Procedure for Cleaning of Production areas after Batch to Batch change over

1.0 OBJECTIVE
To lay down a procedure to keep all production areas free from traces of previous Batch of same Product and Strength.
2.0 SCOPE
This SOP is applicable to Pharmaceutical Production area
2.1 AREAS
Dispensing 1,2 , Module -1,2,3 and Packing Machine rooms.
3.0 RESPONSIBILITY
Concerned Operator
4.0 ACCOUNTABILITY
Production Officer.
5.0 PROCEDURE
5.1.0 Precautions
5.2.0 Equipments and Tools
5.3.0 Cleaning agents.
5.4.0 Disinfectants
5.5.0 Operation
5.1.0 Precautions
5.1.1 While cleaning the walls and floor do not use strong smelling disinfectants.
5.2.0 Equipments and Tools:
5.2.1 Vacuum cleaner
5.2.2 Scrubbing machine
5.2.3 Ordinary mop.
5.2.4 Lint free duster.
5.2.5 Glass cleaning cloth
5.2.6 Sponge rectangular.
5.2.7 Aluminium ladder of suitable size
5.3.0 Cleaning agents:
5.3.1 Alklean as is
5.3.2 Window shine glass cleaner as is.
5.3.3 No rinse hard surface cleaner as is
5.4.0 Disinfectants:
5.4.1 Jeplon - 1 part to 100 parts of water
5.4.2 Dettol H - 1 part to 100 parts of water
5.4.3 Fairgenol - 1 part to 10 parts of water.
5.5 Operation
5.5.1 Aluminium door and wall fittings
5.5.2 Dust and wipe the glove boxes, hanger rod, slipper stand and Return Air Ducts in gowning area
5.5.3 Dust and wipe aluminium doors and glasses in all areas.
5.5.4 Vaccum clean all the Return Air Ducts in above areas.
5.5.5 Floor
5.5.6 Vaccum clean the floor along with Return Air Ducts in all Production areas when ever there is batch to batch change over.
5.5.7 Clean the entire floor with the cleaning agent given, followed by mopping with the diluted disinfectant solution accordingly with the help of Scrubbing Machine.
5.5.8 Waste - Bin
5.5.9 Empty the waste bin into polythine bag, tie the bag with a nylon string and keep it ready for collection at collection point.
5.5.10 Clean and replace the lining (twice in a day).
5.5.11 The extra cleaning tasks are carried out whenever there is batch to batch change over .

Maintenance of dies and punches.

1.0 OBJECTIVE
To lay down a procedure for maintenance of dies and punches.
2.0 SCOPE
Module –2,3,4
3.0 RESPONSIBILITY
Concerned operator.
4.0 ACCOUNTABILITY
Production officer.
5.0 PROCEDURE
5.1 Get required number of punches and dies from Quarantine and make necessary entries in punches and dies stock card and get it checked by production officer.
5.2 Transfer the required punches and dies to the compression area.
5.3 Remove punches from plastic cover and wipe out the oil adhering to the punches and dies.
5.4 Set up and fix punches and dies as per the SOP of compression machine change over operation.
5.5 If any abnormal sound is observed during compression, immediately stop the compression machine to avoid punches and dies damage and inform production officer.
5.6 Examine critically the punches and dies, remove the damaged punches and dies if any from the machine and replace them.
5.7 Remove the punches and dies after the compression.
5.8 Clean thoroughly the punches and dies with lint free duster.
5.9 Smear the punches with oil and put inside the plastic covers.
5.10 Count and keep separately the upper and lower punches and dies in separate boxes.
5.11 Make necessary entries in stock card and transfer to the punches and dies storage area.
5.12 Get the signature in the stock card by production officer.

Procedure for cleaning of HDPE pallets.

1.0 OBJECTIVE
To lay down a procedure for cleaning of HDPE pallets.
2.0 SCOPE
Module -1,2,3,4,5 and raw material stores.
3.0 RESPONSIBILITY
Production officer / Stores assistant.
4.0 ACCOUNTABILITY
Production executive.
5.0 PROCEDURE
5.1 Frequency:- Once in a month (or) when ever necessary.
5.2 Bring the pallet to the washing area.
5.3 Clean the pallets by wiping with lint free duster from all sides.
5.4 Clean with 0.1% teepol solution by using nylon brush.
5.5 Wipe the pallet with wet lint free duster after washing with potable water jet.
5.6 Wipe the cleaned pallet with dry lint free duster.

Cleaning procedure for Inprocess container

1.0 OBJECTIVE
To lay down a procedure for cleaning of in-process containers.
2.0 SCOPE
Module - 1,2,3,4 and 5.
3.0 RESPONSIBILITY
Production officer.
4.0 ACCOUNTABILITY
Production executive
5.0 PROCEDURE
5.1 After usage of the Inprocess container replace the label with “ TO BE CLEANED” label.
5.2 Transfer the container to washing room.
5.3 Remove the “TO BE CLEANED ” label and preserve it with next batch / product document.
5.4 Clean the container by wiping with lint free duster, from outside.
5.5 Clean the container with potable water jet using lint free duster .
5.6 Rinse with purified water jet.
5.7 Dry the container with lint free duster.
5.8 Ensure putting back the same lid to the container.
5.9 Label it as “ CLEANED” with checked by sign and date.
In case of product change over:
-Clean the containers with potable water jet/ hot water using lint free
duster.
-Finally rinse the container with purified water Jet.
-Follow the points from 5.70 to 5.90.

Correction of wrong entry in BMR / BPR

1.0 OBJECTIVE
Procedure for correction of wrong entries in BMR / BPR.
2.0 SCOPE
Module - 1,2,3,4,5, Stores and all Packing areas.
3.0 RESPONSIBILITY
Production officer.
4.0 ACCOUNTABILITY
Production executive.
5.0 PROCEDURE
5.1 Avoid wrong entries in BMR/BPR.
5.2 Make corrections if necessary by putting a straight line across the wrong entry. So that it is clearly visible .
5.3 Write the correct figure/text near the wrong entry.
5.4 Put your signature or initial along with date near the correction.

Procedure for Leak testing of strips / blisters

1.0 OBJECTIVE
To lay down a procedure for leak testing of strips / blisters.
2.0 SCOPE
All packing areas.
3.0 RESPONSIBILITY
Production officer.
4.0 ACCOUNTABILITY
Production executive
5.0 PROCEDURE
5.1 Take the required number of strips / blisters as mentioned in the Annexure – I. Check the quality of strips/ blisters for any damages.
5.2 Tie the collected strips / blisters with a rubber band.
5.3 Ensure that all strips / blisters are dipped in water and close the lid.
5.4 Connect opening of the desiccator to the vacuum pump.
5.5 Apply a vacuum of 300 mm of Hg and close the knob of the desiccator.
5.6 Keep the vacuum for 30sec.
5.7 Release the vacuum by opening the knob of the desiccator slowly and open the lid remove the strips / blisters.
5.8 Wipe out the traces of water from the strips / blisters by using lint free duster .
5.9 Open the pocket of strips by using scissors to remove the tablets / capsules.
5.10 Open the blisters manually.
5.11 Check for any traces of water inside the strips / blisters.
5.12 Number of tablets or capsules, which have become wet, should not be more than 1%. If the leakage is more than the above percentage repeat the leak test.
5.13 Record it in the respective batch packing record, with signature and date.
ANNEXURE -I


Note:
1. Perform leak test at the starting of blistering / strip sealing, operation.
2. If there is machine break down more than 1/2 hour perform leak test immediately after starting the operation.
3. Whenever leakage observed during leak test, ensure that rectification is done.
4. If leak test failure is occurring repeatedly, bring to the notice of Executive / Sr. Executive for corrective action.

Recording and monitoring of differential air pressure

1.0 OBJECTIVE
To lay down a procedure for recording and monitoring of differential air pressure.
2.0 SCOPE
All Modules, Dispensing cubicles, & Primary packing areas.
3.0 RESPONSIBILITY
Concerned officer.
4.0 ACCOUNTABILITY
Concerned executive
5.0 PROCEDURE
5.1 Record the differential pressure between outer corridor and gowning rooms twice daily (Locations of manometers given in Annexure-I ).
5.1.1 Pressure differential limit is 1.0 -1.6mm of water guage.
5.2 Record the differential pressure between Inner corridor and process rooms twice daily (Locations of manometers given in Annexure-I ).
5.2.1 Pressure differential limit is 0.6 -1.0 mm of water guage.
5.3 If any discrepency is observed report to maintenance for corrective action.
5.4 Stop the process till the corrective action is taken.
5.5 If the material is stored in open containers, seal the containers with film / lids.
5.6 Once the corrective action is taken, record pressure differential and start the process.
ANNEXURE - I
LOCATIONS OF MANOMETERS
A. Manometers between outer corridor & adjcent areas

B. Manometers between Inner Corridor / Air lock and Process rooms.

Procedure for defoiling of blisters / strips

1.0 OBJECTIVE
To lay down a procedure for defoiling of blisters / strips.
2.0 SCOPE
All primary packing halls.
3.0 RESPONSIBILITY
Concerned operator.
4.0 ACCOUNTABILITY
Production officer.
5.0 PROCEDURE
5.1 Use clean gloves during defoiling of strips / blisters.
5.2 Cut, rejected strips by using scissors without damaging tablets / capsules over polythene bag lined SS Trays .
5.3 Remove tablets / capsules by hand from cut strips/blisters.
5.4 Sort out good tablets by removing foil pieces and broken tablets / damaged capsules.
5.5 Collect tablets with black particles, oil stains and put them in a bag labelled as “TO BE DESTROYED “.
5.6 Put all Recoverable tablets / capsules in a new polythene bag, properly labelled and tied with nylon thread, and keep in a HDPE container. Put the RR’s label on the container.
5.7 Get the quantity of sorted tablets checked by two production officers or by Quality Assurance officer .
5.8 Pack separately such defoiled, sorted tablets at the end of the batch and indicate in B.P.R shipper weighing log along with the shipper number as “PACKED WITH DEFOILED, SORTED TABLETS”.
5.9 In case it is not packed in the same order. Keep them in double polythene bag and tie with nylon thread, in a HDPE container with proper label containing all details.
5.10 Put all scrap in a poly bag label it and send it for disposal.
5.11 Procedure for defoiling by using deblistering machine.
5.10.1. Set the de-blistering machine for a particular product .
5.10.2.Clean the machine and check for traces of previous product get it counter checked by concerned Junior technical officer visually.
5.10.3. Switch “ON” the machine.
5.10.4 De-blister the rejected blisters.
5.10.5 Follow the procedure given in 5.4 - 5.10 points.
5.10.6 Record the details in respective B.P.R.

