1.0
Objective:
To provide written
procedure for the operation and calibration of Fourier Transform Infrared
Spectrophotometer.
2.0
Scope:
This
SOP covers operation and calibration of Fourier Transform Infrared
Spectrophotometer, model no. : 8400 S
3.0
Responsibility:
Jr.
Research Officer, Research Officer: Responsible for operation, calibration and
maintenance of the instrument as per procedure.
Head of Department: Responsible for calibration and maintenance, timely
as per schedule.
QA Officer/QA Manager: Review the records and governing the document.
4.0
Procedure:
4.1 Ensure that the instrument is clean and free from dust.
4.2 Check and ensure that the instrument is calibrated.
4.3 Ensure that the temperature is between 200 C to 300
C & relative humidity 30 to 70 %
4.4 Switch on the main switch and the power switch of the
instrument.
4.5 Leave the instrument to warm for 30 minutes.
4.6 Turn on the personal computer. The system is swept up to start
up windows automatically.
4.7
Starting Procedure
for solid sample:
4.7.1
Click “Start” Button available
left side corner of the Monitor. Select “Program” on the menu. Select
“IRsolution” in “Shimadzu” group (menu).
OR
Double click on the “IRsolution” Icon on the monitor, display IRsolution
(view) programme.
4.7.2
Click “Measure” button. Select “Measurement” menu on the IRsolution and
click. Select “Initialize” on the menu. The PC automatically initiates
communication with FTIR.
4.8
Scanning :
4.8.1
Comment:
Fill up the information related to Sample i.e. Sample Name, B. No.
4.8.2
Data File:
The IRsolution saves all measured spectra to the hard disk as soon
as measurements are finished. Set and enter the file name in hard disk and
folder.
4.8.3
Auto increment:
Put the check mark to “Auto
increment” to automatically update the file name by putting a number at the end
of the file name in every measurement.
4.8.4 View
Background:
Put the check mark to “View
Background” to display the measured power spectrum for confirmation when the
background measurement is finished. When the check mark is not put, the
measured background spectrum is not displayed (but is used in calculation in sample
measurement).
4.9.1
Measurement Mode:
(% T) or the absorbance (abs) on
the pull down menu.
4.9.2
Apodization:
Click the [ ] button at the right end, and then select
“Happ-Genzel” on the pull-down menu here.
4.9.3
No. of Scans (1-4000) :
Set the number of scans. Click the upper and lower buttons at the right
end or directly enter a numerical value. In normal measurement, set around
“10”. If spectra of better S/N ratio are required, set a larger numerical value
(Maximum 4000).
4.9.4
Resolution:
Open the pull-down menu then set resolution to be used in measurement.
When analyzing gas of low concentration, select “0.85 cm-1 to
accurately measure minute absorption peaks. Sufficient spectra can be acquired
with “4cm-1” or “8cm-1” in measurement of solid or
liquid.
4.9.5
Range (cm-1):
Enter numerical values for the wave
number range in accordance with the measurement method and the used detector.
4.10 Measuring the background:
Click the “BKG” button. The dialog
box appears to give the message “Verify that beam is empty for reference scan”.
Confirm that no sample or only KBr (Pottasium bromide) is set in the sample
holder in the sample compartment, and then click the “OK” button. Background
measurement will be started, after completed background measurement displayed
spectrum on the monitor.
4.11 Setting a sample:
After background measurement is
finished, set a sample. Take about 100 mg KBr in mortar and add about 2 to 3 mg
sample, grind the mixture. Take the mixture in the sample holder in the sample
compartment. Click the “Sample” button. Sample measurement will be
started.
4.12
Confirming and
observing a measured spectrum :
4.12.1 Move the
cursor on the spectrum window, then click and drug the mouse to display
rectangle to a proper size, then drop it.
4.12.2
Move the cursor on the spectrum
window, and right-click the mouse to display the menu. Click “Autoscale” here
to execute the auto scale function.
After zooming in,
click “Full” on the menu, display shows full scale of spectrum.
4.13 Display (View):
4.13.1 Click the
“View” Tab to display the “View” Tab window a measured spectrum in the upper
and lower windows. The upper window is called the Overview window and the lower
one the Zooming window.
4.13.2
Right-click on the Overview
window or zooming window to display the right-click menu. Click “Autoscale”
here to change the vertical axis range while keeping the currently displayed
horizontal axis (wave number) range.
4.13.3
Select the “Range List” on the
right-click menu. Enter the wave number range and the vertical axis range to be
displayed to the Range list Editor dialog, and then click the Add button. To
register two or more ranges, repeat this operation. Select a range to be
displayed and click “Use” button to change the spectrum display range.
4.13.4
Click the “Full view” button on
the right-click menu to return the zoomed in spectrum to the original scale.
4.13.5
Open the right-click menu and
put the cursor on “Vertical Axis” to open the sub menu. Click the “Tra” (Transmission) or “Abs”
(Absorbance) on the sub menu to convert the Transmission (% T) spectrum to the
Absorbance (Abs) spectrum, and vice versa.
