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Dr. Babasaheb Ambedkar Technological University, Lonere, Raigad Maharashtra
Sahyadri College Of Pharmacy, Methwade, Sangola.
Presented By
Miss. Vaishnavi Parmeshwar Chavan
Sem- I 2023-24
Department of pharmaceutical chemistry
1
Flame Emission Spectroscopy
CONTENT
2
 Introduction
 Principle
 Instrumentation
 Interference
 Application
INTRODUCTION
3
 Flame photometry is a branch of spectroscopy in which the species examined in the spectrometer are in the form of atoms.
 Flame photometry is also called as Flame Atomic Emission Spectroscopy because of use of a flame to provide the energy
of excitation to atoms introduced into the flame.
 Flame photometer is an instrument used in inorganic chemical analysis to determine the concentration of certain metal ions
such as sodium, potassium, calcium, lithium, & magnesium.
 Flame photometry is based on the measurement of intensity of the light emitted when a metal is introduced into a flame. The
wavelength of the colour tells about which element is present (QuaLitative) & colour intensity tells about how much
element is presented (QuanTitative).
PRINCIPLE
 Liquid sample containing metal salt solution is introduced
into a flame.
 Solvent is first vaporized, leaving particle of solid salt which
is then vaporised into gaseous state.
 Gaseous molecule dissociate to give neutral atoms and sprayed
into a flame with the help of atomiser/nebulizer which can be
excited (made unstable) by thermal energy of flame.
 The unstable excited atoms emit photons while returning to
lower energy state.
 The intensity of emitted photon is measured by flame photometry. Figure no.1
4
INSTRUMENTATION
5
Figure No. 2:-
1) Sample delivery system :-
6
1. Nebulizer:- It is device used for introduction of a sample into the flame and also breakup the liquid into small droplets.
2. Aerosol modifier :- It remove the large droplet from the stream and allow only small droplet to passes.
3. Atomizer :- It convert analyte into free atoms.
2) Burner :-
In that several burners and fuel and oxidant combination have been used to produce analytical flame.
The burner used are :-
a. Mecker burner
b. Total consumption burner
c. Premix laminar flow burner
d. Lundergarph burner
e. Shielded burner
f. Nitrogen oxide acetylene flame
Figure No.3:- Mecker burner Figure No.4:- Total consumption burner
Figure No.5:- Premix laminar flow burner Figure No.6:- Lundergraph burner
7
3) Sample:-
8
Sample present in the form of liquid contain unknown metal salt.
4) Mirrors:-
The radiation emitted by the flame released in all direction. So, a mirror is placed behind the burner for
reflecting the radiation back to the entrance slits of the monochromators . The mirror is used is concave mirror.
5) Slits :-
The two type of slits used entrance and exist slits before and after the dispersion element. The entrances slits
cuts out most of the radiation from the surrounding allow only the radiation from the flame to pass to monochromator and exist
slits placed after the monochromator and allow only a selected wavelength pass through to the detector .
6) Monochromators:-
9
Monochromators converts polychromatic light into monochromatic light of a desired wavelength.
Prism and grating monochromators used.
7) Filters:-
In some elements, the emission spectrum contain a few lines. In such cases wide wavelength will be allowed to
enter the detector , in this situation filter used in place of the slit and monochromator system. The filter is kept between the
flame and detector, the radiation of the desired wavelength from the flame will be entering the detector and be measured.
8) Detectors:-
Detector convert the radiation coming from the optical system into a electric signals which we can easily
read out through recording system.
Ex. 1) photomultiplier (PMT)
2) Photodetector
10
Figure No. 7
Figure No. 8
INTERFERENCE IN FLAME PHOTOMETRY
11
1) Spectral Interference:-
a) First type:- In this type spectral interference arise due to partly overlapping between the spectra of two elements emitting
radiation at particular wavelength. This type of interfence can be overcome by removing the effect of interfering element by
using extraction method or using calibration curves.
b) Second type:- In this type spectral interference not involve any spectral overlapping but occur due to production of much
closer spectral lines of two or more elements. This type of interference can be overcome by increasing the resolution of the
spectral isolation system.
c) Third type:- This type of spectral interference arise due to high concentration of salts in the sample. It is occur between a
spectral line and continuous background. This type of interference can be corrected by the scanning technique.
