| Operation and Calibration of Fourier Transform Infrared Spectroscopy (FT-IR) |
1.0 OBJECTIVE To lay down the procedure for the operation and calibration of Fourier Transform Infrared Spectroscopy (FT-IR). 2.0 SCOPE This SOP is applicable for Operation and Calibration of Fourier Transform Infrared Spectroscopy (FT-IR) in quality control department. 3.0 RESPONSIBILITY QC – Officer/ Sr. Officer /Executive/Sr. Executive and above. 4.0 ACCOUNTABILITY Head-QC 5.0 PROCEDURE 5.1 Basic Operation 5.1.1 Switch on the instrument and computer attached to the instrument taking care that while switching on the instrument only UATR accessory shall be placed in the instrument. 5.1.2 Double click on the spectrum Icon to enter into software & the spectrum login dialog is displayed. 5.1.3 Enter the user name and password in the new opened window and click . 5.1.4 Now the system shall be asking to select an instrument(If ask). Select an instrument and click on . 5.1.5 Insert the accessory using which sample is to be scanned. 5.1.6 Click on icon the toolbar if the path for the beam is clear otherwise clear it. 5.1.7 System shall be start collecting the background, after background collection is over the system is ready for scanning. 5.2 Measurement using ATR accessory 5.2.1 Background measurement 5.2.1.1 After changing accessory from normal base, accessory the instrument shall be take few seconds to get initialize and after initializing the accessory icon will be displayed in the toolbar. 5.2.1.2 Click on and go to to open instrument Setup window. 5.2.1.3 Click tab and enter start range, end range of wavenumber and check the resolution value shall be 4. 5.2.1.4 Select the scan type and units for measurement by scrolling down the related window and selecting the required parameter and enter the scan number. 5.2.1.5 Click on and then select or press button on the toolbar for collecting background to start collection of background. 5.2.2 Sample scanning 5.2.2.1 Place the sample on the Crystal. 5.2.2.2 Click on tab under the left-hand side layout- and fill the parameters regarding to Sample ID and Description. 5.2.2.3 Ensure that the preview check box is selected(If required). 5.2.2.4 After placing the sample properly, adjust the pressure such that sample is in proper contact with the crystal click on and click on or press the button on the toolbar to begin the data collection. 5.2.3 Comparison of sample spectra with standard spectra or to overlay the spectra 5.2.3.1 Select the spectra to be compared with reference spectra by clicking on & then on & selecting the required spectra from opened window & click on and let is displayed on the screen. 5.2.3.2 Click on and then on to open up the compare set up window. 5.2.3.3 Click on and select and browse to select desired standard and enter the desired correlation value. 5.2.3.4 Select the option for reference Vs spectra and browse the spectra to be taken as reference spectra and click on . 5.2.3.5 Click on and select . 5.2.3.6 The system shall be show compare the spectra and shall be show the comparison report. 5.2.4 Reporting of Fourier Transform Infrared Spectroscopy (FT-IR) 5.2.4.1 To generate the report for the spectra, select and open the respective spectra. 5.2.4.2 Click on file and again click on report 5.2.4.3 In tab select . Select to generate print as soon as the report is generated. 5.2.4.4 Select and either under the section < Template filename> browse for the desired template or select the desired fields to printed on the report from the sections tab. 5.2.4.5 Click on button at the bottom of the screen to generate the report Takeout the print of final report. 5.2.5 Calibration of Fourier Transform Infrared Spectroscopy (FT-IR) 5.2.5.1 Change the Accessory UATR to slide holder accessory. 5.2.5.2 Now go to the instrument verification in instrument verification go to set up instrument verification. 5.2.5.3 Deselect Abscissa, Ordinate, Noise and ASTM. Under Generic Pharmacopeia select European Pharmacopeia. TROUGH Position Peak Position Cm-1 Minimum peak height (A)Limit 2870.00 2849.50 0.33 1589.00 1583.00 0.08 5.2.5.4 Go to setup Pharmacopeia test enable resolution performance and select all peak with limit as bellow: 5.2.5.5 Enable wavenumber verification and select all peak given in tab. 5.2.5.6 Select <Instrument Verification. 5.2.5.7 Click on scan without polystyrene film and after 50% scan completed then place polystyrene film and click on, when scanning completed then report a automatically. 5.2.5.8 At the end closed the window. 5.2.5.9 Compare the wave function accuracy with the following limit. • Limit of Resolution Performance Test of Fourier Transform Infrared Spectroscopy (FT-IR) Test-1Difference between the absorbance of the minimum at nominal 2870cm-1 and the absorption maximum at nominal 2849.5 cm-1 should be greater than from 0.3300. Test-2Difference between the absorbance of the minimum at nominal 1589 cm-1 and the absorption maximum at nominal 1583 cm-1should be greater than from 0.0800. • Limit of Wavenumber Verification Test 3060.0 nm /cm-1 (±1nm /cm-1), 2849.50 nm /cm-1 (±1nm /cm-1), 1942.90 nm /cm-1(±1nm /cm-1),1601.20 nm /cm-1 (±1nm /cm-1),1583.00 nm /cm-1 (±1nm /cm-1),1154.50 nm /cm-1 (±1nm /cm-1), 1028.30 nm /cm-1 ( ±1nm /cm-1) and 906.60 nm /cm-1 ( ±1nm /cm-1) Note: The Validated smart pdf report will calculate the difference between the absorbance/%T values at the absorption minimum or %T maximum at 2870 cm-1 and the absorption maximum or % T minimum at 2849.5 cm-1 and automatically report pass or fail. 5.3 Calibration frequency: Half Yearly. 5.4 After completion of the calibration procedure, make the entries in calibration record of FT-IR (as mentioned in XXX. 5.5 Record all the operational activity in Instrument Usage Log book as per respective SOP. 5.6 If any parameter observed out of limit then follow the procedure of out of calibration as relevant as per respective SOP. 5.7 For Liquids 5.7.1 Prepare the blank and sample solution as directed in the STP. 5.7.2 Fill the blank /test solution into the cell, preferably with a syringe in qc lab. 5.7.3 Rinse the cell 2 times with the solution and finally fill the cell taking care that no air bubble is trapped in quality control department. 5.8 Cleaning and Maintenance 5.8.1 Wipe the outside surface of the instrument with Colin solution. 5.8.2 Clean the sample compartment by moping with Colin solution followed by a dry cloth. 5.8.3 Interior maintenance of the instrument will be done by service engineer as and when required. 5.8.4 The liquid assembly must be thoroughly cleaned to prevent contamination of future samples. Wash several times with solvent that will take off prepared samples in qc lab. 5.9 PRECAUTIONS 5.9.1 Install FT-IR in dust free, shock free and vibration free environment. 5.9.2 Equipment shall be in working and qualified status. 5.9.3 Ensure that area is free from corrosive gases. 5.9.4 Ensure that instrument is kept away from direct sunlight. 5.9.5 Ensure that area is well ventilated with ambient temperature and relative humidity. 5.9.6 Ensure that instrument is attached with a constant voltage transformer. |
