DISTRIBUTION:
It is required to prepare one master copy of the SOP. A soft copy of the Master copy shall be securely maintained with the Head of, QA. A set of Hard Controlled copies shall be issued to the Head of the User departments.
1.0 Purpose:
1.1 To lay down the procedure for the Operation of IR Spectroscopy
2.0 Scope
2.1 This SOP shall be applicable for the Operation of IR Spectroscopy of the quality control department at (name of company and location)
3.0 Responsibilities:
3.1 QC Executive/ Designee: To understand the procedure and to apply it in practice.
3.2 QC-head/Designee: To review the SOP and its implementation.
3.3 QA-Head/ Designee: To approve the SOP and ensure its implementation
4.0 Material and Equipment:
4.1 IR Spectroscopy
5.0 Procedure:
Using a graph of infrared light absorbance on the vertical axis versus frequency or wavelength on the horizontal, one can see the interaction of infrared radiation in an IR spectrum., Typical units of frequency used in IR-Spectra are reciprocal centimeters with the symbol cm-1.
5.1 Precaution:
5.1.1 Ensure the work area is clean.
5.1.2 Handle the instrument carefully.
5.1.3 Solute chemical interaction with the solvent must be taken into consideration, especially for compounds having the property of H-bond.
5.1.4 The solvent should not be absorbed in the studied range.
5.1.5 Do not use explosive or flammable samples.
5.1.6 Nothing should be placed on the electronic cover's top.
5.1.7 Check all cables are working properly
5.1.8 Place the instrument in a well-ventilated room
5.1.9 Direct eye exposure should be avoided.
5.1.10 The availability of a proper safety shield is necessary.
5.1.11 Carefully open and close the chamber.
5.2 Operation:
5.2.1 Connect the power cord of the instrument to the mains and switch ON.
5.2.2 Switch on the PC after the beeping sound is heard.
5.2.3 Double-click the icon (IR solution)
5.2.4 Enter the username and password.
5.2.5 Single-click on the measurement in the Menu bar and then click on Initialize.
5.2.6 Check the instrument status on the monitor on the left side of the screen.
5.2.7 All the items such as light sources, laser, beam splitter, and other accessories should be displayed in green.
5.2.8 Click (Data Tab) on the scan parameters window and feed the values as shown below.
5.2.9 Measurement mode ;: % Transmittance
5.2.10 Apodization-Happ Genzel
5.2.11 No. of scans
5.2.12 Resolution: 4 cm-1.
5.2.13 Range: 4000 to 400 cm-1.
5.2.14 Click the Instrument tab and feed the values as shown below.
5.2.15 Beam-Internal
5.2.16 Detector-Standard
5.2.17 Mirror speed -2.8 mm/sec.
5.2.18 Click on more tab and feed the values as shown below.
5.2.19 Normal
5.2.20 Gain-Auto
5.2.21 Monitor
5.2.22 Gain-1
5.2.23 Mode-Power
5.2.24 Click on the Files Tab and do not checkmark on (locked) so that changes of scan parameters can be done.
5.2.25 Put a tick mark on (View Background) in the measurement files area so that the background spectrum will be displayed as the measurement is finished.
5.2.26 Click on (BKG as background) in the measurement files area, and a dialog box will appear on the screen with a message.
5.2.27 Please prepare a sample compartment spectrum will be a background scan.
5.2.28 Cancel OK
5.2.29 Click on OK and background spectrum will be displayed.
5.2.30 Now prepare the sample hold in the sample holder and place it in the sample chamber.
5.2.31 Enter the ID of the sample to be scanned in Compartment and the file name where the data is required to be stored in Data File by clicking
5.2.32 Click on Sample to scan the sample.
5.2.33 The spectrum will be displayed on the screen and it will be saved as per destination given in the Data File.
5.2.34 Click on the View Tab Window to display the measured spectrum in upper and lower windows. The upper window is known as Overview Window and the Lower Window is the Zooming Window.
5.2.35 Right click on either the overview window or the zooming window and then click on Vertical Axis to change
5.2.36 Open the reference spectrum of the concerned sample from Data /Reference/Spectra/Name of the product.
5.2.37 Drag the reference spectra from the Tree View Window on the left side of the screen and place it on the zooming window to overlay with the sample.
5.2.38 Click on File and then click on the Print Preview, select the required report templates, and out the print by clicking on Print.
5.2.39 Fill in the usage log book.
6.0 Abbreviations:
SOP: Standard Operating Procedure
QC: Quality Control
QA: Quality Assurance
IR: Infra-red
7.0 Reference:
User and Maintenance Manual of Shimandzu
8.0 Annexure:
8.1 Annexure I: Usage log book of IR- Spectrophotometer.
9.0 Summary of Changes:
SOP NO.
Effective from Date
Reason for Revision
10.0 Review Stamp
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