SOPs

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.

Calibration of Hot plate ,Purpose :

Calibration of Hot plate, The purpose of this SOP is to describe the operation, calibration and cleaning of Hotplate with Magnetic Stirrer (Model: Fisherbrand – FB65312).

Calibration of Hot plate, Scope :

This procedure is applicable for Hotplate with Magnetic Stirrer (Model: Fisherbrand – FB65312), installed in the quality control laboratory for general block of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

[][]SOP: Standard Operating Procedure.
[][]QC: Quality Control.
[][]RPM: Rotations per minute.

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 hotplate maintaining 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.
[][]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):

[][]Laboratory coat and thick rubber gloves must be worn while handling the instrument.
[][]Ensure that the main switch and power supply connector are accessible during use.
[][]Remove the plug from the main socket during cleaning.
[][]Never use sharp objects or harsh or abrasive cleaning agents when cleaning.
[][]Spillage must be cleaned up immediately after use.
[][]Do not heat beakers with any type of liquid adhering to backside.
[][]Never touch the top of the plate when the instrument is on.
[][]Never keep the heater in ‘on’ condition, when not in use.
[][]Do not use hotplate until reported faults are repaired.

Operation:

[][]Ensure the equipment is clean, calibrated and free from any dust particle.
[][]Connect the instrument to the main power supply.
[][]Switch ‘ON’ the mains.
[][]Place the beaker containing the solution in the center of the plate.
[][]For stirring option, immerse the Teflon stirring bar into the solution to be stirred.
[][]Switch ‘ON’ the instrument.
[][]Set the required stirring speed (RPM) of stirring bar by means of speed regulator knob. Turn the speed regulator knob clockwise or counter-clockwise to increase or decrease speed respectively.
[][]After stirring is over, slowly decrease the speed to zero by turn knob counter-clockwise.
[][]For heater, set the temperature by rotating the temperature setting knob to the required. It will take 5 to 10 minutes to stabilize. Turn the knob clock wise to increase the temperature or counter clock wise to decrease the temperature.
[][]After heating is over, decrease the set temperature to zero by turn knob counter-clock wise.
[][]Bright red light will flash until surface cools.
[][]After completion of work, switch ‘OFF’ the instrument.
[][]Switch ‘OFF’ the mains when not required.

Calibration:

[][]Calibrate the hotplate once in a year.
[][]Switch ‘ON’ the mains.
[][]Switch ‘ON’ the instrument.
[][]Set the desired temperature using temperature setting knob.
[][]Check the temperature using a duly calibrated thermometer and record the temperature in the calibration information sheet for hotplate with magnetic stirrer (as per Annexure-I).
[][]When instrument do not complies with the specified limits, label “Out of calibration” and get serviced.

Cleaning procedure:

[][]Switch ‘OFF’ the instrument.
[][]Switch ‘OFF’ the mains.
[][]Ensure that the surface of the plate is in room temperature.
[][]De-dust the instrument with a clean dry cloth every day.
[][]Once in a week wet mop the instrument.
[][]Wet mop using a cloth moistened in mild detergent solution and then wipe with a cloth wetted with water.
[][]Afterwards wipe the surface with a clean dry cloth to remove traces of detergent.
[][]Allow to dry the instrument before using it again.

Annexure

Calibration Information Sheet for Hotplate with Magnetic Stirrer

Vortex Mixer , Purpose :

Vortex Mixer , The purpose of this SOP is to describe the operation and cleaning of Vortex mixer (Model: Fisherbrand- ZX Classic), for better or error free use.

Vortex Mixer , Scope :

This procedure is applicable for Vortex mixer (Model: Fisherbrand- ZX Classic) used for mixing the solution or dissolving the various substances into solvent, installed in the quality control laboratory of XX  Pharmaceuticals Limited.

Definitions / Abbreviation:

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

Responsibilities

Executive, QC

[][]To ensure that the instructions of this procedure are correctly followed.
[][]To ensure cleaning of vortex mixer maintaining 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 press the test tube hardly on the mixing head.
[][]Do not vortex any materials for long time.
[][]Maintain the level of test solution into test tube/Vial/test flask to avoid overflow during vortex.
[][]Set the speed control to the minimum, before turning on the mixer.
[][]Disconnect vortex mixer from power source before attempting any cleaning or maintenance procedures.
[][]Never operate without a shaking head securely attached.
[][]Always wear eye protector during use of vortex mixer.
[][]Always have lids on the tubes when solvents and flammables are used on the mixer.
[][]Shake hazardous samples in appropriate containment vessels.
[][]Replace rubber attachments with new ones when these show progressive signs of wear out.
[][]Do not immerse the unit or pour liquids over it as electrical shock may occur.

