SOPs

Calibration of Polarimeter , Purpose :

Calibration of Polarimeter , The purpose of this SOP is to describe the operation, calibration and cleaning of Polarimeter (Model: Rudolph, AUTOPOL IV) used for the determination of the optical rotation in quality control laboratory at XX Pharmaceuticals Ltd.

Calibration of Polarimeter , Scope :

This procedure describes the application of Polarimetric determinations of optical rotation of raw materials (active & excipients), intermediates and drug product etc. in the quality control laboratory of general block at XX Pharmaceuticals Limited.

Definitions/Abbreviation:

Standard Operating Procedure (SOP): A written authorized procedure, which gives instructions for performing operations.

Responsibilities:

The roles and responsibility is as follows:

Officer/Executive/ Sr. Executive, Quality Control

[][]To ensure that this procedure is followed.
[][]To maintain the records properly as per SOP.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]Arrange training on the SOP to all concerned personnel.
[][]To ensure implementation of the SOP after training.
[][]Schedule calibration of the instrument at the defined intervals.

Head of Quality Assurance

[][]Approval of the SOP.
[][]To ensure overall implementation of this SOP.

Procedure:

Precaution(s):

[][]The equipment should not be set near to room heating equipment or direct sunlight.
[][]Not to spill water or sample on the main body of the instrument.
[][]Use the instrument at an ambient temperature of 5°C to 35°C and RH lower than 90%.
[][]Disconnect the power supply before moving or cleaning of the instrument.

General procedure:

Polarimetry is used to measure the effect that an optically active molecule in solution has on polarized light. Specific Optical Rotation is defined as an Observed Optical Rotation, measured at a specific wavelength and temperature, corrected for the path length of the optical cell and concentration of the solution. The sample is normally presented to the Polarimeter as a solution, contained in a thermally controlled optical cell. A beam of polarised light is then passed through this cell and any rotation of this polarised light is measured via a detector

Reagent quality:

[][]If water is used in the preparation of sample solutions, it must be purified by distillation or deionization process.

Instrument equilibration:

[][]The instrument must be equilibrated before use. The polarimeter (set to required wavelength), must be switched on for a minimum of at least 30 minutes before use.

Preparation and storage of samples:

[][]Sample solutions must be prepared in accordance with the analytical method. Sample solutions must be discarded at the end of the working day, unless solution stability has been demonstrated.

Preparation for measurement:

[][]Connect the power cable and turn the Polarimeter ON.
[][]Press Menu to select the measurement settings.
[][]Press Scale button and select the specific optical rotation.
[][]Press Temperature correction and select off mode.
[][]Press Statistics button and select on (n-1).
[][]Exit from the Menu by pressing Exit button.
[][]Fill the Polarimeter cell with sample blank and place it into the sample chamber.
[][]Press Zero button for zeroing the sample blank.
[][]Then remove the cell from the sample chamber and discard the sample blank and rinse the cell with the sample.
[][]Fill the cell with the sample and press Measure.
[][]Type the Lot ID and press Enter.
[][]Input the sample weight and press Enter.
[][]Type the Sample Name again presses Enter.
[][]When the measurement completed, press Print Option to the results.
[][]Remove the polarimeter cell from the chamber.

Calculation of Specific Optical Rotation:
The specific optical rotation of a sample is calculated as follows:

A=αx100/I x c

Where,
[α] = Specific Rotation at Temperature, T°C and wavelength, λ nm
Α = Observed Rotation in degrees (°)
l = Path length in decimeters (dm)
c = Concentration of analyte (g /100 ml)

Cleaning of the instrument:

Cleaning of the cell:

[][]The cell must be cleaned after use. Thoroughly rinse the cell with the same solvent used for the sample, then rinse with purified water followed by methanol.

Cleaning of the sample compartment:

[][]The sample compartment should be cleaned immediately if anything is spilled into it in order to preserve the black matt finish and prevent corrosion or contamination.
[][]Use a soft cloth impregnated with a soapy solution to rub away any foreign material.
[][]Use a clean soft cloth dampened with water to rinse the cleaned surfaces thoroughly.
[][]Finally dry with a lint free cloth or tissue.

Calibration check with sucrose solution:

[][]Frequency: Yearly
[][]The check consists of determining the specific optical rotation of sucrose solution, using 20% w/v solutions. The method is detailed below. All results and calculations must be recorded on the calibration information sheet for Polarimeter.

Procedure:

Apparatus:

1dm Polarimeter tube.
Thermostat bath 20°C ± 0.2°C.

