STANDARD OPERATING PROCEDURE LAB EQUIPMENT FTIR SPECTROPHOTOMETER – OPERATION AND CALIBRATION

STANDARD OPERATING PROCEDURE

SUBJECT :                     LAB EQUIPMENT FTIR SPECTROPHOTOMETER – OPERATION AND CALIBRATION

DEPARTMENT           : QA SOP NO.                      : Page No                       : Effective Date             : Next Review                : Version No                  :

1.0       OBJECTIVE:

To provide guidelines for Operation, Calibration & Maintenance of FTIR Spectrophotometer

2.0       SCOPE: 

To establish a procedure for a operation Calibration & Maintenance of FTIR recording Spectrophotometer.

3.0       PROCEDURE:

1.1              Remove the silica gel bag from the compartment

1.2              Turn on the activation switch on the FTIR recording Spectrophotometer (Right corner)

1.3              Turn on power to P.C double click ‘Lab Solution IR’ program on the desktop.

1.4              Enter a user ID & Password in to the (Login) window & click ok. Then a window display as Shimadzu Lab solution IR.

1.5              Select shortcut & the window displace “Postrun, Spectrum, Quantitation, Photometric, Time course,

Mapping & Easy Macro” selects the program which is needed.  

1.6              For regular analysis select spectrum program. Click initialise than check the status monitor in Log window which display the status of the FTIR’s Interferometer. If it displays green then the instrument is ready for use.

1.7              Select “Measurement” then set scan parameters & select the folder to save the report enter a file name & sample information.

1.8              To perform Background Measurement click Background scan a background spectrum is displayed.

1.9               Click measurement set the sample click “Sample scan” a spectrum of sample is displayed.

1.10          Click “File” click Print with template” selects the template & gives print command.

1.11          \The spectrum will get printed collect the spectrum & attached to the report. 

1.12          The IR graph should be saved with respective templates and kept in a monthly wise folder. The folder will be review once in a month. The data backup is done in hard disk every quarterly.

1.13          Privileges of Admin, Developer & Operators

Admin : Has the right of control of the system.

Developer : Has right to develop a method.

Operators : Has the right to use the Equipment & no changes occurred by Operator.   

Note :   The instrument is covered under annual service contract and it is serviced as and when there

  is a breakdown or requirement.

1.14          PREPARATION OF KBr PLATE TO PERFORM IDENTIFICATION TEST:

·         Clean the plunger and anvil with Solvent to remove Grease.

·         Assemble the top and bottom guide.

·         Insert anvil with polished surface facing with upwards in the top Guide.

·         Fill evenly 200 – 300 mg Kbr + 2mg sample on the Anvil surface and spread it using plunger.

·         Insert plunger facing polished surface towards.

·         Place the small “o” ring around the plunger and push it up to the Top S S Guide.

·         Place the assembled Die on the cover plate of the cylinder of the press. Move the screw with handle (Part No. 1 of the Kbr press Drawing) until it touches the plunger.

·         Apply vacuum.

·         Close the release knob turning clockwise.

·         Apply pressure using pump handle normal pressure required is 8 to 10 Tons. Never exceed 10 ton on the Die though the press is capable of giving 15 ton pressure.

·         Release pressure and vacuum after five minutes.

·         Dismantle Top and bottom guides and using extractor ring provided apply pressure from the reverse side to remove pellet.

·         Clean all traces of Kbr and store the Die in Dessicator.

             

NOTE: For best results use only spectroscopic grade KBr and heat it at 110º C in oven before use.

3.15     CARE OF DIE:

·         All the parts of the Die should be kept absolutely clean by removing traces of KBr & Dirt.

·         Use only soft tissue paper moistened with solvent for cleaning.

·         Do not exceed 10 tons pressure on the Die.

·         Store the Die in Dessicator after cleaning thoroughly. When the Die is not going to be used for long Time, The anvil and plunger should be wrapped in Aluminum foil after applying grease.

·         For daily use keep the Anvil and Plunger Immersed in liquid Paraffin.

·         Use only moisture free dry Spectroscopic Grade KBr if the above instructions are not followed properly, the Die will be permanently damaged.

·         The damage due to lack of observations of above precautions will not be covered under warranty.

3.16     MEASUREMENT OF LIQUID SAMPLE IN FIXED CELL FOR QUANTFICATION:

·                     Prepare the sample as per the specific method.

·         Inject the sample using a syringe cover it with another cell window paying attention not to make bubbles tight or fix the screws fix it to sample compartment & scan Measure the absorbance & print the spectrum with CCl4, CHcl3 clean the cells twice or three times before & after the analysis is performed.

·         Follow the steps as mentioned in the procedure.

Note:   1) Don’t touch the KBr plate with bare hand.

2) Use IR grade KBr & heat it 105º C in over before use.

3) For liquid sample Identification test: Use demountable cell Kbr/ Nacl cells.

Insert the sample between the two cells and close the assembly.

Place the demountable assembly in the sample compartment and follow the steps as mentioned in procedure.

           

3.17     CALIBRATION OF FTIR: 

·                                 Remove the silica gel bag from the compartment

·                                 Turn on the activation switch on the FTIR recording Spectrophotometer (Right corner)

·                                 Turn on power to P.C double click ‘Lab Solutions’ program on the desktop.

·         Enter a user ID & Password in to the (Login) window & click ok. Then a window display as Shimadzu Lab solution.

·         Click on panel and select the USER PC In Panel.

·         Click on panel and select the MACRO.

·         Click on panel and select the EP Validation or JP Validation.

·         Click on panel and select the RUN.

·         Click on panel and select the LOGIN then OK.

·         Click on panel and select the PREVIOUS BACKGOUND DATA click YES.

·         Click on panel and select the EP Validation Parameter Setting click on OK.

·         Set POLYSTERENE FILM into sample compartment click OK

Calibrate with standard Polysterene film supplied by the vendor & perform calibration on the day of use.                           

3.18     PRECAUTIONS:

            

·         Power down the unit to avoid electric shock. Disconnect the power cord from the instrument rear panel before working on the inside the FTIR spectrophotometer

·       Do not use flammable sprays near the instrument. They could ignite and cause a fire.

·       Do not use mobile phones near the product. They may damage data.

·         Light source and light source chamber are very hot. When replacing the light source, be sure to turn OFF the power and check that the light source is completely cooled.

·                     Never use alcohol or thinner solvents for cleaning the instrument

3.19PREVENTIVE MAINTENANCE PROCEDURES:

·                     Do not place heavy objects on the power cord, and keep any hot items away.

·         When using flammable and toxic samples, be sure to install ventilation equipment at installation place.

·   Always wear protective gloves, glasses & prevent exposing of your eyes to ultraviolet radiation while performing the test.

·         Please make sure to use only the power cord specified by Shimadzu

·         After using the Equipment place Silica gel bags in the Sample compartment

·         If a sample is spilled, follow the handling & disposal carefully

4.0       FREQUENCY: 

Internal Calibration:

Once in three months for Calibration with standard Polysterene film.

External Calibration:

Once a year by service Engineer of Shimadzu/ Toshvin Analytical Pvt. Ltd. 

5.0       RESPONSIBILITY:  Executive Q.A

6.0       REVIEW GUIDE: Usage log book.

7.0       ANNEXURE: -------

8.0       SOPs DISTRIBUTION:

            This SOP shall be distributed to following Departments:

Name of the Department	Master Copy	Circulatory Copy
QA/QC	√	√
Production	x	x
Warehouse	x	x
General	x	x
Maintenance	x	x