Operation:

[][]Switch ‘ON’ the mains.
[][]The yellow light will be illuminated.
[][]Use the ‘continuous’ key to select the automatic vortex or manual vortex.
[][]Set the desired speed with the help of the ‘control’ knob.
[][]In case of automatic vortex option, touch test tube/vial on the mixing head to start the vortex automatically.
[][]For manual vortex, place the test tube on the mixing head and then press ‘continuous’ button.
[][]Adjust the vortex speed by turning ‘control’ knob clockwise to increase speed or anti-clockwise to decrease speed.
[][]Vary the speed and/or the angle of contact and pressure against the mixing attachment to achieve the desired mix.
[][]On completion, turn the ‘control’ knob anticlockwise to the minimum.
[][]Remove the test tube at the end of vortex.
[][]Stop the vortex by press ‘continuous’ button.
[][]Switch ‘OFF’ the mains.

Cleaning procedure:

[][]Switch ‘OFF’ the mains and disconnect the power plug.
[][]After each use, wipe down the mixer with a soft, dry cloth.
[][]Keep the unit clean by immediately blotting any spills. Remove the shaking head, if required. Clean the head with mild detergent. Dry thoroughly, before replacing the head on the unit.
[][]Clean the outer surface of the instrument properly with a non-abrasive cloth or sponge, moistened in mild detergent water, once in a week or when required.
[][]Never use harsh or abrasive cleaning agents.
[][]Allow to dry before use it again.

Calibration of orbital shaker, Purpose :

Calibration of orbital shaker, The purpose of this SOP is to describe the operation, calibration and cleaning of Orbital Shaker (Model: Stuart SSL1), used for shaking flask, bottle and beaker to dissolve solids in liquid.

Calibration of orbital shaker, Scope :

This procedure is applicable for Orbital Shaker (Model: Stuart SSL1), installed in the quality control laboratory XX Pharmaceuticals Limited.

Definitions / Abbreviation:

[][]SOP: Standard Operating Procedure.
[][]QC: Cephalosporin Quality Control.
[][]RPM: Rotations per minute.

Responsibilities:

Executive, QC

[][]To ensure that the instructions of this procedure are correctly followed.
[][]To maintain the records properly as per SOP.
[][]To ensure cleaning of orbital shaker maintaining 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.

Procedure:

Precaution(s):

[][]Laboratory coat and safety glasses 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 and splashing if containers are over filled and shaken at high speed. Always gradually increase the speed to the desired level. Never set the speed beyond the maximum limit.
[][]Remove the plug from the main socket during cleaning.
[][]The shaker should not be operated at the maximum RPM without a load.
[][]Do not leave the shaker unattended when starting the unit. Be sure all flasks are firmly seated in the platform and securely clutch between screwing bars.
[][]Ensure the speed controller knob are turned off before switch on the instrument.

Operation:

[][]Check the calibration sticker to ensure that the instrument is within due date of calibration.
[][]Place the apparatus on a firm level surface ensuring the platform is free from vibration.
[][]Fit the flasks or bottles or beakers to be shaken between two rubber cushioned horizontal screwing bars and adjust to hold them tightly.
[][]Switch ‘ON’ by pressing the ‘control’ knob.
[][]Red dot in the display shows RPM is selected; this can be adjusted by turn the ‘control’ knob to the right up to desired shaking speed (in rpm). Once the correct speed is displayed press the ‘start/stop’ button to begin motion.
[][]In order to use the timer and RPM press the ‘mode’ button. The red dot on the display moves over to time. The display will show the last stored time in minutes.
[][]Select the desired count down time using the control knob. When the display shows the correct time in minutes.
[][]Rotation can be paused at any time by pressing the ‘start/stop’ button.
[][]Rotation will start again by pressing ‘start/stop’ button and the timer will continue to count down.
[][]The timer can be adjusted without halting the unit. When the timer reaches zero, the unit will be automatically halted and alert will sound.
[][]Press ‘start/stop’ button to revert back to the last time and speed values set or select new value.
[][]The shaking will stop automatically after the desired period and sounds an alert.
[][]Switch OFF completely by pressing the ‘control’ knob. The display will show OFF

Calibration:

[][]Calibrate the orbital shaker once in a year.
[][]Switch ‘ON’ the mains.
[][]Switch ‘ON’ the instrument by pressing ‘control’ knob.
[][]Set the desired time (most commonly used time range) using time setting button.
[][]Check the time using a calibrated stop watch and record the time in the calibration information sheet for Orbital shaker as per Annexure-I.