2) Ionisation Interference:-
Ionisation interference arises due to metal atoms ionise in high temperature flame which decreases the radiant power of
atomic emission. Ionisation interference is eliminated by adding an excess of an elements which is easily ionized thereby
creating a large number of free electrons in the flame and suppressing ionization of the analyte.
12
3) Chemical Interference:-
The chemical interferences arise due to reaction between different interferents and the analyte. There are three chemical
interference as following :-
a) Cation – anion interference:- The presence of certain anions, such as oxalate, phosphate, sulphate, aluminate in a solution
may affect the intensity of radiation emitted by an element. E.g. calcium in the presence of the phosphate ion forms a stable
substance, which does not decompose easily, resulting in the producing of lesser atoms. This type of interference can be remove
either by extraction of the anion or by using calibration curves.
b) Cation – cation interference:- This type interferences neither spectral nor ionic in nature and mechanisms of their
interaction ate unknown. It occurs in sample containing sodium and calcium having comparatively closer emission
wavelength. It is prevented by using effective monochromators.
c) Oxide formation interference :- This type of interference arises due to the formation of stable oxide with free metal atoms
if oxygen is present in the flame. Thus, the emission intensity is lowered because a large percentage of free metal atoms
have been removed form the flame. It is overcome by applying very high temperature flame.
APPLICATION
14
1.Flame photometry can be used for both qualitative and quantitative analysis.
2.It can be used for the determination of alkali and alkaline earth metals.
3.It can be used in determination of lead in petrol.
4.Flame photometry used in the study of equilibrium constants involving in ion exchange resins.
5. Analysis of soft drinks, fruit juices and alcoholic beverages can also be analysed by using flame photometry.
6.In agriculture, the fertilizer requirement of the soil is analysed by flame test analysis of the soil.
REFERENCES
15
 Gurdeep R. chatwal, Sham K. Anand. Instrumental Method of Chemical Analysis. Himalaya publishing
house:2008:2.367-2.382.
 Dr.shashikant D. Barhate ,et.al. Textbook of modern pharmaceutical analytical technique ; Pee vee publication
page.no.97-106.
16

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Flame Atomic Emission Spectroscopy.-pptx

  • 1. Dr. Babasaheb Ambedkar Technological University, Lonere, Raigad Maharashtra Sahyadri College Of Pharmacy, Methwade, Sangola. Presented By Miss. Vaishnavi Parmeshwar Chavan Sem- I 2023-24 Department of pharmaceutical chemistry 1 Flame Emission Spectroscopy
  • 2. CONTENT 2  Introduction  Principle  Instrumentation  Interference  Application
  • 3. INTRODUCTION 3  Flame photometry is a branch of spectroscopy in which the species examined in the spectrometer are in the form of atoms.  Flame photometry is also called as Flame Atomic Emission Spectroscopy because of use of a flame to provide the energy of excitation to atoms introduced into the flame.  Flame photometer is an instrument used in inorganic chemical analysis to determine the concentration of certain metal ions such as sodium, potassium, calcium, lithium, & magnesium.  Flame photometry is based on the measurement of intensity of the light emitted when a metal is introduced into a flame. The wavelength of the colour tells about which element is present (QuaLitative) & colour intensity tells about how much element is presented (QuanTitative).
  • 4. PRINCIPLE  Liquid sample containing metal salt solution is introduced into a flame.  Solvent is first vaporized, leaving particle of solid salt which is then vaporised into gaseous state.  Gaseous molecule dissociate to give neutral atoms and sprayed into a flame with the help of atomiser/nebulizer which can be excited (made unstable) by thermal energy of flame.  The unstable excited atoms emit photons while returning to lower energy state.  The intensity of emitted photon is measured by flame photometry. Figure no.1 4
  • 6. 1) Sample delivery system :- 6 1. Nebulizer:- It is device used for introduction of a sample into the flame and also breakup the liquid into small droplets. 2. Aerosol modifier :- It remove the large droplet from the stream and allow only small droplet to passes. 3. Atomizer :- It convert analyte into free atoms. 2) Burner :- In that several burners and fuel and oxidant combination have been used to produce analytical flame. The burner used are :- a. Mecker burner b. Total consumption burner c. Premix laminar flow burner d. Lundergarph burner e. Shielded burner f. Nitrogen oxide acetylene flame
  • 7. Figure No.3:- Mecker burner Figure No.4:- Total consumption burner Figure No.5:- Premix laminar flow burner Figure No.6:- Lundergraph burner 7
  • 8. 3) Sample:- 8 Sample present in the form of liquid contain unknown metal salt. 4) Mirrors:- The radiation emitted by the flame released in all direction. So, a mirror is placed behind the burner for reflecting the radiation back to the entrance slits of the monochromators . The mirror is used is concave mirror. 5) Slits :- The two type of slits used entrance and exist slits before and after the dispersion element. The entrances slits cuts out most of the radiation from the surrounding allow only the radiation from the flame to pass to monochromator and exist slits placed after the monochromator and allow only a selected wavelength pass through to the detector .