Reagent:

Sucrose Solution

Loss on Drying:

[][]Accurately weigh approximately 1g of sucrose into a clean dry weighing bottle that has previously been dried at 105°C, cooled in a dessicator for half an hour and weighed.
Dry in an oven at 105°C±2°C for 2 hours, then cool in a desiccator and reweigh.
[][]Calculate the loss in weight as a percentage and record the result on the polarimeter calibration check sheet using the following calculation:

LOD=Weight loss(g)/Weight taken(g)x100

Determination of Specific Optical Rotation at 20°C:

[][]Accurately weigh about 20 g of Sucrose into three separate 100 ml volumetric flasks. Dissolve in 80 ml of water and dilute to 100 ml with water.
[][]Zero the polarimeter using purified water in the 1dm polarimeter tube.
[][]Determine the optical rotation of each solution at 20°C ± 0.5°C in the 1dm tube.
[][]Record and calculate the results obtained for each solution on the polarimeter calibration check sheet using the following calculation:

A=αx100x100/I x c x(100-%LOD)

Where,
[α] = Specific Rotation at Temperature, 20°C and wavelength, 589.3 nm
A = Observed Rotation in degrees (°)
l = Path length in decimeters (dm)
c = Concentration of analyte (g/100 ml)
The specific optical rotation for each solution should be in the range +66.3° to +67.0° (reference the current European Pharmacopoeia).

Calibration check with Quartz Control Plate:

Frequency: Yearly
Apparatus:
Quartz Control Plate
[][]Check that the instrument and the Quartz Control Plate are at room temperature and that the instrument has been on for at least 10 minutes with the Quartz control Plate resting in the back of the sample chamber.
[][]Press Menu button to select Measurement Settings.
[][]Press Scale to select Optical Rotation.
[][]Press Temperature Correction and select Quartz.
[][]Press Statistics and select on (n-1).
[][]Press Exit button to return Manu.
[][]Press zero for zeroing the instrument.
[][]Place the Quartz Control Plate in to the sample chamber.
[][]Press Measure to measure the Quartz Control Plate.
[][]Type the Lot ID and press Enter.
[][]Type the Sample ID and press the Enter.
[][]Type the Sample Name and press the Enter.
[][]When the measurement completed press Print/Send key to print the measurement results.
[][]Remove the Quartz Control Plate form the chamber and return it to its container.
[][]Review the measurement results. Verify the Quartz Control Plate measure is within the tolerance specification.

Annexure:

[][]Annexure-I: Calibration Information Sheet for Polarimeter with Sucrose Solution
[][]Annexure-II: Calibration Information Sheet for Polarimeter with Quartz Control Plate
[][]Annexure-III: Log Book for Polarimeter

Water Purification System, Purpose :

Water Purification System, This purpose of this SOP is to describe the operation of Water Purification System (Model: Barnstead Easy Pure II 7136).

Water Purification System, Scope :

This procedure is applicable for Water Purification System (Model: Barnstead Easy Pure II 7136), installed in the quality control laboratory  of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

[][]SOP: Standard Operating Procedure
[][]QC: Quality Control

Responsibilities:

The roles and responsibility is as follows:

Executive/ Sr. Executive, QC

[][]Ensure that the instructions of this procedure are correctly followed

Manager, Quality Control

[][]Ensure that this procedure is kept up to date.
[][]Ensure appropriate personnel from the section are trained on this procedure.
[][]Ensure the instrument safety information is maintained as per manual.
[][]Ensure that the water system is ready for use.
[][]Ensure that the water system is sanitized properly at due time.
[][]Confirm that SOP is technically sound and reflects the required working practices.

Head of Quality Assurance

[][]Approval of the SOP
[][]To ensure the overall implementation of the SOP.

Annexure:

N/A

Procedure:

General precaution:

[][]Use a properly grounded electrical outlet of correct voltage and current handling capacity.
[][]Do not locate your EASY pure II directly over equipment that requires electrical service. Routine maintenance of this unit may involve water spillage and subsequent electrical shock hazard, if improperly located.
[][]Replace fuses only with the same type and rating of fuse.
[][]Do not assemble water lines or remove cartridges where spilled water could contact equipment that requires electrical service. Electrical shock could result.
[][]Disconnect from the power supply prior to maintenance and servicing.
[][]Does not use in the presence of flammable or combustible materials; fire or explosion may result. This device contains components which may ignite such materials.
[][]Do not use in the presence of highly corrosive substances such as bleach or acid baths; fire may result.
[][]This device is to be used with water feeds only. Cleaning agents must be used in compliance with instructions in this manual. Failure to comply could result in explosion and personal injury.
[][]Avoid splashing cleaning solutions on clothing or skin.
[][]Ensure all piping connections are tight to avoid chemical leakage.
[][]Ensure adequate ventilation.
[][]Carefully follow manufacturer’s safety instructions on labels of chemical containers and material safety data sheets.
[][]Depressurize system prior to opening cartridge access door or removing top cover.
[][]This unit may be equipped with an ultraviolet lamp. Ultraviolet radiation is harmful to the eyes and skin. Do not observe the lamp directly.

