‫ م‬1:47 2023/‫‏‬7/‫‏‬30 SOP on Operation and Calibration of Melting Point Apparatus - Pharmaceutical Guidelines

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SOP on Operation and Calibration of Melting Point Apparatus

SOP on Operation and Calibration of Melting Point

Apparatus
Leave a Comment / By Admin / September 12, 2020

Standard Operating Procedure (SOP) for Operation and Calibration of Melting Point
Apparatus used for analysis / identification of starting materials (Raw Material – API &
Excipient) in Quality Control Laboratory.

Table of Contents
1. Operation and Calibration of Melting Point Apparatus
1.1. 1.0 PURPOSE:
1.2. 2.0 SCOPE:
1.3. 3.0 REFERENCES – SOP FOR MELTING POINT APPARATUS:
1.4. 4.0 RESPONSIBILITY – SOP FOR MELTING POINT APPARATUS:
1.5. 5.0 PROCEDURE – MELTING POINT APPARATUS:
1.5.1. NOTE: Be sure about the settings (initial temperature and °C/min) as they cannot be
viewed or changed while heating process is ON.
1.6. 6.0 ANNEXURES – MELTING POINT APPARATUS:
1.6.1. Annexure -1 : Format for Calibration Record of Melting Point Apparatus
1.6.2. Annexure -2 : Format for Calibration Status label

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Operation and Calibration of Melting Point Apparatus

1.0 PURPOSE:

The purpose of this SOP is to describe the procedure for operation, calibration
and maintenance of Melting Point Apparatus.

2.0 SCOPE:

This SOP is applicable to the following Melting point apparatus at Quality

Control Department in pharmaceutical for Make : Polmon and Model MP-96.

3.0 REFERENCES – SOP FOR MELTING POINT APPARATUS:

Operation Manual supplied by the manufacturer

SOP for Maintenance of Laboratory Instruments

SOP for Preparation of internal and external (Third Party) Calibration schedule
and calibration practices

4.0 RESPONSIBILITY – SOP FOR MELTING POINT APPARATUS:

Analyst shall be responsible for:

To operate the instrument as per the SOP.

Calibrate the instrument as per the SOP.

To carry out the documentation as per the SOP.

Quality Control Head or Designee shall be responsible for :

To approve the calibration of instrument verifying against SOP.

To provide training to all the concerned persons before implementing the SOP.

Execute the out of calibration in case of calibration failure and in case of

breakdown, intimate to Quality Head.
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To ensure the operation and calibration of the instrument is carried out as per
the SOP.

To ensure proper documentation as per the SOP.

Quality Assurance shall be responsible for:

To ensure the implementation of the system as per the SOP.

5.0 PROCEDURE – MELTING POINT APPARATUS:

General Procedure for handling of Melting Point Apparatus

Follow the SOP on Instrument/Equipment usage log book, for the entry of
usage of the instrument.

In case of any maintenance of instrument, follow SOP on Maintenance of

Laboratory Instrument.

Maintain the third party calibration schedule and the internal calibration
schedule for the instrument as per SOP, Preparation of internal and external
(Third Party) calibration schedule and calibration practices.
Operational procedure

Check the calibration status of the instrument.

Switch ON power supply by switching on the main supply and switch provided
on backside of the instrument.

Press the “FUNCTION” Key to set initial temperature. The “INI TEMP” LED blinks
and parameter is displayed in the display.

Use “↑ ” or “ ↓ “ keys to set the initial temperature.

Set the initial temperature to 10°C below the expected melting point and the
initial temperature should be (15 – 25 )°C above the bath temperature to
overcome undershoot or overshoot of temperature, the maximum melting
range for the operation of the instrument is 350°C.
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Press the “FUNCTION” key to set “°C/min”, “°C/min” LED blinks and the
parameter is displayed in the display.

Use “↑” or “↓” keys to set the rate of heating.

Press “FUNCTION” key. The bath temperature is displayed.

Press “START” key. The “INI TEMP” and “°C/min” LED blinks one after another
displaying the corresponding setting with an interval of 2.5 sec.

