Category: QC SOP

SOP Title: Management of Laboratory Instruments

1. Objective:

To lay down the procedure for management of laboratory instruments.

 

2. Scope:

This procedure is applicable for management of laboratory instruments in the Quality Control Department.

 

3. Responsibility:

• Quality Control Department: To prepare and review the SOP. To follow the procedures laid down for management of laboratory instruments in Quality Control Department as per this SOP.
• Quality Assurance Department: To review and approve the SOP and Annexure.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department.

5. Procedure

 

5.1	Installation and Qualification of Instrument and Equipment :
5.1.1	For all new instrument and equipment received in the laboratory allocate an identification number.
5.1.2	Get the instrument and equipment installed and qualified as per individual installation and qualification protocols, which is either provided by manufacturer/service provider or prepared in house and approved.
5.1.3	Prepare operating procedure including calibration parameters and performance verification parameters along with acceptance criteria and frequency schedule based on pharmacopoeia, regulatory guidelines and instrument manufacture/ service provider’s guidelines etc.
5.1.4	Perform complete calibration/ performance verification as mentioned in relevant instrument/ equipment SOP. In case parameter are listed under multiple schedules, then perform all parameters listed under all schedule/ frequency.
5.1.5	While using the instrument, usage entry shall be done in instrument usages logbook/ log sheet.
5.1.6	Incorporate the instrument/ equipment in master plan for performance verification and get the same also included in the master maintenance schedule available with the maintenance department, if applicable.

  

6. Definitions / Abbreviations:

• Definitions :

 

• Abbreviations:

Abbreviation	Expansion
QC	Quality Control
QA	Quality Assurance
SOP	Standard Operating Procedure
i.e.	That is

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Operation, Cleaning and Calibration of Muffle Furnace

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Muffle Furnace.

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Muffle Furnace located in Quality Control Laboratory

 

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of Muffle Furnace as per this SOP.
• Engineering Department: To carry out preventive maintenance as per schedule and procedure defined.
• Quality Assurance Department: To review and approve the SOP and Annexures.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department.

 

5. Procedure:

 

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the muffle furnace is fixed in the socket properly.
5.1.2	Wear personal protective equipments such as safety glasses, heat resistant gloves during operation of equipment.
5.1.3	Ensure that the ON/OFF switch is working properly by switching “ON” the muffle furnace.
5.2	Operation:
5.2.1	Switch ON the main switch.
5.2.2	The main indicator red light and yellow light will glow and the temperature panel display will show the temperature in o C.
5.2.3	Set the required temperature on the digital temperature controller by pushing red key present at the left side of “Temp. SET” knob and rotating the “Temp. SET” knob.
5.2.4	Relieve the red key button after the required temperature is set.
5.2.5	Move the “Energy Regulator” knob clockwise to corresponding temperature.
5.2.6	Wait till the temperature controller display shows the set temperature.
5.2.7	Open the door of the muffle furnace by pushing the lever upwards and place the crucible containing sample inside the muffle furnace with the help of long pair of tongs.
5.2.8	Immediately close the door.
5.2.9	Allow the substance under test to remain inside muffle furnace at a specified temperature and specified time as mentioned in the respective pharmacopoeia or specification.
5.2.10	After completion of analysis, Switch OFF the mains of the muffle furnace.
5.2.11	Open the door of the muffle furnace, remove the crucible containing sample and place it in desiccator till it attains the room temperature.
5.2.12	Immediately close the door of the muffle furnace.
5.2.13	Update the “Instrument/Equipment Usage Log Book” as per SOP “Calibration of Instruments and Equipment’s”.
5.3	Cleaning Procedure:
5.3.1	Switch OFF the mains of the muffle furnace.
5.3.2	Ensure that the temperature of the muffle furnace is nearly at room temperature when cleaning inside.
5.3.3	Clean the inside and outside of muffle furnace with lint free cloth or soft brush before and after use.
5.4	Calibration Procedure:
	Frequency:  Once in a year by external agency.
5.4.1	Calibration is carried out by external agency as per SOP “Calibration of Instruments and Equipment’s”.
5.4.2	Refer Annexure for calibration test to be performed and acceptance criteria. Sr. No. Tests Set value Acceptance Criteria (± 2%) 1. Temperature Verification 200oC ± 4oC 400°C ± 8oC 800oC ± 16oC 1000oC ± 20oC 1100oC ± 22oC
5.4.3	Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP and give requisition to QA department for calibration formats of instruments/equipments on the due date of calibration.
5.4.4	For issuance of calibration report refer SOP “Control of documents, Preparation, Approval, Issuance and Maintenance.
5.4.5	Update “Annual Calibration Schedule” and “Monthly Calibration Schedule” as per SOP “Calibration of Instruments and Equipments”.
5.5	Preventive Maintenance:
5.5.1	Perform the preventive maintenance as per define Annexure.
5.5.2	If preventive maintenance activity is outsourced, the observations are to be transcribed in the Annexure and external party certificate to be attached.
5.5.3	If any breakdown occurs, follow procedure as per SOP “Calibration of Instruments and Equipments”.

 

6. Definitions / Abbreviations:

• Definitions:
• Calibration: Tests performed to ensure that the instrument/equipment is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.
• Preventive Maintenance: Maintenance activity performed to ensure that the equipment will function smoothly and to avoid breakdowns. These activities are performed as per predefined frequency.
• Abbreviations

 

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
A. R. No	Analytical Reference Number
No.	Number
oC	Degree Celsius
PM	Preventive Maintenance

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Operation, Cleaning and Calibration of Bursting Strength Apparatus

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Bursting Strength Apparatus.

 

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Bursting Strength Apparatus located in Quality Control Laboratory.

 

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of Bursting Strength Apparatus as per this SOP.
• Engineering Department: To carry out preventive maintenance as per schedule and procedure defined.
• Quality Assurance Department: To review and approve the SOP and Annexures.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

 

5. Procedure:

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the Bursting Strength Apparatus is fixed in the socket properly.
5.1.2	Wear personal protective equipments such as safety glasses during operation of instrument.
5.1.3	Ensure that the ON/OFF switch is working properly by switching “ON” the Bursting Strength Apparatus.
5.2	Operation  Procedure:
5.2.1	Check the validity of Calibration before starting any operations.
5.2.2	Introduction to the Keys: MAIN ON:  ON/OFF switch. PUSH FOR BRUST: Press button to apply pressure for bursting. GAUGE I (Left side): To select the pressure gauge 0 to 8.0 kg/cm2. GAUGE II (Right side):  To select the pressure gauge 0 to 40.0 kg/cm2.
5.2.3	Switch ON the main switch and “MAINS ON” switch of the instrument.
5.2.4	Raise the tripod and upper clamping by rotating clamp wheel.
5.2.5	Place the representative sample of the material to be analysed over the diaphragm between the upper and lower clamping plates.
5.2.6	Lower the tripod plate applying sufficient clamping pressure to prevent slip of the sample between lower and upper clamping plates during analysis.
5.2.7	While analysing corrugated board, it is recommended that tripod plate be lowered to position where it rests on top of the sample.
5.2.8	Select the GAUGE I or GAUGE II depending up on the strength of sample by moving the lever.
5.2.9	If bursting strength of the sample is below 8.0 kg/cm2, then turn the lever to GAUGE I.
5.2.10	If bursting strength of the sample is above 8.0kg/cm2, then turn the lever to GAUGE II.
5.2.11	Set the needle pointer of the gauge at zero position.
5.2.12	Push the “PUSH FOR BURST” button and keep it pressed so that plunger will start rotating in clock wise direction at constant speed till sample bursts.
5.2.13	Release pressed push button as soon as the sample bursts.
5.2.14	Record the bursting strength at which the needle pointer on the gauge stops when the sample bursts.
5.2.15	This will automatically reverse the direction of plunger, and it will come and stop to its starting position.
5.2.16	The motor will stop at this position.
5.2.17	Update the “Instrument/Equipment Usage Log Book” as per SOP No. QC/009 “Calibration of Instruments and Equipments”.
5.3	Cleaning Procedure:
5.3.1	After completion of the test clean the plunger with lint free nylon cloth.
5.4	Calibration Procedure:
	Frequency:  1) Once in a year by external agency.
	2) In-house calibration to be performed half yearly or after carrying out any major maintenance work.
5.4.1	For external calibration refer Annexure for calibration test to be performed and acceptance criteria. Sr. No. Tests Set value Acceptance Criteria 1. Pressure Verification of Pressure Gauge – Ι   0.0 Kg/cm2 ± 2 % 2.0 Kg/cm2 ± 2 % 4.0 Kg/cm2 ± 2 % 6.0 Kg/cm2 ± 2 % 8.0 Kg/cm2 ± 2 % 2. Pressure Verification of Pressure Gauge – ΙΙ   0.0 Kg/cm2 ± 2 % 10.0 Kg/cm2 ± 2 % 20.0 Kg/cm2 ± 2 % 30.0 Kg/cm2 ± 2 % 40.0 Kg/cm2 ± 2 %
5.4.2	Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP and give requisition to QA department for calibration formats of instruments on the due date of calibration.
5.4.3	For issuance of calibration report refer QA SOP “Control of documents, Preparation, Approval, Issuance and Maintenance.
5.4.4	Perform the Inhouse calibration of instrument as per Annexure and procedure mentioned below.
5.4.5	Calibration of bursting strength is performed by standard aluminium foil.
5.4.6	Repeat the procedure from point 5.2.5 to point 5.2.16.
5.4.7	Enter the details in calibration report as per Annexure. Ensure that the results obtained, comply with the acceptance criteria. Sr. No. Parameters Acceptance Criteria (As per Supplier Specification) Observed Values Complies / Does Not Complies 1. Bursting Strength of Standard Aluminium foil
5.4.8	Update the “Instrument/Equipment Usage Log Book” as per SOP “Calibration of Instruments and Equipments”.
5.4.9	Affix the “Calibration Status Label” on the Instrument as per SOP “Calibration of Instruments and Equipments”.
5.4.10	If calibration activity is outsourced, the values are to be transcribed in the Annexure, and external party certificate to be attached.
5.5	Preventive Maintenance :
5.5.1	Perform the preventive maintenance and record in Annexure.
5.5.2	If preventive maintenance activity is outsourced, the observations are to be transcribed in the Annexure and external party certificate to be attached.
5.5.3	If any breakdown occurs, follow procedure as per “Calibration of Instruments and Equipments”.

