Operation and Calibration of DSC apparatus

 
1.0    PURPOSE: 

1.1    To lay down the procedure for operation and calibration of  Mettler Toledo DSC Apparatus.

2.0    SCOPE.

2.1    This SOP is applicable for operation and calibration of Mettler Toledo DSC apparatus in Quality control lab.

3.0    RESPONSIBILITY

3.1    Executive-QC

4.0    ACCOUNTABILITY

4.1     Asst. Manager-QC

5.0    PROCEDURE

5.1    Operation of DSC apparatus.

5.1.1    Switch on the computer.
5.1.2    Press the main power supply switch, located on the rear panel of the module to on the instrument.
5.1.3    Double click the STARe software icon on the desktop to start the software.
5.1.4    The STARe soft ware main menu bar appears.
5.1.5    Click DSC822e/500/850 icon on the scroll bar to display the main windows. 

5.2    Operation using existing method:

5.2.1    Click File/open method, methods shall be displayed.
5.2.2    Select the required method, Click ok to open the method.
5.2.3    Enter the sample name and size.
5.2.4    Place the reference and sample crucibles in the sample chamber.
5.2.5    Click control/start experiment and then send experiment.
5.2.6    “Wait for insert temperature” message shall be displayed on the bottom left corner of the screen. , Click OK.
5.2.7    “Wait for insert sample” message shall be displayed on the bottom left corner of the screen. , Click OK.
5.2.8    The messages “ Going to start the temperature” “ Setting and measurement ” shall be displayed and the measurement starts.
5.2.9    After completion of measurement reset the furnace to room temperature and switch off the instrument.

5.3    Creating new method:    

5.3.1    Click File/New method, new method window shall be displayed.
5.3.2    Select “Add Dyn” icon and enter the required parameters i.e Temp.start,
Temp.END and Heating rate.
5.3.3    Click on” Gas” icon, segment gas window displays and select the required gas.
5.3.4    Click on “Pan” icon, select the type of pan required and click ok.
5.3.5    Select save icon and save the method with method name.

5.4    Sample preparation:

5.4.1    Weigh an empty crucible and record the weight.
5.4.2    Place the crucible on the crucible holder and fill the sample using the funnel.
5.4.3    Weigh the crucible with sample and record the sample weight.
5.4.4    Keep the crucible in the matrix of the crucible sealing press.
5.4.5    Place a crucible lid on the crucible holder perforated by using the needle provided in the kit.
5.4.6    Close the sample crucible with lid and rotate the lever of the sealing press once.
5.4.7    With plunger pressure the crucible in matrix and crucible gets sealed.
5.4.8    Place the sealed sample crucible and empty crucible in the sample chamber indicated by “S” and “R” respectively.

5.5    Evaluation:

5.5.1    After completion of measurement click “database1” icon on the scroll bar.
5.5.2    Select “Functions/ Evaluate” and STARe evaluation window shall be displayed.
5.5.3    Click “File/Open curve “, to display the list of measurements.
5.5.4    Select the required curve measurement and click open to display the curve window.
5.5.5    Double click on X -axis and Y- axis to display full scale graph
5.5.6    Click “TA/Integration”, the peak gets integrated and result shall be displayed.
5.5.7    Click “File/ Plot”  for report print out.
5.5.8    Selcet save icon and save the Evalution method with name.

5.6    Calibration of DSC apparatus:

5.6.1    Indium Check:

5.6.1.1    Select method check DSC ˆ exo In.
5.6.1.2    Set the start temperature of the furnace as 120°C and end temperature as 180°C.
5.6.1.3    Weigh about 4 to 8 mg of Indium standard in a crucible and seal it with the perforated lid using the sealing press.
5.6.1.4    Place the reference and sample crucible in the sample chamber and record the measurements.

5.6.2    Zinc check:

5.6.2.1    Select method check DSC ˆ exo In.
5.6.2.2    Set the start temperature of the furnace as 370°C and end temperature as 450°C.
5.6.2.3    Weigh about 2 to 5 mg of Zinc standard in a crucible and seal it with the perforated lid using the sealing press.
5.6.2.4    Place the reference and sample crucible in the sample chamber and
 record the measurements.
5.7    Record the results in the format No.xxxxx.
5.8    Calibration frequency: Once in 6 months.
5.9    Acceptance criteria:

Dsc apparatus, mettler toledo, add dyn, gas, pan, perforated