Cleaning procedure:

[][]Clean the instrument once in a week or when required.
[][]Switch ‘OFF’ the instrument and switch ‘OFF’ the mains.
[][]Clean the instrument properly with a non-abrasive cloth moistened in detergent water.
[][]Never use harsh or abrasive cleaning agents.
[][]Allow to dry before use it again.

Annexure:

Annexure-I: Calibration Information Sheet for Orbital Shaker.

Calibration of Ultrasonic Bath, Purpose :

Calibration of Ultrasonic Bath, The purpose of this SOP is to describe the operation, calibration and cleaning of Ultrasonic Bath (Model: Clifton DU-14), used for degassing liquids, dissolving solids in solutions and cleaning laboratory apparatus.

Calibration of Ultrasonic Bath, Scope :

This procedure is applicable for Ultrasonic Bath (Model: Clifton DU-14), installed in the quality control laboratory of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

[][]SOP: Standard Operating Procedure.
QC: Quality Control.
[][]Sonication: The act of applying sound energy (usually of the ultrasound type) to agitate particles in a sample.

Executive, QC

[][]To ensure that the instructions of this procedure are correctly followed.
[][]To maintain the records properly as per SOP.
[][]To ensure cleaning of ultrasonic bath maintaining 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.
[][]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):

[][]Never put hands in the bath during operations.
[][]Always maintain the liquid level above the minimum level mark.
[][]Disconnect the power supply before moving, emptying or cleaning of bath.
[][]Never operate the unit when dry.
[][]Allow the liquid in the bath to cool down before draining.
[][]Never block or restrict ventilation slots.
[][]Do not place item directly on the bottom of the bath, always make use of the stainless steel basket to suspend the item.
[][]Do not use cleaning fluids which contain concentrations of halogen ions, low pH values or high temperatures when operating the bath for cleaning purposes as these will all increase the risk of corrosion.

Operation:

[][]Check the calibration sticker to ensure that the instrument is within due date of calibration.
[][]Fill the bath with purified water above the ‘MIN’ level mark.
[][]Switch on the bath using the ‘ON/OFF’ switch, located at the rear of the bath.
[][]Place the stainless steel basket into position.
[][]Switch ‘ON’ the heater and press ‘■’ menu button to display “SP1”. Set the desired temperature using ▲ or ▼ key button. Maximum setting 69° C.
[][]After setting temperature, display will flash the temperature four times and then it will be automatically set.
[][]Press ‘■’ menu button twice to display “t”. Set the time using ▲ or ▼ key button.
[][]After setting time, display will flash the time four times and then it will be automatically set or press ‘■’ menu button to set manually.
[][]Place the glassware containing sample onto the stainless steel basket, to prevent touching the bottom of the tank.
[][]To start sonication, press and hold ‘Ο’ button until the Time LED is blinking.
[][]Instrument will stop after set time finished.
[][]Wait until the operation process is completed.
[][]To stop sonication, press and hold ‘Ο’ button until the Time LED is off.
[][]Use suitable tongs to remove the hot glassware from the bath.
[][]Allow the bath to cool.
[][]After completion of work, switch off the bath.
[][]Finally switch off the instrument.

Calibration:

[][]Calibrate the water bath once in a year.
[][]Fill purified water in the bath above the ‘MIN’ level mark.
[][]Switch ‘ON’ the mains.
[][]Switch ‘ON’ the mains of instrument.
[][]Set the desired temperature. Follow operation procedure 7.1.5 to 7.1.6.
[][]Allow 30 minutes to equilibrate.
[][]Check the temperature using a calibrated thermometer/digital thermometer and record the temperature in the calibration information sheet for Ultrasonic bath (as per Annexure-I).
[][]Set the desired time. Follow operation procedure 7.1.7 to 7.1.8
[][]Check the time using a calibrated stop watch and record the time in the calibration information sheet for Ultrasonic bath as per Annexure-I.