Procedure for handling of finished goods

1.0 OBJECTIVE
To lay down a procedure for handling of finished goods.
2.0 SCOPE
All packing halls.
3.0 RESPONSIBILITY
Production officer.
4.0 ACCOUNTABILITY
Production executive
5.0 PROCEDURE
5.1 Raise production transfer slip and get it cleared timings.
5.2 Send approved shippers on a pallet to bond room on hydraulic trolley.
5.3 Check the number of shippers physically to be transferred to bonded storage area and tally the same with details in the batch packing record, duly checked and dated.

Returning of unused Raw and Packing materials

1.0 OBJECTIVE
To lay down a procedure for returning of unused raw and packing materials.
2.0 SCOPE
Module 1,2,3,4,5 and packing areas.
3.0 RESPONSIBILITY
Production officer / Executive.
4.0 ACCOUNTABILITY
Production manager.
5.0 PROCEDURE
5.1 Returning of unused Raw materials.
5.1.1 Return unused materials along with stock return note as per format No: xxxxx
5.1.2 Ensure all unused raw materials are tied in separate poly bags with stock return labels and keep them in in-process container and send them to dispensing area along with stock return note or through system generated stock return note.
5 .2 Returning of unused packing materials.
5.2.1 Return unused packing material along with SRN as per (Annexure-I).
5.2.2 Ensure that all the packing materials are properly labelled.
5.2.3 Place them in a trolley / crates and send to stores with an authorized stock return note duly approved by production Officer.
Annexure-I
STOCK RETURN NOTE
No:
Module:
Product:
B.No:
Date:


Returned by with date:
Received by with date:
Verified by with by:

Date: Date: Date:

Destruction of old, torn rejected FBD and FEM bags

1.0 OBJECTIVE
To lay down a procedure for destruction of rejected FBD & FEM bags.
2.0 SCOPE
Module - 1,2,3 & 4.
3.0 RESPONSIBILITY
Concerned Junior Technical officer / Operator.
4.0 ACCOUNTABILITY
Production officer.
5.0 PROCEDURE
5.1 Wash the torn , old FBD / FEM bags with potable water jet.
5.2 Dry the washed FBD/FEM bags in FBD using steam.
5.3 Cut the torn, old FBD/FEM bags into pieces and send to house keeping department with label for disposal, with a disposal note duly authorized by Sr. Executive.
5.4 Record the same destruction details in the FBD / FEM bag control card.

Transferring of Materials from Dispensing to Module, Module to Hold area and Hold area to Primary Packing

1.0 OBJECTIVE
To lay down a procedure for transfer of materials from dispensing to module, from module to hold area and to primary packing.
2.0 SCOPE
Module - 1,2,3,4 and 5.

3.0 RESPONSIBILITY
Concerned production associate / operator.
4.0 ACCOUNTABILITY
Production officer
5.0 PROCEDURE
5.1 Transfer of raw materials to module
5.1.1 Ensure that all the dispensed materials are kept in labelled in-process containers (IPC).
5.1.2 Clean the IPC wheels with lint free duster before transferring.
5.1.3 Transfer the IPC to module raw material hold room with batch document.
5.2 Transfer of material from module to hold area (Quarantine).
5.2.1 Ensure that all HDPE drums are properly labelled and are clean from outside.
5.2.2 Transfer all HDPE drums containing materials in an SS trolley from module air lock to quarantine with batch document.
5.2.3 Keep drums separately lot wise and keep batch document on the top of drums.
5.2.4 Keep recoverable residues drums separately.
5.2.5 Make necessary entries in hold area stock card and get it checked by production officer.
5.3 Transfer of recoverable residues to module for recovery.
5.3.1 Check the weight of recoverable residues both from manufacturing and packing areas.
5.3.2 Whenever required transfer recoverable residues drums to module for recovery.
5.3.3 Make necessary entries in hold area card and get it signed by production officer.
5.4 Transfer of material from quarantine to primary packing.
5.4.1 Transfer the material as per work order on SS trolley to the respective packing area.
5.4.2 Make necessary entries in the hold area stock card and get it signed by production officer.
5.4.3 Weigh the packing recoverable residues and enter in the hold area stock card and keep separately with proper labelling.

Cleaning procedure for New Equipment

1.0 OBJECTIVE
To lay down a procedure for cleaning of new equipment.
2.0 SCOPE
Module 1,2,3,4 & 5 and Packing areas.
3.0 RESPONSIBILITY
Production officer / Executive.
4.0 ACCOUNTABILITY
Sr. Executive - Production.
5.0 PROCEDURE
5.1 De-dust the equipment with vacuum cleaner / lint free duster
5.2 Clean the equipment with potable water jet (where ever applicable) using scrubber.
5.3 Clean the equipment with 0.5% teepol solution using scrubber.
5.4 Rinse the equipment with potable water jet (where ever applicable).
5.6 Use IPA / Acetone to clean the parts where ever applicable.
5.7 Finally rinse the equipment with purified water jet (where ever applicable).
5.8 Verify that cleaning is appropriate and satisfactory by visual inspection.
5.9 Get ‘CLEANED’ label signed by the production officer and fix it to the machine.
5.10 Use the equipment only after completion of IQ, OQ and PQ by validation department

Transferring of machine under major break downs

1.0 OBJECTIVE
To lay down a procedure for transferring of machine under major break down.
2.0 SCOPE
Module -1,2,3,4 and 5.
3.0 RESPONSIBILITY
Production officer.
4.0 ACCOUNTABILITY
Executive / Sr. Executive.
5.0 PROCEDURE
5.1 Raise major breakdown request to maintenance through engineering helpdesk.
5.2 Transfer the machine to the respective module air lock.
5.3 Maintenance department transfers the machine from air lock to the repair bay.
5.4 Concerned production officer shall examine the machine after necessary repairs.
5.5 After getting clearance from concerned production officer, transfer the machine to the respective area.

Place the caution while in operation as follows
CAUTION:ENSURE NOT TO DAMAGE EPOXY FLOORING.

Procedure for Inventory of Sieves

1.0 OBJECTIVE
To lay down a procedure for maintaining inventory of sieves.
2.0 SCOPE
Module - 1,2,3,4 and 5.
3.0 RESPONSIBILITY
Production officer.
4.0 ACCOUNTABILITY
Production executive
5.0 PROCEDURE
5.1 Check the sieves against indent for required numbers and sizes and enter the details in the sieve inventory record.
5.2 Sieves inventory to be maintained as per the details mentioned in the Annexure -I .
5.3 If any sieve observed damaged discard immediately and replace with new approved sieve and enter the details in the sieve inventory record.
5.4 Module wise sieve inventory record to be maintained by production department as per Annexure – I every month.
5.5 Sieve size should be measured by counting the no of apertures per linear inch.
5.6 All the sieves should be of ASTM/ BSS standards.

ANNEXURE - I
Module :

Month:

Date:

Maintenance of Dies and Punches stock card.

1.0 OBJECTIVE
To lay down a procedure for maintenance of dies and punches.
2.0 SCOPE
Module- 2,3 & 4
3.0 RESPONSIBILITY
Production officer
4.0 ACCOUNTABILITY
Production Executive
5.0 PROCEDURE
5.1 Check all the punches and dies immediately after receiving from stores, count them and record in punches and dies stock card (Annexure - I) in format No.: xxxx
5.2 Inform immediately if any damaged punches and dies are found and record the number of damaged punches and dies, in stock cards.
5.3 Send to Engineering department for defacing along with stock return note.
5.4 Keep all good upper punches, lower punches and dies and labelled the box with details of product, size, shape and number. Keep them in quarantine.
5.5 When punches and dies are required, take required number of punches and dies to the production area and make entry in stock card.
5.6 Get stock card checked & signed by production officer.
5.7 If any damage of punches and dies occurred during compression, inform immediately to production officer and make necessary entry in the stock card and sign and place the damaged punches and dies in separate box.
5.8 Investigate the cause of damages to the punches and make necessary action plan to avoid in future.
5.9 After removing punches and dies from the machine clean them with lint free duster and smear the punches with oil and put into the plastic covers. Keep them in respective boxes.
5.10 Transfer punches to the storage area.
5.11 Make necessary entries in stock card and get it signed by production officer.
ANNEXURE - I
PUNCHES AND DIES STOCK CARD
PRODUCT: ………..

SIZE : ………..
SUPPLIER: ………..

DATE OF RECEIPT : ………..

IN REMARKS PLEASE GIVE THE DETAILS OF BATCH NO. AND ACTION TAKEN IF PUNCH/ DIE IS REJECTED DURING COMPRESSION


UP: - UPPER PUNCH

LP :- LOWER PUNCH

D :- DIES

Returning of on-line rejected packing material

1.0 OBJECTIVE
To lay down a procedure for returning of on-line rejected packing materials.
2.0 SCOPE
All packing areas.
3.0 RESPONSIBILITY
Production officer and Quality assurance chemist.
4.0 ACCOUNTABILITY
Production executive and Quality Assurance executive.
5.0 PROCEDURE
5.1 Any packing materials are observed to be defective on - line, such as having shade variation, printing, lamination problems with foils and locking, printing problems with cartons.
5.2 Paste the on-line rejection label and keep the material aside.
5.3 Weigh the quantity / count the number to be rejected on-line.
5.4 Inform to quality assurance and get the approval for the same.
5.5 Raise the on-line rejection format as per Annexure-I in triplicate and enclose the rejected material samples and get it checked by production executive and QA executive.
5.6 Return the material to the stores by SRN as per Annexure -II.
5.7 Once again ensure the A.R.No of on-line rejected material, before returning to the stores.
5.8 If the over printed shippers and cartons are to be rejected on –line, follow the procedure from 5.2 to 5.7.

