Calibration of Melting Point Apparatus , Purpose :
Calibration of Melting Point Apparatus, The purpose of this SOP is to describe the operation, calibration and cleaning of Automatic Melting-point apparatus (Model: BUCHI M-565) used for the determination of the melting point of raw materials in the quality control laboratory at XX Pharmaceuticals Ltd.
Calibration of Melting Point Apparatus, Scope :
This procedure is applicable to the Automatic Melting-Point Apparatus (Model: BUCHI, M-565), installed in the quality control laboratory of XX Pharmaceuticals Limited.
Definitions / Abbreviation:
[][]SOP: Standard Operating Procedure.
[][]QC: Quality Control.
[][]Melting point or Melting range: Melting point or Melting range is defined as the point at which or those points of temperature within which, the solid coalesces and is completely melted. The optical properties of most substances change at this transition.
Responsibilities:
The roles and responsibility is as follows:
Sr. Executive/Executive, QC
[][]To ensure that this procedure is followed.
[][]To maintain the records properly as per SOP.
[][]To ensure cleaning of Melting point apparatus 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.
[][]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 the overall implementation of the SOP.
Procedure:
Precautions:
[][]Laboratory coat and safety glasses (to protect eye from capillary tube) must be worn while handling the instrument.
[][]Always ensure that the cooling air outlet at the back of the instrument is not covered so that the air can flow.
[][]Use only the BUCHI sample tubes provided, as other tubes may not correctly fit in the sample holder. Always handle these glass tubes with care.
[][]Never touch the furnace or sample just removed from the furnace. The temperature of the furnace can reach 400°C.
[][]Care should be taken while inserting the capillary into its cavity or taking out from the cavity to avoid breaking, take it out vertically.
[][]Check always colour of the silicone oil. Normally it is colourless. If it observed as yellow or brown, discard the oil. And take fresh oil in that container.
[][]Disconnect the power supply before moving or cleaning of the instrument.
[][]When not in use, keep the Instrument in a safe place.
[][]Prior to use, user must ensure that equipment is calibrated.
Operation:
[][]Check the machine is clean and calibrated.
[][]Prepare the sample to make it powder, if required with an agate mortar.
[][]Fill the sample in capillary tube to a height of approximately 3 – 6 mm with the help of sample loader.
[][]Plug the instruments into an acceptable power source.
[][]Turn the instrument ON by using ‘I/O’ switch in front of the machine.
[][]Choose the Melting Point settings for melting point determination by rotary knob.
[][]Make sure that all samples are removed.
[][]To create a new melting parameter, press ‘Edit’.
[][]Select Start temperature with the rotary knob and press ‘Next’.
[][]Select Stop temperature with the rotary knob and press ‘Next’.
[][]Select Temperature gradient with the rotary and press ‘Save’.
[][]Press ‘START’ to start the determination.
[][]Turn the rotary knob to select a sample ID/Lot. Press ‘Enter’ after selecting each word/number by rotary knob.
[][]When machine reaches the set the temperature, a beep sound will be given and display will show ‘Insert sample & START’.
[][]Insert three capillary tubes containing sample and press ‘START’.
[][]To register additional temperature stamps manually, see the tube through the front window, press the ‘Set’ button for related sample. Each button can be pressed three times. Registered temperature stamps are displayed in green.
[][]After finish, machine will show the result.
[][]To run through the result, rotate the rotary knob.
[][]To replay the recorded melting process, press ‘Relay’.
[][]Press ‘End’ or ‘STOP’ to return to the idle screen.
[][]The result will be printed out automatically or by print option.
[][]Fill up the Log book for Automatic Melting point Apparatus ( as per Annexure-II)
[][]For creating a method:
[][]Press ‘Method’ to enter the method menu.
[][]Press Options-New-ok.
[][]Enter a method name and press ‘SAVE’.
[][]Adjust Start temperature, Stop temperature and Gradient temperature by using rotary knob. Use ‘Next’ button to move from one option to another. After setting the all parameter press ‘SAVE’.
Calibration:
[][]Calibrate the Automatic Melting Point Apparatus once in a year.
[][]Determine the melting point of 4-Nitotolune, Diphenyl acetic acid, Caffeine, potassium nitrate standard.
[][]To start calibration, turn the rotary knob to calibration. Press ‘START’. The instrument automatically heats to the start temperature of the first substance (4-Nitrotolune). Prepare at least six sample of each substance standard.
[][]Press ‘START’ to start the determination. Turn the rotary knob to select a lot/Sample ID and press ‘Enter’. Press ‘Save’ after giving Lot/Sample ID.
[][]Choose the correct Pharmacopoeia melting point value with the rotary knob. The Pharmacopoeia melting point is written on the certified of analysis. Press ‘SAVE’.
[][]Press ‘START’ to continue. Insert three samples and press ‘START’ to start the determination.
[][]After determination, press ‘START’ again to continue and wait for the beep sound and then insert three more samples and press ‘START’.
[][]After each run, the current result is indicated. After six results are obtained with in a standard deviation of ± 0.2°C. The process moves on to the next substance. The process identical for Diphenylacetic Acid, Caffeine and potassium Nitrate and save.
[][]After determination of the melting point of all four standards, compile the results and record the results in Calibration Information Sheet for Automatic Melting Point Apparatus (as per Annexure-I).
Cleaning:
Clean the instrument once in a week or in between when water becomes dirty.
Switch ‘OFF’ the instrument.
De-dust the instrument daily externally with a clean dry cotton cloth.
Remove the glass window from the heating block periodically and wipe it clean with alcohol or acetone. Replace the window with a new one if it will not come completely clean.
Once in a week remove adhered dust by wet mopping using detergent solution. Afterwards wipe the surface with a clean dry cloth to remove traces of detergent and moisture.
Annexure:
Annexure-I: Calibration Information Sheet for Automatic Melting Point Apparatus.
Annexure-I: Operation Log book for Automatic Melting Point Apparatus.