STANDARD OPERATING PROCEDURE

Procedure: Operating Differential Scanning Calorimetry (DSC) Analyser

Department/Section
R&D / Instrumental Analysis Laboratory
:
SOP prepared by: Jayshree Gogoi, Subodh Purohit
Version: 1

Purpose:

This Standard Operating Procedure (SOP) states the procedure for analysis carried out using
Differential Scanning Calorimetry (DSC) analyser. DSC is used to measure the amount of
energy absorbed or released by a sample when it is heated or cooled, providing quantitative
data on endothermic and exothermic process i.e. WAT(Wax Appearance Temperature) which
is an exothermic process and WDT( Wax Dissolution temperature) which is an endothermic
process. This SOP must be read and understood prior to the commencement of analysis using
DSC.

Safety Precautions:

1. Before starting any laboratory experimental work, involving the operation of DSC
analyser, the user must ensure that at least the following protective equipment is being
used:
i. Safety Goggles that seal around glasses (not prescription glasses)
ii. Gloves – preferably nitrile
iii. Long pants
iv. Closed-toe shoes
v. Lab Coat
vi. Hair is tied back (if long)

2. Material Safety Data Sheet (MSDS) for each of the hazardous materials that are to be
used must be read thoroughly by the user before the commencement of work.

3. Location of the nearest fire extinguisher must be well known to the user.

4. To avoid condensation of fluids in experimental methods operating at temperature

below 25°C, purging the surroundings of the instrument’s furnace with a dry gas ( N 2
or Ar) is necessary. The flow rate of the dry gas must be maintained at 200 ml/min as
it aids in creating a definite furnace atmosphere in the sample chamber by flushing out
air and any volatile products that are evolved from the sample.

Potential Hazards:

1. The SOP outlined for handling, storing and use of gas cylinders must be thoroughly
read, understood and followed while working with gas cylinders required in DSC
analysis.

Last review date: 02.07.2020

Creation date: 02.07.2020 Page 1 of 3
Next review date: 01.07.2021
 STANDARD OPERATING PROCEDURE
2. The equipment may operate at high temperature range based on specific experimental
parameters and hence use of forceps for placing or removing the crucible in the
carousel/sample holder is compulsory.

Operation:

1. Before sampling, the sample must be homogenised by heating at constant temperature

depending on specific sample requirement in a constant heating water bath with
occasional stirring by a glass rod.
2. Free water present in the sample, if any, must be separated using a separating funnel,
which may otherwise lead to erroneous result.

3. For liquid sampling, a micro syringe must be used to place the sample in the crucible.
The user must prudently choose the correct size of the micro syringe and crucible to
meet the experimental requirement.

4. The user must ensure that the instrument is first plugged in and then the main power
supply is switched on. The user must then turn on the instrument mains.

5. The user must also ensure that the specified flow rate of the dry gas viz. 200 ml/min.
is maintained for proper functioning of the instrument.

6. The sealed reference crucible must be placed in the reference slot and must not be
removed frequently so that multiple runs can be performed with the same reference
crucible.

7. The sealed crucible containing the test sample must be placed in the designated
sample carousel and the chiller connected to the system must be powered on.

8. The user must open the STARe software on the desktop of the computer to connect
the software and DSC analyser.

9. The user must then create a new method for the experiment and fill in the required
experimental parameters or select from the existing methods and start the
measurement.

10. During a measurement, data is continuously transferred from the DSC module to the
software and is presented as an online curve in the module control window. The
original model-specific operation manual may be referred for details on method
selection, data analysis and more.

Cleaning/ Spills/ Incidents:

1. The special brush located in the DSC kit must be used to clean the inside of the
equipment if required.

Last review date: 02.07.2020

Creation date: 02.07.2020 Page 2 of 3
Next review date: 01.07.2021
 STANDARD OPERATING PROCEDURE
2. The outer surface of the instrument must be wiped with lint free cloth on weekly basis
so that there is no dust particles on the instrument.

3. If a FIRE breaks due to technical fault in the instrument, the area should be evacuated
immediately. The user must ACTIVATE THE FIRE ALARM, AND CALL
7333/2800444. The user should stay close to the building to inform emergency
personnel of what started the fire and what other items are in the immediate area of
the fire

Departmental Safety Committee Signature & Date

Shri P. K. Dhodapkar
GM – R&D (IOR/EOR) & Chairman

Shri Shivananda Boruah

Dy. CRS and DSO – R&D

Sectional In-charge (OFO)

Approving Authority

Dr. Neeraj Mathur

CGM – R&D and HoD

Last review date: 02.07.2020

Creation date: 02.07.2020 Page 3 of 3
Next review date: 01.07.2021