SOP for Operation of Shimadzu IRSpirit-X FTIR Spectrophotometer

PURPOSE

To lay down a procedure for the Operation of the FTIR Spectrophotometer, Model: IRSpirit-X, Make: Shimadzu

SCOPE

This SOP applies to the operation of the FTIR spectrophotometer, with the model IRSpirit-X and the make Shimadzu.

RESPONSIBILITY

• QC Analyst: Operation of an instrument as per SOP.
• Senior Analyst: Reviewing of recorded data and implementation of the SOP.
• Manager QAD/QCD: Approval and responsible for implementing the SOP.

PROCEDURE

Security Policy

• The administrator (QA/QC Manager or Asst. Manager) shall log in with his/her credentials and shall set the system policies.
• To set the ‘Security Policies’, go to ‘Administration’ and click on ‘Security Policy’.
• The policies of System, Account and Instrument shall be set as per the below screens.

System Policies

Account Policies

Instrument Policies

User Group & Privileges

• The administrator (QA/QC Manager or Asst. Manager) shall login with his/her credentials to create a user group and to set the user privileges.
• Three User group(s) are configured in the software and privileges shall be assigned to a respective user group.
• Created user accounts shall be added to the appropriate user group to get the privilege to perform the activity (as per the following table).

Sr. No.	User Group	Shall be assigned to
1.0	Administrator	QA/QC Manager or Asst. Manager
2.0	Operator	Who performs the analysis, shall be from site quality control and perform review of raw data.
3.0	Guest	Other site(s) employee/ third party analyst(s)/ Service engineer.
NOTE: Based on the activity to be performed by the service engineer, his/her user account can be added to the Administrator group to perform the service-relevant activities. However, no batch sample shall be used to complete the service activity.

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• Each user must belong to a group and cannot belong to more than one group.
• To create a new group, go to, ‘Administration’ and click on ‘User Administration’.
• Then, double-click on ‘Rights Group Administration’ to open the ‘Rights Group Administration’ window.
• Click on ‘Add’. The ‘Add Rights Group’ window will appear.
• Enter the Group Name, comments, add the necessary rights and click on ‘OK’ to save the new user group.

User Account Maintenance

• The administrator (QA/QC Manager or Asst. Manager) is responsible for the maintenance of the user accounts in the software application.
• For user account creation/deactivation/modification/password change, the user shall submit the authorized ‘User Account Request Form’ to the Administrator as the SOP of Computer System Policies SOP.
• The administrator shall login with his/her credentials to create user accounts.
• To create a new user account, go to ‘Administration’ and click on ‘User Administration’.
• Then, double-click on ‘User Administration’ to open the ‘User Administration’ window.

• Click on ‘Add’. The ‘Add User’ window will appear.
• Enter User ID, User Name, and first login password, add the necessary rights group, and click on ‘OK’ to save the new user account.

General Precautions

• Always keep samples with a worksheet in a tray labeled as ‘Samples to be analyzed (For FTIR Identification Test)’.
• Ensure that the instrument is clean before use, including the surrounding area.
• Check the calibration status.
• Ensure that the electrical connections are proper.
• Change desiccant if the indicator color changes to pink.
• If any discrepancy is observed during use, then inform the Head of Quality Control. Meanwhile, affix the ‘Instrument Under Breakdown/Under Maintenance’ label on the instrument.

Operating procedure through PC with LabSolutions Software

• Ensure that the instrument is properly connected to the power supply.
• Turn on the IRSpirit-X interferometer.
• Double-click on the ‘LabSolutions’ Icon.

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• Enter the Individual User name and password. Click ‘OK’ to access.

• Go to ‘Instruments’ and double-click on the selected instrument to open the “LabSolutions IR’ application window to perform the analytical work.

• Click on the ‘Spectrum’ icon, and the following window will be displayed.

• Go to the Measurement toolbar, click on the ‘Instrument’ icon, then click on ‘Initialize’, The Instrument will start initialization for 20 seconds and show status on the screen with green indications.
• When Windows asks for confirmation on whether to remove or keep previous background data will be displayed, click on ‘YES’. The instrument will get initialized. ‘Initialization success’ will be shown in the status window.
• After initialization, boxes in green color will be shown in the status monitor window.
• If any of these boxes are red in color, means the instrument is not ready for use. In such cases, perform the initialization again after rectifying the error, with the help of the service engineer.
• Analyst must ensure that the initialization is succeeded, before starting the measurement of the sample.

• Click on ‘Load Parameters’ to load the required method with the specified parameters.
• Select the appropriate method and click on the ‘Open’ button.

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• Thus, the method will be loaded.
• Before starting the sample analysis, every user should make a Background correction.
• Click on ‘BKG Scan’ to record the background spectrum. Then Background spectrum will be recorded and stored.
• After the background (BKG) measurement is complete, keep the sample spectra in the sample holder.
• Click on the ‘File Name’ browse icon and enter the file name as shown below.

• Enter the file name as Product/Material Name_L.R.No/B.No._Description(SPL/STD)_Date.

Where,

1. Material/Product Name- Enter the name of Material or Product, as applicable.
2. L.R.No./B.No.- Enter the L.R. Number or batch number for Sample analysis.
3. Description- Enter the sample description as ‘STD’ for standards and ‘SPL’ for the sample.
4. Date- Enter the current date.

• Enter the ‘Test Name’ in the ‘Comment’ column, ‘Sample Description and Name’ in the ‘Sample Name’ column, and ‘L.R. Number’ in the ‘Sample ID’ column.
• Then, click on the ‘Sample Scan’ to record the spectra of the standard/sample materials. Once the measurement is completed, the pellet shall be removed from the sample holder.
• After completion of the activity make necessary entries in the instrument log sheet as per ‘Instrument Usage Log for Instruments with labSolutions Software’.

Calculation of Sample Peak Purity (Correction):

• Open the standard as well as sample spectra.
• Go to ‘Data Processing’, and click on ‘Purity’.

• Right-click on the sample file name, and select on ‘send to source’.

• Right-click on the standard file name, and select ‘send to reference’.

• Click on ‘Calc’ & ‘OK’.

• The report will give the value of the Purity Index. Purity Index should be greater than 0.9. If the purity index is less than 0.9, an investigation shall be carried out.
• Labeling the peaks: Click on ‘Data Processing’ and then on ‘Peak Pick’ to detect peaks. Set the ‘Noise’, ‘Threshold’, and ‘Min Area’ in the parameter. Click on ‘Calc’ and then on ‘OK’.

Cleaning of Accessories of FTIR

• Take out the sample holder from the compartment.
• Wipe the sample holder with tissue paper with having smooth texture.

ABBREVIATIONS

QAD: Quality Assurance Department

QCD: Quality Control Department

SOP: Standard Operating Procedure

ANNEXURE

Nil

REVISION HISTORY

Nil

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