Operation:

[][]Turn main power on at power entry module.
[][]Switch on the Water Purification System located on the upper left side of the instrument.
[][]The Barnstead EASY pure II 7136 control panel incorporates three switches ‘STOP’,’STAND BY’, ‘START’ and a digital display.
[][]Connect the instrument with purified water supply by feed water tubing.
[][]Pressing the ‘START’ when the unit is in either the stop or standby mode will put the instrument into Run Mode.
[][]When the display will show the resistivity 18.2 MΩ-cm at 25°C, the water can be taken from the instrument for different purposes by pushing down the Draw-off Valve Lever.
[][]To reserve the RO water for further use, connect the Water purification system with Barnstead 30 liter Storage reservoir with water inlet tubing.
[][]Push down the Draw-off Valve Lever to transfer the RO water from Water purification system to Barnstead 30 liter Storage reservoir by water inlet tubing.
[][]Use the water from the Barnstead 30 liter Storage reservoir for different purposes by Draw Off Valve.
[][]Use Product water outlet to drain the RO water if necessary.
[][]Finally power off Water Purification System.
[][]Unplug the instrument from the main power connection.

Temperature Monitoring of Refrigerator, Purpose :

Temperature Monitoring of Refrigerator, This purpose of this SOP is to describe the operation of Refrigerator for preservation of reference standard and others temperature sensitive materials in Quality Control Laboratory and Microbiology Laboratory.

Temperature Monitoring of Refrigerator, Scope :

This procedure is applicable for the preservation of reference standard and others temperature sensitive materials into Refrigerator in Quality Control Laboratory and Microbiology Laboratory of XX Pharmaceuticals Ltd.

Definitions / Abbreviation:

[][]SOP: Standard Operating Procedure
[][]QC: Quality Control

Responsibilities:

The roles and responsibility is as follows:

Executive, QC

[][]Ensure that the instructions of this procedure are correctly followed.

Manager, Quality Control

[][]Ensure that this procedure is kept up to date.
[][]Ensure that the materials are preserved at defined temperature.
[][]Ensure appropriate personnel from the section are trained on this procedure.
[][]Confirm that SOP is technically sound and reflects the required working practices.

Head of Quality Assurance

[][]To ensure the overall implementation of the SOP.
[][]Approval of the SOP.

Procedure:

Precaution(s):

[][]Do not store articles on the top of the refrigerator.
[][]Do not put a container filled with water on the refrigerator. If spilled, there is a risk of fire or electric shock.
[][]Do not insert your hands into the bottom area under the refrigerator.
[][]Do not overfill the refrigerator with the material.
[][]Do not touch the inside walls of the freezer or products stored in the freezer with wet hands.
[][]Never put fingers or other objects into the water dispenser hole, ice chute and ice maker bucket.
[][]Do not spray inflammable gas near the refrigerator.
[][]Do not store volatile or flammable substances in the refrigerator.
[][]Do not reset the temperature without approval.

Operation:

[][]Connect and switch on the power of Refrigerator.
[][]Set the temperature within 2-8°C.
[][]After stable of the temperature, keep the items into the chamber at specific area.
[][]Check that the chamber temperature is within the setting value by standard calibrated thermometer.
[][]Record the temperature in Temperature log sheet for refrigerator (Annexure-I).
[][]Read the label of the materials to confirm the storage temperature.
[][]Store materials in refrigerator as per label.
[][]Minimize the door opening and closing to protect the chamber temperature increasing.

Cleaning procedure:

[][]Clean the inside walls and accessories with a mild detergent and then wipe dry with a soft cloth.
[][]Wipe the digital panel and display panel with a clean, soft cloth.
[][]Spray water onto the cleaning cloth instead of spraying directly on the outer surface of the refrigerator.
[][]The doors, handles and cabinet surfaces should be cleaned with a mild detergent and then wiped dry with a soft cloth.
[][]Keep the door seals free of grit or grime by cleaning the doors with a mild detergent and damp cloth then wipe with dry, clean and soft cloth.

Maintenance:

[][]If Refrigerator shows any mechanical, electrical or any others problem, inform to the supplier or Engineering Department for maintenance.

Annexure:

Annexure-I: Temperature Log Sheet for Refrigerator.