Annexure-I

ON-LINE REJECTION FORMAT

Date:____________
Location:__________
Name of the Material:_______________________
B.No:_________________________
A.R.No.___________
Quantity:_____________
Mfg.B.No:____________________
Suppliers:__________
Batch Qty:___________
DCNo.:_______
GRN No.:____

Observations:

Production:

Executive :

Quality Assurance:
Group Leader:

Remarks:
By Quality control executive Production

By Stores-QC

Annexure - II

STOCK RETURN NOTE

No:

Module:

Product:

B.No:
Date:

Returned by with Date:
Received by with Date:
Verified by with Date:
Authorized by with Date:

Packing line start up and closing procedure

1.0 OBJECTIVE
To lay down a procedure for startup and closing of packing line.
2.0 SCOPE
All packing areas.
3.0 RESPONSIBILITY
Production officer.
4.0 ACCOUNTABILITY
Production executive
5.0 PROCEDURE
START UP
5.1 Ensure the cleanliness of the area before starting of the operation.
5.2 Ensure that all packing materials are belonging to the respective product and batch number.
5.3 Ensure that line clearance is given by two production officers or by Q.A.
5.4 Put the equipment status label on the machine.
5.5 Switch “ON” the machine. Note down the sealing temperature and environmental conditions in batch packing record with sign and date also check the foil proof for batch details against PWO by two production officers or by QA.
5.6 Check the leak test for strips / blisters / quality of packs and give the clearance to start the belt.
CLOSING:
5.7 Clear off the packing material from the belt during lunch break and at the end of the shift.
5.8 Switch “OFF” machine and packing belt.
5.9 Clean the equipment and areas.
5.10 Put the ‘CLEANED’ label.

Handling of New Machines

1.0 OBJECTIVE
To lay down a procedure for handling of new machines.
2.0 SCOPE
Module-1,2,3,4,5, packing areas and stores.
3.0 RESPONSIBILITY
Maintenance executive / Production executive.
4.0 ACCOUNTABILITY
Maintenance manager / Manager - Production.
5.0 PROCEDURE
5.1 Maintenance executive along with the packing list shall examine the machine.
5.2 If the packing list is reconciling with the machine / parts, transfer the machine to finished goods store.
5.3 If the packing list is not reconciling with the machine / parts, maintenance executive shall generate a report and send to the supplier.
5.4 If the machine is small use battery operated pallet truck to transfer the machine into the respective area.
5.5 If the machine is big use sufficient manpower to transfer the machine into the respective area, manually.
5.6 While transferring manually use PVC sheet / Rubber mat on the floor.
CAUTION: NEVER KEEP THE MACHINE DIRECTLY ON THE FLOOR.
5.7 Dedust the machine with lint free duster before transferring to shop floor.
5.8 After transferring into respective area use PVC sheet to keep the machine on the floor.
5.9 After proper placing of the machine on the floor, check the level of the machine.
5.10 If machine is properly placed inform maintenance for necessary utility connections.

Procedure for Indenting of Stereos

1.0 OBJECTIVE
To lay down a procedure for indenting the rubber stereos to be used for over printing purpose.
2.0 SCOPE
Formulation Unit xx
3.0 RESPONSIBILITY
Packing Officers.
4.0 ACCOUNTABILITY
Production Executives.
5.0 PROCEDURE
5.1 After receiving the production month plan from PPIC, the number of batches to be manufactured in the month will be identified by concern production executive, along with Manufacturing and Expiry details.
5.2 The above will be informed to concern production officer.
5.3 Production officer will indent the stereos accordingly for
5.3.1 Foil over printing stereos for blister / strip machine.
5.3.2 Carton over printing stereos.
5.3.3 Shipper coding stereo required if any.
5.4 The indent will be checked by Production Executive.
The indent will give through Fax or E.Mail to stereo Manufacturer

Returning of on-line rejected raw Material

1.0 OBJECTIVE
To lay down a procedure for returning of on-line rejected raw material.
2.0 SCOPE
Module 1,2,3,4 and 5.
3.0 RESPONSIBILITY
Production officer / QA officer.
4.0 ACCOUNTABILITY
Production Executive, Group leader / Quality Assurance.
5.0 PROCEDURE
5.1 If the raw materials are observed to be defective on - line, such as having lumps or foreign materials, paste the on-line rejection label and keep the materials aside.
5.2 Weigh the quantity / count the number to be rejected and check the AR Number of the materials.
5.3 Enter the details in online rejection format as per Annexure –I.
5.4 Inform to Quality assurance officer / executive and get the approval for the same.
5.5 Enter the details of materials rejected on-line in stock return note as per Annexure –II and take authorized sign by production officer / executive and Quality assurance officer / Executive.
5.6 Return the materials to stores.
Annexure-I
ON-LINE REJECTION FORMAT
Date :____________
Location :__________
Name of the Material:_______________________
B.No:_________________________
A.R.No.___________
Quantity:_____________
Mfg.B.No:____________________
Suppliers:__________
Batch Qty:___________
DCNo.:_______
GRN No.:_______
Observations:
Production:

Signed by Executive:

Quality Assurance:

Signed by Group Leader:

Remarks:
Quality control executive

Production/Stores @ QC

Annexure - II

Procedure for Disposal of Materials

1.0 OBJECTIVE
To lay down a procedure for disposal of material.
2.0 SCOPE
Module - 1,2,3,4,5 and packing areas.
3.0 RESPONSIBILITY
Production officer / House keeping officer.
4.0 ACCOUNTABILITY
Production executive
5.0 PROCEDURE
5.1 Used stereos:
5.1.1 Cut the stereos into pieces after each campaign and hand over to House keeping department for disposal with proper label.
5.2 Left-over overprinted cartons / labels after batch completion:
5.2.1 Send all used / Unused discarded cartons / Labels having Company's logo for shredding to house keeping department for disposal.
5.3 Empty strips / blisters and defoiled strips / blisters:
5.3.1 Collect all empty strips / defoiled strips / blisters at the end of the shift / end of the batch, weigh and record the weight in the batch packing record.
5.3.2 Send the same to the house keeping department for shredding and disposal with proper labelling.
5.4 Used polythene bags:
5.4.1 Keep all used poly bags in a one poly bag and send to house keeping department for disposal with label as “Used polybags to be destroyed”.

Exit Procedure - Annexure Y

1.0 OBJECTIVE
To lay down a procedure for exit from,
1) Secondary packing halls.
2) Secondary packing material store.
3) Finished goods stores.
2.0 SCOPE
Applicable to all the personnel who are leaving the areas mentioned in objective.
3.0 RESPONSIBILITY
Concerned person.
4.0 ACCOUNTABILITY
Workmen(T)/Production Associates/Technical Associates/ Jr. Technical Officers-Production officer
Officers-Executive
Executive and above-Plant Manager
5.0 PROCEDURE
5.1.0 Precautions
5.2.0 Exit procedure.
5.1.0 Precautions
5.1.1 Keep the slippers in the rack in orderly manner.
5.1.2 Every alternative day / Product change over / Whenever necessary put the dress in the bin marked as uniform for cleaning.
5.1.3 Do not dump the removed uniform in the locker, which is to be used next day.
5.1.4 Fold the dress gently and keep it in the locker.
5.1.5 Do not cross the bench with the primary dress.
5.1.6 Entry of gents into ladies change rooms or vice-versa is strictly prohibited.
5.2.0 Exit procedure
5.2.1 Enter primary change room through external corridors.
5.2.2 Remove your slippers and keep them in slipper rack in an orderly manner.
5.2.3 Remove the headgear, shirt and trouser.
5.2.4 Place them in the locker and lock it.
5.2.5 Cross the step over bench by sitting on it (Do not jump over the bench)
5.2.6 Put on the street clothes.
5.2.7 Put on the footwear.
5.2.8 Collect ornaments or any other personal belongings from your locker identified by your code number and lock it.
5.2.9 Leave the change room.

Entry Procedure - Annexure Y

1.0 OBJECTIVE
To lay down a procedure for primary changing before personnel entering into,
1) Secondary packing halls.
2) Secondary packing material ware house
3) Finished goods ware house.
2.0 SCOPE
Applicable to all the personnel who are entering into the areas mentioned in objective.
3.0 RESPONSIBILITY
Concerned person.
4.0 ACCOUNTABILITY
Workmen(T) /Production Associates/Technical Associates/ Jr. Technical Officers-Production officer.
Officers-Executive.
Executive and above-Plant Manager.
5.0 PROCEDURE
5.1.0 Precautions.
5.2.0 Entry procedure.
5.1.0 Precautions
5.1.1 There is a separate entry available for Ladies and Gents.
5.1.2 Entry of Gents into Ladies change rooms or vice-versa is strictly prohibited.
5.1.3 Ensure the air curtains and insecticutors are working (in all working shifts).
5.1.4 If not working inform maintenance for rectification.
5.1.5 Any authorized person wishes to enter into pharma Secondary packing areas, canteen, Packing material stores, Finished goods stores.
5.1.6 Jewellery, watches and cosmetics should be removed in the primary change room only.
5.2.0 Entry Procedure
5.2.1 For Gents follow annexure-I : Pictorial display of dressing procedure in sequence for gents entry procedure and For Ladies annexure-II: Pictorial display of dressing procedure in sequence for ladies entry procedure.
5.2.2 Change dress every alternative day / during product change over /whenever necessary.
5.2.3 Visit toilet if necessary.
5.2.4 Wash your hands with soap thoroughly.
5.2.5 Remove the street footwear, place them in bottom rack of the locker.
5.2.6 Remove the street clothes, fold and hang them properly in the upper rack of the locker.
5.2.7 Remove your personal belongings like purses, coins, bangles, rings, chains, wrist watches and place them in the upper rack of the locker.
5.2.8 Lock the locker.
5.2.9 Cross the step over bench by sitting on it. (Do not jump over the bench).
5.2.10 Collect the dress from the locker identified by your code number.
5.2.11 Put on shirt, trouser and headgear.
5.2.12 Shirt should be tucked into the trouser.(for Gents).
5.2.13 Collect the slippers from the slipper rack and wear them.
5.2.14 Walk through the corridor to the respective area.

