- 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.
- The 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 > scan > Instrument > Advanced.
- Keep Apodization ‘none’ & scan speed 0.1cm/s.
- The instrument may ask for collecting new background, then click OK.
- Go to Instrument > Validate > system Suitability & click OK.
- The instrument should display ‘System suitability test pass’.
- Scroll the report from the 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 wavenumbers & find out the difference between two %T.
- The 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.
- The difference should be not less than 18%T.
- Then adjust the scale to 4000 to 450 cm-1 & take printouts.
- Verification of wave number scale.
- Go to Process > Peak table & take its print.
- Peaks (transmission minima) should be observed at the wave numbers as follows, within the tolerance limit.
Wave number cm-1 Minimum Tolerance cm-1 Maximum Tolerance cm-1
3060.0 3058.5 3061.52849.5 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
After repair calibrate the instrument before use.
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.
- The instrument should display ‘System suitability test passes.
- The report will be displayed, click print icon & take print out.
Maintenance/ Repairs
Whenever the 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
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Reference –
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Date -
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Frequency - Once in three Months.
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Instrument No. -
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Make –
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Model –
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1.0
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Resolution:
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Difference Between % T at 2851 cm-1 and 2870 cm-1
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Difference Between % T at 1583 cm-1 and 1589 cm-1
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Limit
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NLT 18%
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NLT 12%
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Actual
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2.0
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Verification of Wave Number Scale -
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Observed Wave Number cm-1
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Minimum Tolerance
cm-1
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Maximum Tolerance
cm-1
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3058.5
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3061.5
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2848.0
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2851.0
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1941.4
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1944.4
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1600.2
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1602.2
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1582.0
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1584.0
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1153.5
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1155.5
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1027.3
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1029.3
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3.0
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System suitability after attachment of diffuse reflectance sampling accessory : Complies / Does Not Comply.
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4.0
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Conclusion : Calibration is satisfactory / Not satisfactory.
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5.0
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Next Calibration Due On :
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Done By :
Date :
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Checked By :
Date :
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This is exactly what I've been looking for.
ReplyDeleteThanks!
In the SOP of my labs tolerance limits for 1942, 2849 and 3060 wavelength is just ± 1.0, however in this example you use ±1.5, which is the source of that difference. Because my equipment has -1.13 at 3060.0. Thanks in advance
ReplyDelete