6. Definitions / Abbreviations:

• Definitions:
• Breakdown: Any activity leading to operation of instrument/equipment other than the set parameters or unusual sound or vibration observed in the instrument/equipment.
• Calibration: Tests performed to ensure that the instrument/equipment is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.
• Preventive Maintenance: Maintenance activity performed to ensure that the instrument/equipment will function smoothly and to avoid breakdowns. These activities are performed as per predefined frequency.

 

• Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
Kg/cm2	Kilogram per centimetre square
PM	Preventive Maintenance

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Operation, Cleaning and Calibration of Refrigerator  

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Refrigerator.

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Refrigerator located in the wet chemistry area of Quality Control Department.

 

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of Refrigerator as per this SOP.
• Quality Assurance Department: To review and approve the SOP and Annexures.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department.

 

5. Procedure:

 

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the refrigerator is fixed in the socket properly.
5.1.2	Ensure that the ON/OFF switch is working properly by switching “ON” the refrigerator.
5.1.3	Place the refrigerator at least 30 cm away from the adjacent side wall and 10 cm away from the backside wall for free circulation of air.
5.1.4	Ensure that refrigerator is placed away from direct heating sources.
5.1.5	Do not use the extension board to connect refrigerator plug.
5.1.6	Levelling should be done with rotation of front leg to avoid imbalance of the refrigerator.
5.1.7	Do not place the heavy object or the dangerous object in the refrigerator or on the refrigerator.
5.1.8	Do not modify power cord length or share the outlet with other appliances.
5.1.9	Do not operate with wet hands or in damp environment.
5.1.10	Do not splash water on refrigerator.
5.1.11	Do not leave refrigerator open for long time. Don’t open the refrigerator door too often, hot air will enter and increases the temperature.
5.1.12	Never overload refrigerator or cover the shelves with paper or plastic sheets as it will reduce its efficiency.
5.1.13	Close the door properly; make sure that there is no gap between the gasket and the cabinet of refrigerator.
5.2	Operation:
5.2.1	Connect the refrigerator to electric power supply.
5.2.2	Switch “ON” the mains of the refrigerator.
5.2.3	Adjust the refrigerator knob to attain temperature i.e. 20C to 8°C according to the season as mentioned below. 1)      In summer season set the refrigerator knob in between 5 – 7. 2)      In rainy season set the refrigerator knob in between 3 – 5. 3)      In winter season set the refrigerator knob in between 1 – 3.
5.2.4	Place the items required to be stored into the refrigerator and close the door properly.
5.2.5	Ensure that the lamp inside the refrigerator glows when door is open.
5.2.6	Push the defrost knob when ice level reaches to defrost indicator.
5.2.7	Record the temperature twice in a day by using calibrated thermometer as per Annexure  i.e. in first half and in second half of the day.
5.2.8	For issuance of ‘Temperature Monitoring Record’ refer SOP ‘Control of documents, Preparation, Approval, Issuance and Maintenance’.
5.3	Cleaning Procedure:
5.3.1	Disconnect electric power supply of refrigerator before cleaning.
5.3.2	Use dry cloth only for cleaning exterior and interior.
5.3.3	Replace all the items back into the refrigerator and put ON the refrigerator.
5.3.4	Do not use mechanical devices to accelerate the defrosting process.
5.4	Calibration Procedure:
	Frequency:  Once in a year
5.4.1	Calibration shall be carry out by external agency OR by using calibrated thermometer as per SOP “Calibration of Instruments and Equipments”.
5.4.2	Refer Annexure for calibration test to be performed and acceptance criteria. Sr. No. Tests Acceptance Criteria Observations 1. Temperature Verification 5oC ± 1.0oC
5.4.3	For issuance of calibration report refer QA SOP “Control of documents, Preparation, Approval, Issuance and Maintenance.
5.4.4	If any breakdown occurs, follow procedure as per SOP number “Calibration of Instruments and Equipments”.

  

6. Definitions / Abbreviations:

• Definitions:

  

• Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
No.	Number
°C	Degree centigrade
±	Plus or minus
cm	Centimetre
i.e.	That is
%	Percentage
Hrs	Hours

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Operation, Cleaning and Calibration of Vacuum Oven

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Vacuum Oven.

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Vacuum Oven located in Quality Control Laboratory.