Note: User Should Prepare annexure-I and II pictorial display as per their Dressing Design

Procedure for cleaning of Production Aids

1.0 OBJECTIVE
To lay down a procedure for cleaning of production aids.
2.0 SCOPE
Module - 1,2,3,4 and 5
Process
Applicable to S.S.scoops, S.S.spatullas, beakers, S.S containers SS bowls, flexible hoses and silicon tubes.
3.0 RESPONSIBILITY
Concerned operator.
4.0 ACCOUNTABILITY
Production officer.
5.0 PROCEDURE
5.1 Clean with potable water jet and lint free duster to remove adhering material.
5.2 Use purified water and nylon brush to clean them.
5.3 Rinse with purified water.
5.4 Dry with lint free duster.

Procedure for Maintaining Environmental Conditions

1.0 OBJECTIVE
To lay down a procedure for maintaining environmental conditions.
2.0 SCOPE
Module - 1,2,3,4,5,6 , Quarantine, primary packing rooms and secondary packing areas.
3.0 RESPONSIBILTY
Concerned operator.
4.0 ACCOUNTABILITY
Production Officer / Executive.
5.0 PROCEDURE
5.1 Record the environmental condition two times in a day.
5.2 Preferably take one reading in the morning and one reading in the afternoon.
5.3 If the conditions are more than the R&D specified limits / B.M.R, stop the operation and intimate to maintenance department for necessary rectification.
5.4 Start the operations only after attaining the required conditions and make the record of the same.

Gowning room Exit Procedure

1.0 OBJECTIVE
To lay down an exit procedure before the personnel leaving from
A) Pharma manufacturing modules.
B) Dispensing rooms.
C) Primary packaging machine rooms.
D) Raw material sampling room.
2.0 SCOPE
Applicable to all persons who are leaving the above mentioned areas.
3.0 RESPONSIBILITY
Concerned persons.
4.0 ACCOUNTABILITY
Workmen(T) /Production associates/Technical associates/ Jr. Technical officers-Production officer
Officers-Executive
Executive and above-Plant manager.
5.0 PROCEDURE
5.1.0 Precautions.
5.2.0 Exit procedure.
5.1.0 Precautions.
5.1.1 The soiled gowns (boiler suits) to be washed are to be put in separate bin Identified for that purpose.
5.1.2 Hang your gown (boiler suit) to the hanger.
5.2.0 Exit procedure
5.2.1 Enter the gowning room through process corridor of the module.
5.2.2 Remove the gloves and put them in SS box labelled as ‘used gloves’.
5.2.3 Remove the headgear and hang it to the hanger.
5.2.4 Remove the booties and keep them in a separate bin identified for that purpose.
5.2.5 Remove the boiler suit and hang it to the hanger.
5.2.6 Cross the step over bench gently by sitting on it.
5.2.7 Put on slippers from slipper rack.
5.2.8 Open the door, ensure that second door is closed, then enter the external corridor.

Gowning room Entry Procedure

1.0 OBJECTIVE
To lay down a procedure before the personnel entering into:
A) Pharma manufacturing modules.
B) Dispensing rooms.
C) Primary packing machine rooms.
D) Raw material sampling room.
2.0 SCOPE
2.1.1 Applicable to all persons who are entering in to the above mentioned areas.
3.0 RESPONSIBILITY
Concerned persons.
4.0 ACCOUNTABILITY
Workmen(T) /Production associates/Technical associates/ Jr. Technical officers-Production officer
Officers-Executive
Executive and above-Plant Manager
5.0 PROCEDURE
5.1.0 Precautions.
5.2.0 Entry procedure.
5.1.0 Precautions
5.1.1 The person allotted to one module or work place should not enter into the other Modules or work place without proper reason or until and unless authorized by the concerned department heads.
5.1.2 Every alternative day / product changeover or whenever necessary the boiler suit should be changed.
5.2.0 Entry procedure
5.2.1 Enter respective gowning rooms through external corridors (through personnel entry only).
5.2.2 Remove the factory slippers.
5.2.3 Keep them in the slipper rack.
5.2.4 Cross the step over bench gently by sitting on it.
5.2.5 Collect the boiler suit from hanger.
5.2.6 Put on the boiler suit
5.2.7 Put on clean booties and tie them properly over the boiler suit.
5.2.8 Put on the headgear and tie it properly.
5.2.9 Wash your hands with the disinfectant.
5.2.10 Collect the gloves from SS box.
5.2.11 Ensure that personnel entry door is closed and open the door which takes you into the module.
5.2.12 Put on the gloves in the process corridor (before entering into respective rooms).

Exit Procedure - Annexure X

1.0 OBJECTIVE
To lay down a procedure for exit from
a) Pharma production.
b) Ware house (raw and primary packing materials).
c) Primary packing.
2.0 SCOPE
Applicable to all the personnel who are leaving the areas mentioned in objective.
3.0 RESPONSIBILITY
Concerned person.
4.0 ACCOUNTABILITY
Workmen(T) /Production associates/Technical associates/ Jr. Technical officers -Production officer
Officers-Executive
Executive and above - Plant Manager
5.0 PROCEDURE
5.1.0 Precautions.
5.2.0 Exit procedure.
5.1.0 Precautions
5.1.1 Keep the slippers in the rack in orderly manner.
5.1.2 Every alternative day / product change over / whenever necessary put the dress in the bin marked as uniform for cleaning.
5.1.3 Do not dump the removed uniform in the locker, which is to be used next day.
5.1.4 Fold the dress gently and keep it in the locker.
5.1.5 Do not cross the bench with the primary dress.
5.1.6 Entry of gents into ladies change rooms or vice versa is strictly prohibited.
5.2.0 Exit procedure
5.2.1 Enter primary change room through external corridors.
5.2.2 Remove your slippers and keep them in slipper rack in orderly fashion.
5.2.3 Remove the headgear, shirt and trouser.
5.2.4 Place them in the locker and lock it.
5.2.5 Cross the step over bench by sitting on it (Do not jump over the bench).
5.2.6 Put on your street clothes.
5.2.7 Put on your footwear.
5.2.8 Collect ornaments or any other personal belongings from the locker identified by your code number and lock it.
5.2.9 Leave the change room.

HVAC SYSTEM - BASIS OF DESIGN PARAMETERS & EQUIPMENT SPECIFICATIONS

1.0 AIM:
The basic aim behind this exercise is to provide Terminal HEPA Filters for the Compression Area, with Overhead Feeding Room & Airlock and provide temperature and humidity control so that the product passing through shall remain under the same conditions as that of manufacturing areas.
Based on the actual observations of the present operating system it was decided to form the System Design Basis on following assumptions:
1.1 To provide Terminal HEPA filters in the Supply air path so as to achieve most effective Air Filtration System within the given limitations.
1.2 The air changes will be kept as minimum 25 air changes per hour.
1.3 Pressure Gradient shall be maintained from Passage to Compression Area to prevent cross contamination and to prevent ingress of untreated external air.
1.4 Heating Coil with Hot water shall be provided to maintain the required Relative Humidity.
1.5 The return air risers shall be provided with Grilles for pick up of room Air.
1.6 The motor of Air- Handling Unit will be provided with frequency drive so as to control the air quantity through variation in fan speed.
2.0 System Designation & Areas Covered under designated System:
2.1 System Location: Contractor Company
2.2 System Designation: AHU - XX
2.3 Areas covered:

COMPRESSION AREA
OVERHEAD COMPRESSION AREA
AIRLOCK

3.0 Design Parameters:
3.1 Area, Height & Volume:

3.2 Out Side Conditions:

3.3 In Side Conditions:

3.4 Fresh Air Quantity: 60 CFM
3.5 Lighting Load: 1.5 Watts / Sqft.
3.6 Roof Insulation:
Sun Exposed Roofs shall be insulated with 50 MM THK Expanded Polystyrene / Equivalent
3.7 Chilled Water Temperature - Not to exceed 8.50C at Inlet to Chilled Water Coil
3.8 Equipment Load, Occupancy, Room volume, Design Air changes and air quantity requirements.

4.0 Calculated Refrigeration Load & Air Quantity:

Note: 1. FA – Fresh Air
2. Deh. – Dehumidified Air Quantity
(i.e. Calculated Air Quantity based on Area Heat Load)
3. TR – Refrigeration Tonnage
(Calculated on the basis of Area Heat Load)
4. AHU Capacity – Air Quantity in CFM.
(Selected from Higher of Design Air Changes required &
Calculated Air Quantity based on Area Heat Load)
5.0 Differential Room Pressure Gradient:

6.0 Air Filters:

7.0 Temperature & Humidity Control:
Temperature and Relative Humidity Control to achieve the desired room conditions is achieved by a combination of Cooling and Heating Coil. Sensible & latent heat is removed from the Air Stream by the Chilled Water Cooling Coil. A three way proportionate balancing valve with temperature controller has to be provided at the chilled water cooling coil outlet connection.
The sensor of this valve senses the return air temperature and humidity proportionately controls the chilled water flow to chilled water coil in such a way that when the room temperature drops and/or the Relative Humidity decreases, the chilled water flowing through cooling coil is reduced proportionately to the setting and when the room temperature or Relative Humidity rises, the chilled water flowing through cooling coil is increased proportionately to the setting to achieve desired range of room temperature / Humidity.
The necessary Re-heat is provided to maintain desired Room Temperature through a heating coil. A Three Way proportionate balancing valve is provided at the outlet of the hot water coil, to regulate the hot water flow control as per the temperature requirements.

