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Operation And Calibration Of FTIR Spectrophotometer

Quality control
To provide a procedure to operate and Calibrate the
spectrophotometer xxxxx (Perkin Elmer, Spectrum one).

I.    PURPOSE :

     To provide a procedure to operate and Calibrate the

spectrophotometer xxxxx (Perkin Elmer, Spectrum one) 

 II.    SCOPE:
        This procedure is applicable to the FTIR Spectrometer
(Perkin Elmer) used in the Quality Control department 

III.    RESPONSIBILITY:
        It is the responsibility of the Quality Control personnel
involved in the calibration of FTIR Spectrometer (Perkin
Elmer) to follow the procedure and schedule as mentioned in
this Standard Operating Procedure

 IV.    DOCUMENT REFERENCE:

SOPs    :    Core procedure, Calibration of Equipment
                  Operation of KBr Pellet Press    
Forms    :    Calibration of FTIR Spectrometer 

V. OPERATION:

1.0      General     

1.1.    Before use, ensure that the instrument is clean and
free from dust.  Ensure that the instrument 
             is connected to a stabilized ( U.P.S. ) power supply.
1.2    Avoid touching optical surfaces.
1.3    Do not carry out operations involving water or
corrosive liquids near the instrument.
1.4    Ensure that the instrument is located and maintained
at a temperature between 19°C and 30°C and at a relative
humidity not exceeding 60 percent.

2.0    STARTING UP:

2.1    Connect the instrument to the main power supply.

2.2    Switch on the instrument using the switch provided on

the right side of the instrument.

2.3    Switch on  C.P.U., Monitor . Wait to start Windows

software.

2.4    Double Click on Spectrum one icon on the main screen.

2.5   Select ‘Spectrum One’ and click ‘OK’. Click

BACKGROUND, background will be stored automatically, and
then click ‘OK’.

    Note :    The instrument is always kept ON to get optimum

performance.

3.0       CHECKING ENERGY LEVEL

3.1    To see the energy level   click  “Instrument” from menu
bar and then click “Monitor”.
3.2    Wait till the energy level is displayed on the monitor.  It
must be more than 2500.If the energy is less than 2500,
then the instrument hould not be used and Service engineer
should be called.
3.3    [If current intensity is displayed as ‘0000’ or the error
‘Scan failed – Source failed’, is displayed on the screen, this
indicates that the source filament needs to be replaced.]

3.4    Click  “ Exit “ to come out of the test mode.

    [Note:  Perform this test whenever the power is switched

off and put on again]
4.0    TAKING BACKGROUND SPECTRUM

4.1    Ensure there is no sample in the sample compartment.

4.2    Go to  SET UP => INSTRUMENT & fill the  following
 informations.
4.3    Click SAMPLE => Type name (Background)  SCAN =>
Background   UNIT => Energy (EGY). RANGE  => Start:
4000 cm-1 End: 400 cm-1, SCAN NO=> 4. Click Apply &
then scan.
4.4    A blank background scan is done and automatically
stored.

5.0    STANDARD AND SAMPLE PREPARATION IN POTASSIUM

BROMIDE (KBr)

5.1    Make sure that the pestle mortar and the pellet maker
used for preparing KBr disk is clean, if it is not, clean it.
5.2    Weigh 4 to 5 mg of the standard in a mortar and grind
the standard until it takes a glossy appearance.
5.3    Weigh 400 to 500 mg of KBr into the same mortar so
that the concentration of standard is about 1 %  (For 5 mg
standard take 500 mg of KBr).
5.4    Grind the standard thoroughly to get a uniform mixture
unless otherwise specified in the specification.
5.5    Assemble the die by inserting the shiny stainless steel
disc into the barrel with the polished side up.
5.6    Take care not to touch the polished surface.
5.7    Transfer the powder from mortar into the barrel using
a spatula and rotate the assembly such that a thin uniform
surface is obtained.  Insert the plunger.
5.8    Place the die assembly in hydraulic, press and rotate
the screw on top clockwise until it holds the die assembly
tightly.
5.9    Close the pressure valve and apply by moving the lever
up and down.  Apply to 10 tons pressure and wait for 2
minutes.
5.10    Release the pressure gently by opening the valve.
5.11    Separate the barrel from the base and place the
barrel with the plunger on the hydraulic press such that the
plunger is touching the base of the hydraulic plate.  Place the
disc removed over the top and rotate the screw on top
clockwise till the disc comes out.
5.12    Place the KBr disk in the sample holder.
5.13    Carry out same procedure for the sample preparation.

