Procedure for operation and calibration of IR Spectro Photometer (SHIMADZU). Quality assurance

• OBJECTIVE
• To lay down the procedure for operation and calibration of Fourier Transform Infrared Spectrophotometer (Shimadzu)
• SCOPE
• This SOP shall be applicable for Quality Control in Quality Assurance department.
• RESPONSIBILITY
• Quality Control Executive/Officer.
• ACCOUNTABILITY
• Head Quality Control.
• PROCEDURE FOR CLEANING
• Check that the power supply to the instrument is switched ‘ OFF ‘ before cleaning. Clean the instrument with a clean dry cloth every day. Occasionally wet cloth dipped in dilute soap solution may be used. Precaution has to be taken to clean the instrument immediately with dry cloth to remove the moisture.
• PROCEDURE FOR OPERATION
• Switch on the main power switch of the instrument.
• Switch on the PC after the beeping sound is heard.
• Double click the icon [IR solution]
• Enter the username and password.
• Single click on Measurement in the Menu bar and then click on Initialize.
• Check the instrument status on the status monitor on the left side of the screen. All the items such as light source , laser , beam splitter And other accessories should be displayed in green.
• Click [ Data Tab ]  on the scan parameters window and feed the values as shown below

1.  Measurement mode –  % Transmittance
2. Apodization – Happ Genzel
3.  No. of scans -16
4.  Resolution – 4 cm-1
5.  Range   – 4000 – 400 cm-1
6. Click  Instrument tab and feed the values as shown below

1. Beam –  Internal
2. Detector -Standard
3. Mirror speed – 2.8 mm/sec
4. Click on More tab and feed the values as shown below

• Normal

1. Gain – Auto
2.  Aperture – Auto

•  Monitor

1. Gain – 1
2. Mode – Power

• Click on [ BKG ] in the measurement file area , a dialog box will appear on the screen with a     message
• Put a tick mark on [ View Background ] in the measurement file area so that the background    spec trum will be displayed as the measurement is finished.
• Click on Files Tab and do not check mark on [ locked ] so that changes of scan parameters can be done.
• “ Please prepare sample compartment for background scan “
• Cancel                                                           OK
•     Click on OK  and background spectrum will be displayed.
• Now prepare the sample and hold in sample holder and place in sample chamber.
• Enter the ID of the sample to be scanned in Comment and the file name where the data is required to be stored in Data File by clicking on … Button.
• Click on  Sample      to the scan the sample.
• The spectrum will be displayed on the screen and  it will be saved as per destination given in the Data File.
• Click on [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 known as Zooming window.
• Right click on either overview window or zooming window and then click on Vertical Axis to change the spectrum in    absorbance mode if required.

• Open the reference spectrum of the concerned sample from D:\Data\Reference Spectra\Name of the product.

• Drag the reference spectra from the Tree View window on the left side of the screen and place it on zooming win dow to overlay with the sample.
• Click on File and then click on print preview, select the required report template and take out the print by clicking on  print option.

• Preparation of Sample: Prepare the sample as follows
• For Solids

• Dry potassium bromide ( Spectroscopic grade ) in an oven at 105° C for one hour.

• Triturate about 1 mg of the substance with approximately 300 mg of the dry , finely powdered potassium bromide. Grind the mixture gently and thoroughly , spread it uniformly in a die and compress under vacuum at a pressure of about 10 tons.
• Use a clean S.S spatula and transfer the disc into S.S pellet holder and place it in sample compartment.

• For Liquids

• Prepare the sample solutions as directed in the STP.

• Fill the test solutions into the cell, preferably with a syringe. Rinse the cell 2 times with the solution and finally fill the cell taking care that no air bubble is trapped inside.

• For samples in mineral oil dispersion

• Triturate 200 to 300 mg of the sample in a clean mortar with the minimum amount of liquid paraffin ( 8 to 10 drops )

• To give smoothy paste.

• Compress a portion of the mull between the two Sodium Chloride plates

• Now place the sample holder in the sample compartment and record the spectra.
• PROCEDURE FOR CALIBRATION
• Click on Measurement in the Menu  Bar and then click on JPEP 2000 validation , a dialog box will appear on the screen with a message
• Click on Measurement and feed the informations related to instrument . User ID , Temperature , Sample name , Relative humidity and Inspected by, and click OK.
• Immediately two messages will appear on the screen
• Test 1 – Form of Power Spectrum⇒ OK
• Remove sample from Sample Chamber ⇒ OK
• Remove sample from sample chamber if any and click OK to start the scanning for Power Spectrum.
• After the scanning for   Power spectrum , a message will appear on the screen
• Set Polystyrene film into sample chamber⇒ OK

• Place the polystyrene film in the sample chamber and click OK to start the scanning for Resolution, Wave number, Accuracy, Reproducibility of Wave number and Reproducibility of Transmittance.

• After the completion of scanning report will be printed of its own, otherwise go to Measurement, click on report viewer, select the data and take out the print.

• Forms and Records (Annexures)
• Not Applicable
• Distribution
• Master copy –  Quality Assurance
• Controlled copies- Quality Assurance, Production, Quality Control.engineering
• History
  

  Date	Revision Number	Reason for Revision
  –	00	New SOP

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