 

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of Vacuum Oven as per this SOP.
• Engineering Department: To carry out preventive maintenance as per schedule and procedure defined.
• Quality Assurance Department: To review and approve the SOP and Annexures.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

 

5. Procedure:

 

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the vacuum oven is fixed in the socket properly.
5.1.2	Wear personal protective equipments such as safety glasses, heat resistant gloves during operation of equipment.
5.1.3	Ensure that the ON/OFF switch is working properly by switching “ON” the vacuum oven.
5.2	Operation:
5.2.1	Switch ON the main switch.
5.2.2	Switch ON the ‘ON/OFF’ knob in ON position.
5.2.3	The main indicator red light will glow and the temperature panel display will show the temperature in oC.
5.2.4	Set the required temperature on the temperature panel with ‘TO SET’ key.
5.2.5	Adjust the required temperature with the ‘COARSE’ and ‘FINE’ keys.
5.2.6	Wait till the vacuum oven attains the set temperature.
5.2.7	The Temperature indicator green light will glow when the required temperature is reached.
5.2.8	Open the door of the vacuum oven by rotating the 3 screw knobs in anti clockwise direction.
5.2.9	Place the sample to be dried inside the vacuum oven on a stainless steel plate provided.
5.2.10	If the sample is placed in LOD bottle or any other closed glass apparatus, open the lid of the bottle and place in the vacuum oven.
5.2.11	Immediately close the door and tighten the 3 screw knobs tightly.
5.2.12	To apply pressure to the vacuum oven, connect the vacuum pump to the vacuum nozzle of the vacuum oven provided at the right side corner of the equipment.
5.2.13	For operation of vacuum pump refer SOP ‘Operation, Cleaning and Calibration of Vacuum Pump’.
5.2.14	Open the pressure ‘IN’ knob and start the vacuum pump.
5.2.15	Check the vacuum gauge dial of the equipment till the needle reaches at the required vacuum.
5.2.16	As soon as the required vacuum is reached, close the pressure ‘IN’ knob tightly and switch OFF the vacuum pump.
5.2.17	Allow the substance under test to remain under vacuum at a specified temperature and specified time as mentioned in the respective pharmacopoeia or specification.
5.2.18	After completion of analysis, slowly release the vacuum by opening the pressure ‘OUT’ knob till the pressure needle on vacuum gauge dial comes to zero position.
5.2.19	Switch OFF the ‘ON/OFF’ knob in OFF position.
5.2.20	Open the door of the vacuum oven, remove the sample and place it in dessicator till it attains the room temperature.
5.2.21	Close the door of the vacuum oven and switch OFF the mains.
5.2.22	Update the “Instrument/Equipment Usage Log Book” as per SOP “Calibration of Instruments and Equipments”.
5.3	Cleaning:
5.3.1	Switch OFF the mains of the vacuum oven.
5.3.2	Clean the inside and outside of vacuum oven with lint free cloth before and after use.
5.4	Calibration Procedure:
	Frequency:  Once in a year
5.4.1	Calibration is carried out by external agency as per SOP “Calibration of Instruments and Equipments”.
5.4.2	Refer Annexure for calibration test to be performed and acceptance criteria.   Sr. No. Tests Set value Acceptance Criteria (± 2%) 1. Temperature Verification 50oC ± 1oC 100oC ± 2oC 150oC ± 3oC 200o C ± 4oC 280oC ± 6oC   Sr. No. Tests Set value Acceptance Criteria 1. Pressure Verification of vacuum gauge 0 inHg ± 2 % – 5 inHg  ± 2 % – 10 inHg ± 2 % – 15 inHg ± 2 % – 20 inHg ± 2 % – 25 inHg ± 2 %
5.4.3	Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP and give requisition to QA department for calibration formats of instruments/equipments on the due date of calibration.
5.4.4	For issuance of calibration report refer SOP “Control of documents, Preparation, Approval, Issuance and Maintenance.
5.5	Preventive Maintenance
5.5.1	Perform the preventive maintenance as per Annexure.
5.5.2	If preventive maintenance activity is outsourced, the observations are to be transcribed in the Annexure, and external party certificate to be attached.
5.5.3	If any breakdown occurs, follow procedure as per SOP “Calibration of Instruments and Equipments”.

 

6. Definitions / Abbreviations :

• Definitions :
• Breakdown: Any activity leading to operation of instrument/equipment other than the set parameters or unusual sound or vibration observed in the instrument/equipment.
• Calibration: Tests performed to ensure that the instrument/equipment is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.
• Preventive Maintenance: Maintenance activity performed to ensure that the equipment will function smoothly and to avoid breakdowns. These activities are performed as per predefined frequency.

 

• Abbreviations :

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
A. R. No	Analytical Reference Number
No.	Number
oC	Degree Celsius
LOD	Loss on Drying
PM	Preventive Maintenance

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Rounding and Reporting of Test Results

 

1. Objective:

To lay down the procedure for Rounding and Reporting of Test Results in the Quality Control Department.

2. Scope:

This procedure is applicable for Rounding and Reporting of Test Results in the Quality Control Department.

