To lay down the procedure for operation and calibration of Perkin-Elme.
1.0 PURPOSE:
1.1 To lay down the procedure for operation and calibration of Perkin-Elmer FT-IR Spectrometer.
2.0 SCOPE:
2.1 This procedure is applicable in Quality Control Department (Block-D).
3.0 RESPONSIBILITY:
3.1 Junior Assistant/Senior Assistant – QC
3.2 Senior Executive – QC
4.0 ACCOUNTABILITY:
4.1 Manager – QC
4.2 Asst. Manager – QC
5.0 PROCEDURE:
5.1 Spectrum measurement of samples as KBr pellet:
5.1.1 Turn on the P.C.
5.1.2 Double click on the spectrum icon.
5.1.3 Login window appears. Enter the login name and click O.K.
5.1.4 Background correction window appears with the message ‘New back ground required collect a background’. Click background.
5.1.5 Background correction window appears with the message ‘Please ensure sample area is empty and beam path is not obstructed’.
5.1.6 Open the sample chamber at the front side by lifting it upwards. Check and ensure that the pellet holder is not having any pellet and is empty. Then click O.K.
5.1.7 Background correction window appears with message ‘Collecting background spectrum’. Once the background collection is over, then the message will be ‘Ready for sample scan’. Click O.K.
5.1.8 Spectrum v5.0.1 – [Graph#1] window appears. Now place the working standard pellet in the pellet holder and keep it inside the chamber. Click instrument menu in the menu bar and click scan.
5.1.9 Spectrum one scan and instrument set up window appears. Enter the sample name, description and comment as required.
5.1.10 Click on scan icon in the menu bar. Set the scan parameters as per STP.
5.1.11 Click on instrument icon in the menu bar. Set the instrument parameters as per STP.
5.1.12 Click on the scan button in the right side of the window above exit scan.
5.1.13 Scanning takes place spectrum one scan and instrument set up window appears showing spectrum and data regarding number of scanning.
5.1.14 Once scanning is over, instrument auto-save to disk window appears with overwrite and cancel icons. Click on overwrite icon.
5.1.15 Spectrum v5.0.1 – [Graph#1] window appears with spectrum and name at the bottom left corner.
5.1.16 Click process in the menu bar and go to baseline/automatic correction and click it.
5.1.17 The original spectrum is shown in black colour and the baseline corrected spectrum is shown in blue colour. The names also are shown with corresponding colors at the bottom left corner. Click on the name shown in black and delete it using keyboard button.
5.1.18 Click process in the menu bar and go to smooth/automatic smooth and click it.
5.1.19 The baseline corrected spectrum is shown in blue colour and the smoothened spectrum is shown in black colour. The names also are shown with corresponding colors at the bottom left corner. Click on the name shown in blue and delete it using keyboard button.
5.1.20 Click on the name of the sample in the bottom left corner. Click view in the menu bar and go to label peaks and click it. The peaks are labeled with peak numbers.
5.1.21 Click file in the menu bar and go to save as and click it. Enter the standard name in the file name field and click save. The standard spectrum is saved.
5.1.22 Replace the working standard pellet with the sample pellet in the chamber.
5.1.23 Click instrument menu in the menu bar and click scan.
5.1.24 Repeat points 5.1.9 to 5.1.20.
5.1.25 Click file in the menu bar and go to save as and click it. Enter the sample name in the file name field and click save. The sample spectrum is saved.
5.2 Spectrum measurement of liquid samples:
5.2.1 Instead of placing pellet holder in the chamber, place NaCl cell with standard and sample and follow the same procedure as described for above KBr pellet.
5.3 Spectrum measurement of Polystyrene film:
5.3.1 Set the resolution of 2.00 cm-1 instead of 4.00 cm-1.
5.3.2 Click on the symbol given below in Beam tab.
Select polystyrene and click OK.
5.3.3 Perform scanning in replicate.
5.4 Comparing sample spectrum with standard spectrum:
5.4.1 In the spectrum v5.0.1 – [Graph#1] window, click set up in the menu bar and go to compare and click it.
5.4.2 Compare set up window appears. Click on browse icon. Select the appropriate standard spectrum by clicking on it and click open.
5.4.3 The name of the selected spectrum appears in the reference part of the compare set up window. Click O.K.
5.4.4 In the spectrum v5.0.0 – [Graph # 1] window. Click file in the menu bar and go to open and click it. Select the appropriate sample spectrum by clicking on it and click open.
5.4.5 Click process in the menu bar and go to compare and click it.
5.4.6 Spectrum v5.0.1 – [Graph # 2] Window appears with comparative spectrums. Click file in the menu bar and go to copy to report and click it. The report builder window appear and after few seconds the spectrum appears in the lower part of the report format.
5.4.7 Click on the compare – (Standard Name) window. Click file in the menu bar and go to copy to report and click it. Report builder window appears with spectrum in the lower part and comparative report.txt in the upper part of the report format.
5.4.8 Click layout in the menu bar of the report builder window and go to actual size and click it. Check the report.
5.4.9 Click file in the menu bar of report builder window and go to print and click it.
5.5 Calibration:
5.5.1 The following parameters shall be checked in the calibration of the instrument.
5.5.2 Wave number accuracy and repeatability:
5.5.2.1 Accuracy: Difference between the observed wave numbers and standard wave numbers as per annexure – I for two successive scans shall not be more than ± 1.5 cm-1 for the wave numbers 3060.00, 2849.50 and 1942.90 cm-1 and not more than ± 1 cm-1 for the wave numbers 1601.20, 5832.00, 1154.50 and 1028.30 and 1028.30
5.5.2.2 Repeatability: Difference between the wave numbers of two successive scans is not more than ± 1 cm-1.
5.5.3 Resolution:
5.5.3.1 Difference between the %T of base and peak shall be not less than 18% for the wave numbers 2851.00 cm-1 and shall be not less than 12% for the wave numbers 1583.00 cm-1.
5.6 Calibration frequency: Once in a three months.
5.7 Making the print out of the report:
5.7.1 Click file in the menu bar and go to open and click it. Select the spectrum by clicking it and click O.K. Click view in the menu bar and go to label peaks and click it. The peaks are labeled with peak numbers.
5.7.2 Click file in the menu bar and go to copy to report and click it.
5.7.3 Report builder window appears and after few seconds the spectrum appears in the lower part of the report format.
5.7.4 Select the required template from file menu as per requirement.
5.7.5 Click file in the menu bar of the spectrum window and go to status and click it.
5.7.6 Status window appears. Click on to report.
5.7.7 Report builder window appears with spectrum in the lower part and report.txt in the upper part of the report format.
5.7.8 Click layout in the menu bar of the report builder window and go to actual size and click it. Check the report.
5.7.9 Click file in the menu bar of report builder window and go to print and click it. The report is printed.
Note: 1. Do not switch off the instrument.
2. Close the sample compartment chamber immediately after placing and after removing the samples.
Calibration, perkin elmer, spectrometer