NOTE: Be sure about the settings (initial temperature and °C/min) as they cannot be
viewed or changed while heating process is ON.

Press “START” key. The oil bath temperature is raised to the initial During this
period “INI TEMP” LED glows continuously and “HEATER” LED glows
continuously or blinks.

Insert the capillaries in the bath.

Press “FUNCTION” key to start Rate of heating (i.e. °C/min). During this period
“°C/min” LED glows continuously and “HEATER” LED blinks.

Watch the sample through magnifying lens.

Press “STORE” key at the beginning of Melting point, “T1” LED glows
continuously indicating that initial melting temperature is stored.

Press “STORE” key again to store final melting point. “T2” LED glows
continuously indicating that final melting point temperature is stored.

To view initial and final melting point temperatures press “STORE” key to view
initial melting point temperature, “T1” blinks to indicate that the displayed
temperature is initial melting point.

Press “STORE” key again to view final melting point temperature, “T2” LED blinks
to indicate that the displayed temperature is final melting point
Calibration Procedure of Melting Point Apparatus

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Calibrate by using Melting Point reference standard.

Calibration Frequency: Monthly ± 3 days.

The four Melting Point standards Vanillin, Caffeine, Acetanilide and

Sulfanilamide shall be used.

Reduce the reference standard to very fine powder.

Treat the reference standards as given below:

Vanillin: Do not dry.

Caffeine: Dry portion over silica gel for 16 hours.

Sulfanilamide: Dry portion over silica gel for 16 hours.

Acetanilide: Dry portion over silica gel for 16 hours.

Charge the capillary, one end of which is sealed with sufficient quantity of
reference standard to form a column in the bottom of the tube 2.5 mm to 3.5
mm height when packed down as closely as possible by moderate tapping on
a solid surface. Surface. (There should not be gap in the column).

Heat the block until the temperature is about 10°C below the expected melting
point and continue heating at a rate of temperature increase of about 1° C per
minute.

Insert the capillary tube in the melting point apparatus when the temperature is
about 5° C below the lower limit of the expected melting range and continue
heating until melting is complete.

Follow the above steps given in the procedure part.

Note the melting point of the reference substance.

Record the same in the calibration record.

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6.0 ANNEXURES – MELTING POINT APPARATUS:

Annexure -1 : Format for Calibration Record of Melting Point Apparatus

Instrument Melting Point

Name Apparatus

Instrument
Make/Model
Code

Calibration Monthly ± 3
Location
frequency days

Calibration Next Calibration due

Date on

Procedure

Reduce the standard to very fine powder or as recommended on the label of

respective reference standard.

Treat the reference standards accordingly.

Charge the capillary, one end of which is sealed with sufficient quantity of
reference standard to form a column in the bottom of the tube 2.5 mm to 3.5
mm height when packed down as closely as possible by moderate tapping on a
solid surface. (There should not be gap in the column.)

Heat the block until the temperature is about 10° C below the expected
melting point and continue heating at a rate of temperature increase of about
1° C per minute.

Insert the capillary tube in the melting point apparatus when the temperature is
about 5°C below the lower limit of the expected melting range and continue
heating until melting is complete.

Record the temperature at which the last particle passes into the liquid phase.

Remove the capillary tubes care fully and dispose it off after cooling.
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Observation Table:

Melting Point Calibration Observed

Sr.No. Limit
Standard Standard No. Melting Range

81°C to
1 Vanillin
83°C

112°C to
2 Acetanilide
115°C

163°C
3 Sulfanilamide
to166°C

235°C to
4 caffeine
239°C

Remarks : The instrument is calibrated & qualified / Out of calibration & not
qualified for use.

Calibration : Scheduled / Not scheduled ( Reason : ______________________

Annexure -2 : Format for Calibration Status label

CALIBRATION STATUS

Instrument : ___________________________ ___________ Code :

___________________ Model: ______________________
Frequency______________________________________________ Done on :
____________________________ Due on :____________ Status : Instrument found
satisfactory for analytical use Done By : __________________________ Checked By :
__________ Date : ___________________________ Date : ________________

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