SOP - OPERATION AND CALIBRATION PROCEDURE FOR INFRA RED SPECTROPHOTOMETER (MAKE: BUCK SCIENTIFIC)

1.0 OBJECTIVE

To ensure that the instrument performs satisfactorily and gives accurate and reproducible results.

2.0 SCOPE

This SOP covers operation and calibration procedure for Infra red spectrophotometer and this SOP is applicable to Quality control department.

3.0 RESPONSIBILITY

Officer / Executive.

4.0 ACCOUNTABILITY

Department Head

5.0 PROCEDURE

5.1 PROCEDURE FOR GENERAL CLEANING

5.1.1 Ensure that the power supply to the instrument is switched OFF before cleaning.

5.1.2 De-dust the instrument with a clean dry cloth every day.

5.1.3 Once in a week remove adhered dust by wet mopping using detergent solution.
Afterwards wipe the surface with a clean dry cloth to remove traces of detergent.

5.1.4 Caution to be taken to clean the oven immediately with dry cloth to remove the moisture.

5.2 PROCEDURE FOR OPERATION

5.2.1 Switch on the instrument and wait for 30 minutes for heating and stabilizing the lamp.

5.2.2 Then turn on P.C and the Printer.

5.2.3 Go to ‘Buck IR’ icon and double click, and Wait for software initialize with following Word Checking For attached instruments please wait……..

5.2.4 Click on ‘instrument ,’and also Click on ‘Adjust parameters’ and Give the Following parameters For Set up Options .

Optical Mode : Transmission
Scan time : 3
Gain setting : 0
Pen Responsive : 0.1
Scan type : Reference.

5.2.5 In case of Liquid cell, Change Optical Mode to Absorbance by keeping the rest of the parameters as such.

5.2.6 After Setting this, Instrument shows this parameters in its Screen.

5.2.7 5.2.7 Click Instrument and go to Communication parameters . Give Following parameters as a Communication parameters.

Communication Configuration

COM Port : COM1
Baud Port : 2400
Parity : none
Stop bits : 1
Data bits : 8

Click OK for Setting the above parameters in Instrument.

5.2.8 Click on ‘Instrument’ and Go to ‘Scan Sample’
This system Will assign Scan sample.

5.2.9 In Scan Sample, Give 4000 ,600 for start & end wave numbers respectively.


5.2.10 System will show Single beam energy profile and will beep during scan. This is considered as Blank Spectrum.(Air back ground spectrum)

5.3 PREPARATION SAMPLE PELLET:

5.3.1 Weigh about 400 mg of potassium bromide (IR spectroscopy grade, previously dried in-between 1200-1300 C ).

5.3.2 Transfer the weighed material to porcelain mortar & pestle.

5.3.3 Weigh accurately 4 mg of testing sample and transfer it to potassium bromide containing mortar.

5.3.4 Grind and mix well.

5.3.5 Weigh accurately 150 mg of mixed sample and transfer this to the pellet making accessory, using KBr press instrument as per SOP.No: BGQC009-00 pellet is
prepared.

5.4 SAMPLE MEASURMENT

5.4.1 Place the sample pellet, in pellet terminal and give the file name in Scan sample (procedure same as described in air spectrum) and Click OK.

5.4.2 System will show single beam energy profile and will give beep during scan. After scan processing, Go to Arithmetic function .Click Transmission, and select the Correct background(Air spectrum) file from file list . Click on OK. Software will generate the % of Scan for that Sample. This is considered as Sample spectrum.

5.4.3 Go to peak function, adjust peak-threshold and Click on View peaks.

5.4.4 Go to File, select File information and give the following parameters:

Memo : Name of sample analyzed
Method : KBR PELLETE
Instrument : BUCK IR

5.4.5 Click on OK. This is useful for future reference.

5.4.6 Go to View function, Select Overlaid Option for Comparison with Reference spectrum.

5.4.7 Go to File function, select print set-up& print for taking print-out of Scanned spectrum

5.4.8 Go to peak function select print peaks report for peaks report of scanned spectrum.

5.5 CALIBRATION

5.5.1 RESOLUTION

Record the spectrum of a polystyrene film 0.05 mm in thickness.

5.5.2 ACCEPTANCE CRETERIA

5.5.2.1 The depth of the trough from the maximum at about 2851 cm-1 and 2870cm-1 should be greater than 18 % transmittance

5.5.2.2 The depth of the trough from the maximum at about 1586 cm-1 and 1589cm-1 should be grater than 12% transmittance

5.5.3 WAVE NUMBER ACCURACY

5.5.3.1 Record the spectrum of a polystyrene film 0.05 mm in thickness.

5.5.4 ACCETANCE CRITERIA

5.5.4.1 It should give the maxima at the following wave numbers within the acceptable range.


S. No: 1.
WAVE NUMBER 2850.7
ACCEPTABLE RANGE 2846.7 ----- 2854.7

S. No: 2.
WAVE NUMBER 1601.4
ACCEPTABLE RANGE 1597.4 ----- 1605.7

S. No: 3.
WAVE NUMBER 906.7
ACCEPTABLE RANGE 902.7 ----- 1000.7

5.5.5 Record the results in the calibration record as per Annexure-1

5.5.6 Affix a ‘CALIBRATED’ label on the instrument.

5.6 Report any discrepancy observed during calibration or operating the instrument to Department Head and notify the defect to utility / service engineer to rectify the defect. Affix “BREAK DOWN” label on the instrument till it gets rectified.

5.7 FREQUENCY OF CALIBRATION
Once in three months and after each maintenance job.


6.0 REASON FOR REVIEW:

First time issue.