Vacuum Drying Oven Calibration, Purpose :

Vacuum Drying Oven Calibration, The purpose of this SOP is to describe the operation, calibration and cleaning of Vacuum Drying Oven (Model: VO 200S) used for drying of the raw materials in the quality control laboratory at XX Pharmaceuticals Ltd.

Scope :

Vacuum Drying Oven Calibration, This procedure is applicable for the Vacuum Drying Oven, installed in the quality control laboratory for general block at XX Pharmaceuticals Limited.

Definitions/Abbreviation:

[][]QC: Quality Control

Responsibilities:

The roles and responsibility is as follows:

Officer/Executive/Sr. Executive, Quality Control

[][]To ensure that this procedure is followed.
[][]To maintain the records properly as per SOP.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]Arrange training on the SOP to all concerned personnel.
[][]To ensure implementation of the SOP after training.
[][]Schedule calibration of the instrument at the defined intervals.

Head of Quality Assurance

[][]Approval of the SOP.
[][]To ensure overall implementation of the SOP.

Annexure:

[][]Annexure-I : Log Book for Vacuum Drying Oven
[][]Annexure-II: Calibration Record of Vacuum Drying Oven

Procedure:

Precaution(s):

[][]Wear the temperature resistance gloves to keep or remove materials from Vacuum Drying Oven.

Operation:

[][]Operation in normal mode
[][]Switch on the main switch of the Vacuum Drying Oven.
[][]Open the door and place the samples into the Vacuum Drying Oven.
[][]Press push/turn control key to put on the main power switch in front of the Vacuum Drying Oven. The Vacuum drying oven will start in normal mode with the display of timer, the chamber temperature, alarm temperature (red color indication).
[][]Select operating mode “Normal operation”. Press and hold on the SET key (approx. 3 sec) until the current operating option is flashing.
[][]Select temperature set point. Hold down the SET key and use the push/turn control key clockwise or anticlockwise to select the required temperature set point.
[][]After the SET key has been released the Vacuum drying oven briefly flashes the temperature set point. Set the temperature as per requirement. Heating is indicated by the orange heater symbol.
[][]Select the fan speed. Turn the push/turn control clockwise until the fan symbol is flashing. While the holding down the SET key. Use the push/turn control to set 50% fan speed.
[][]Select the alarm temperature. Turn the push/turn control clockwise until the monitor temperature display is flashing. Hold down the SET key and use the push/turn control to set the alarm temperature.
[][][][]The display then changes to the actual current temperature and starts to the setting temperature. The temperature will be automatically increased at setting temperature and display the setting temperature digitally.
[][]Observe the display temperature until stable position.
[][]At the end of drying, remove dried materials from Vacuum drying oven.

Operation in cyclic mode :

[][]Press push/turn control key to put on the main power switch in front of the instrument. The Vacuum drying oven will start in normal mode with the display of timer, the chamber temperature and alarm temperature (red color indication).
[][]Hold down SET key and turn the push/turn control key at the clockwise or anti clockwise for setting date, local time, operating temperature, alarm temperature. After setting, SET key will be released the display briefly flashes the set point.
[][]Press and hold down SET key to select the program and rotate push/turn control key at clockwise and select “Ramp timer” mode.
[][]Hold down the SET key and set the work day’s group using the push/turn control. Press push/turn control to select the ramp segment “t1” If the day is not required, it will be off position.
[][]Hold down the SET key and set the time using push/turn control.
[][]Select the ramp segment “t2” using the push/turn control. Hold down the SET key and using the push/turn control set the time.
[][]Turn push/turn control clockwise until the temperature display is flashing. Hold down the SET key and set the required temperature set point using push/turn control.
[][]Select the set point waiting time. Hold down the SET key and set on using the push/turn control. After the SET key has been released the function for set point waiting time is stored.
[][]Select hold time “t3”. Hold down the SET key and set the time using the push/turn control.
[][]Select the cooling time “t4”. Hold down the SET key and set time using push/turn control.
[][]Select program repeats “loop”. Hold down the SET key and set 2 for repeats using the push/turn control.
[][]Select the fan speed to set the air changes. Turn the push/turn control clockwise until the fan
[][]symbol is flashing. Hold down the SET key and set fan speed 50% suing the push/turn control.
[][]Select the alarm temperature. Turn the push/turn control clockwise until the monitor temperature display is flashing. Hold down the SET key and set the alarm temperature using the push/turn control.
[][]Turn the push/turn control at clockwise until the fan symbol flashing to move the air slider opens and closes the air valve to control the supply and discharge of air.
[][]Start the program. Turn the push/turn control clockwise until the stop symbol ▀ is flashing. Hold down the SET key and select start ► using the push/turn control. On releasing the SET key the program
starts to run.

