5 Utility Verification Report

Sr. No.	Utility	Acceptance criteria	Observation	Checked by sign/date
1	Electricity	Single phase, 230 + 10% V AC and 50 + 5% Hz

 5.6 Eccentricity Test Report

5.6.1 Procedure

Eccentricity test is carried out by placing 1/3 rd weight of maximum capacity i.e. 20.00 Kg on weighing platform at 5 different locations (four corners & center) and Values displayed by Balance against standard weight are recorded in a following table.

Location ID	Standard Weights	Observation/Weight Displayed	Checked by sign/date
1	20.00 Kg
2	20.00 Kg
3	20.00 Kg
4	20.00 Kg
5	20.00 Kg

• Acceptance Criteria: 19.18 Kg to 20.02 Kg

• Remark: ______________________________________________________________________________________________________________________________________________________

5.7 Linearity Test Report

5.7.1 Procedure

Linearity test is carried out by placing 4 different standard weights i.e. 0.50 Kg, 15.00 Kg, 30.00 Kg and 50.00 Kg one by one on weighing platform in ascending order and by removing the placed standard weights in descending order. Values displayed by Balance against standard weights area recorded in a following table

Sr. No.	Standard Weights	Observation/Weight Displayed	Checked by sign/date
A	Ascending order
1	0.50 Kg
2	15.00 Kg
3	30.00 Kg
4	50.00 Kg
B	Descending  order
1	50.00 Kg
2	30.00 Kg
3	15.00 Kg
4	0.50 Kg

• Acceptance Criteria:     0.49 Kg to 0.51 Kg for 0.50 Kg

   14.98 Kg to 15.02 Kg for 15.00 Kg

   29.97 Kg to 30.03 Kg for 30.00 Kg

   49.95 Kg to 50.05 Kg for 50.00 Kg

• Remark: ________________________________________________________________________________________________________________________________________________________________________________________________________

5.8 Repeatability Test Report

5.8.1 Procedure:

Repeatability test is carried out by placing minimum i.e. 0.50 Kg, optimum i.e. 25.00 Kg and maximum i.e. 50.00 Kg weight of capacity of balance 5 times on weighing platform and values displayed by Balance against standard weight are recorded in a following table.

Sr. No.	Standard Weights	Observation/Weight Displayed	Checked by sign/date
1	0.50 Kg
2	0.50 Kg
3	0.50 Kg
4	0.50 Kg
5	0.50 Kg
6	25.00 Kg
7	25.00 Kg
8	25.00 Kg
9	25.00 Kg
10	25.00 Kg
11	50.00 Kg
12	50.00 Kg
13	50.00 Kg
14	50.00 Kg
15	50.00 Kg

• Acceptance Criteria:     0.49 Kg to 0.51 Kg for 0.50 Kg

                                                 24.97 Kg to 25.02 Kg for 25.00 Kg

                                                 49.95 Kg to 50.05 Kg for 50.00 Kg

• Remark: ______________________________________________________________________________________________________________________________________________________

6.0 DEVIATION REPORT:

Sr. No.	Deviation (s)	Justification for acceptance criteria	Impact on installation, operation and performance

7.0 CHANGE CONTROL:

8.0 LIST OF ANNEXURE:

9.0 SUMMARY AND CONCLUSION OF QUALIFICATION

10.0 CERTIFICATION OF QUALIFICATION:

        Qualification is satisfactory.                                     Yes/No

        Hence Balance can be used for routine use.             Yes/No

                                                                                                            Head- Q.A.

1.0   OBJECTIVE:

Objective of this report is to provide documented evidence through the verification of  installation, operation &  performance of Tablet Friability Tester to show that the instrument  installed, operated and consistently performed according  to predetermine specifications.

2.0   SCOPE :

The scope of this Report is limited to Id No. XYZ

3.0  QUALIFICATION TEAM AND RESPONSIBILITIES:

DEPARTMENT	NAME & SIGNATURE	RESPONSIBILITY
Maintenance		To prepare qualification report. To co-ordinate the entire qualification activity.
Quality Assurance		To execute qualification study in co-ordination with other departments.
Production		To execute qualification study in co-ordination with other departments.
Maintenance		To review the qualification documents.
Head – Quality Assurance		To approve qualification protocol & report.