6.0    STANDARD AND SAMPLE PREPARATION IN NUJOL

(Mineral oil / Liquid paraffin oil)

6.1    Weigh about 10 to 20 mg standard into a mortar.

6.2    Grind the standard thoroughly to get a glossy
appearance unless otherwise specified in the specification.
6.3    Add two drops of nujol (liquid paraffin of spectroscopic
grade is suitable) and mix thoroughly to get a uniform
smooth creamy consistency.
6.4    Collect this mull from the mortar and place it on a NaCl
window cell (previously cleaned in carbon tetrachloride).
6.5    Place the second window on top.  Lightly press the two
windows together so as to get an evenly spread layer of
sample between the NaCl windows.  Wipe away the NaCl
cells with excess split mull with a soft tissue paper and place
in the cell holder and tighten lightly.
6.6    Carry out the same procedure for the sample
preparation.

7.0    TO OBTAIN A SPECTRUM

7.1    Keep the holder containing the pellet in the sample

compartment and close the compartment.
7.2         Go to  SET UP => INSTRUMENT & fill the  following
 information
7.2.1    Click SAMPLE =>Type Sample Name    Description
 =>About sample (About AR No.) 
              Click SCAN => Select Sample      UNITS  => % T
              RANGE   =>  Start : 4000 cm-1  End : 500  cm-1 
SCAN  NO   =>  4. Click Apply & then scan.
7.2.2      Click Instrument
             Resolution: Select 4.00
7.2.3    Click Beam
           Select None.    
7.3     TO GIVE THE CORRECT PATH. 
Go to beam and click on filter. select  none
While performing internal calibration select polystyrene
filter. 
Instrument will scan the spectrum  & will be displayed on the
screen. If needed smooth the spectrum in seq, Go to
PROCESS=>SMOOTH=>AUTOMATIC SMOOTH
7.4    Similarly obtain the spectrum of related working
standard material. 

8.0    SUPERIMPOSING TWO SPECTRA

8.1    Select the Raw material spectrum & related WS

spectrum from C:Pel_dataspectraws and click ‘OK’
9.0    OPTIMUM GRAPHICS DISPLAY

9.1    Select one of the spectra  & adjust using arrow keys on
the screen.

9.2    To mark the peaks of interest select VCURSR => drag
to desired peak and double click. 

9.3    To remove the vertical line click VCURSR again.

10.0    PRINTING
    
10.1         Click setup and then Report Template. A Report
Builder opens on the main screen. Click ‘File’ and then ‘Open
Template’. Open the template ‘HET.pfm’. 
10.2     From the main screen click ‘File’ and then ‘copy to
report’. The spectrum gets copied to    the ‘HET’ Report
Template. Give print from the Report Builder print option. 
10.3    Close the Report Builder icon.
11.0       Maintenance:
11.1    Change the purge desiccant kits after every six
months to control the humidity inside 
     the instrument, failing which can cause extensive damage
to the hygroscopic parts.
11.2    While operations dehumidifier must be kept on.

12.0   Assembling and application of HATR accessory:

12.1    Raise the sample cover to the vertical position, press
the release clip and lift the cover upwards  
          as shown in the figure given below.
12.2    Reach in under the base of current accessory and pull
the blue release towards you to release the accessory.