Qualification Protocol of Heating, Ventilation and Air Conditioning (HVAC) System - overview

Purpose :
To provide the documentary evidences that the HVAC system of System No. even numbered...
· Designed as per XXXX requirement
· Installed as per design specification
· Operating as per set parameters and
· Performing as per its intended use.
Scope:
This qualification protocol is applicable to the HVAC system of XXX Drug Area designed by M/s. (Contracting company) and installed by them.
Intended Use :
· To supply the required air quantity to the Compression Room to provide product protection from air borne contamination.
· To maintain the temperature and humidity for process as required by the product specification.
· To provide room pressure gradient to prevent ingress of contaminant
Location :
Service floor, XXXX, (Place).
Reference :
NA
Attachments :
Ducting Layout As Attachment (User Should attach one layout)
G.A. Drawing for Air Handling Unit As Attachment (User Should attach one layout)
Air Flow Diagram As Attachment (User Should attach one layout)

Study for qualification :
IQ:
To check all parts of AHU are as per predefined specification
To review proper installation as per protocol.
OQ:
To operate the AHU system as per proposed procedure and record.
To challenge the operating parameters of AHU and record.
To challenge the safety operation and record.
PQ:
HEPA filters integrity leak test by cold DOP test and air velocity shall be checked during performance.
Temperature and Humidity for three consecutive days shall be checked.
Air pressure, Air pattern and Air movement shall be checked for three consecutive days.
Air changes for the room shall be calculated to meet predefined specification.
Responsibilities :
M/s. (Contracting company)
· To install the HVAC system as per approved designed specification and at designated
Place.
· To prepare qualification protocol.
· To submit qualification protocol to 'XXXX company' for approval.
· To record the observation alongwith 'XXXX company' as per predefined specification.
· To submit final qualification reports to 'XXXX company' for approval.
Quality Assurance
· To review qualification protocol and approval.
· To record the observation along with production and engineering as per designed protocol.
Engineering
· To prepare the Qualification protocol.
· To install the system as per the design specification.
· To provide utilities and supportive services for qualification.
· To arrange for the calibration of the instruments for qualification study.
· To assist QA/Production while qualification study.

SOP - PAINTING OF THE FACILITY

1.0 PURPOSE :
To provide proper guidelines for painting.
2.0 SCOPE:
Whole plant.
3.0 RESPONSIBILITY:
Maintenance department.
4.0 ACCOUNTABILITY:
Head of Maintenance department.
5.0 DEFINITIONS:
Nil.
6.0 PROCEDURE:
6.1 GENERAL:
6.1.1 In manufacturing, filling, coating, sampling, dispensing areas and corridor, air lock the flooring is epoxy. Concrete pillars and beams are painted with PU Paint. All other areas (Store, Packing hall, Corridors) wall and ceiling is painted with Acrylic Emulsion paint. All utility areas and structure are painted with synthetic enamel paints.
6.2 FOR PU PAINTING:
6.2.1 The area is properly leveled with terraco plaster. On the prepared surface poly urethane primer is applied with brush. The surface is dried for 3 to 4 hours. When surface is tacky the first coat of PU paint is applied with brush. Three such coats are applied. Each coat is allowed to dry for 8 to 10 hours.
6.3 FOR EPOXY FLOORING:
6.3.1 The flooring is properly cleaned with wire brush to remove all dust particles from flooring. The pothole in flooring is leveled with epoxy mortar. The epoxy mortar is prepared by mixing quartz sand (No.10) in sterile paint. The surface is leveled with water papers. On the prepared surface 2 mm self leveling epoxy is applied. This floor is allowed to dry for 2 days.
6.4 FOR ENAMEL PAINT:
6.4.1 The surface is cleaned with wire brush and two coats of primer is applied. Each coat is allowed to dry for 10 to 12 hours. Then another two coats of enamel paint are applied.
6.5 SURFACE PREPARATION:
6.5.1 PIPELINES AND STRUCTURAL SUPPORTS:
Where corrosion in pipelines and pipeline supports is noticed, clean the surface thoroughly with chipping hammer and wire brush to bare metal. Apply appropriate primer (zinc primer for enamels paints) as base coat; allow drying for at least 24 hours and overcoat with recommended paint as required.
6.6 EQUIPMENTS:
6.6.1 Where corrosion in equipment is noticed remove all traces of oil or grease with cotton waste and scrap thoroughly to clean the surface. Touch up with appropriate primer and over coat with recommended paint as required.
6.7 WALLS, DOORS AND WINDOWS:
6.7.1 Remove all loose and flaked paint with scrapper or emery paper, level with putty as required and over coat with recommended paint.
6.8 SPECIFICATIONS AND PREPARATION OF PAINT:

6.9
COLOUR CODES FOR PIPELINES:
6.9.1 Steam - Red Bands over Aluminum Cladding
6.9.2 Potable - Water Yellowish (CPVC Pipe)
6.9.3 Chilled - Water Dark Blue
6.9.4 Cooling - Water Blue
6.9.5 Fire Water - Postal Red
6.9.6 Compressed Air - Sky Blue
6.9.7 Drains line - Black
6.9.8 Vacuum - Ivory
6.9.9 Nitrogen - Yellow
6.9.10 Diesel - Brown
6.10 HANDING OVER PROCEDURE:
6.10.1 After painting, the surface should be allowed to cure for at least 24 hours with paints like enamel, and ordinary aluminium paints and 2 to 3 hours for paints like snowcem. High temperature resistant aluminum paint will be cured only after the painted surface reaches that particular temperature. After painting the near by area should be cleaned by removing spillage of any paint. The equipment / area which was painted is now ready for use.
7.0 REFERENCES:
Nil.
8.0 ENCLOSURES:
Nil.
9.0 ABBREVIATIONS:
9.1 PU - Poly Urethane

INSTRUMENT OPERATION PROCEDURE DISSOLUTION APPARATUS

1.0. PURPOSE:
To provide a procedure for operating dissolution test apparatus.
2.0. SCOPE:
This covers the procedure for operating dissolution test apparatus
MAKE : ELECTROLAB
MODEL : TDT-08 L
3.0. RESPONSIBILITY:
3.1. Officer-Quality Control
3.2. Executive-Quality Control
4.0. ACCOUNTABILITY:
Manager-Quality Control
5.0. DEFINITION:
Nil
6.0. PROCEDURE:
6.1. Ensure the calibration status is valid and make sure that the instrument is properly placed for use.
6.2. Fill the distilled water in the tank up to the mark level without jars. Place the tank on the base of the instrument such that four screws at the bottom of the tank fits in to the holes on the base plate and heater cable is at the rear side of the instrument.
6.3. Connect the heater plug in the socket provided at the right hand side of the stirrer unit, fill the tank with water up to the level marked without placing any jar in the bath .Add 0.01%cetyl puridinium chloride or sodium benzoate or Bronidiol to prevent fungal growth in the water bath.
6.4. Set the temperature by pressing the SET TEMP and followed by pressing 3,7 and ENTER in number keys, Press START/STOP TEMP start temperature controller will start the controller making the TEMP ON LED glow once the temperature of the water bath has reached to the set value of the temperature, the READY LED will glow on the front panel of the instrument.
6.5. Set the rotation by pressing SET RPM and followed by pressing number keys ex : 50 RPM is required press ‘5’ and ‘0’ then ENTER.
6.6. Set the timer by pressing SET TIMER and followed by pressing number keys ex : i) 30 min is required press 3,0 and ENTER,
ii) 1 hour is required press 1,0,0 and ENTER,
iii) 5 hour is required press 5,0,0 and ENTER.
6.7. Fill the jar with dissolution medium as per the specification and place them in tank and fix the jar holder.
6.8. Fix all the stirrer with paddles or basket carefully.
6.9. Bring the stirrer with using the DOWN KEY.
6.10. Press START/STOP when the READY LED glowing on the front panel. If the water bath temperatures has not reached the set value of the temperature, then temperature display will flash “rd”. In this case press START key again after the READY LED on the front panel is on.
6.11. After end of the timing the buzzer beeps for 10 seconds.
6.12. Draw the sample as per the specification.
6.13. Lift the stirrer using the UP KEY.
6.14. Put ‘OFF’ the instrument after use.
6.15. PRECAUTIONS
6.15.1. Do not start the heater if there is no water in the tank up to the marked level.
6.15.2. The water bath should be filled with RO water only.
6.15.3. To clean the jar and water bath do not use any aggressive material or strong solvent
6.15.4. Do not pull or force the paddle or basket
6.15.5. Do not hold the stirrer while in operation
6.15.6. After every 4 month, put 6 to 8 drops of oil in lifting arrangement for smoother operation (oil parts are provided on the top of the lifting column ).
6.15.7. For lifting up the stirrer, make sure the paddles are stop.
6.15.8. Do not disturb the sensor tube while cleaning the tank.
6.15.9.
6.15.10 External probe should be handled with care.
Replace & clean the water from water bath fortnightly.
7.0. REFERENCES:
Instrument Manual
8.0. ENCLOSURES:
Nil
9.0. ABBREVIATIONS:

INSTRUMENT CALIBRATION DISINTEGRATION TEST APPARATUS

1.0 PURPOSE :
To provide a procedure for calibrating Disintegration tester.
2.0 SCOPE :
This covers the procedure for calibrating Disintegration tester ( QCI – 21 ).
MAKE & MODEL : Electrolab, ED-2L (USP).
3.0 RESPONSIBILITY :
QC officer.
4.0 PROCEDURE :
4.1 TEMPERATURE CHECK :
4.1.1 Keep about 800 ml of water in 1 liter beaker in the water bath.
4.1.2 Set the temperature to 37°C.
4.1.3 Wait until the set temperature reaches.
4.1.4 Observe and record the temperature,
Acceptance limit : 37°C ± 0.5°C.
4.2 STROKE HEIGHT:
4.2.1 Measure the distance between lowest and highest stroke,
Acceptance limit : 53mm to 57 mm.
4.3 CYCLES
4.3.1 Count the number of cycles per minute,
Acceptance limit : 28 – 32 cycles/minute.
5.0 FREQUENCY OF CALIBRATION :
Once in a month.