4.0    INSTRUMENT DESCRIPTION:

  For instrument description, should match as per re qualification protocol

 5.0   ACCEPTANCE CRITERIA:

Qualification of  the instrument shall be in accordance with the parameters given in Annexures – A, B, C, D, E, F, G, H, I & J of this report.

 6.0   OBSERVATIONS:

 Qualification shall be executed using following forms:

• Installation verification checklist – Refer Annexure – A.
• Calibration of measuring device– Refer Annexure – B.
• Site inspection checklist – Refer Annexure – C.
• Utility verification checklist – Refer Annexure – D.
• Technical specification checklist – Refer Annexure – E.
• Drum specification checklist – Refer Annexure – F.
• Operation verification checklist – Refer Annexure – G.
• Parameter challenge study –  Refer Annexure – H.
• Power failure challenge study – Refer Annexure – I.
• Performance of instrument –   Refer Annexure- J.

Annexure- A

INSTALATION VERIFICATION CHECK LIST

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.

Annexure- B

CALIBRATION OF MEASURING DEVICES

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 within calibration period.
3	Stopwatch	It   should   be calibrated within calibration period.
4	Multimeter	It   should   be calibrated within calibration period.

Annexure- C

SITE INSPECTION CHECKLIST

Sr.No.	Parameter	Acceptance criteria	Observation	Checked by/ Date
1	Room Temperature	15 to 30°C
2	Room Humidity	40 to 70 % RH
3	Room environmental checks	– Away from direct sunlight. – Free from vibration. – No corrosive gases. – Free from excess dust and moisture.
4	Table space	Width :15” Length : 18” Height :  20”

Sr.No.	Parameter	Acceptance criteria	Observation	Checked by/ Date
5	Point for electrical connection	Single phase of 230 V AC 50 Hz
6	Base/table level	Levelled sturdy, with no vibration.
7	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 VAC, 50/60 Hz.

Annexure- E

TECHNICAL SPECIFICATION CHECKLIST

Sr. No.	Test	Acceptance criteria	Observation	Checked by/ Date
1	Speed	25 Revolutions per minute (RPM)
2	Speed Accuracy	± 1 RPM
3	Time range	01 Sec. to 09 Hrs.59 Min. 59 Sec.
4	Count Range	01 to 99999 revolutions.
5	Motor	DC Stepper Motor of 3.5 KgCm Torque, 6 Volts
6	Type of the 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	350mm (L) X 310mm X 430mm (H)
10	Weight	12 Kg. (approx.)
11	No. of Drums	02 Nos.
12	No. of Discharge Trays	02 Nos.

Annexure- F

DRUMS SPECIFICATION CHECK LIST

Sr. No.	Name	Acceptance criteria (As per USP General Chapter – 1216)	Observation	Checked by / Date
1	Drums	– One side removable.
—	—	—	Drum 1 and Drum 2	—
–	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.
–	–	–	–

Annexure- G

OPERATIONL VERIFICATION CHECKLIST

Sr. No.	Operation	Acceptance criteria	Observations	Checked by/ Date
1	Switch ‘ON’ the power switch.	– The drum shall initialize itself to the  loading position. – The 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 the desired value by using numerical keys. Press ‘ENTER’ key to register the 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.	The instrument shall initialize and will stop at the loading position.
3	a) Press ‘COUNT’ key to select the “COUNT MODE”.	– The MODE indicator LED shall    indicate the “COUNT MODE”. – The display shall show the previous count values.
	b) Enter the desired value by using numerical keys. Press ‘ENTER’ key to register the value.	The display shall show ‘00’.
	c) Press ‘RUN/HALT’ key.	– The drum shall start rotating in forward direction. – The display shall show elapsed count. – 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 test over shall show “END”.
	d) Press ‘RESET’ key.	The instrument shall initialize and the will stop at the loading position.

POWER FAILURE CHALLENGE STUDY (Annexure- I)

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 resumes from the stop condition with all the parametrs found as before POWER – OFF.