 

3. Responsibility:

• Quality Control Department: To prepare and review the SOP. To follow the procedures laid down for Reporting of Test Result in Quality Control Department as per this SOP.
• Quality Assurance Department: To review and approve the SOP and Annexure.

 

4. Accountability:

Head Quality  Control Department, Head Quality  Assurance Department.

5. Procedure:

5.1	Significant figure determination :
5.1.1	Number of digit in a decimal or whole number, to be considered as significant or representative of the real value, specification limit or a result of a particular method, operation or process is called as significant figure.
5.1.2	In case there is no decimal place mentioned in specification, no decimal place should be reported.
5.1.3	In case the signification limit is expressed in decimal place the result obtained shall also be documented in decimal place, following the same number of decimal place.
5.1.4	The analytical result which is above 1.0 percent, the result shall be reported up to specification limit.
5.1.5	The analytical result which is equal to or below 1.0 percent, the result shall be reported up to two digit after decimal place.
5.1.6	The balance/equipment used for the process, must provide accuracy up to the last digit established by the current specification.
5.2	Rounding :
5.2.1	Abbreviate to one digit beyond the significant digit required.
5.2.2	Illustration of Rounding Numerical Values for Comparison with Requirements Compendial Requirement Unrounded Value Rounded Result Conforms Assay limit ≥ 98.0% 97.96% 98.0% yes 97.92% 97.9% No 97.95% 98.0% yes Assay limit ≤ 101.5% 101.55% 101.6% No 101.46% 101.5% yes 101.45% 101.5% yes Limit test ≤ 0.02% 0.025% 0.03% No 0.015% 0.02% yes 0.027% 0.03% No Limit test ≤ 3ppm 3.5 ppm 4 ppm No 3.4 ppm 3 ppm yes 2.5 ppm 3 ppm yes
5.3.3	( Example :- If that digit is 0,1,2,3,4 than the previous digit remain same and if that digit is 5,6,7,8,9 than the previous digit increase by one.). Specification Limit NMT 1.0 Specification Limit NMT 1.00 Calculated Result Rounded value     Calculated Result Rounded value 0.90 0.9 0.950 0.95 0.91 0.9 0.951 0.95 0.92 0.9 0.952 0.95 0.93 0.9 0.953 0.95 0.94 0.9 0.954 0.95 0.95 1.0 0.955 0.96 0.96 1.0 0.956 0.96 0.97 1.0 0.957 0.96 0.98 1.0 0.958 0.96 0.99 1.0 0.959 0.96
	Exceptions :
5.2.4	In case of reporting where the result becomes “zero” after rounded value, the result shall   be reported up to least calculated numeric value.
5.2.5	To calculate the Assay on anhydrous basis, moisture content/LOD shall be taken in to report calculated value as per specification. Specification Limit NMT 1.0 Calculated Result Rounded value 0.1446 0.1 0.1486 0.1 0.0652 0.1 0.0446 0.04 0.0057 0.01 0.0041 0.004 0.0026 0.003 0.0006 0.001 0.0002 0.0002     Parameter Specification limit Calculated result Reported value Value for assay calculation Loss on drying 1.0 0.3456 0.35 0.35 Water content 1.0 0.7327 0.73 0.73
5.2.6	In case specification limits containing two specification limits, first result  shall be reported more than one decimal of specification limit, the second result shall be considered as final result and will be reported after rounding off up to same decimal of specification limit. Parameter Specification limit Calculated result Reported value Assay 4.75 mg to 5.25 mg 5.0428 5.043 95.0 % to 105.0 % 100.856 100.9
5.2.7	In case reported result is close to specification limit and after rounded value the results is same as specification limit, the result shall be reported more than one decimal of specification limit. e.g. In case, the specification limit is 15.0 and the observed result without rounded value is within 14.95 to 15.04 than the result shall be reported more than one decimal of specification limit.

 

6. Definitions / Abbreviations :

• Definitions :
• Interpretation: Analytical results observed in the laboratory (or calculated from experimental measurements) are compared with stated acceptance criteria to determine whether the article conforms to compendia requirements.

The reported value, which often is a summary value for several             individual determinations, is compared with the acceptance criteria.      The reportable value is the end result of a completed                      measurement procedure, as documented.

Where acceptance criteria are expressed numerically herein through specification of an upper and / or lower limit, but no value outside the limit(s). Acceptance criteria are considered significant to the last digit shown.

• Rounding Rules: The observed or calculated values shall be rounded off to the number of decimal places that is in agreement with the limit expressions for the reportable value have been completed. Intermediate calculations (e.g. slope for linearity) may be rounded for reporting purpose, but the original (not rounded) value shall be used for any additional required calculations. Acceptance criteria are fixed numbers and are not rounded.

 

• Abbreviations:

Abbreviation	Expansion
QC	Quality Control
QA	Quality Assurance
e.g.	Example
No.	Number
NMT	Not more than
LOD	Loss on drying
%	Percent
USP	United State of Pharmacopoeia

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Operation and Calibration of Stop Watch

1. Objective:

To lay down the procedure for Operation and Calibration of Stop Watch.