Vacuum pump operation:

[][]After setting the drying temperature, switch on the vacuum pump.
[][]After completion of vacuum drying, turn the push/turn control knob until the Open door option is displayed. Press SET key to release the vacuum. Switch off the vacuum pump. Then the door of Vacuum drying oven can be opened.

Calibration:

[][]Frequency: Perform calibration of the instrument once in a year or if the system has been moved, serviced or a malfunction is suspected.

Temperature Calibration

[][]Insert the standard thermometer or thermocouples into the chamber.
[][]Press and hold down SET key until the normal mode light blinking.
[][]Turn push/turn control key clock wise to reach SETUP light.
[][]Select Calibration to rotate push/turn control key.
[][]Use three calibration temperatures as below :
CAL.1 : 30°C
CAL.2 : 100°C
CAL.3 : 200°C
[][]Select the required calibration temperature in SETUP key and set the corresponding calibration correction to 0.0°C.
[][]Measure the deviation from the selected calibration temperature under the steady conditions, using a reference instrument.
[][]Set the calibration correction in SETUP key. If the measured reference temperature is too low, the calibration correction setting is negative sign.
[][]Adjust the temperature if require from adjusting value of calibration temperature (CAL). The correction value should not more than ±0.50C.
[][]Carry out the check measurement using the reference thermometer.
[][]Carry out others two calibration temperatures in the same manner.
[][]Measure the vacuum pressure and input the data on calibration record.
[][]In case of internal calibration, record calibration data in Vacuum drying Oven Calibration Record, as per Annexure-II.

Calibration of pressure for vacuum chamber

[][]Calibrate pressure of vacuum chamber by calibrated multi-functional calibrator using five calibration pressures as below :
CAL.1 : 10 mbar
CAL.2 : 50 mbar
CAL.3 : 100 mbar
CAL.4 : 500 mbar
CAL.5 : 900 mbar
[][]Record calibration data in Vacuum drying Oven Calibration Record, as per Annexure-II.
[][]Cleaning of Vacuum Drying Oven :
[][]Clean the inner part of Vacuum drying oven with a cleaned cloth.
[][]Disinfect the inner surfaces with 70% IPA or ethanol when required.
[][]Clean the outer surfaces with dry cleaned cloth.

Maintenance :

[][]If Vacuum drying oven shows any mechanical, electrical or any others problem, inform to supplier or Engineering Department for maintenance.
[][]After maintenance, recalibrate the Vacuum drying oven.

Muffle furnace, Purpose :

Muffle furnace, The purpose of this SOP (Standard Operating procedure) is to describe the operation and maintenance of Muffle furnace for the determination of Ash, Sulphated ash/residue on ignition and Loss on ignition and other tests (which required higher temperatures and furnace) of the materials under specified condition.

Muffle furnace, Scope :

This procedure is applicable for Muffle furnace (Model: Carbolite, CWF1200), installed in the quality control laboratory for general block of  XX  Pharmaceuticals Limited.

Definitions:

SOP: Standard Operating Procedure.
QC: Quality Control.

Responsibilities:

The roles and responsibility is as follows:

Executive, QC

[][]To ensure that the instructions of this procedure are correctly followed.
[][]To ensure cleaning of Muffle Furnace safety rules.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.

Head of Quality Assurance

[][]To ensure the overall implementation of the SOP.
[][]Approval of the SOP.

Procedure:

Precaution(s):

[][]Do not open the door during operation of Muffle Furnace.
[][]Always wear vinyl/heat resistance gloves to put and to remove the crucible from the furnace using the long tongs.
[][]Ensure that heating elements are isolated from the door and the inner surface of the chamber.

Operation:

[][]Connect the instrument to the main power supply.
[][]Switch ‘ON’ the mains.
[][]Press “■” key button.
[][]Display will show SPºC.
[][]Use “▲” up or “▼” down arrow key button to set the required temperature.
[][]Press “■” key button.
[][]Then display will show SPrr.
[][]Use “▲” up or “▼” down arrow key button to set ram temperature.
[][]Press “■” key button.
[][]Display will show t S.
[][]Use “▲” up or “▼” down arrow key button to set the time (Hr:Min) by a single press.
[][]Machine will automatically increase the temperature according to ramp temperature.
[][]After reach the set temperature, machine will hold that temperature according to set time.
[][]Then display will show ‘End’.
[][]Switch OFF the instrument and mains.

Cleaning procedure:

[][]Insure that main power switch of the equipment is “OFF” position and at room temperature.
[][]Clean the outer surface of the furnace with a damp cloth.
[][]Clean the inner surfaces with dry cleaned cloth or soft nylon brush.