PERFORMANCE OF INSTRUMENT (Annexure- J)

1.0  Procedure:

Performance of instrument is checked by taking different size or shape of tablets   ( different size or shape of tablets 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 minute i.e. 100 rotations. Calculated the friability and result is recorded in following tables.

 a) For regular tumbling, set the instrument at normal position, as there is no any irregular tumbling of tablets.

b) For irregular tumbling, set the instrument with 10° tilt with the bench top to prevent any irregular tumbling of tablets.

 1.1    Acceptance criteria:  Performance of instrument shall be found satisfactory.

 1.2   For Normal Position: 

 Product Name: 

 Batch No.:

Sr. No.	Time Set in Minute	Initial weight	Final weight	Friability	Checked by/Date
1
2
3

1.3   For 10° Tilt Position: 

Product Name: 

Batch No.:

Sr. No.	Time Set in Minute	Initial weight	Final weight	Friability	Checked by/Date
1
2
3

7.0 DEVIATION REPORT:

Sr. No.	Deviation (s)	Justification for acceptance criteria	Impact on installation, operation and performance

8.0   CHANGE CONTROL:

9.0   LIST OF ANNEXURE:

10.0   SUMMARY AND CONCLUSION OF QUALIFICATION:

11.0   CERTIFICATION OF QUALIFICATION:

        Qualification is satisfactory                                          Yes/No

        Hence instrument can be used for routine use.           Yes/No                                            

1. OBJECTIVE:

Objective of this report is to check and provide documented evidence of its performance as per the predetermined acceptance criteria.

Refer working and principle of RMG https://pharmaceuticalupdates.com/2020/04/27/working-and-principle-of-rapid-mixer-granulator-rmg/

2.   SCOPE:

The scope of this report is limited to equipment ID No. XYZ.

3. QUALIFICATION TEAM AND RESPONSIBILITIES:

DEPARTMENT	NAME AND SIGNATURE	RESPONSIBILITY
Quality Assurance		To prepare performance qualification protocol and report. To co-ordinate the entire qualification activity.
Production		To execute qualification study in co-ordination with other departments.
Quality Assurance		To execute qualification study in co-ordination with other departments.
Maintenance		To review the qualification documents.
Head – Quality Assurance		To approve qualification protocol & report.

4. EQUIPMENT DESCRIPTION:

Equipment description shall be match as per design qualification protocol.

5.  ACCEPTANCE CRITERIA:

Performance Qualification of the equipment shall be in accordance with the parameters given in FORM – A of this report.

6.  PROCEDURE:

Perform the qualification as per following form,

Performance of Equipment

PERFORMANCE OF EQUIPMENT

Performance of the equipment is verified by simulating the normal operation for dry mixing, granulation and milling of the ingredients. While doing the exercise consideration is given to the operational range of the equipment that is at minimum level (20% of capacity), optimum level (50% of the capacity) and maximum level (80% of the capacity). At the end of the granulation process wet mass is checked for its physical appearance.

  1.0 Minimum Level: (20 % of capacity)

Product Name              :

Batch No.                     :

 Theoretical Batch Size  :

Practical Batch Size      :

1.1 Dry Mixing:

Uniform mixing of raw materials i.e. active and inactive materials is checked by collecting samples from 10 different locations for blend uniformity test. The result of blend uniformity test, process parameters of equipment i.e. mixer speed, chopper speed and end point ampere reading are recorded in following tables.

1.1.1 Acceptance Criteria:     

Mixing of active material shall be uniform.

  Blend Uniformity: 90.0 % to 110.0 %

  % RSD: NMT 6.0 %

1.1.2 Process Parameters Data:

sr no.	Step	Mixer Slow	Mixer Fast	Chopper Slow	Chopper Fast	End Point  Ampere	Observation entered by/date
1	Dry mixing cycle

1.1.3 Blend Uniformity Test Result:

Sr. No.	Locations	Assay in %	Result  entered by/date
1	Left – Top
2	Left – Bottom
3	Right – Top
4	Right – Bottom
5	Middle – Top
6	Middle – Bottom
7	Front – Top
8	Front – Bottom
9	Back – Top
10	Back – Bottom
	Minimum
	Maximum
	Average
	% RSD

1.2 Wet Mixing (Binder Addition):

After addition of binder solution, checked the wet mass, process parameters of equipment i.e. binder solution temperature, mixer speed, chopper speed and end point ampere reading. The observations are recorded in following tables.