2. Scope:

This SOP is applicable for Operation and Calibration of Stop Watch located in Quality Control Laboratory .

  

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for operation, cleaning and calibration of Stop Watch as per this SOP.
• Quality Assurance Department: To review and approve the SOP and Annexures.

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

5. Procedure:

 

5.1	Operation:
5.1.1	The stopwatch consist of  two  dials,  Big dial shows the time in ‘seconds’ and small dial shows time in ‘minutes’.
5.1.2	Further one second divided in 10 parts i.e. 1 second = 1/10 parts. Hence time can be measured as min;sec:1/10 parts of second. Example: Small dial on 2 and big dial on  9th line after crossing 10 then time can be measured as below:- 02 minutes: 10 seconds :1/9 parts of second or 02 minutes: 10 second : 900 milli seconds. 1 Second = 1000 milli second, one line on stop watch = 100 milli seconds.
5.1.3	One key is provided on the top of the stopwatch to start and stop the counts.
5.1.4	If  the  needle  of  both  dials  are  not  vertically  align  to  ‘ZERO’  press the key twice to bring both the dials to zero position.
5.1.5	To start the stop watch, press the key once and the clock starts.
5.1.6	To stop the stop watch once again press the key of the stopwatch and stop the watch.
5.1.7	To reset the time to ‘ZERO’, press the key twice.
5.2	Calibration Procedure:
	Frequency:  Once in a year
5.2.1	Calibration is carried out by external agency as per SOP “Calibration of Instruments and Equipments”.
5.2.2	Refer Annexure for calibration test to be performed and acceptance criteria. Sr. No. Tests Set Value min : sec : 1/10 sec Acceptance Criteria (± 1%) (min : sec : 1/10 sec or  min : sec : milli seconds ) Acceptance Criteria Range ± 1% 1. Time Verification 01 : 00 : 00 ± 00:00:06 or 00:00:600 00 min : 59 sec : 400 milli sec To 00 min : 06 sec : 600 milli sec 03 : 00 : 00  ± 00:01:08 or 00:01:800 2 min : 58 sec : 200 milli sec To 3 min : 01 sec  : 800 milli sec 06 : 00 : 00 ± 00: 03:06 or 00:03:600 5 min : 56 sec : 400 milli sec To 6 min : 03 sec  : 600 milli sec 09 : 00 : 00 ± 00:05:04 or 00:05:400 8 min : 54 sec : 600 milli sec To 9 min : 05 sec  :400 milli sec 12 : 00 : 00 ± 00: 07:02 or 00: 07:200 11 min : 52 sec : 800 milli sec To 12 min : 07 sec  :200 milli sec 15 : 00 : 00 ± 00:09:00 or 00:09:000 14 min : 51 sec : 000 milli sec To 15 min : 09 sec  : 000 milli sec
5.2.3	Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP and give requisition to QA department for calibration formats of instruments/equipments on the due date of calibration.
5.2.4	For issuance of calibration report refer QA SOP.
5.2.5	If any breakdown occurs, follow procedure as per SOP “Calibration of Instruments and Equipments”.

 

6. Definitions / Abbreviations :

• Definitions :
• Abbreviations :

Abbreviation	Expansion
A. R. No	Analytical Reference Number
No.	Number

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Operation, Cleaning and Calibration of TLC UV Cabinet

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of TLC UV Cabinet.

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of TLC UV Cabinet located in Quality Control Laboratory.

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of TLC UV Cabinet as per this SOP.
• Engineering Department: To carry out preventive maintenance as per schedule and procedure defined.
• Quality Assurance Department: To review and approve the SOP and Annexures.

 

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

 

5. Procedure:

 

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the TLC UV Cabinet is fixed in the socket properly.
5.1.2	Wear personal protective equipments such as hand gloves during operation of equipment.
5.1.3	Ensure that the ON/OFF switch is working properly by switching “ON” the TLC UV Cabinet.
5.2	Operation:
5.2.1	Check the validity of calibration before starting any operations.
5.2.2	Ensure that the equipment should be cleaned before operation.
5.2.3	Switch ‘ON ‘the main electrical switch.
5.2.4	Open the door of ultra violet cabinet.
5.2.5	Keep the thin layer chromatography plate inside the cabinet.
5.2.6	UV cabinet is suitable for wavelength 254 nm and 365 nm.
5.2.7	Switch ON the required UV lamp, as per standard testing procedure.
5.2.8	View the TLC plate and check the results obtained.
5.2.9	After completion, open the door of ultra violet cabinet and remove TLC plate.
5.2.10	Switch OFF the UV lamp and switch OFF the main electrical switch.
5.2.11	Update the “Instrument/Equipment Usage Log Book” as per SOP.