  • 9. 6) Monochromators:- 9 Monochromators converts polychromatic light into monochromatic light of a desired wavelength. Prism and grating monochromators used. 7) Filters:- In some elements, the emission spectrum contain a few lines. In such cases wide wavelength will be allowed to enter the detector , in this situation filter used in place of the slit and monochromator system. The filter is kept between the flame and detector, the radiation of the desired wavelength from the flame will be entering the detector and be measured. 8) Detectors:- Detector convert the radiation coming from the optical system into a electric signals which we can easily read out through recording system. Ex. 1) photomultiplier (PMT) 2) Photodetector
  • 11. INTERFERENCE IN FLAME PHOTOMETRY 11 1) Spectral Interference:- a) First type:- In this type spectral interference arise due to partly overlapping between the spectra of two elements emitting radiation at particular wavelength. This type of interfence can be overcome by removing the effect of interfering element by using extraction method or using calibration curves. b) Second type:- In this type spectral interference not involve any spectral overlapping but occur due to production of much closer spectral lines of two or more elements. This type of interference can be overcome by increasing the resolution of the spectral isolation system. c) Third type:- This type of spectral interference arise due to high concentration of salts in the sample. It is occur between a spectral line and continuous background. This type of interference can be corrected by the scanning technique.
  • 12. 2) Ionisation Interference:- Ionisation interference arises due to metal atoms ionise in high temperature flame which decreases the radiant power of atomic emission. Ionisation interference is eliminated by adding an excess of an elements which is easily ionized thereby creating a large number of free electrons in the flame and suppressing ionization of the analyte. 12 3) Chemical Interference:- The chemical interferences arise due to reaction between different interferents and the analyte. There are three chemical interference as following :- a) Cation – anion interference:- The presence of certain anions, such as oxalate, phosphate, sulphate, aluminate in a solution may affect the intensity of radiation emitted by an element. E.g. calcium in the presence of the phosphate ion forms a stable substance, which does not decompose easily, resulting in the producing of lesser atoms. This type of interference can be remove either by extraction of the anion or by using calibration curves.
  • 13. b) Cation – cation interference:- This type interferences neither spectral nor ionic in nature and mechanisms of their interaction ate unknown. It occurs in sample containing sodium and calcium having comparatively closer emission wavelength. It is prevented by using effective monochromators. c) Oxide formation interference :- This type of interference arises due to the formation of stable oxide with free metal atoms if oxygen is present in the flame. Thus, the emission intensity is lowered because a large percentage of free metal atoms have been removed form the flame. It is overcome by applying very high temperature flame.
  • 14. APPLICATION 14 1.Flame photometry can be used for both qualitative and quantitative analysis. 2.It can be used for the determination of alkali and alkaline earth metals. 3.It can be used in determination of lead in petrol. 4.Flame photometry used in the study of equilibrium constants involving in ion exchange resins. 5. Analysis of soft drinks, fruit juices and alcoholic beverages can also be analysed by using flame photometry. 6.In agriculture, the fertilizer requirement of the soil is analysed by flame test analysis of the soil.
  • 15. REFERENCES 15  Gurdeep R. chatwal, Sham K. Anand. Instrumental Method of Chemical Analysis. Himalaya publishing house:2008:2.367-2.382.  Dr.shashikant D. Barhate ,et.al. Textbook of modern pharmaceutical analytical technique ; Pee vee publication page.no.97-106.
  • 16. 16