INSTRUMENT OPERATION PROCEDURE DISINTEGRATION TEST APPARATUS

1.0. PURPOSE:
To provide a procedure for operation of Disintegration tester.
2.0. SCOPE:
Applicable to Disintegration tester
MAKE & MODEL : Electrolab, ED-2AL
3.0. RESPONSIBILITY:
3.1. Officer-Quality Control
3.2. Executive-Quality Control
4.0. ACCOUNTABILITY:
Manager-Quality Control
5.0. DEFINITION:
Nil
6.0. PROCEDURE:
6.1. Ensure the calibration status is valid and make sure that the instrument is clean and free from dust.
6.2. Switch on the main switch and put on the ‘ON/OFF’ switch at the rear panel to ‘ ON’ position Follow the procedure to set the temperature.
6.3. For setting the temperature select the BATH probe by pressing PROBE key. This key toggles between BATH probe EXTSEL
a) Press SET key – LED to the right of the key will glow.
b) Press TEMP key- Temperature display shows previous set temperature with right most digit flashing.
c) Press ▲ key –Flashing digit value will show increment for every key press. OR
d) Press ▼ key - Flashing digit value will show decrement for every key press. Set the value for flashing digit.
e) Press DISP key - Next significant digit flashes .Repeat the above step.
f) Repeat the step c & d till the desired temperature is set.
g) Press ENTER key –Set temperature value will be registered and SET LED will be off.
To confirm the set value of temperature, press SET key first and TEMP key next. See the set value. Press ENTER key to come out from set mode.
NOTE: After pressing the SET key one should start the settings within 10 seconds other wise the set mode will be terminated automatically.
Press the TEMP key to start temperature controller. The LED above TEMP key will start glowing.
Select the bath temp indicator using PROBE SEL key. Once the bath temperature reaches the set value , you are ready to start the test by pressing START/STOP key.
There are two modes of operation.
a) Timer mode b) Manual mode
a) Select mode by pressing TIMER key, if the TIMER LED is on, then timer mode is selected. If the TIMER LED is off & Timer display shows “…….. then manual mode is selected. TIMER key toggles between TIMER mode and MANUAL MODE.
In timer mode two time ranges are possible.
1) 1 sec to 99 min & 59 sec.
2) 1 min to 9 hrs & 59 min(if this range is selected the forth (left most) digit of timer display will show “….”).For changing the timer range press SET key first and the ENTER key. Once the test is started range cannot be altered. After range is selected now set the desired time as mentioned. Step No 8.
Timer settings can be done only in timer mode. To set the timer follow the instructions given below.
a. Press SET key- SET LED will start glowing.
b. Press TIMER key – Timer display shows last set value with right most digit flashing. To set the digit go to step c
c. Press ▲ key –Flashing digit value will show increment for every key press.
OR
Press ▼ key - Flashing digit value will show decrement for every key
press. Set the value for flashing digit.
d. Press DISP SEL next significant digit will flash. Now repeat step c to set the value. Repeat step d to set all digits. Press ENTER to accept the value .
e. Press ENTER key to complete the timer setting. Set LED goes off.
f. Start the test using START/STOP key. TIMER display shows the elapsed time starting from “00.000” if the timer range is min , sec(“-0.00” if the timer range is hrs . min)
In any mode , to START or to STOP the test press the START/STOP key.
Warm distilled water to 37±2°C and take in 1000ml beaker. The volume of the water should be such that the wire mesh of the moving basket at its highest point is at least 25mm below the surface of the liquid and at its lowest point is atleast 25mm above the bottom of the beaker.
Place the beaker in the disintegration test apparatus. Suspend the basket assembly in to the beaker by fixing it in to the moving shaft.
Introduce one tablet in each of the six tubes of the basket of the assembly and place the disc in each.
Press START/ STOP button and note the time.
Run the instrument for required period and switch off. Lift the basket and observe for completion of disintegration.
Cleaning:
Empty the beaker and clean.
Remove the discs and clean the disintegration test apparatus.
7.0. REFERENCES:
Instrument Manual
8.0. ENCLOSURES:
Nil
9.0. ABBREVIATIONS:
Nil

INSTRUMENT OPERATING PROCEDURE UV-SPECTROPHOTOMETER

1.0. PURPOSE:
To provide a procedure for operating the UV – VIS Spectrophotometer.
2.0. SCOPE:
This covers the procedure for operating UV–VIS Spectrophotometer.
MODEL : UV-1700 with PC software
MAKE : Shimadzu.
3.0. RESPONSIBILITY:
3.1. QC-Chemist
3.2. QC-Officer
4.0. ACCOUNTABILITY:
Manager-Quality Control
5.0. DEFINITION:
Nil
6.0. PROCEDURE:
6.1. For PHOTOMETRIC
6.1.1. Switch on the instrument and computer
6.1.2. Check the connection cable to the PC is properly connected or not.
6.1.3. Select the icon of UV probe and click double
6.1.4. Press PC control (F4) in the instrument.
6.1.5. Select the icon Photometry.
6.1.6. Click the CONNECT icon.
6.1.7. Place the blank solution in sample compartment
6.1.8. Click the method icon(M).The page will be opened enter the wavelength & add the parameter, select calibration and enter raw data and close the window and method should be saved in method folder( which is suitable for name of the sample).
6.1.9. Keep blank and perform AUTOZERO
6.1.10. To read the samples keep the test solution and enter the sample ID in sample table and click the Read unknown icon.(If the method is already exists open the method file place the blank and make AUTOZERO).
6.1.11. To take print out click on REPORT icon and go to file open , select “ B & B PHOTOMETRIC DISSOLUTION” .Change the necessary information and save the report in data folder as XYZ. Where X is name of the sample or code, Y is batch No & Z is date, month & data.
6.1.12. Then preview the report and give the print out command.
6.2. FOR SPECTRUM
6.2.1. Switch on the instrument and computer.
6.2.2. Check the connection cable to the PC is properly connected or not.
6.2.3. Select the icon of UV probe and click double.
6.2.4. Press PC control (F4) in the instrument.
6.2.5. Select the icon Spectrum and click.
6.2.6. Place the blank solution in sample compartment
6.2.7. Click the method icon(M).The page will be opened, enter the wavelength range & scan at medium speed, and enter the necessary information which are relevant then click and the method should be saved as name of the sample and do the base line correction. (If the method is already exists open the method file , place the blank and do the base line correction).
6.2.8. To read the sample spectrum place the sample solution in sample compartment and click the START icon.
6.2.9. After spectrum scanning completion new data set will appear on screen automatically. Enter the file Name :dzu\uvprobe\data\xyz where X is sample name or code, Y is B.No , Z is date and Month and data, data storage to be same enter the analyst name and enter the analyst name and comment if required, click ok and should be saved
6.2.10. After completion of scanning go to operation click on peak pick, pick table will appear on monitor.
6.2.11. To take print out click on REPORT icon and go to file open select “ B& B SPECTRUM PEAK PICK”
6.2.12. Change the necessary information allotted space and save the report
6.2.13. Then preview the report and then give print out command.
7.0. REFERENCES:
Instrument Manual
8.0. ENCLOSURES:
Nil
9.0. ABBREVIATIONS:
Nil

OPERATION OF HIGH PRESSURE LIQUID CHROMATOGRAPHY

1.0. PURPOSE:
To provide procedure for Operation of High Pressure Liquid Chromatography.
2.0. SCOPE:
Applicable to HPLC (CodeNo. ) :
Make : Shimadzu
Model : LC-2010A
Pump : LC-10Atvp Detector : SPD-10Avp
System Controller : SCL-10Avp
Auto Injector : SIL-10Advp
3.0. RESPONSIBILITY:
3.1. QC- officer
3.2. QC- Executive
4.0. ACCOUNTABILITY:
Manager-Quality Control
5.0. DEFINITION:
Nil
6.0. PROCEDURE:
6.1.1. Check and ensure that the instrument is clean and calibration is valid.
6.1.2. Switch on SCL10Avp system control,SPD 10Avp UV-Visible detector, followed bySQL/10ADvp autoinjector & followed by LC10ATvp pump.
6.1.3. Then start the computer (Softwere),wait for a while;Till enter Password, appear on the monitor.
6.1.4. Enter the password -On screen WELCOMES TO WINDOWS appear.
6.1.5. Enter Esc wait for a while.
6.1.6. Icons appear. Then double click on class-vp system & wait for a while.
6.1.7. Class -vp system will open.
6.1.8. Choose Auto Sampler with double click.
6.1.9. On monitor login appear,enter the users name & Password . Enter User name as System , Password as 2001
6.1.10. Then Icons appear on the screen click on File,choose for METHOD, open a New file or stored file & same by going back to method.
6.1.11. Once again go back to file, Choose the SEQUNCE & save,enter file name data name & save.
6.1.12. Next go to METHOD icon on the screen click over method.
6.1.13. Choose INSTRUMENT SETUP then PUMPS/ SPD 10 AVP (Detector-A) will appear.
6.1.14. Set the Pump for flow rate & max pressure.
6.1.15. In SPD10VP (Detector-A),choose for wavelength & click APPLY followed by DOWNLOAD & save the method.
6.1.16. Once again come back to main screen,then choose icon on the main screen.
CONTROL,run down click over DIRECT CONTROL the series of icons appear on the screen.
6.1.17 Click icon on instrument ON/OFF Now the system is ready for operation Once analysis is over close the system as follows.
6.1.18. Click over file run down to EXIT.
6.1.19. Click once again on screen SHUTDOWN the computer,it's now safe to turn off your computer message appear.
6.1.20. Similarly switch off SCL10AVP system controller, followed by SPD10AVP, UV-VISIBLE DETECTOR followed by Auto-Injector, & then LC10ATVP pump.
Acceptance criteria : maximum pressure variation must not exceed 5.0 Kgf/cm2.
6.1.21. SELECTION OF COLOUMN: Check for the coloumn specified in the individual Monograph, and wash properly with solvents specified to get the proper resolution.
6.1.22 SYSTEM SUITABILITY: Carry out the system suitability test mentioned in individual Monograph.
6.1.23 ‘Frequency of washing’ : Column washing should be carried out after each analysis .
6.1.24 Extra washing should be carried ,whenever abnormal pressure variation or distortion of peaks occurs during analysis.
7.0. REFERENCES:
Instrument Manual
8.0. ENCLOSURES:
HPLC usage log
No.SOP:QCOP:00x6:xx
9.0. ABBREVIATIONS:
Nil

