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.