Melting Point Apparatus

Standard Operating Procedure (SOP) for Operation and Calibration of Melting Point Apparatus in Quality Control Laboratory.

1.0 Objective :

- To lay down a procedure operation and Calibration of Melting Point apparatus.

2.0 Scope :

- This SOP is applicable for operation and calibration of Melting point apparatus in Quality Control.

3.0 Procedure : Operation and Calibration of Melting Point Apparatus :

- OPERATION – Melting Point Apparatus:
- Ensure that Melting Point Apparatus is clean and free from dust.

- When the Melting Point Apparatus is Powered On or Reset key is pressed, it gets initialized and display reads,

LABINDIA MELTING RANGE APPRATUS

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MODEL: MR-Vis+ Version: V X.X

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1) Prog 2) Run 3) Print 4) Config T°C: XX.X

- Main Menu Functions of Melting Point Apparatus software.

Prog’: To Add (create) / edit, view, copy, delete programs.

Run’: To start the RUN desired program for Melting range determination.

Print’: To view the results of last sample Run ; To obtain a hard copy of program parameter listing, Result report, Graph print out (for AUTO operation only) & Calibration report.

Config’: To set date & time and to select data transfer to PC/Printer.

- Procedure for the operation of Software – Melting Point Apparatus :

- Turn on the Melting Point Apparatus system and windows shall display EDC icon

- Then double click the icon EDC icon for further proceeding

- After opening the icon on window, window will display another screen showing LABINDIA EDC 21 as shown below in the image.

- Go to the file and file shall display four options as user Account Window, Front Panel, Audit Trial and Exit.

- Then double click on front panel for the next step.

- After opening front panel, window shall display front panel screen.

- Then click Connect Option

- After connecting the Melting Point Apparatus instrument new screen shall open requiring User Name and Password.

- Then go to the Instrument Name shown as MRVIS +.

- After clicking MRVIS + option bulb shall glow green and it indicates right selection of the Melting Point Apparatus instrument under operation.

- Ensure following before the Sample Analysis run is Started on Melting Point Apparatus.

- - The round Cover-slip on the Furnace Lid is clean (not foggy)

- - The surface of the Furnace shall be clean from any foreign particles for a good thermal contact of the slide.

- - The presence of foreign particle will create the thermal difference and leads to erroneous results.

- - There shall not be Direct Air Draft in the furnace direction.

- To Select ‘RUN’ from main menu options press ‘2’.

- The Lamp will be switched ON automatically as soon as the Furnace temperature reaches 5°C below Set Temperature.

- In AUTO operation, as soon as the sample starts melting, the Photo Sensor detects the start and instrument automatically records it and displays this temperature as ‘Set Temperature’ Display reading,

- After melting of sample test is getting completed out, now, print the result by selecting the concerned results.

CALIBRATION OF MELTING POINT APPARATUS :
- Frequency : 6 Month ±3 days

- Tolerance:

1	Vanillin	81°C to 83°C
2	Sulphanilamide	163.5 °C to166.0°C
3	Acetanilide	114 °C to 116°C
4	Caffeine	234°C to 237°C

- Set The Method Using Following Parameter:
- Select program from main menu options by pressing <1> key.

- Select ADD from menu by pressing 1 and enter by pressing enter button.

- Obtain program no., say 1 and press enter key.

- Enter sample name by using alphanumeric keys and then press enter.

- Select the sample preparation type by selecting 1 for Slide and 2 for Capillary and then press enter.

- Select mode of heating by selecting 1 for Heat mode and 2 for Heat & Cool mode and then press enter.

- Ten select operation (1) Auto (2) Manual and press enter key.

- Use numeric keys to enter set temperature value & press enter key.

- Enter the Furnace temperature cut off limit using numeric keys.

- Enter heating rate 1ºC.

- Press escape to return to main menu screen.

- Ensure the sample is in the form of fine powder.

- Use only standard capillary tubes with one end sealed.

- Take the fine powder of vanillin about 3 to 4mm height in capillary tube and packed down as closely as possible by moderate tapping on a solid surface.

- Operate the instrument and set the melting range of vanillin.

- Keep the capillary tube filled by vanillin; wait for the material to melt and after sometimes instrument display the melting range of vanillin.

- Repeat the procedure for Acetanilide, Sulfanilamide and Caffeine respectively.

- Enter details in instrument log book.

- Record the observation in Annexure – I

- Prepare the calibration tag and affix it on the equipment.

- Enclose the old calibration tag with record and don’t throw it.

- If the variation is not within the specified tolerance limit:

- Label the equipment with a tag “out of calibration”

- Inform to the department head

- Don’t use equipment until all errors are rectified

- After rectification ,again calibrate the equipment and record the observations

- If any discrepancy is observed during calibration or operation of the instrument affix the under maintenance label on the instrument.

4.0 Annexure

Annexure – I : Calibration Record of Melting Point Apparatus

Make : ………………. Eq. No. : ……………….

Model No. : ………………. Calibration Frequency : 6 Month ± 3 days

Date of Calibration : ………………

Sr. No.	Reference Standard	Sample detail	Observed Melting Point (°C)	Limit
1.	Vanillin	B. No.: Mfg. Date:		81 – 83°C
2.	Acetanilide	B. No.: Mfg. Date:		114 – 116°C
3.	Sulphanilamide	B. No.: Mfg. Date:		164.5 – 166.5°C
4.	Caffeine	B. No.: Mfg. Date:		234 – 237°C

Remarks: The observed values comply / does not comply the acceptance criteria and the equipment can be / cannot be used for routine analysis.

Next Calibration due date : ………….

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