INSTRUMENT CALIBRATION PROCEDURE GAS CHROMATOGRAPHY

1.0 PURPOSE :
To provide a procedure for Calibration of Gas Chromatography
2.0 SCOPE:
This covers the procedure for operating Gas Chromatography
MAKE: Shimadzu, MODEL : GC-2010.
3.0 RESPONSIBILITY:
3.1. Officer-QC
3.2. Executive-QC
4.0. ACCOUNTABILITY:
Manager-Quality Control
5.0. DEFINITION:
Nil
6.0. PROCEDURE:
6.1. SYSTEM SUITABILITY
Run for every analysis in replicate 4 at the beginning and 2 at the end. Calculate RSD for retention time.
6.2. COLUMN AND INJECTION PORT
6.2.1. Inject 1ml of mixture of methanol and toluene (1:10) at the following conditions.
a. Mobile phase : Nitrogen gas,
b. Injector port temperature : 150°C,
c. Detector temperature : 150°C FID,
d. Column temperature : 120°C.
Inject in replicate and calculate the RSD for retention time.
Limit : NMT 2.0
Incase of abnormality.
a. Change the septum,
b. Clean the injection port
d. Purge the nitrogen gas through column for 2 hours
6.3. FREQUENCY OF CALIBRATION: Once in 3 months
7.0. REFERENCES:
Nil
8.0. ENCLOSURES:
Report format
9.0. ABBREVIATIONS:
Nil
NAME OF THE INSTRUMENT : GAS CHROMATOGRAPHY
INSTRUMENT CODE : xxxx
MODEL : GB-14
MAKE : SHIMADZU
CALIBRATION SOP No. : SOP:QCCB:xxx
INSTRUMENT OPERATION SOP No.: SOP:QCOP:xxx
A. R. No. :
DATE OF CALIBRATION :
NEXT CALIBRATION DUE ON :
CALIBRATION :

REMARKS:

CALIBRATION OF FLUID BED DRIER TEMP GUAGE

1.0 PROCEDURE :
1.1 Clean the drier, the air filters and exhaust system thoroughly,
1.2 Ensure that the air dampers are kept open fully,
1.3 Ensure that the dial gauge is clean,
1.4 The probes of inlet thermometer and outlet thermometers of the fluid bed drier are kept in oil bath along with standard thermometer and heated to note down the readings at various temperatures.
1.5 Record the temperature shown on the dial thermometer of the drier at an interval of 10 degree centigrade and corresponding temperature on the standard thermometer,
1.6 Calculate the percentage variation and check with the limits,
2.0 DOCUMENTATION :
2.1 F:Sxxxx/FBR - Fluid bed drier Temperature Guage Calibration Record.

CALIBRATION OF 6- STATION DISSOLUTION APPARATUS

1.purpose : Cleaning, Calibration and operational procedure of 6- Station Dissolution Apparatus.
2.Scope : This procedure is applicable to clean, calibrate and operate 6- Station Dissolution Apparatus.
Instrument:Dissolution Apparatus
Make: Electrolab
3.Reference / Attachments :
3.1 Reference
3.1.1 None
3.2 Attachments
3.2.1
Attachment – I : Instrument Usage Log
Attachment – II : Calibration Label
Attachment – III : Monthly calibration log for pH meter
Attachment – IV : History Card
Attachment – V : periodic Cleaning
4.Responsibility
4.1 Quality Head location
4.1.1 To review, audit and approval of SOP
4.1.2 Implementation of system as per SOP.
4.1.3 Training to the concern before implementation of SOP.
4.1.4 To ensure the operation, calibration and maintenance of the instrument is as per recommended Procedure.
4.2 Head Quality control
4.2.1 To ensure proper documentation as per SOP
4.2.2 To initiate the maintenance activity while breakdown.
4.3 Quality control officer / chemist
4.3.1 Operation of the instrument.
4.3.2 Calibration of the instrument.
4.3.3 Recording all document related to calibration and maintenance.
5.Calibration frenquency :
Calibrate the instrument once in 3 months or immediate after any maintenance.
6. Distribution
6.1 Quality control
6.2 Quality Assurance
6. Procedure
6.1 Clean the 6-Station Dissolution Apparatus and surroundings
6.2 Ensure that the Apparatus consists of following equipment.
6.2.1 Jars
6.2.2 Paddles
6.2.3 Baskets
6.2.4 pH meter
6.3 Place the tank on the base of the instrument such that four screws at the bottom of the tank fits into the holes on the base plate and heater cable is at the rear side of the instrument.
6.4 Connect the heater plug in the socket provided at the rear right hand side of the stirrer unit. Fill the tank with water upto the level marked without placing any jar in the bath. Add 0.01% cetyl pyridinium chloride or sodium benzoate or bronidiol to prevent fungal growth in water bath.
6.5 Plug in the mains chord a 230 V/ A. C./15 Amp. Power supply socket. Switch on the power switch and heater switch provided at the back side of the stirrer unit.
6.6 Press set temperature push button and adjust the set temperature knob till the digital reading shows 37 degree Celcious. Lock the knob after setting.
6.8 Make entry of the usage in the instrument log Register.
6.9 Always keep the lifting switch situated at the instrument in center when not in use.
7. Operation procedure:
7.1 Ensure, that the instrument is calibrated.
7.2 Fix the paddle or basket as per the test requirement. Do not overtighten.
7.3 Start the stirrer by pressing the RUN switch.
7.4 Set thr RPM by turning RPM knob clockwise to increase the RPM and anti-clockwise to decrease the RPM. After setting the RPM, lock the knob and stop the stirrer by pressing the reset switch. Do not turn the knob when it is in LOCK position always unlock the knob and turn.
7.5 Set the time as specified in individual specification/monograph by using thumb wheel switch.
7.6 Select the manual mode using the auto manual switch. This switch illuminates in auto mode. In auto mode the instrument will give an alarm after every set interval and the stirrer will keep on running.
7.7 Add the required volume of the deaerated dissolution medium in the jars as specified in the individual specification / monograph.
7.8 Bring the stirrer unit down by using up – stop – down switch. Run the apparatus to equibrate dissolution medium in the jars and check the temperature with a calibrated theromometer.
7.9 If baskets are used, lift the stirrer unit, down by using up – stop – down switch. If paddle is used, place one tablet / capsule in the jar. Care to be taken : The inside distance between paddle or basket to the jars should be maintained at 25mm +2mm, during the test.
7.10 Cover the jars containing dissolution medium with the lids provided.
7.11 Start the stirrer by pressing the start switch. Run the apparatus for the set time.
7.12 Collect the sample within +2% of specified time. [ For eg If time is 30 mts., sample to be taken within 36 seconds.]
7.13 Withdraw sample from a zone midway between the surface of the dissolution medium and the top of the rotating basket or blade, not less than 1cm. From the vessel wall and filter the solution.
7.14 Lift the stirrer by using the up – stop – down switch at the end of the set time.
7.15. Switch off the Instrument.
8. Calibration Procedure:
8.1 At start set the Revolutions per minute to 50 and Start the instrument and check the initial RPM. At the end of 1 hour stop the instrument and check for number of revolutions per minute. Continue for another 1 hour and check for the number of revolutions per minute. Like wise the procedure is to be repeated for 100 RPM. The limit for the revolutions is ± 2% of the set value.
8.2 At start set the temperature to 37° C and start instrument and check the initial temperature. At the end of 1 hour stop the instrument and note the temperature of the medium. Continue for another 1 hour and check the temperature of the medium. The limit of the temperature should be between 36.5°C to 37.5°C. Check the temperature of the dissolution medium by a calibrated thermometer.
8.3 The wobbling of each shaft is measured by placing the Wobblometer at the center of the shaft of the paddle/Basket and note the value observed in the guage of the wobblometer keeping the instrument on 50 RPM.
9. Cleaning procedure:
9.1 After use clean the jars(Test Vessels) with water and rinse with distilled water.
9.2 To clean the marlon jars and water bath do not use any abrasive material
9.3 Clean the tank at least once in a week. Add 0.01% cetyl pyridinium chloride or sodium benzoate or bronidiol to prevent fungal growth in water bath.
9.4 Do not disturb the sensor tube while cleaning the tank.
9. Cleaning procedure:
9.1 After use clean the jars(Test Vessels) with water and rinse with distilled water.
9.2 To clean the marlon jars and water bath do not use any abrasive material
9.3 Clean the tank at least once in a week. Add 0.01% cetyl pyridinium chloride or sodium benzoate or bronidiol to prevent fungal growth in water bath.
9.4 Do not disturb the sensor tube while cleaning the tank.

CALIBRATION OF DRIER TEMPERATURE GUAGE

1.0 PROCEDURE :
1.1 Clean the drier, the air filters and exhaust system thoroughly.
1.2 Ensure that the air dampers are kept open fully,
1.3 Ensure that the probe of the dial guage is clean.
1.4 Start the drier and keep a standard thermometer of 110°C range near the probe.
1.5 Check the temperature shown on the dial thermometer on the drier at an interval of 10 degree centigrade and the corresponding temperature on the standard thermometer.
1.6 Record and calculate the percentage variation and check with the limits.
2.0 DOCUMENTATION :
2.1 F:Sxxxx/DTR - Drier Temperature Guage Calibration Record.