12.3    Hold the HATR accessory as shown in the figure given

below, rest the back of it on the 
           ledge in the sample area and slide it into the position

12.4   After assembling the HATR accessory, software will

recognize, and displays the message
         “ Ensure top plate in position’.
12.4    Remove the cover and place the Zinc selenium
sulphide plate on the HATR accessory, with arrows     pointing
towards the back.
12.5    Collect the new background scan and place the
sample on ZNS plate and place the cover on it.

12.6   Apply the force by using force gauge screw and adjust
the screw to 60% force and then proceed for sample scan. 

 13.0    Qualification of KBr

13.1     Check the surroundings for cleanliness or if it is not

clean, clean with soft clean 
 duster.
13.2   KBr bottle should be stored in dry box.
13.3   Scan of KBr should be taken after opening the bottle
to check any interfering  
   absorption bands. Note the lot number of the bottle and
give the validity period of 
   3 years on the bottle.
13.4       Make a disc about 2 mm thick from material.

13.5       Set measuring mode absorbance.

13.6       Place the KBr pellet inside the interferometer and

give background scan.

13.7       Do not remove the KBr pellet. Then given sample

scan.

13.8      Acceptance Criteria:  The spectrum should have a

substantially flat baseline over 
             the range 4000 to 620  cm-1.  It should exhibit no
maxima with an absorbance 
             greater than 0.02 above the baseline with the
exception of maxima due to water at 
             3440 and 1630 cm-1 . 

VI.       CALIBRATION                                Calibration frequency:

First week of every month

1.0       Control of Wave numbers:

1.1       Record the spectrum of polystyrene film4000 cm-1

to 650 cm-1 after the routine  
            Background correction.  The film should be stored
carefully in desiccator over silica gel 
            when not in use.
1.2    The following bands should appear at the frequencies
indicated below and should not deviate from the designated
frequency by more than the tolerance indicated.

S.No.    Wave-number (cm-1)    Acceptable Tolerance (cm-1)

01.    3060.0    ± 1.0       (3059.0 –3061.0)
02.    2849.5    ± 1.0       (2848.5 – 2850.5)
03.    1942.9    ± 1.0       (1941.9 – 1943.9)
04.    1601.2    ± 1.0       (1600.2 – 1602.2)
05.    1583.0    ±  1.0       (1582.0 –1584.0)
06.    1154.5     ± 1.0      (1153.5 – 1155.5)
07.    1028.3    ±  1.0       (1027.3 – 1029.3)

2.0     Control of resolution performance:

2.1    Expand the recorded polystyrene spectrum in the

region 3200 cm-1 to 2600 cm-1 as follows : Go to  “ FORMAT
“ icon ,  enter  3200  in  LEFT  block, 2600  in RIGHT & click
 OK .  

2.2    Note down the absorption at wave numbers 2870 cm-1

(tolerance ± 1 cm-1) and 2849.5 cm-1  (tolerance ± 1
cm-1).  The difference of between the absorbances at the
absorption minimum at 2870 cm-1 and absorption
maximum at 2849.5 cm-1  should be greater than   0.33.

2.3    Expand the polystyrene spectrum in the wave number

region 1800 cm-1 to 1400 cm-1      cm-1 as follows: Go to
FORMAT icon, enter 1800 in LEFT block, 1400 in     RIGHT    
 & Click OK.

2.4    Note down the absorption at wave numbers the

difference the absorption at 1583 cm-1 (tolerance ± 1
cm-1) and 1589 cm-1 (tolerance ± 1 cm-1). The difference
of between the     absorbances at the absorption maximum
at 1583 cm-1 and the absorption     minimum at    1589
cm-1  should be greater than 0.08.

3.0      Io-line Flatness test:  

3.1     Scan the background from 4000 cm-1 to 650 cm-1

after the routine Background correction. adjust the  Y axis to
99.5% - 100.5% transmittance.

3.2      Acceptance criterion: The Io -line should not cross

99.5% and 100.5% transmittance range.    

Note:     If the instrument fails in calibration, proceed as per

the Core Procedure, “Calibration of Equipment”.

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FTIR, spectrophotometer, Pellet Press , automatically, barrel

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