SOP FOR OPERATION AND CALIBRATION OF FOURIER TRANSFORM INFRARED SPECTROPHOTOMETER

1. OBJECTIVE:

1. To lay down the procedure for Operation & Calibration of Fourier Transform Infrared Spectrophotometer.

2. SCOPE: 

1. This procedure is applicable for the Operation & Calibration of Fourier Transform Infrared Spectrophotometer in Laboratory 

3. RESPONSIBILITY:

1. Quality Control Officer / Executive are responsible to follow procedure as per the procedure mentioned in this SOP. 

2. QC Head is responsible for implementation and compliance of the procedure as per this SOP.

4. ABBREVIATIONS

1. SOP    :    Standard Operating Procedure

2. QC    :    Quality Control

3. No.     :     Number 

4. °C        :    Degree centigrade

5. NA      :    Not Applicable

6. Temp.    :    Temperature

7. &        :     And

8. %        :    Percentage

9. CFR    :    Code of federal regulation

10. FT-IR    :    Fourier Transmission Near-Infra Red

11. cm-1    :    Centimeter inverse

12. Rev.    :    Revision

5. PROCEDURE: 

1. Pre-requisites

1. Equipment shall be in working and qualified status.

2. Check the instrument for the cleanliness and free from dust.

2. Operation 

1. Switch on the instrument and computer attached to the instrument taking care that while switching on the instrument only normal base accessory shall be placed in the instrument.

2. Double click on the spectrum Icon to enter into software & the spectrum login dialog is displayed.  

3. Enter the user name and password in the new opened window and click <OK>.

4. Now the system shall be ask to select an instrument. Select an instrument and click on <Connect>.

5. Insert the accessory using which sample is to be scanned.   

6. Click on <Background> icon the toolbar if the path for the beam is clear otherwise clear it. 

7. System shall be start collecting the background, after background collection is over the system is ready for scanning.

3. Measurement using normal base accessory

1. Back ground measurement 

1. Click on setup <Instrument> and go to basic instrument setting to open Instrument Setup window. 

2. Click on <Setup Instrument Basic>  settings tab and enter start range, end range of wave number , resolution value shall be 4.00 and scan type and units for measurement by scrolling down the related window and selecting the required parameter and enter the scan number.

3. As the scan type selected is background to measure the background, the units for measurement shall be automatically get converted to energy <EGY>.  

4. Now click on background the system shall be start background collection and shall be shown on the screen after complete collection.

2. Sample Scanning 

1. Click on sample table under the left hand side layout  tab- Data Explorer and fill the parameters regarding to Sample ID and Description.

2. After placing the sample properly click on <Measurement> and click on <Scan> or press the <Scan> button on the toolbar to begin the data collection.

4.  Measurement using MIR acle ATR accessory

1. Background measurement

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.   

2. Click on <Setup> and go to <Instrument> to open instrument Setup window.

3. Click <Setup Instrument Basic> tab and enter start range, end range of wavenumber and check the resolution value shall be 4

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. Place spectral on standard on the platform taking care that is shall be placed properly covering beam path completely.

6. Click on <Measurement>and then select <Background> or press <Background> button on the toolbar for collecting background to start collection of background.

2. Sample scanning 

1. Place the sample on the Crystal.

2. Click on <Sample Table> tab under the left hand side layout- <Data Explorer> and fill the parameters regarding to Sample ID and Description.

3. Ensure that the preview check box is selected

4. After placing the sample properly, adjust the pressure such that sample is in proper contact with the crystal click on <Measurement> and click on <Scan> or press the <Scan> button on the toolbar to begin the data collection.

5. Processing generated spectra

1. To process the generated spectra, get it displayed on the screen. Select the spectra to be processed by clicking on <File> and then on <open> and selecting the required spectra from opened window and click on <Open>.

2. Go to <Process> and then to <Baseline Correction> to select the <Automatic correction> & delete the initial under process spectra.

3. Now again select the spectra under processing and click on <Process> and go to <Smooth> to select the automatic smooth.

4. Now again select the spectra under processing and click on <Process> and click on <Normalize> and enter the required value for ordinate limits as per requirements and click on <OK>.

5. Once again select the spectra under processing and click on <Process> and then click on <Peak Tables>. To change the value of threshold as per requirement click on <Setup> and select  <Peak able>

6. Select the finally processed spectra and save it.

6. Comparison of sample spectra with standard spectra or to overlay the spectra

1. Select the spectra to be compared with reference spectra by clicking on <File> & then on <open> & selecting the required spectra from opened window & click on <open> and let is displayed on the screen.

2. Click on <Setup> and then on <Compare> to open up the compare set up window. 

3. Click on <Add> and select <Single Spectrum> and browse to select desired standard and enter the desired correction value.

4. Select the option for reference Vs spectra and browse the spectra to be taken as reference spectra and click on <Open>.

5. Click on <Process> and select <Compare>.

6. The system shall be show compare the spectra and shall be show the comparison report. 

7. Reporting 

1. To generate the report for the spectra select and open the respective spectra. 

2. Click on <File> and again click on <Report >

3. In <Report Option> tab select <Save Report>. Select <Print> to generate print as soon as the report is generated.

4. Select <Report Template> 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. Click on <Report> button at the bottom of the screen to generate the report Takeout the print of final report

8. Calibration: 

1. Remove the sample holder, if any, and measure the back ground for the system.

2. Place the Polystyrene film in the sample holder.

3. Click on  <Setup> and select <Instrument Verification>

4. Deselect Abscissa, Ordinate, Noise and ASTM. Under Generic Pharmacopeia select European Pharmacopeia. 

5. Select <Measurement>  <Instrument Checks> <Instrument Verification>

6. ANNEXURES/REFERENCES :

1. Annexure I : Calibration of FTIR Spectrophotometer.