Operation & Calibration of Melting Point Apparatus

Operation & Calibration of Melting Point Apparatus

SOP

1.0 WHAT
This document details the procedure for the Operation of Melting Point Apparatus
2.0 WHY
It is the policy of  the written procedure will be followed for the Operation of Melting Point Apparatus and its use monitored in order to ensure that the operation is carried uniformly by any of the analyst so as to avoid any deviation from the procedure.
3.0 WHEN
This procedure is to be applied at the time of Operation of Melting Point Apparatus
4.0 RESPONSIBILITY
Persons along with their responsibilities are given below:

S.
No

Designation

Responsibility

 

01

Analyst

To prepare the
SOP and follow the SOP.

02

Section In Charge

To ensure
implementation of SOP.

03

QA In Charge

To ensure
implementation of SOP.

5.0 PROCEDURE

5.1 OPERATION

5.1.1 Powder the sample as fine as
possible.

5.1.2 Dry it at a temperature if specified
in the individual monograph.

5.1.3 Heat
the bath until the temperature is about 10 below the expected melting  temperature.

5.1.4 Continue
the heating and note the temperature at which the column of the sample 

collapse  definitely against the side of
the tube at any point, when melting may be considered to have 

begun and note also the temperature at
which the sample becomes liquid throughout as seen by the 

formation of a
definite meniscus.

5.1.5  Record
the reading of Melting point.

5.1.6  After
observation remove the capillaries/ sample column from oil bath.

5.1.7  After
completing the test switch off the instrument properly.

5.2 CLEANING

5.2.1  Clean
the instrument  with Clean Cloth

5.2.2  Remove
the  Silicon  Oil frequently

5.3   Precaution:

5.3.1 Keep the instrument
clean and Dust free.

5.3.2  Do
not go to the over limit of temperature as prescribed.

5.3.2 All
the knobs are very delicate and should be handled carefully.

6.0 CALIBRATION

6.1  PROCEDURE

6.1.1  Melting point apparatus is calibrated
by taking the melting points of vanillin, acetanilide, 

sulphanilamide and
caffeine anhydrous.

6.1.2  Using the standard calibrated
thermometer the temperatures at which the materials start 

melting, & at
which they completely melt, are read and recorded.

6.1.3  The melting points of these materials
should fall within the given limits; then the instrument is

calibrated.

S. No.

SUBSTANCE

LIMITS

 

1.

 

Vanillin

 

81 to 83 Deg. C

2.

Acetanilide

114 to 116 Deg. C

3.

Sulphanilamide

164.5 to 
166.5 Deg. C

4.

Anhydrous Caffeine

234 to 237 Deg.C

6.2 FREQUENCY OR CALIBRATION: 

Quarterly or after any maintenance work.

Record the data on APPENDIX I Format                                                                                       

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