4.14 Displaying spectra:
4.14.1 Click “File” on the menu bar
and select “Open” on the pull-down menu in the same way as many other software
to open and display a spectrum measured before then dialog box
appears. On this dialog box,
select the file name of the spectrum. To open plural spectra at a time, use the
“Shift” or “Ctrl” key.
4.14.2 Open the pull-down menu of “File” at
the left end of the menu bar and click “Close” to close the open data in the
same way. Click “Close All” to close all open data.
4.15
Overlay of Spectra:
Click “Join visible” on the pull-down menu of “Window” on the menu bar
to overlay
all displayed
spectra.
4.16
Peak Table:
4.16.1
When plural spectra are displayed in the view mode, click the tab of a
spectrum to make peaks and activate it. After that click “Peaktable” on the
pull-down menu of “Manipulation 1” to automatically switch to the
“Manipulation” Tab and display the peak detection screen.
4.16.2
Peaks to be detected can be set
using “Noise”, “Threshold” and “Min. Areas”. Enter a numerical value to each
parameter and click the “Calc” button to display the peak detection result. To
increase or decrease detected peaks, change a numerical value of each parameter
and click the “Calc” button.
4.16.3
Open the right-click menu of
the mouse on the spectrum window and click “Show Peak
4.17
Purity :
4.17.1 Spectrum has been
created by measurement or data processing and displayed on the “View” Tab.
4.17.2 Open the reference spectrum as per step
4.14.1
4.17.3 Click “Join visible” on the pull-down menu of
“Window” on the menu bar to overlay
all displayed spectra.
Select “Manipulation 2” and click
on “Purity”. Select “Window” menu and click ok
“Show tree
view”. Display shows two-spectrum file on left side of the display window.
4.17.4
Select measured sample spectrum file and
right-click and select “Send to Source”, and then select another measured
reference spectrum file and right-click “Send to reference”. The purity graph
display on the screen, then click “OK” button the display shows two overlay
spectrum.
4.18 Print:
4.18.1
Select measured sample spectrum
file and reference spectrum file on the “File” menu. Select the “File”-“Print
Preview” command from the menu bar to display the output preview so that the
format of print layout can be confirmed by click ‘File”-“Open” from the menu
bar to open the dialog box for selecting print layout.
4.18.2
Click the “Print” button on the
preview window to open the “Print” window. If the print preview is not
required, execute the “File”-“Print” command from the menu bar.
4.18.3
Creating a New Print Layout :
4.18.3.1 Select and click “PrintForm” Tab to display
the standard set layout. To create a new layout, select “Print”-“New Template”
from the menu or click the button on the print toll bar.
4.18.3.2
Right-click the page image to
open the right-click menu, and select “Page Setup”, set sheet direction to
portrait or landscape and the margin of the sheet.
4.18.3.3
Select “Print” – “Template” –
“Sizes” and set the header and footer sizes.
4.18.3.4
Click (+) on the “Keywords”
window before “View”, “Manipulation” or “Purity” and select require parameter.
Then save the layout file in “Print Template” menu.
4.19
For Liquid analysis :
4.19.1
Take the kit of sample preparation for liquid and clean
it.
4.19.2 Fix liquid sample holder and apply screws of
stainless steel and tighten them.
4.19.3 Now, inject sample solution through the
injection hole and then apply the Teflon lid.
4.19.4 Press scan “BKG” (Make sure that the sample
slide is empty ) to take a background.
4.19.5 Follow the procedure for solid sample.
4.20 Record the details in FTIR usage
logbook as per given in Annexure – 1.
5.0 Calibration:
5.1
Start and operate the Instrument as per
procedure 4.1 to 4.7.
5.2
Configuration of IR Solution :
5.2.1
Open any spectrum and click on “View” tab.
Select the “Environment”-“Graph Preferences”.
5.2.2
Select the “Style” tab on the 2D Graphic
Preferences dialog box. Put check marks on the “Show peak borders” and the
“Peak label on top of peak”, and then click the OK button.
5.2.3
Now display setting of background spectrum,
click the “Measure” tab and Put the check mark on the “View background” on the
screen. Click the “Monitor” button to execute the monitor scan, and stop. (It
is an operation necessary to make the setting effective.)
5.3
Start the Validation program :
5.3.1
The program starts when the
[Measurement]-[EP/JP2000 Validation] is selected.
5.3.2
Selection menu display on the screen. Click
on Setting button, Setting parameter display on the screen feed the require
parameter i.e. Instrument, Language, Change-Beam etc., after adding this
parameter close the menu.
5.3.3
Now click on Measurement button, Parameter
Setting menu display on the screen. Feed the parameters i.e. Instrument, User
ID, Temperature, Sample Name, Relative Humidity, Inspected by etc. then click
on OK button.
5.3.4
The message “Form of a power spectrum” is
displayed. The power spectrum inspection starts when the OK button is clicked
or within 5 seconds.
