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Thursday, September 26, 2013

CALIBRATION OF FT-IR SPECTROPHOTOMETER

Check that all the connections of the instrument are proper.
Ensure that printer is attached to the instrument.
Attach sample compartment.
Log in the software.

Go to set up > Validation > System suitability.
Instrument may ask for gathering the configuration, and then click OK.
System suitability set up will appear.
Go to checks & select only Abscissa, screen report.
Go to archive & set archive prefix as required & click OK.
Resolution
Go to instrument > Scan > Instrument > Advanced.
Keep Apodization 'none’ & scan speed 0.1 cm/s
Instrument may ask for collecting new background, then click OK.
Go to instrument > Validate > system Suitability & click OK.
Instrument should display ‘ system suitability test pass’.
Scroll the report from original path for display, click print icon & take print out.
Abscissa spectrum of polystyrene film will be displayed.
Go to graph format icon & select the range 1600 to 1580.
Zoomed spectrum will appear, then collect the continuous curser & label at about 1583 cm-1 & 1589 cm-1, find out %T at these wave numbers & find out the difference between two %T.
Differences should be not less than 12%T.
Similarly zoom between 2840 cm-1 to 2880 cm-1 & label at 2851 cm-1 & 2870 cm-1, find out %T at these wave numbers & find out difference.
Difference should be not less than 18%T.
Then adjust the scale to 4000 to 450 cm-1 & take print outs.
Verification of wave number scale
Go to Process > Peak table > take its print.
Peak (transmission minima) should be observed at the wave numbers as follows, with in the tolerance limit.
Wave number cm-1
Minimum Tolerance cm-1
Maximum tolerance cm-1
3060.0
3058.5
3061.5
2849.5
2848.0
2851.0
1942.9
1941.4
1944.4
1601.2
1600.2
1602.2
1583.0
1582.0
1584.0
1154.5
1153.5
1155.5
1028.3
1027.3
1029.3

Remove sampling compartment.
Attach the diffuse reflectance sampling accessory.
Collect the background with KBr.
Go to set up > Validation > System suitability.
Set up will appear.
Go to checks & select only Abscissa, screen report.
Go to archive & set archive prefix as required & click OK.
Go to Instrument > Validate > System suitability.
Click OK.
Instrument should display System suitability test passes.
Report will be displayed, click print icon & take print out.
Maintenance / Repairs
Whenever instrument is out of order, then put the tag as Out of Calibration & get it repaired. After repair calibrate the instrument before use.
Frequency:
Once in three months.
Attachments
Enclose following attachments with the calibration report.
-          System suitability check report for side holder instrument configuration.
-          Abscissa spectrum of polystyrene film with identified peaks table for wave number calibration.
-          Abscissa spectrum of polystyrene film (showing %T at 2851 cm-1, 2870 cm-1, 1583 cm-1, 1589 cm-1).
-          System suitability check report for diffuse reflectance instrument configuration.
Note: Words in italics stand for instrument tabs.

 

CALIBRATION REPORT OF FT-IR SPECTROPHOTOMETER


Reference -                                                                                                Date –
Frequency – Once in three Months.                                                Instrument No. –
Make –
   1.0   Resolution:

Difference Between % T at 2851 cm-1 and 2870 cm-1
Difference Between %T at 1583 cm-1 and 1589 cm-1
Limit
NLT 18%
NLT 12%
Actual


   2.0   Verification wage Number Scale:
ObservedWave number cm-1
Minimum Tolerance cm-1
Maximum tolerance cm-1
3060.0
3058.5
3061.5
2849.5
2848.0
2851.0
1942.9
1941.4
1944.4
1601.2
1600.2
1602.2
1583.0
1582.0
1584.0
1154.5
1153.5
1155.5
1028.3
1027.3
1029.3
   3.0   System suitability after attachment of diffuse reflectance sampling accessory: Complies / Does Not        Comply.
   4.0   Conclusion: Calibration is satisfactory / Not satisfactory.
   5.0   Next Calibration Due On:

Done By:
Date:
Checked By:
Date:

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