SOP for Operation of Shimadzu IRAffinity-1S Fourier Transform Infrared Spectrophotometer

OBJECTIVE:
To lay down a procedure for the Operation of Shimadzu IRAffinity-1S system using LabSolutions software. 

SCOPE:
This is applicable for the operation of Shimadzu IRAffinity-1S system using LabSolutions software for IRAffinity-1S system. 
RESPONSIBILITY:
It is the responsibility of QC Executive to follow this procedure accurately and precisely fully without any deviation. 

ACCOUNTABILITY:
Assistant Manager – Quality Control 
Manager – Quality Assurance 

PROCEDURE:
Operation of Shimadzu Fourier Transform InfraRed spectrophotometer (FTIR)
  • Before starting analysis, ensure that the FTIR System is placed on a clean and dust free platform. 
  • Ensure that the instrument has been connected to power supply. Ensure that the all communication cords between the units are connected properly. 
  • Turn on the computer and then switch on the FTIR by clicking the power switch at the front right side. The green LED is lit when the instrument is powered. There are two indicators – an orange lamp as Dry indicator and green lamp as Power indicator on the front. Dry indicator light shows the humidity in the interferometer of the FTIR even if it is off. Always confirm that the Dry indicator is on. 
  • Double click the LabSolutions icon on desktop screen to open the LabSolutions software & Logging in. 
  • Click on Instrument -à Double click on FTIR -à LabSolutions IR -à Click on the Spectrum icon. The system will then initialize automatically. 
  • Click the [Data] tab and then set scan parameters such as the number of scans and resolution. 
  • Enter filename and sample information to save in a specific folder. 
  • Click [BKG Scan] icon to perform background scan measurements.  
Sample Preparation Method
  • Prepare samples according to the following procedure by using a Mini Hand Press Model MHP-1. 
  • Clean the top and bottom dice set and tablet frame surfaces with small piece of cloth or paper. 
  • Insert the tablet frame on the thicker pedestal bottom side of the dice set. (The tablet frame may be set with either side up.) 
  • Put the mixture of powder KBr and solid sample in the frame hole, normally, in the ratio of 3:1. Remove the mixed powder sample spilled on the tablet frame surface. (For liquid samples spread a portion of the sample on the KBr discs provided and attach them to the demountable cell then insert in the sample chamber cassette of the FTIR for measurements). 
  • Insert the top dice set protrusion in the tablet frame hole. 
  • Place the tablet frame assembled with top and bottom dice set at the center of the V-groove in the base body of the Mini Hand Press. 
  • Let down the handle of the Mini Hand Press quietly, and press the top and bottom dice set slowly with hand. (A yardstick pressing load is about 20kg.) 
  • Disassemble the top and bottom dice set to take out the tablet frame. 
  • Set the tablet frame in the pellet holder and insert in the sample chamber cassette of the FTIR and start measurements. 
  • Click [Measurement] and then click [Sample Scan] to measure the sample. (A spectrum of the sample is displayed). 


Postrun / View 
  • Postrun is done to perform operations such as searching and printing with respect to spectra. 
  • Double click the LabSolutions icon on desktop screen to open the LabSolutions software & Logging in. 
  • Click on Instrument Ã  Double click on FTIR Ã  LabSolutions IR Ã  Click on the Postrun icon. 
  • Open data folder and select the desired spectrum file (A spectrum of the sample is displayed). 
  • Click [Search] Ã  Go to [Spectrum Search] Ã  Click [Fix search result] Ã  Click [Save] Ã  Click [Print Preview] and then print. 
Procedure for System Shutdown 
  • Confirm that all necessary LabSolutions IR data has been saved. 
  • Quit LabSolutions IR with the [File] -à [Exit] command. 
  • Shutdown windows 
  • Turn off the power switch at the front right side of the IRAffinity-1S. The power (green) should turn off. 
  • Enter the instrument usage details in the logbook. 

ABBREVIATIONS:
QC – Quality Control 
QA – Quality Assurance 
FTIR – Fourier Transform InfraRed spectrophotometer 
IR - Infrared 
BKG Scan – Background Scan 
MHP-1 –Mini Hand Press 
KBr – Potassium Bromide

 

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