1.2.1 Acceptance Criteria:  Wet mass shall be coherent.

 1.2.2 Process Parameters Data:  

              Binder solution temperature:

Sr No.	Steps	Mixer Slow	Mixer Fast	Chopper Slow	Chopper Fast	End Point  Ampere	Observation entered by/date
1	During binder solution addition.
2	After completion of binder solution addition.
3	Additional purified water, if added. Quantity :

1.2.3 Physical Appearance of Wet Mass:

Sr.No.	Test	Observation	Checked by/date
1	Physical appearance

1.3 Wet Mass Milling:

The wet mass after granulation is passed though the cone mill and the same is checked visually for its size and uniformity.

1.3.1 Acceptance Criteria:  Wet granules size shall be uniform.

1.3.2 Physical Appearance of Wet Mass:

               Sieve details:

Sr.No.	Test	Observation	Checked by/date
1	Visually check wet granules for its size.

Repeat the above mentioned process for optimum level (50% of the capacity) and maximum level (80% of the capacity).

7. Deviation Report:

Any deviation reported during process with respect to acceptance criteria shall be justified and it’s it’s impact on equipment qualification shall be evaluated.

8. CHANGE CONTROL:

Change control number shall be mentioned.

9. List of Annexures:

Annexures shall be attached to the PQ Report.

10. Summary and Conclusion of Performance Qualification:

The results and final conclusion shall be mentioned that the equipment performance is found satisfactory at load condition and analytical and physical parameters performed at different capacities are found satisfactory.

11. Certification of Performance Qualification:

Performance Qualification is satisfactory Yes/No

Hence equipment can be used for routine use Yes/No.

Certification shall be taken from Quality Assurance before use.

1.0	Objective :
	To lay down a procedure for Training and Qualification of Quality Control Analyst.
2.0	Scope :
	The scope of this document is to provide the procedure for Training and Qualification of Quality Control Analyst.
3.0	Responsibility :
3.1	Quality Control Personnel :
3.1.1	To undergo Training and Qualification.
3.2	Quality Control Head / Designee :
3.2.1	To review and monitor the procedure for Training and Qualification of Quality Control Personnel.
5.0	Procedure :
5.1	Training shall be conducted by Manager / Designee for relevant core/ as per SOP, “Procedure for Training of Plant Personnel.
5.2	Incase of SOP training the trainee shall be considered as ‘trained’ if analyst gets the qualifying score (> 80%) and should be evaluated through assessment questionnaire as per SOP, “Procedure for Training of Plant Personnel otherwise retraining shall be considered.
5.3	Upon completion of training program, the new joinee shall undergo qualification process for all tests / techniques relevant to that area in which analyst is supposed to work.
5.4	Based on the category to which the analyst belongs as per the discussion with the Head of Department, the tests in which the analyst shall be trained and qualified depending on the job responsibilities shall be identified.
5.5	Non Complex Analytical Techniques are those for which a practical demonstration shall be provided by the trainer as per Annex – 1. As part of demonstration of these techniques, the Manager / Designee shall explain the test procedure to the analyst who is under training.
5.6	Trainee shall enter the key learning points in the Analyst Qualification report.
5.7	The details of the analytical techniques in which the analyst is trained and qualified shall be recorded in the current version of the “Analyst Qualification Record”,
5.8	For complex analytical techniques the analyst shall be trained by Manager / Designee and key points of the analytical techniques shall be recorded by the trainer in “Analyst Qualification Record” during training.
5.9	The analyst shall perform the test as per STP / Specification / GTP and qualification under the supervision of trainer and the qualification shall be verified as per the acceptance criteria.
5.10	The trainer shall use the checklist provided in Annex – 3 to verify that the analyst undergoing qualification performs correct unit operations.
5.11	Manager / Designee shall generate the Analyst Qualification Number (A.Q. No.) for each analyst as per procedure given below and this number shall be referred in analyst qualification raw data.
5.11.1	AQXXYYY, Where AQ stands for Analyst qualification, XX denotes the last two digits of calendar year (20 for 2020) & YYY denotes the serial number.
5.11.2	e.g. The Analyst qualification number for the first Analyst qualified in the year 2020 will be AQ20001
5.12	For each analytical technique, the details such as “Name of Analytical Technique”, “Product” / “Material Name”, “Batch” / “Lot Number”, “A. R. Number” of the previous analysis shall be recorded in the “Analyst Qualification Register”.
5.13	The details of analysis shall be recorded in the “Calculation Sheets” / “Test Data Sheets”. In case the qualification is performed on routine samples, the A.R. Number of the sample being analyzed shall also be recorded in the “Analyst Qualification Register” as a reference.
5.14	The trainer shall review analytical results and consider the analyst as qualified, if the result of the test performed is complying with the acceptance criteria.
5.15	Head of Department or his designee shall review the data of technique for which the analyst is under qualification and provide comments as “Qualified” or “Not Qualified” in the “Analyst Qualification Register”.
5.16	At the beginning of every calendar year Manager / Designee shall prepare a schedule for re-training of relevant analytical techniques for each of the qualified personnel in the section in “Analytical technique Schedule”.
5.17	The trainee shall be considered as trained only after the trainee qualifies as per the questionnaire.
5.18	If the Analyst is having more than 2 years and above experience and have performed the similar analysis in previous organisation then depending upon the evaluation of previous experience and his expertise in the respective analytical technique, complex analytical technique need not be performed. In this case Analyst can directly put on the job by giving respective analysis of ongoing samples in presence of trained analyst and if the result meets the acceptance criteria then the analyst can be considered as Qualified Analyst.
5.19	Requalification of the Analyst shall be carried out if the analyst is absent for more than 60 working days.

6.0 Distribution :

This SOP (Controlled Copy) shall be distributed to Quality Control Department.

7.0 Annexures :

Annex-1 Non Complex Analytical Techniques for Qualification of Analyst

Annex-2 Complex Analytical Techniques for Qualification of Analyst

Annex-3 Checklist for Analyst Qualification.

8.0 Abbreviation :

Nil

9.0 Reference(s) :

Nil

10.0 SOP Revision History Record :

Revision No.

Details for Revision(s) with Change Control No.

Effective Date (Sign. / Date)

                                                               Annex-1

                           Non Complex Analytical Techniques for Qualification of Analyst

Sr. No.	Analytical Technique
1	Description / Characteristics
2	Solubility of Solution
3	Appearance of Solution / Colour and Clarity of Solution
4	pH of Solution
5	Loss on Drying
6	Sulphated Ash
7	Residue on Ignition / Loss on Ignition
8	Heavy Metals
9	Limit tests such as Chloride, Sulphate, Nitrate, Lead, and Arsenic.
10	Bulk Density (Tapped / Untapped)
11	Distillation range
12	Melting Point
13	Sieve Analysis
14	Disintegration test
15	Friability
16	Thin Layer Chromatography
17	Preparation and Standardization of Volumetric solutions.
18	Determination of conductivity
19	Identification (FTIR, UV)

• 

• 

Annexure-3    Checklist for Analyst Qualification
Name of the Analyst	:
Product / Material/ Batch / Lot Number/ A. R.No.	:
Test being performed	:
Name of the Supervisor & Date	:

Sr. No.	Checklist	Observation     (Yes / No / NA)
1	Is the analyst using the correct analytical method for performing the analysis?
2	Is the analyst using calibrated equipment / instrument for performing the analysis?
3	Is the analyst using the correct working standard / reference standard?
4	Is there evidence that the solutions/ reagents used during the analysis were within their validity period?
5	Is it evident that the analyst is taking all the safety precautions?
6	Is the analyst using the analytical balance correctly?
7	Is the analyst using clean weighing accessories, like spatula, Butter paper, etc.?
8	Is the solution prepared by the analyst labeled appropriately?
9	Is the analyst using the correct glassware / reagents / chemicals / as mentioned in the analytical method?
10	Is the analyst making concurrent documentation of the activity being performed?
11	Are samples/ solutions stored appropriately during the analysis?

Specific Observations for the Analytical Technique

Supervisor (Sign) & date:

ALCOA and CCEA (complete, consistent, Enduring and Available)

• 

• 

• 

• 

• 

• 

• 

CCEA (++++ Complete, Consistent, Enduring and Available)

What is Fluid Bed Dryer :

FBD is used for drying of different pharmaceutical materials or products and it can easily achieve specific moisture content in granules and powders.

FBD is able to remove excess moisture from different materials and its working principle is so precise and focused on drying the materials without changing their physical attributes.

FBD is used in different industries like Pharmaceutical, Chemical, Food Processing, Fertilizer and dairy industry.

What is the Purpose of Drying of Material in Pharmaceutical using FBD :

Here are the main functions as to why you should perform solid drying.

• It increases the shelf life of the products

• It helps in the improvement of different product properties such as compressibility and flow ability.

• It will also make the materials more suitable for handling and it helps in proper preservation of the materials.

What is Fluidization Principle :

In fluidization process, hot air is introduced at high pressure through a perforated bed of moist solid particulate. The wet solids are lifted from the bottom and suspended in a stream of air (fluidized state). As the hot air passes between the particles it takes the excess moisture from the particles thus drying the particles.

Heat transfer is accomplished by direct contact between the wet solid and hot gases.

Steps of Fluidization :

Step 1: Fluidized bed dryer loading :

Loading of materials involves adding a fresh batch of wet granules into the product chamber through negative pressure feeding, materials can be sucked from the high shear  mixer chamber through a feeding tube.

Step 2: Air inlet (intake) :

Switching the blower unit on is done from the control panel. Once the blower is operational, the air is drawn continuously from the Air Handling unit and into the tower through the lower plenum.

Step 3: Fluidization :

Inlet air is blown up through the static power bed as the velocity of the air increases so does the space between powder particles until the particles become suspended in a bed the fluidization process is through to occur in five stages including smooth  fluidization, bubbling  fluidization, turbulent fluidization and first  fluidization.  

Step 4: Drying:

The drying process takes place in three stages until the end point is reached (At the end point the solid particles moisture level is equal or less than 1%)

Step 5: Pre heating:

Wet particles are suspended in hot and dry air stream. Moisture on the particles surface evaporates as heat flows through the body  (conventional heating) the rate of drying slowly increases as the particles absorb more heat.

The moisture lost during preheating is still small but the temperature of the bed rises steadily.

Step 6: Filter bag shaking:

The blower continuously draws and excels air from Fluidized bed dryer. The airstream may contain very small particles called fines. The filter bags capture the fines in their pores but this cause the formation of a dust layer that clogs the filter bags causing a pressure drop.

Mechanical shaking is the best way to remove the dust layer and it is done by the pneumatic cylinder at the set intervals and seems we have two filtering chamber the shaking is alternated between the two.

Refer Fluid Bed Dryer Filter Bag

https://pharmaceuticalupdates.com/2020/10/05/procedure-for-indent-receipt-usage-and-specifications-of-fluid-bed-drier-filter-bag/

 Step 7: Discharging of dried material:

Discharging refers to the removal of dried materials from fluidized bed dryer. It can be done manually by unlocking and wheeling the product container on its trolley to the next process equipment.

Alternatively, vacuum conveying can be carried out by connecting the product container with a tube and creating negative pressure for suction using a vacuum transfer system. After drying, the next process is milling.

What are the main disadvantages of using the fluid bed dryer :

Not Ideal for Organic Solvents :

You cannot use the fluid bed dryer for reducing excess moisture in organic solvents or substances containing organic solvents.

This is because the organic solvents usually dissolve in the products thus making it very difficult to dry.

Risk of Fire Explosion:

Fluid bed dryers use high levels of hot gas and air thus making it difficult to dry toxic or flammable materials.

This may place the lives of the people operating the machine or around the machine in great danger.

Electrostatic Build-up :

When we use the fluid bed dryer there are high chances of electrostatic build up during the drying process.

It is a phenomenon that will happen especially when we are drying organic particles.

We should, therefore, go for the fluid bed dryers with electrical earthing elements to avoid this problem.

Difficulty in Drying Sticky Particles :

The main principle of drying using the fluid bed dryer is the movement of particles as it takes away excess moisture.

We will, therefore, experience a lot of problems when it comes to drying sticky materials as they don’t move freely.

Material of Construction of FBD:

For the contact parts of FBD we should use  AISI 316 and non-contact parts AISI 304.