5.3.5
The following message “Remove Sample from
Sample Chamber” is displayed. Confirm that no sample is set on the sample
compartment and then click the OK button.
5.3.6
After the power spectrum measurement, the
polystyrene measurement starts. The correctness of the resolution and wave
number by polystyrene film”. Click OK button or wait 5 seconds for the message
“Set a Polystyrene Film into Sample Chamber” to be
displayed.
5.3.7
Set a polystyrene film in sample chamber and
click OK button. The polystyrene measurement is done twice.
5.3.8
When the measurement is finished, calculation
for the inspection is done automatically. The validation program inspected 5
tests. When all the tests are passed, the validation is passed. The judgment
dialog box shows “PASS” and a validation report is printed out.
5.3.9
If one of the tests is not passed,
validation fails. The judgment dialog box shows “FAIL” and a validation report
is printed out. The message closes when the OK button is clicked.
5.4
VERIFICATION OF WAVE NUMBER SCALE :
5.4.1
Check
the transmission minima obtained as shown below.
Sr. No.
|
Transmission Minima
(Absorbance Maxima) in cm-1
|
Acceptance Tolerance
Limit in cm-1
|
5.5 RESOLUTION PERFORMANCE OF THE APPARATUS :
5.5.1 Record the maximum absorption at 2849.5 cm-1 and 1583.0 cm-1.
5.5.3 In the same way record the minimum absorption at 2870.0 cm-1
and 1589.0 cm-1 respectively.
5.5.4 Calculate the difference in % transmittance as follows :
5.5.4.1 Difference : 2870.0 -
2849.5 = _______ %
Limit : Not less than 18.0 % transmittance.
5.5.4.2 Difference : 1589.0 - 1583.0 = _______ %
Limit
: Not less than 12.0 % transmittance.
5.6
Record the calibration as given format in the Annexure - 2.
5.7 Calibration frequency : Once in a
Month
5.8
Calibration is satisfactory when the observed transmission minimum is
within the acceptable limits.
6.0 Routine maintenance:
6.1
Clean the system by dry cloth. If the outside
of the interferometer becomes dirty, wipe it clean with a soft cloth or tissue;
soak the cloth in water or detergent, and wring it out. Do not use organic
solvents and avoid contact with mirrors and other internal component.
6.2
Inspect the colour of silica gel and replace
the silica gel if necessary. (The colour of the silica gel should be blue)
7.0 Documentation:
7.1 Annexure – 1 - FTIR
usage log book. XXX/FRM/ 000-00
7.2 Annexure
– 2 - FTIR calibration Format. XXX/FRM/ 000-00
7.3 Annexure
-3 – FTIR Temperature and Humidity Record XXX/FRM/ 000-00
Annexure – 1
|
|||||
Date
|
A. R. No.
|
Name of Sample
|
B. No.
|
Used by
|
Remark
|
SOP No. : XXX/SOP/000-00 Format
No. : XXX/FRM/000-00
|
|||||
Annexure – 2
|
|||||||||
CALIBRATION DATA OF
|
Page
No. :
01 of
02
|
||||||||
Calibration Date : Next
Due date for Calibration :
|
|||||||||
Model
no. : INS.ID :
Make
: Balance ID
:
Polystyrene film
Part
No :
Make
:
Thickness :
(1) VERIFICATION OF WAVE NUMBER SCALE :
The wave-number scale may be verified using a
polystyrene film, which has transmission minima (absorption maxima) at the
wave-number (in cm-1) shown in table.
Calculation status :
Satisfactory/Not satisfactory
|
|||||||||
Calibrated by :
Checked
by :
|
|||||||||
SOP No. : XXX/SOP/000-00 Format
No. : XXX/FRM/000-00
|
|||||||||
Annexure – 2
|
|
CALIBRATION DATA OF
|
Page
No. :
02 of
02
|
Calibration Date : Next
Due date for Calibration :
|
|
(2)
RESOLUTION PERFORMANCE OF THE APPARATUS :
(I) Maximum transmittance at 2870 cm-1 :
Minimum transmittance at 2849.5 cm-1 :
Difference transmittance =
Limit : Should be greater than
18.0 % transmittance
(II) Maximum transmittance at 1589 cm-1 :
Minimum transmittance at 1583 cm-1 :
Difference transmittance =
Limit : Should be greater than
12.0 % transmittance
|
|
Calculation status :
Satisfactory/Not satisfactory
|
|
Calibrated by :
Checked by :
|
|
SOP No. : XXX/SOP/000-00 Format
No. : XXX/FRM/000-00
|
|
Annexure – 3
FTIR TEMPERATURE & HUMIDITY RECORD
Equipment Identification No :
Limit: Temperature: 20° to 30°C
Month:
Relative Humidity: 30 to 70%
Date
|
Time
|
Temp (°C)
|
Humidity (RH%)
|
Done by
|
Remark
|
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