 

5.3	Cleaning Procedure:
5.3.1	Clean the instrument with lint free cloth inside and outside before and after completion of the test.
5.4	Calibration Procedure:
	Frequency:  Once in a Year or after carrying out any major maintenance work.
5.4.1	Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP number and give requisition to QA department for calibration formats of instruments on the due date of calibration.
5.4.2	For issuance of calibration report refer QA SOP.
5.4.3	Perform the calibration of instrument as per Annexure  and procedure mentioned below.
5.4.4	Preparation  of  95%  ethanol: Add  10 ml  purified water  to 200 ml   volumetric  flask  and  make  up  the  volume  with ethanol and mix.
5.4.5	Preparation  of  0.04% w/v  of  Sodium  Salicylate  in  95%  ethanol: Weigh  accurately  40 mg  of  Sodium  Salicylate  in  clean  and dry  100 ml  volumetric  flask  add  about 50 ml  of  95%  ethanol,  shake  to  dissolve and   make  up  the  volume  to  100 ml   with  95%  ethanol and mix.
5.4.6	Preparation of 0.2% w/v  of  Sodium  Salicylate  in  95%  ethanol: Weigh accurately 100 mg of Sodium  Salicylate  in  clean  and dry  50 ml  volumetric  flask  add  about 30 ml  of  95%  ethanol,  shake  to  dissolve and  make  up  the  volume  to  50 ml   with  95%  ethanol and mix.
5.4.7	Draw a line on the Silica gel 60 F254 and Silica gel 60 TLC plate in pencil at 1.5 cm from the bottom of the plate.
5.4.8	Spot with glass syringe 5 micro litre of 0.04%w/v solution on Silica gel 60 F254 and 0.2%w/v solution on Silica gel 60 TLC plate of sodium salicylate on the line drawn of TLC plate.
5.4.9	Put identification mark for the spots and allow the spots to dry in air.
5.4.10	Examine the plate at 254 nm for 0.04%w/v spot and 365 nm for 0.2%w/v spot.
5.4.11	Follow the same procedure from point no. 5.2.2 to 5.2.10.
5.4.12	Enter the details in calibration report. Ensure that the results obtained, comply with the acceptance criteria. Sr. No. Standards Acceptance Criteria Complies / Does Not Complies 1. 0.04% w/v  of  Sodium  Salicylate  in  95%  ethanol The UV light at about 254 nm should reveal a standard spot of Sodium Salicylate with a diameter of about 5 mm on a TLC plate.   2. 0.2% w/v  of  Sodium  Salicylate  in  95%  ethanol The UV light at about 365 nm should be capable of revealing standard spot of Sodium Salicylate with a diameter of about 5 mm on a TLC plate.
5.4.13	Update the “Instrument/Equipment Usage Log Book”, “Annual Calibration Schedule” and “Monthly Calibration Schedule” as per “Calibration of Instruments and Equipments”.
5.4.14	Affix the “Calibration Status Label” on the Instrument as per SOP “Calibration of Instruments and Equipments”.
5.4.15	If calibration activity is outsourced, the values are to be transcribed in the Annexure and external party certificate to be attached.
5.4.16	If any breakdown occurs, follow procedure as per SOP number “Calibration of Instruments and Equipments”.

 

6. Definitions / Abbreviations :

 

• Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
0C	Degree Celsius
No.	Number
w/v	Weight by volume
nm	nanometer
TLC	Thin Layer Chromatography
UV	Ultra violet

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Operation, Cleaning and Calibration of  Magnetic Stirrer

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Magnetic Stirrer.

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Magnetic Stirrer located in Quality Control Laboratory.

 

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for Operation, Cleaning and Calibration of Magnetic Stirrer as per this SOP.
• Engineering Department: To carry out preventive maintenance as per schedule and procedure defined.
• Quality Assurance Department: To review and approve the SOP and Annexures.

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

5. Procedure:

 

