Sop for Operation and Calibration of FTIR

This Document describes (Standard Operating procedure) Sop for Operation and Calibration of FTIR

Sop for Operation and Calibration of FTIR

I. Purpose & Scope:

• The Purpose of this SOP is to lay down the procedure to lay down a procedure for Operation, Cleaning & Calibration of FTIR
• This procedure is applicable for Operation, cleaning & Calibration of FTIR used in Quality Control Department

II. Responsibilities:

• All Quality Control personnel’s shall be responsible to follow and implement this SOP.

III : Introduction and Procedural Part :

GENERAL CLEANING :

• Clean the instrument with a clean dry cloth every day. Occasionally wet cloth dipped in dilute soap solution or IPA may be used for cleaning of outer surface of instrument.
• A precaution has to be taken to clean the instrument immediately with dry cloth to remove the moisture.

PRECAUTIONS :

• Do not touch to clean any optical surface while cleaning.
• Do not stare into the internal laser beam under the instrument cover.
• Do not use a flammable gas to purge the instrument.
• Do keep the spectrum one dry and avoid spilling liquid into the instrument.
• Do not keep any traces of materials on the sample port of Instrument, as excess humidity may damage sensitive optics.

BASIC OPERATION OF FTIR :

• Ensure that the power supply to the instrument is ON and Select the Peak Miracle IR ‘Instrument setup.
• Select Software icon ‘Horizon MB’ & Open, select the Instrument configuration as MAC-00-02-2C-001CB2.
• Fill the sample information for background (Blank) first, with comment as background.
• Select the Instruments Parameters
• Resolution = 4
• Scan          = 16
• Click on acquisition mode as Single Beam
• Click on icon ‘Reference’ Instrument scanning is started for Blank.
• After the completion or Back ground, Start for Sample set up & preparation.
• Put sample/ Standard on zinc mirror to the Peak Miracle, Take care the Zinc mirror is covered by the sample.
• Fill the sample/ Standard information for with name of sample with batch details or Analytical report number & comment as the test name.
• Select the Instruments Parameters
• Resolution = 4 and Scan = 16
• Click on acquisitions mode as Transmittance.
• Click on icon ‘Measure’ Instrument scanning is started for Sample & saves with given name.
• Select icon for Print ‘Window –Project- Measure Data – Data, Click on the sample/ Standard file, open it & take print for the same Take print & compare the test sample & standard sample.
• Clean the sample port with Isopropyl alcohol (IPA) after the use of instrument.

CALIBRATION OF FTIR :

Calibration of FTIR Frequency: Once in months and after each maintenance job

Verification of the wave-number Scale:

• Select the sample compartments for polystyrene film.
• Take Blank is air and take scan for 4000 – 400 cm^-1.
• Insert the polystyrene film in sample compartments and go to beam and select polystyrene for scan with following set up.
• Go to scan and give the following parameters
• Range                          –           4000 – 400 cm^-1
• Scan type                    –           Background/Sample
• Units                           –           % T
• Scan No.                     –           1
• Click to scan
• The peak data of the spectrum of the polystyrene film is displayed on the screen.
• Print all the data from peak tables from ‘view’. And check limits of wave number, Accuracy, Compare the wave number accuracy with following limit.
• 3060.0 ± 1.0 cm^-1
• 2849.5 ± 1.0 cm^-1
• 1942.9 ± 1.0 cm^-1
• 1601.2 ± 1.0 cm^-1
• 1583.0 ± 1.0 cm^-1
• 1154.5 ± 1.0 cm^-1
• 1028.3 ± 1.0 cm^-1
• Record the observations as per Annexure I during calibration of FTIR.

Control of resolution performance :

• Select the sample compartments for polystyrene film.
• Take Blank is air and take scan for 2900 cm^-1 to 2800 cm^-1 &  1600 cm^-1 to  1500 cm^-1 separately one by one.
• Insert the polystyrene film in sample compartments and go to beam and select polystyrene for scan with following set up during calibration of FTIR.
• Go to scan and give the following parameters
• Range               –   2900 cm^-1 to 2800 cm^-1 & 1600 cm^-1 to 1500 cm^-1
• Scan type        –           Background/Sample
• Units               –           % T
• Scan No.         –           1
• Click to SCAN
• The peak data of the spectrum of the polystyrene film is displayed on the screen.
• Print all the data from peak tables from ‘view’. And check limits of wave number.
• The difference between the absorbance at the absorption minimum at 2870 cm^-1 and the absorption maximum at 2849.5 cm^-1 is greater than 0.33. The difference between the absorbance at the absorption  minimum at 1589 cm^-1 and the absorption maximum at 1583 cm^-1 is greater than  08.
• Record all the calibration data in Annexure-I during calibration of FTIR
• Handle the out of calibration results as per respective SOP
• If any discrepancy observed during operating the instrument report to QC Manager & notify the defect to Maintenance Manager to rectify the defect. Affix ‘Under Maintenance Label’ on the instrument.
• Maintain the instrument usage log book as per SOP Handling of instrument usage log book

ANNEXURE:

Annexure I      :  Instrument Calibration Record

ANNEXURE-I

  Calibration of FTIR Record

1. A) Cleanliness of the Instrument:

Observation: Clean / Not Clean

2. Any other maintenance:

Observation: Required / Not required

1. B) VERIFICATION OF WAVE NUMBER SCALE:

1. CONTROL OF RESOLUTION PERFORMANCE:

Remark: The calibration of FTIR performed as per SOP and Complies / does not comply with the acceptance criteria.

Calibrated By:                                      Checked By:                               Approved By:

 Date                                                       Date:                                            Date: