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1.0 OBJECTIVE
To set up a procedure for the operation and cleaning procedure of Melting Point apparatus (Model: M-565)
2.0 SCOPE
This SOP is applicable for operation and cleaning procedure of Melting Point apparatus (Model: M-565, Eq. ID.: QC/248) at Quality Control Department (Company Name).
3.0 RESPONSIBILITY
3.1 Operating personnel responsible for carrying out the procedure.
3.2 Overall responsibility for training, implementation & follow-up with the Head of QC or his/her nominee.
4.0 ACCOUNTABILITY
4.1 Head of Quality.
5.0 PRECAUTIONS
5.1 The melting point apparatus should never be operated without the sample holders inserted. The sample holders protect the apparatus from dust and smaller particles.
6.0 PROCEDURE
6.1 Preparation of samples: Crush the granular, crystalline and inhomogeneous sample into fine powder in a mortar and fill into the melting point capillary to at least 4 to 6 mm or as per STP or Pharmacopoeia.
6.2 Connect the power cord of the instrument to the main power supply.
6.3 Switch on the power key that is on the front side of the machine.
6.4 Display shows the menu for melting point.
6.5 Press on Method to create a new method. Pres Option New then OK.
6.6 Enter a method name. To finish press Save.
6.7 Enter start temperature, end temperature and gradient of increment press Next then Save.
6.8 Using and Handling methods
6.8.1 Turn the rotary knob to select a method.
6.8.2 Press Start to start the determination.
6.8.3 Use Edit to adjust method parameters.
6.8.4 Press the Option key to get further functions.
6.8.5 New: Create a new Method.
6.8.6 Delete: Deletes the Method.
6.8.7 Rename: Changes the method name.
6.9 Press start key. The unit will heat up to the previously selected set point. The display will show the temperature gradient.
6.10 The machine will give a beep when the set point has been reached. Place the sample into the sample holder.
6.11 Press starts key to run the test.
6.12 See the sample through the magnifying glass as required.
6.13 The result is print out automatically.
6.14 Press stop key. The machine will cool down automatically to the previously used set point.
6.15 Record the information’s in the operational log book- “LOG BOOK FOR MELTING POINT APPARATUS” as per FRM No.: FQC/245.
6.16 Calibration
6.16.1 To start calibration, turn the rotary knob to calibration. Press START and follow the instruction on display.
6.16.2 The instrument automatically heats to the start temperature of the first substances. In the meantime, prepare at least 6 samples of the given substances.
6.16.3 Choose the correct pharmacopoeia melting point value with the rotary knob. The pharmacopoeia melting point is written on the certificate of analysis. Press SAVE.
6.16.4 Follow the instruction on the display. After each run the current result is indicated. Press start to perform the next measurement.
6.16.5 After 6 results are obtained within a standard deviation of ± 0.2°C, the process moves on to the next substance. The process is identical for the other substances.
6.16.6 As soon as a complete calibration is obtained, the new calibration date is saved automatically. Press oK. All results obtained are displayed.
6.16.7 Use the print key to print out the data.
6.17 Verification
6.17.1 To verify the calibration measure the melting point of all standards (BUCHI recommended) or internal standards.
6.17.2 When all measuring results were within the required tolerance, click on verified. one screen appears.
6.17.3 Enter the password VER. The current date is now indicated under “Last Verification”.
6.17.4 Record the result as per Annexure-II.
6.18 Calibration frequency: 6 months ± 10 days.