CALIBRATION OF DRY AND WET BULB THERMOMETER

1.0 PROCEDURE
1.1 Place the standard dry wet bulb thermometer in the area along with the dry wet bulb thermometer used is to be calibrated.
1.2 Record the wet and dry bulb temperature of the thermometers at various intervals during the course of the day (at least five readings)
1.3 Calculate the percentage relative humidity by taking the difference of dry and wet bulb thermometers by referring to table of wet and dry bulb thermometer readings with corresponding percentages of humidity as read in the standard hygrometer.
1.4 Calculate the percentage variation and check with limits,
1.5 Reference table attached,
Limits : Relative humidity 50 ± 2%
2.0 DOCUMENTATION :
F:Sxxxx/WBR - Dry and Wet bulb Calibration Record.

CALIBRATION OF FLAME PHOTOMETER

1.0 PROCEDURE
1.1 PREPARATION OF STANDARD STOCK SOLUTIONS
1.1.1 Potassium chloride stock solution
Weigh accurately 0.75 g of KCl to a 1000 ml volumetric flask, shake well, to dissolve and make up the volume with the distilled water.
1.1.2 Sodium chloride stock solution
Weigh accurately 1.170 g of sodium chloride to a 1000ml volumetric flask, shake well to dissolve and make up the volume with the distilled water.
For calibration dilute the above stock solution as follows

CALIBRATION OF FLUORIMETER

1.0 PROCEDURE :
1.1 PREPARATION OF STANDARD STOCK SOLUTION OF QUININE SULFATE:
Weigh accurately 10mg of Quinine sulfate and dissolve in 0.1N Sulfuric acid and make up to volume with 0.1N Sulfuric acid to 1000mL. Preserve this solution, protected from light, in a refrigerator.
For calibration, dilute the above stock solution as follows:
Soln. 1.5ml - 200ml with 0.1 N Sulfuric acid (0.25 mcg/ml)
Soln. 2.4ml - 200ml with 0.1 N Sulfuric acid (0.20 mcg/ml)
Soln. 3.3ml - 200ml with 0.1 N Sulfuric acid (0.15 mcg/ml)
Soln. 4.2ml - 200ml with 0.1 N Sulfuric acid (0.10 mcg/ml)
Soln. 5.1ml - 200ml with 0.1 N Sulfuric acid (0.05 mcg/ml)
1) Select the instrument as per the Operating Procedure.
2) Select Primary filter (366 nm) and Secondary filter (4308 nm)
3) Adjust the blank to zero with 0.1 N Sulfuric acid.
4) Place the diluted solution 1 in the cuvette. Adjust the reading to 100 and place the other diluted solutions in the cuvette and note down the readings.

CALIBRATION OF HPLC

1.0 PROCEDURE
1.1 CALIBRATION OF PUMP :
Start the HPLC pump as per IOP and check the flow rate by collecting water in a 10ml measuring cylinder. Using a stop watch set the time for 5 minutes and measure the volume collected for 1.0ml/ minute 1.5/minute and 2.0ml/minute flow rates respectively. Note the readings in duplicates.

1.2 CALIBRATION OF DETECTOR
To a clean, dry 100ml volumetric flask, add 0.1ml of Benzene and 0.1ml of Toluene. Mix by adding mobile phase and make up to volume. Inject equal quantities three times and record the ratio of the peak area.
Chromatographic conditions
Detector : 254nm
Flow Rate : 1.0 ml/minute
Mobile Phase : Methanol : Water = 80 : 20
Absorbance Scale : 0.02
Attenuation : 5
Injection Volume : 20micro litre
Column : C-18 (Shim-pak)
Area of first peak
Calculation : = Ratio
Area of second peak


2.0 DOCUMENTATION
2.1 F:Sxxxx/HCR - HPLC Calibration Record.

CALIBRATION OF INFRA RED SPECTROPHOTOMETER

1.0 PROCEDURE:
Spectrophotometers for recording spectra in the infra red region consists of an optical system capable of providing monochromatic light in the region of 4000 to 670 cm-1 (about 2.5 to 15mm) or in some cases down to 200cm-1 (50mm) and a means of measuring the Quotient of the intensities of the transmitted light and the incident light.
1.1 Resolution Performances of the Apparatus:
The instrument used for recording infrared spectra should comply with the following test for resolution. Record the spectrum of the polystyrene film 0.05mm thick. The depth of the through from the maximum absorption at 2851 cm-1 (3.51mm) to the minimum at 2870 cm-1 (3.48mm) should be greater than 18% transmittance and that from the maximum at 1583 cm-1 (6.23mm) to the minimum at 1589 cm-1 (6.29mm) should be greater than 12% transmittance.
Verification of the wave-number scale
The wave number scale may be verified using a polystyrene film which has maxima at the wave-number (in cm-1) 8 hours.

The numbers in parentheses indicate the accuracy with which these values have been established.
1.0 DOCUMENTATION
1.1 F:Sxxxx/ICR - Infra red Spectrophotometer Calibration Record.

CALIBRATION OF MIXING TANK (GRADUATED)

1.0 SETTING OF TANK :
1.1 Clean the tank throughly using water.
1.2 Place the tank in a particular place and level it using a spirit level.
1.3 Mark the position of the wheel on all the four sides.
2.0 STANDARDISATION OF WATER :
2.1 Take a clean 20-L stainless steel (S.S) Vessel.
2.2 Weigh and note down the empty weight (B)
2.3 Add about 15-L water and note down the total weight (A). Check temperature (T degree C).
2.4 Note down the weight of water (C) Taken by subtracting B from A.
2.5 Calculate the specific gravity of water,
2.6 Calculate the quantity of water in terms of Liter equivalent to the weight taken using the following formula.
Volume of water in Liters = Weight of water (C) in kg / Specific gravity of water at temp T°C

CALIBRATION OF pH METER

1.0 PURPOSE : To provide a procedure for periodic calibration of pH meter.
2.0 SCOPE : Covers procedure for the calibration of pH meter (daily and monthly) and also for the activation of electrode and maintenance of electrode.
3.0 DEFINITION :
3.0.1 pH: pH value conventionally represents the acidity or alkalinity of an aqueous solution.
3.0.2 CALIBRATION : The set of operations which establish, under specified conditions, the relationship between values indicated by a measuring instrument or measuring system or values represented by a material measure and the corresponding known values of a reference standard. 4.0 PROCEDURE :
4.1 PREPARATION OF BUFFER SOLUTION
Buffer solution D: (pH 4.01) Dissolve 10.21 g of potassium hydrogen phthalate, previously dried at 110 degree to 130 degree for 2 hours in sufficient carbondioxide free water to produce 1000mL.
Buffer solution E: (pH 6.87) Dissolve 3.40 g of potassium dihydrogen phosphate and 3.55 gram of anhydrous disodium hydrogen phosphate previously dried at 110 degree to 130 degree for 2 hours both in sufficient carbondioxide free water to produce 1000mL.
Buffer solution G: (pH 9.18) Dissolve 3.814 gram of borax in sufficient carbondioxide free water to produce 1000.0 ml.
Store all the above solutions in alkali free glass. Label the bottle as follows:



Frequency of preparation : Monthly
Every week transfer 250ml of this buffer to the secondary bottle after checking for clarity and label the bottle with details as under :



Solution showing precipitation, haziness or growth of fungus shall be discarded.
4.2 CALIBRATION OF Ph METER :
Use the service beaker provided for each buffer and do not transfer the buffer from service
beaker back to the bottle. Discard after every use.
Calibrate the apparatus using 25ml from the stock solution of buffer solution D as the primary
standard adjusting the meter to read appropriate pH 4.01 Plus or minus 0.05 corresponding to the temperature of solution (25degreeCPlus or minus 2 degree C). To set the scale use a second reference buffer solution
either E (6.87) or G (9.18).
If the difference between this reading and the original value is greater than 0.05, the set of
measurements must be repeated.
When measuring pH values above 10.0 ensure that the glass electrode is suitable for use under
alkaline conditions and apply any correction that is necessary.
IMPORTANT CONDITIONS :
a) All solutions of substances being examined must be prepared using carbon dioxide free
water.
b) pH determination is carried out at a temperature of 25degreeCPlus or minus 2 degree C.
c) Buffer solutions should be stored in bottles made of alkali free glass.
5.0 ACTIVATION OF ELECTRODE :
FREQUENCE : EVERY 15 DAYS
5.1 COMBINED GLASS ELECTRODE.
Soak the electrode overnight in 6 M Hydrochloric acid, next day wash repeatedly with distilled
water and immerse the electrode in distilled water.
5.2 GEL FILLED ELECTRODE
5.2.1 Between measurements (upto 1 hour)
leave the electrode in an open air lab environment not in distilled water.
5.2.2 Short term storage (upto one week)
Soak electrode in 200ml pH 7 buffer added with 1 g potassium chloride.
5.2.3 Long term storage (over one week).
Cover the electrode tip with a protective cap used for shipment.
6.0 MAINTENANCE OF ELECTRODE :
CLEANING PROCEDURE
6.1 GLASS ELECTRODE
6.1.1 General : Soak electrode in 0.1 M HCl or 0.1 N HNO3 for 15 minutes.
6.2 GEL FILLED ELECTRODE :
6.2.1 Removal of Deposits
6.2.2 Protein : Digest with 1% pepsin in 0.1 M HCl.
6.2.3 Inorganic : Rinse with 0.1 M tetra sodium EDTA solution.
6.2.4 Grease and oil : Rinse with mild detergent or methanol solution.
7.0 RECORDS :
7.1 Record the pH calibration & activation of electrode in form F:Sxxxx/DPHR/A.
7.2 Record the monthly calibration in form F:Sxxxx/PHR/A
7.3 Record the pH of all solutions checked in daily pH log book.
8.0 DOCUMENTATION :
8.1 F:Sxxxx/PHR/A pH Meter calibration record
8.2 F:Sxxxx/DPHR/A Daily pH checking record.