Maintenance:

[][]If Muffle furnace shows any mechanical, electrical or any others problem, inform to supplier or
[][]Engineering Department for maintenance.

Calibration of Digital Hygrometer, Purpose :

Calibration of Digital Hygrometer, This purpose of this SOP is to describe to operate of Hygrometer for the determination of temperature and humidity of Quality Control Laboratory, Microbiology Laboratory, and Product Development.

Calibration of Digital Hygrometer, Scope :

This procedure is applicable for the determination of room temperature and humidity by digital hygrometer used in Quality Control Laboratory, Microbiology Laboratory, and Product Development of  XXP Pharmaceuticals Ltd.

Definitions/Abbreviation:

N/A

Responsibilities:

The roles and responsibility is as follows

Officer/Executive/Sr. Executive, Quality Control

To ensure that the instructions of this procedure are correctly followed

Manager, Quality Control

[][]To ensure that SOP is kept up to date.
[][]To ensure appropriate personnel from the section are trained on this procedure.
[][]To confirm that the SOP is technically sound and reflects the required working practices.

Head of Quality Assurance

[][]To ensure the overall implementation of the SOP.
[][]Approval of SOP

Procedure:

Precaution(s):

[][]Keep the sensor’s protective cap closed to extend the sensor’s life when the meter is not in use.
[][]Do not use for cleaning abrasive or solvents on these instruments.
[][]Do not store or use the meter outside the operating/storage environment.
[][]Allow time to stabilize the meter, when moving from one temperature/humidity extreme to other.

Operation:

[][]Check the calibration sticker to ensure that the instrument is within due date of calibration.
[][]Remove the RH sensor protective cap before use.
[][]Press Power button to turn the meter on.
[][]Setting Time-of-Day:
[][]Slid the CLOCK SET switch, located on the back of the unit to the CLOCK SET position
[][]Press HR and MIN button to set the hours and minutes respectively;
[][]Press and hold the button to rapidly advance the display.
[][]Setting 12/24 Hour Display:

[][]Slide the 12HR/24HR switch, located on the back of the unit to the desired position. In 12 hour format, “AM/PM” will appear on the display.
Selecting °C or °F:
[][]To display the temperature reading in Celsius or Fahrenheit, slide the °C/°F switch, located on the back of the unit, to the desired position.

Viewing the Humidity Memory:

[][]To view the humidity memory, press the HUMIDITY MEMORY button. The maximum humidity reading achieved will be displayed (“MAX” will appear on the display)
[][]Press the HUMIDITY MEMORY button a second time, within 10 seconds, to view the minimum humidity achieved (“MIN” will appear on the display)
[][]Press the HUMIDITY MEMORY button a third time, within 10 seconds, to return the current reading.

Clearing the humidity memory:

The maximum and minimum humidity memory may be cleared individually. To clear the desired humidity memory (MIN or MAX), press the CLEAR button while the memory value is being displayed (follow 7.1.7 to view the Humidity Memory)

Viewing the Temperature Memory:

[][]To view the temperature memory, press the TEM MEMORY button. The maximum temperature reading achieved will be displayed in the middle display (“MAX” will appear to the right of the value);
[][]The minimum temperature reading achieved will be displayed in the top display (“MIN” will appear to the right of the value);
[][]Press the TEM MEMORY button a second time, within 5 seconds, to return the current temperature and time-of-day display.

Clearing the humidity memory:

[][]To clear the temperature memory (MIN and MAX), press the CLEAR button while the memory value is being displayed (follow 7.1.9 to view the temperature Memory)
[][]Use annexure-I for recording of temperature and relative humidity, and use annexure-II for recording of temperature only as per requirements.

Calibration Procedure:

[][]Check the temperature and humidity using a digital thermo hygrometer and record the temperature and humidity in the calibration certificate. as per Annexure-V of Engineering.

[][]Calibrate the digital hygrometer once in a year ± 15 days.

Maintenance:

[][]If Humidity meter shows any mechanical, electrical or any others problem, inform to the supplier or
Engineering Department for maintenance.

Annexure

Annexure-I : Temperature and Humidity Record Sheet
Annexure-II : Temperature Record Sheet

Calibration of Potentiometric Titrator, Purpose :

Calibration of Potentiometric Titrator, The purpose of this SOP is to define the current procedure for the operation, calibration and cleaning of Potentiometric Titrate (Mettler-Toledo, Model: T50) within Analytical laboratory at XX  Pharmaceuticals Ltd.