Cleaning procedure:

[][]Clean the instrument once in a week or in between when water becomes dirty.
[][]Switch ‘OFF’ the instrument and switch ‘OFF’ the mains.
[][]Remove the basket from the ultrasonic bath.
[][]Wash the basket properly with purified water.
[][]Drain the water from the ultrasonic bath.
[][]Wipe the inner surface of the bath with a non-abrasive cloth moistened in water.
[][]Use 10% nitric acid on a cloth (wear suitable gloves) to remove any scale or deposits.
[][]Fill purified water in the bath above the ‘MIN’ level mark.
[][]Put the basket in to the bath.

Annexure:

Annexure-I: Calibration Information Sheet for Ultrasonic bath.

Tap Density Apparatus Calibration, Purpose :

Tap Density Apparatus Calibration, The purpose of this SOP is to describe the operation, calibration and cleaning of Bulk density apparatus (Model: Electrolab ETD-1020) used for the Bulk density test of raw materials in the quality control laboratory at XX Pharmaceuticals Limited.

Tap Density Apparatus Calibration, Scope :

This procedure is applicable for Bulk density apparatus (Model: Electrolab ETD-1020), installed in the quality control laboratory of XX Pharmaceuticals Limited.

Definitions / Abbreviation:

[][]SOP: Standard Operating Procedure.
[][]QC: Quality Control.
[][]USP: United State Pharmacopoeia

Responsibility

Executive, QC

[][]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.
[][]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

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

Procedure:

Precaution(s):

[][]The equipment should not be set near to room heating equipment or direct sunlight.
[][]Use mask, gloves and safety goggles during handling the instrument.
[][]Disconnect the power supply before cleaning of the instrument.
[][]Prior to use, user must ensure that equipment is calibrated.
[][]Avoid any dust gathering on the bearings.
[][]Do not lubricate the bearings.
[][]Keep the shaft of the cylinder holder and the tip of the cylinder holder clean.
[][]Do not press the cylinder holder when the tapping base of cylinder holder is not touching the anvil.
[][]Place the cylinder in the holder only when the holder is placed on the anvil.

Operation:

[][]Ensure that working area is clean.
[][]Connect power cord of the instrument to mains and switch ‘ON’ the instrument.
[][]Instrument will initialize itself and the display will flash and show the start up screen.

[ELECTROLAB TAP DENSITY
ETD-1020 VER 3.0

[][]Set the mode of operation as USP or USER using the ‘DIGIT SCROLL’ key on the front panel.
[][]In USP mode, instrument will stop after every program and validation; report is available at the end of test.
[][]In USER mode, instrument will stop after the set tap value and no validation and result screen will be available. This method is used only when no. of taps are specified in the method.
[][]Press the ‘METHOD’ key to toggle between USP-I and USP-II method and select the required method.
[][]Press ‘SET’ key to set the test parameter.
[][]Display reads

[TAP COUNT 1: # # # # ▲▼◄
SET : EXIT / Enter : SCROLL

[][]Set the TAP COUNT 1.
[][]Enter the Tap count 1 within 1 to 9999 using the ‘UP/DOWN’ & ‘DIGIT SCROLL’ key.
[][]Press ‘ENTER’ key to go next parameter.
[][]Similarly set TAP COUNT 2 and TAP COUNT 3.
[][]In USP method, set TAP COUNT 1 as 250 taps, TAP COUNT 2 as 500 taps and TAP COUNT 3 as 500 taps.
[][]Set the date and time using the ‘UP/DOWN’ & ‘DIGIT SCROLL’ key.
[][]Select the print option & press ‘SET’ key to scroll back to main menu.
[][]Pass a quantity of material sufficient to perform the test through 20-mesh screen to break up any agglomerates.
[][]Transfer about 100 g sample into a dry 250 ml graduated cylinder with 2 ml accuracy.\
[][]Alternatively transfer a small quantity (less than 100 g) of sample into a 100 ml cylinder with 1ml accuracy to minimize the sample quantity.
[][]Press the ‘START’ key.
[][]Weigh the test sample and enter the weight of test sample.
[][]Press the ‘ENTER’ key to register the weight.
[][]Level the sample without tapping or compacting.
[][]Read the unsettled apparent volume to the nearest graduated unit and enter the volume using the ‘UP/DOWN’ & ‘DIGIT SCROLL’ key.
[][]Press the ‘ENTER’ key to register the volume.
[][]Fix the measuring cylinder into the holder provided for holding the measuring cylinder on the instrument.
[][]Lock the holder assembly.
[][]Press the ‘START’ key again to run the test.
[][]Display will show the elapsed taps and drops per minute.

