To lay down the procedure for Calibration of Melting Range/Melting Point Apparatus.
1.0 PURPOSE
1.1 To lay down the procedure for Calibration of Melting Range/Melting Point Apparatus.
2.0 SCOPE
2.1 This procedure is applicable for Calibration of all Melting Range/Melting Point Apparatus located in quality control lab.
3.0 RESPONSIBILITY
3.1 Assistant-QC
4.0 ACCOUNTABILITY
4.1 Sr.Executive-QC
5.0 PROCEDURE
5.1 Operate the instrument as per the SOP for operation of melting range/point apparatus.
5.2 Perform the temperature check for calibration of the instrument.
5.3 Dry the reference/standard material as per their specified condition.
5.4 Perform the test with each selected reference/standard material.
5.5 Pack dry powder of Vanillin, Sulfanilamide and Caffeine reference materials in the capillary tubes such that a 3 mm packed columns are made.
5.6 Start the apparatus, put ‘on’ the heater and stirrer (as applicable).
5.7 Heat the sample plate / silicon oil by setting the control parameter/knob.
5.8 Vanillin
5.8.1 Insert the three capillary tube filled with sample.
5.8.2 Set the temperature program as below.
Initial temperature 70°C
Rate 1°C/min
Final temperature 87°C
5.8.3 Note down the temperature at which the first and last particle
Of Vanillin melts.
Acceptance criteria: Vanillin : between 81°C to 83°C.
5.9 Sulfanilamide
5.9.1 Insert the three capillary tube filled with sample.
5.9.2 Set the temperature program as below.
Initial temperature 155°C
Rate 1°C/min
Final temperature 170°C
5.9.3 Note down the temperature at which the first and last particle of
Sulfanilamide melts.
Acceptance criteria: Sulfanilamide : between 164.5°C to 166.5°C.
5.10 Caffeine
5.10.1 Insert the three capillary tube filled with sample.
5.10.2 Set the temperature program as below.
Initial temperature 225°C
Rate 1°C/min
Final temperature 245°C
5.10.3. Note down the temperature at which the first and last particle of
Caffeine melts.
Acceptance criteria: Caffeine : between 234°C to 237°C.
5.11 Record all the results in Format No.xxxxx
5.12 Frequency: Once in three months.
point apparatus, range melting, temperature, reference