Calibration of Potentiometric Titrator, Scope :

This procedure is applicable to the determination of the potency and/or purity of raw materials (Active & Excipients), intermediates and drug product etc. in the quality control laboratory of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

N/A

Responsibilities:

The roles and responsibility is as follows:

Executive, QC

[][]To ensure that this procedure is followed.
[][]To maintain the records properly as per SOP.

Manager, Quality Control

[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]Arrange training on the SOP to all concerned personnel.
[][]To ensure implementation of the SOP after training.
[][]Maintaining calibration schedule of the instrument at the defined intervals.

Head Quality Assurance

[][]Approval of the SOP.
[][]To ensure overall implementation of the SOP.

Procedure:

Precaution(s):

[][]Laboratory coat, safety glasses and must be worn while handling the instrument.
[][]Ensure that the main switch and power supply connector are accessible during use.
[][]There is a chance of liquid spillage at high speed. Always gradually increase the speed to the desired level.
[][]Remove the plug from the main socket during cleaning.

General procedure:

[][]Titration is a technique for determining the potency and/or purity of synthetic raw materials, intermediates, drug substances, excipients and drug products, and for standardizing volumetric solutions. Although less specific than chromatographic techniques it is useful for quality control purposes where more details impurity quantization is not requested. Titration for assay of active substances is frequently used in pharmacopoeia monographs for drug substance and drug product.

[][]Samples are quantified by reaction in solution with a volumetric solution of known strength. A graduated glass tube fifed with a stopcock and fine tip is used to deliver deliver variable amounts of titrant, accurately measured, until the point at which the stoichiometric analytical reaction is complete. The endpoint may be determined use of color indicators or electrochemically. Where electrochemically endpoint detection is employed, automated burettes and endpoint detection may be used.

Automatic Burettes:

[][]This type of burette is found on automatic titration and dilution equipment. These devices are capable of very high precision volumetric measurements.

Automatic Titrates:

[][]Two types of automatic titrates are recorded the electrode potential differences during the course of titration as the expected sigmoid curve. This type is recommended for purchase and use since it offers greater accuracy and precision. In the second type, titrant addition is performed automatically until a pressed potential or pH, representing the endpoint, is reached, at which point the titrant addition ceases.

Indicator electrode:

[][]Choice of indicator electrode depends on the substance being examined and be a glass or metal electrode. The reference electrode is generally a calomel or silver-silver chloride electrode. Ensure that electrodes are in good condition. Electrode for non-aqueous titration must be dedicated and not utilized for any aqueous titration techniques.

Overview of titration chemistries:

[][]Titrimetric analyses utilize one of four basic chemistries, Reduction-oxidation, Complex metric, Precipitation and Acid-base, which may also be subdivided into non-aqueous and aqueous titrations.

Operations:

Manual Operation:

Enter the following parameters
[][]Stirrer
[][]Sensor
Temperature sensor
Potentiometric sensor
Polarized sensor
Conductivity sensor
[][]Burette
Rinse burette
Rinsing several burette at the same time
Dispense
Manual titration
[][]Pump
[][]Auxiliary instrument
[][]Sample Changer

You can determine the following parameters:

[][]Press ‘Manual’ to select Parameters.
[][]To ’Set’ parameters and input data. You would like to use and adjust the parameters.
[][]Press “Start’ to start the parameters procedure.
[][]You can select ‘Stop’ to terminate the procedure at any time.
[][]Press ‘Exit’ to end the manual operation.
[][]Press ‘Home’ and retune to main menu.

Methods:

Loops:

[][]There are the following loop types.
[][]A sample loop is for analyzing a sample.
[][]A calibration loop is for calibrating a sensor.
[][]A titer is for determining the titer of a titrate.

Types of Methods

[][]GT: Method for general titration (contains only sample loops or mixed loops).
[][]Calibration: Method for sensor calibration (contains only calibration loops).
[][]Titer: Method for titer determination(contains only titer loops)
Create a new method for general Titrant:
[][]Press ‘Method’
[][]Choose ‘New’ to create a new method on the basis of a template.
[][]From the available templates, choose method template EP by pressing ( ).Then press ok and exit.
You can modify this method in line with your requirements by inserting removing method functions or modify its parameters.
[][]Press ‘Title’ method function, enter a new method ID. After wards, a new method will be stored under this Method ID. Press ok and exit.
[][]Assign a ‘title’ to your new method.
[][]Press Sample button and input Sample ID, Entry Type, Density, Correction factor, Temperature and Entry in line with your requirements. Press ok and exit.
[][]Press Titrant Stand button and select manual stand. Press ok and exit.
[][]Press stirrer button and select stirrer speed and duration. Press ok and exit.
[][]Press Titration [EQP] [1].Press ok and exit.
[][]Input titrant and concentration by pressing titrant button.Press ok and exit.
[][]Press Sensor key and then input type, sensor and unit. Press ok and exit.
[][]Input stirrer speed by pressing stirrer. Press ok and exit.
[][]Input mode and wait time after pressing pre-dispensing key. Press ok and exit.
[][]Input Control and Mode after pressing control. Press ok and exit.
[][]Input molecular weight of the materials after pressing calculation. Press ok and exit.
[][]After inserting all required method function, you can store the new method in the titrator by choosing ‘Save’.