ELAPSED TAP: # # #
Drops / Min. : # # #

[][]After programmed TAP COUNT 1 is over, measure the tapped volume to its nearest graduated unit.
[][]Enter the measured tapped volume using ‘UP / DOWN’ & ‘DIGIT SCROLL’ Keys.
[][]Press ‘ENTER’ key to register the value.
[][]Press ‘START’ key to continue TAP COUNT 2 program.
[][]Measure the tapped volume at the end of TAP COUNT 2 program and enter the value using ‘UP / DOWN’ & ‘DIGIT SCROLL’ Keys.
[][]The difference between the two counts will be displayed as a result.
[][]If the result after the completion of TAP COUNT 2 is less than 2.0%, press ‘STOP’ key to end the operation and to get the results.
[][]If the result is more than 2.0%, then press ‘START’ key again to start the TAP COUNT 3 program to get a new value.
[][]Repeat the operation till the difference between two succeeding measurements is less than 2.0%.
[][]Press ‘STOP’ key once the desired difference is obtained instrument will display the results.
[][]The results of Bulk density or initial density, tapped density and Hausner ratio and compressibility index will be displayed one after another by using ‘DOWN’ key.
[][]The results shall be recorded separately or taken as a print out.
[][]After operation enter usage details in Operation Logbook of Bulk Density Apparatus as per Annexure – II.

Calibration:

[][]Calibration of Drop distance
[][]Calibrate the instrument once in a year or whenever there is a major maintenance.
[][]Disconnect the instrument from mains.
[][]Gently disassemble the sample holder assembly.
[][]Remove the top cover by unscrewing the holding screws given on the bottom of the instrument i.e. the screws given on the four sides and one screw given on the backside near the power switch. The places are marked for convenience.
[][]Place the sample holder in the slot of USP I and manually rotate the cam wheel so that the holder is at the highest position.
[][]The stem of the holder is now on the top of the highest position of the cam (which is marked as a groove on the wheel.
[][]Measure the distance from base to the bottom of the holder (h1) using a suitable vernier caliper.
[][]Rotate the wheel to get the lowest position, the position from which it started to raise again.
[][]Measure the distance from base to the bottom of the holder (h2) using a suitable vernier caliper.
[][]The difference between the h1 and h2 gives the drop distance.
[][]Record the observations in the calibration information sheet (Annexure –I).
[][]Repeat the same procedure on the USP-II slot.
[][]Record the observations in the calibration information sheet (Annexure –I).
[][]When the distance is not within the prescribed limit, change the teflon bottom of the stem to get the required height.
[][]Carefully replace the top cover and close.
[][]Calibration of Drop rate
[][]Connect the instruments for main and proceed for the calibrations for drops rate.
[][]Switch ‘ON’ the mains.
[][]Select USP-I or USP-II method using ‘METHOD’ key
[][]The indicator light glows in USP-I or USP-II on the front panel
[][]Using ‘SCROLL BAR’ keys, select the USER method and press ‘SET’ key.
[][]Enter the number of taps to 100
[][]Press ‘START’ key and simultaneously start the stopwatch.
[][]Record the time at which the tapping stops in the calibration information sheet (Annexure –I).
[][]Similarly perform the test using 250, 750 and 1250 taps and note the timings
[][]Calculate the drops per minute in both USP-I and USP-II method.
[][]Record the drops per minute in the calibration information sheet (Annexure –I)
[][]If the instrument is out of calibration, inform the Manager, Quality Control.

Cleaning Procedure:

[][]Clean the instrument after every use.
[][]Switch ‘OFF’ the instrument and switch ‘OFF’ the mains.
[][]Remove the cylinders from the apparatus and clean the cylinder.
[][]Clean the apparatus with cotton cloth.
[][]Clean the surrounding areas of instrument with a cloth dampen in water.

Annexure:

Annexure-I: Calibration Information Sheet for Tap Density Apparatus.
Annexure-II: Operation Logbook of Tap Density Apparatus