Fluid Bed Dryer Quality Standards and Certifications:

The main quality standard and certification are

• Current Good Manufacturing Practices (cGMP)

• International Standards Organization (ISO) Quality Certification

• Food and Drug Administration Quality Certifications

• CE quality certification for the electrical appliances

Below given are the details of causes and solutions of defects in tablet Manufacturing.

The defects are capping, Lamination, Picking, Sticking, Cracking and Chipping.

1. OBJECTIVE

1.1 To lay down a procedure for operation of Friabilator, Make: Electro lab

2.0       RESPONSIBILITY

2.1 Technical Assistant / Production Executive / IPQA Executive – To Perform as per SOP.

2.2 Production / IPQA In-charge – To ensure the compliance.

3.0 PROCEDURE

3.1   OPERATION :

3.1.1     Switch ON the mains.

3.1.2    Press the START/STOP switch on the rear right hand side of the instrument base, then the drum will initialize itself to the loading position and simultaneously display shows START.

3.1.3 Mode setting – TIME, COUNT key are toggle keys to set in Timer mode or Count mode of operation.   3.1.4   Set the Time in the following procedure:

 3.1.4.1  Press “RESET” key.

 3.1.4.2  Press “TIME” key.

 3.1.4.3  Enter the required duration of time by pressing the numeric digits.

 3.1.4.4  Press “ENTER” key to set the time.

3.1.5     Set the Count in the following procedure:

  3.1.5.1  Press “RESET” key.

  3.1.5.2  Press “COUNT” key.

  3.1.5.3  Enter the desired number of rotations by pressing the numeric digits.

 3.1.5.4  Press “ENTER” key to set the count.

 3.1.5.5  After completing the parameter settings, slide the tablets gently into the drum from the side slit provided on the drum. 

3.1.5.6  Select the Time mode or Revolution count mode as desired by pressing the “TIME / COUNT” key respectively.

PRECAUTIONS:

1. Make sure the knob is properly fitted on the shaft to assure the drum is held in position.
2. Do not hold the drums while they are rotating.

3.1.6 Weigh the quantity of tablets to be tested as per the BPRR specification from LHS and RHS of compression machine.

3.1.7 Record the weights of tablets in BPRR if provided and load the tablets to  friabilator drum.

3.1.8 Press “RUN / HALT” key to start the test.  “RUN / HALT” is a toggle key to start and stop the test.

3.1.9 Drums rotate in forward direction as per the set (TIME/COUNT) mode.

3.1.10 Completion of test is indicated by an audible beep and the display shows “END”.

3.1.11 When the test is over, the drums rotate in the reverse direction for discharging the tablets into the trays.  After discharge of tablets drums initialize to loading position and the display shows “START” indicating the instrument is ready for next test.

3.1.12 Slide out the tray and take out the samples for weighing.

3.1.13 Dedust the tablets using nylon brush, weigh and record  in BPRR.

3.1.14 Calculate and record the friability as per BPRR.

Note:

1. If tablet size or shape causes irregular tumbling, adjust the drum base so that the base forms an angle of about 10⁰ with the table surface and the tablets no longer bind together when lying next to each other, which prevents them from falling freely.
2. Adjustment of the drum base can be done by opening the two flaps, which are situated at the front bottom side of the instrument.

3.2    CLEANING :

3.2.1     Clean the Friabilator frequently by following procedure.

3.2.2     Switch off the power supply to the instrument before cleaning the equipment.

3.2.3     Remove the trays in the tray holders.

3.2.4     Remove the drums from the shaft by pressing the button on the knob and pull   out  the knob.

3.2.5 Clean the drums, trays and knob with lint free cloth dipped purified water and wipe with dry lint free cloth.

3.2.6 Wipe off the exterior of the equipment with lint free wet cloth.

3.2.7 Reassemble the drums and tray in the reverse order of dismantling.

3.2.8 Update the status label as CLEANED.

3.2.9 Switch off the mains of the tablet friability apparatus after the days operation.

Frequency   :   After every batch irrespective of product, or Weekly (if machine is in

operation), or Monthly (if machine is idle) which ever is the earlier and as and when   required.

4.0       ABBREVIATIONS

Nil

5.0       REFERENCES

Nil

6.0       ANNEXURES

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