Annexure:

Annexure-I: Calibration Information of Potentiometric Titrator.
Annexure-II: Log Book for Potentiometric Titrator.

Calibration of Fume Hood, Purpose :

Calibration of Fume Hood, The purpose of this SOP is to describe the operation, calibration and cleaning of Fume Hood (Model: ESCO – EFD-4B1).

Calibration of Fume Hood, Scope :

This procedure is applicable for Fume Hood (Model: ESCO – EFD-4B1), installed in the quality control laboratory of  XX Pharmaceuticals Limited.

Definitions/Abbreviation:

[][]SOP: Standard Operating Procedure
[][]QC: Quality Control
[][]Face velocity: Face velocity is the average air flow speed at the sash opening of the fume hood into the work chamber. The measurement is expressed in m/sec or fpm.

Responsibilities:

The roles and responsibility is as follows:

Officer/Executive/Sr. Executive, Quality Control

[][]To ensure that the instructions of this procedure are correctly followed.
[][]To ensure the equipment is left clean and tidy after use.

Manager, Quality Control

[][]To ensure that this procedure is kept up to date.
[][]To confirm that the SOP is technically sound and reflects the required working practices.
[][]To arrange training on the SOP to all concerned personnel and to ensure implementation of the SOP after training.
[][]Schedule calibration of the instrument at the defined intervals.

Head of Quality Assurance

[][]To ensure the overall implementation of the SOP.
[][]Approval of the SOP.

Procedure:

Precaution(s):

[][]Relevant safety data sheet and safety guidelines must be followed when handling chemicals and reagents.
[][]Hazardous and fuming materials must be handled in fume hood.
[][]Wear appropriate personal protective equipment (PPE) while performing laboratory tasks in a fume hood.
[][]Keep head outside of the hood.
[][]Leave the front sash at the safe working height, when not in use.
[][]Follow laboratory procedure on the use of fume hood.
[][]Ensure the exhaust is operating before commencing work.
[][]Do not use the hood as storage area. Items can block airflow and interfere with containment.
[][]Do not leave uncapped bottles of chemicals in the hood.

Operation:

[][]Switch ‘ON’ the fluorescent lamp of the fume cupboard.
[][]Switch ‘ON’ the external exhaust blower/ fan.
[][]Lift the front sash to access in work area but not beyond the working height marked with yellow tape (30 cm).
[][]Work with the sash as fully lowered as possible, utilizing the sash as natural barrier to accidents which may occur in the hood.
[][]Plug in any electrical equipment used within the cabinet with electrical socket.
[][]Work as far into the hood as possible and with slow, deliberate movements, to minimize the external airflow disturbances.
[][]If performance is suspected, or an airflow alarm is triggered, terminate usage, close the sash completely and cease work.
[][]Report any fault regarding operation, maintenance or cleanliness of the cupboard to the supervisor.
[][]Leave the fume cupboard clean & dry after use.
[][]Turn the external exhaust blower/fan switch ‘OFF’.
[][]Turn the fluorescent lamp switch ‘OFF’.

Calibration:

[][]Calibrate the air flow (face velocity) of the fume cupboard six monthly.
[][]Switch ‘ON’ the fan.
[][]Open the window sash by sliding upward, 30 cm from the bottom.
[][]Take the reading by flow meter at left, right & middle of the fuming hood & record it in the calibration information sheet for Fume Hood (as per Annexure-I) for calculation.
[][]When instrument do not complies with the specified limits, label “Out of calibration” and get serviced.

Cleaning procedure:

[][]Clean the instrument once in a month or when required.
[][]Clean the work surface and walls with appropriate disinfectant agent and soap water.
[][]Clean the sash window using an appropriate agent disinfectant and glass cleaner.
[][]Use clean water to finish the cleaning and wash away any residue of disinfectant agent, soapy water and glass cleaner.
[][]Use a damp cloth to clean the exterior surface of the fume hood, particularly on the front and top in order to remove dust.
[][]Use Methyl-Ethyl-Ketone to remove stain or spot on the stainless steel surface as soon as possible.

Annexure:

Annexure-I: Calibration Information Sheet for Fume Hood.