SOP operation and calibration of melting point apparatus.
OBJECTIVE:
To ensure that there is a standard procedure followed for Operating & Calibrating the Melting point Apparatus to ensure efficient working of the instrument.
SCOPE:
Operation & Calibration of Melting point Apparatus for checking Melting Point / Boiling point of raw Materials / Finished product.
REFERENCE:
Instrument operating manual.
RESPONSIBILITY:
QC – officers, executives – To follow the procedure as per SOP.
QC Head – To ensure proper execution of SOP.
QA – To ensure SOP is being properly implemented.
DISTRIBUTION :
NA
ABBREVIATION:
SOP – Standard operating procedure,
QC – Quality Control,
QA – Quality assurance,
NA – Not applicable,
MP – Melting Point.
INSTRUMENT DETAILS :
Instrument Name Melting point apparatus Make: VEEGO
Model No. : MP-OM Sr. no.: 12/12-11
Instrument ID No.:STSP/QC/MP/01 Location: Instrument room
PROCEDURE:
1. Ensure that the instrument is clean & free from dust.
2. Ensure that the plug is connected to the mains.
3. Switch ON the mains.
4. Set the speed of stirrer motor. To change the speed press STIRRER SPEEDE key or F2 KEY from PS-2 KEY BOARD the cursor will move to the displayed numeric value from 1 to 4.
5. confirm that the speed of the stirrer is uniform.
6. Press start key the display should as follows
7. Set the Test method from PRODUCT SEETINGS.
8. Select PRODUCT SEETING and press ENTER KEY or press 3 no. key, or F5 key from PS-2 key board.
9. Enter 6 digit password.
10. Press key no. 1.
11. With the help of PS-2 key board enter product name and Expected melting point in range.
12. Press enter key and data will save.
13. Similarly enter remaining 98 product name with their expected melting or Boiling point.
14. Enter the Operator’s name and Company name with Instrument no.
15. Press 3 key and select the NAME ENTRIES option.
16. Select OPERATOR NAME option by pressing ‘1’ key. And press enter.
17. Enter the password.
18. Enter OPERATORS’S name with Ps-2 key board. Press enter.
19. Select COMPANY NAME option by pressing ‘2’ key.
20. Enter Company’s name and Address with PS-2 key board.
21. Press enter.
22. Write Instrument no. with PS-2 key board.
23. Exit from above menu press ( BACK) key or ESC KEY from PS-2 key board.
24. Press menu key.
25. Press key No. 1 or press ENTER key.
26. Display OPTIONS: 1) SAMPLE TEST: to test sample for M.P. or B.P.
2) INSTRUMENT VALIDATION: To validate the instrument with standard powders.
a) VANILLIN M.P. – 81.00C – 84.00C
b) ACETANILLIDE M.P. – 113.00C – 116.00C
c) CAFFEINE M.P. – 234.00C – 238 0C
d) New reference standard
3) UNKNOWN SAMPLE TESTING: to test the sample which M.P. or B.P. is not known. The temperature will increase by approx 3.00C/min. up-to 300.00C.
27. Press ‘1’ key or ENTER key when ‘SAMPLE TEST’ message is flashing.
28. Press ‘1’ key or ENTER key when ‘MELTING POINT TEST’ message is flashing.
29. Select the test no. with the help of UP or DOWN key or enter the number with numeric key pad.
30. Enter Batch no. in alpha and numeric.
31. Press ENTER key and then select the OPERATOR NAME.
32. Fill the powder in one end sealed capillary about 3 to 4 mm and insert in one of the hole provided on the heater stand.
33. Heater temperature starts increasing. The green indicator lamp starts blinking and on the display actual temperature is indicated.
34. First buzzer sound approximately 15.00C before set temperature. From this point of temperature, the rate of increase is 1.00C/min.
35. The second buzzer sound before 5.00C.
36. For unknown sample the temperature will start increasing at approx. 3.00C/min. Observe melting point of sample manually, and when it melts Press Record key.
37. When melting point of a sample is observed, Press ‘RECORD’ key. TO observe START OF MELTING POINT.
38. When sample completely melted, press ‘RECORD’ key.
39. Connect DOT MATRIX 80 COLUMN PRINTER and take out the printed report.
40. Switch OFF the apparatus.
Calibration:
1. Determine the melting range of the following reference substances following the operating procedure. The substance should melt to the nearest of the std. Range.
REFERENCE SUSTANCES STANDARD RANGE
VANILLIN 810 C to 840 C
ACETANILIDE 1120 C to 1160 C
CAFFEINE 2340 C to 2380 C
2. Label the instrument as calibrated if within range.
FREQUENCY :
i) Operational frequency:- As & when required.
ii) Calibration frequency:- Once in three months.
ANNEXURE:
Annexure 1 – Melting point calibration report.
ANNEXURE 1
Instrument Name Melting point apparatus Make: VEEGO
Model No. : MP-OM Sr. no.: 12/12-11
Instrument ID No. STSP/QC/MP/01 Location: Instrument room
Calibration frequency: after 3 month Calibration done on:
Calibration due on
Parameters and acceptance criteria :
Sr. No. Parameter stated Acceptance criteria
1 Melting Point vanillin 81 to 84 0C
Acetanilide 112 to 116 0C
Caffeine 234 to 238 0C
Observations and results :
Sr. No. Reference Substance Std. MP Range Observed MP Result
1 Vanillin 81 to 84 0C
2 Vanillin 81 to 84 0C
3 Vanillin 81 to 84 0C
Sr. No. Reference Substance Std. MP Range Observed MP Result
1 Acetanilide 112 to 116 0C
2 Acetanilide 112 to 116 0C
3 Acetanilide 112 to 116 0C
Sr. No. Reference Substance Std. MP Range Observed MP Result
1 Caffeine 234 to 238 0C
2 Caffeine 234 to 238 0C
3 Caffeine 234 to 238 0C
CONCLUSION :
Done By: Checked By: Approved By :
Date Date Date