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the centrifuge apparatus is fixed in the socket properly.
5.1.2	Ensure that the ON/OFF switch is working properly by switching “ON Magnetic Stirrer.
5.1.3	Wear personal protective equipments such as safety glasses, hand gloves during operation of equipment.
5.1.4	Before instrument is put ON check that the speed  and  heat   control  knobs  are in  “0”  position  and  the  corresponding  switches  are  in  OFF  position.
5.2	Operation:
5.2.1	Check the validity of Calibration before starting any operations.
5.2.2	Switch ON the main switch of the equipment and then the ON/OFF switch on the equipment.
5.2.3	The orange light indicator on the equipment will glow.
5.2.4	Insert the magnetic bid slowly in the sample solution to be stirred.
5.2.5	Place the sample solution on the equipment at room temperature or at specified temperature on the top flat surface of the equipment approximately in the centre.
5.2.6	Set the required speed by rotating ‘SPEED’ knob.
5.2.7	To increase the speed of stirring, rotate the ‘SPEED’ knob in clockwise direction and to decrease the speed of stirring, rotate the ‘SPEED’ knob in anti-clockwise direction.
5.2.8	If heating is required then set the required temperature on the ‘HEAT’ knob. The red light indicator on the equipment will glow.
5.2.9	Ensure that there is no spillage of sample solution on the equipment during speed adjustment.
5.2.10	After stirring is completed, remove the sample solution from the magnetic stirrer.
5.2.11	Turn off ‘HEAT’ knob and ‘SPEED’ knob by rotating them in anticlockwise  direction and bring at “0” position.
5.2.12	Switch OFF the ON/OFF switch on the equipment and the main switch.
5.3	Cleaning Procedure:
5.3.1	Disconnect the equipment from the switch.
5.3.2	Clean the top flat surface with wet cloth to remove debris and finally clean with lint free dry cloth.
5.3.3	Clean the equipment after use.
5.4	Calibration Procedure:
	Frequency:  Once in a year
5.4.1	Calibration is carried out by external agency as per SOP.
5.4.2	Refer Annexure for calibration test to be performed and acceptance criteria. Sr. No. Tests Set value Acceptance Criteria 1. Temperature Verification 30oC ±3oC 60oC ±3oC 90oC ±3oC
5.4.3	Generate the A. R. No. on the “Instrument/Equipment Calibration Register”
5.4.4	For issuance of calibration report refer QA SOP.
5.4.5	If any breakdown occurs, follow procedure as per SOP

 

6. Definitions / Abbreviations :

• Definitions :
• Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance
A. R. No.	Analytical Reference Number

 

*Note – Ready to use SOP available in “DOWNLOAD” Section.

 

SOP Title: Operation, Cleaning and Calibration of Water Bath

 

1. Objective:

To lay down the procedure for Operation, Cleaning and Calibration of Water Bath.

 

2. Scope:

This SOP is applicable for Operation, Cleaning and Calibration of Water Bath located in Quality Control Laboratory.

3. Responsibility:

• Quality Control: To prepare and review the SOP. To follow the procedures laid down for operation, cleaning and calibration of Water Bath as per this SOP.
• Engineering Department: To carry out preventive maintenance as per schedule and procedure defined.
• Quality Assurance Department: To review and approve the SOP and Annexures.

  

4. Accountability:

Head Quality Control Department, Head Quality Assurance Department

5. Procedure:

 

5.1	Safety Precautions/Instructions:
5.1.1	Ensure all the electrical connections are properly earthed. Ensure the power plug of the water bath is fixed in the socket properly.
5.1.2	Wear personal protective equipments such as safety glasses, hand gloves during operation of instrument.
5.1.3	Ensure that the ON/OFF switch is working properly by switching “ON” the water bath.
5.2	Operation:
5.2.1	Check the validity of calibration before starting any operations.
5.2.2	Ensure that the equipment should be cleaned before operation.
5.2.3	Fill the water bath with sufficient purified water (i.e.  2/3 of its capacity).
5.2.4	Switch ON the ON/OFF knob provided on the water bath.
5.2.5	Close all the rings which will facilitate the boiling faster.
5.2.6	The  lid  has  got  six  holes  which  can  be  closed  and  opened  by  means  of  ring.
5.2.7	Maintain the required temperature of the water bath with the help of temperature knob provided on the water bath.
5.2.8	Red light on the “Thermostat indicator” and “Line indicator” will glow when the required temperature is reached.
5.2.9	Ensure that the heater of the bath is immersed below the water level.
5.2.10	Open the rings and place the sample on the water bath for heating.
5.2.11	Refill the purified water in the water bath if the water level is decreased.
5.2.12	Use only purified water to refill water bath.
5.2.13	Switch OFF the mains of the instrument after heating is over.
5.3	Cleaning Procedure:
5.3.1	Drain the purified water and clean the water bath thrice in a week.
5.4	Calibration Procedure:
	Frequency:  Once in a year
5.4.1	Calibration is carried out by external agency as per SOP
5.4.2	Refer Annexure for calibration test to be performed and acceptance criteria. Sr. No. Tests Set value Acceptance Criteria 1.   Temperature Verification 50oC ±5oC 100oC ±5oC
5.4.3	Generate the A. R. No. on the “Instrument/Equipment Calibration Register” as per SOP number and give requisition to QA department for calibration formats of instruments on the due date of calibration.
5.4.4	For issuance of calibration report refer QA SOP.
5.4.5	If any breakdown occurs, follow procedure as per SOP “Calibration of Instruments and Equipments”.

 

 

6. Definitions / Abbreviations:

• Definitions:
• Breakdown: Any activity leading to operation of instrument/equipment other than the set parameters and/ or unusual sound or vibration observed in the instrument/equipment.
• Calibration: Tests performed to ensure that the instrument/equipment is functioning as per set parameters. These tests are performed as per predefined frequency and also after any major repair or replacement of parts.

  

• Abbreviations:

Abbreviation	Expansion
SOP	Standard Operating Procedure
QC	Quality Control
QA	Quality Assurance

 

No.	Number
A. R. No.	Analytical Reference Number
i.e.	That is

  

*Note – Ready to use SOP available in “DOWNLOAD” Section.