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Calibration of FT-IR Spectrophotometer


Learn how to calibrate the FT-IR Spectrophotometer used in identification of Pharmaceutical products.

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 upÞ validation Þ System suitability.
Instrument may ask for gathering the configuration, 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 Þ scan Þ Instrument Þ Advanced.
Keep Apodization ‘none’ & scan speed 0.1cm/s.
Instrument may ask for collecting new background, then click OK.
Go to Instrument Þ Validate Þ 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.
Difference 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 Þ Peak table & take its print .
Peaks (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 Þ validation Þ 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 Þ validate Þ 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 slide holder instrument configuration.
· Abscissa spectrum of polystyrene film with identified peaks’ table for wave number calibration.
· Abscissa spectrum of polystyrene film (showing %T at 2851cm-1, 2870cm-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 – 

  Model – 

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 of Wave Number Scale -
Observed Wave Number cm-1
Minimum Tolerance
cm-1
Maximum Tolerance
cm-1
3058.5
3061.5
2848.0
2851.0
1941.4
1944.4
1600.2
1602.2
1582.0
1584.0
1153.5
1155.5
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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Anonymous said...

This is exactly what I've been looking for.

Thanks!

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