FLAME EMISSION SPECTROSCOPY

CONTENTS
Introduction Principle Instrumentation Interferences Applications References
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Introduction
It is based on the measurement of intensity of light emitted when a metal is introduced into a flame. The elements can be found by wave length of colour and the amount of element can be found out by colour intensity. It determining the total concentration of sample but not about the molecular form of sample. The elements such as Na, K, Li, Ca, Mg, and transition elements such as Cu, Fe and Mn can be determined by this method.
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Principle
When a liquid sample containing a metallic salt solution is introduced into flame the following events take place.
Solvent get vaporised form solid salt Salt is vapourised then to gaseous state Gaseous molecule dissociate to free neutral atom These neutral atom excited by flame. Excited atom which are unstable and emit photons reaching the unexcited state.
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Block Diagram of Flame Photometer

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Boltzman distribution law

Liquid sample containing elements Formation of liquid droplets Fine residue Decomposion of residue Formation of exited atom
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N* N0

= e-e/Kt

N* = Number of atoms in excited state N0 = Number of atoms in ground state T = flame temperature K= boltzman constant e = Difference in energy level of excited and ground state

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Instrumentation
Burner Total consumption burner Laminar flow burner Lundergarph burner Mirors Slits Monochromator Filter detector
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Burner
Flame should evaporate the liquid droplet The flame should decompose that compound result in formation atom And flame must have to excite the atom and cause them to radiant energy

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Total consumption burner

Liquid sample is drawn into flame. From the site hydrogen and oxygen are entering and produce the flame. As soon as liquid sample enters into flame it form solid residue
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Merits and demerits

Merits
The design is simple and the entire sample is consumed

Demerits
Uniform and homogenous flame is not obtained

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Laminar flow burner

In this type fuel and oxidant are before reaching the burner and enter into the flame Only 5% reaches into the flame remaining 95% of the sample wasted result in the loss of sensitivity.
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Mirrors
Flame is emitted in all direction in order to maximize the radiation the mirror is located behind the burner. It reflects the radiation back to monochromator

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Slits
Entrance slits and exit slits are used Entrance slits
Cut the radiation around surroundings and allow only the radiation from flame.

Exit slits
It allows only selected wavelength range to pass detector
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Filters & Detectors

Filter is kept in between flame and detector Desired wave length from flame enter into the detector and the undesired one will be absorbed by the filter and not measured. Detector
The detector is to measure the intensity of radiation coming from optical system
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First Type
Sample solution aspiration take place. Emitted radiation collected by mirror Then pass through prism Then read out was calculated
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Internal standard flame photometer

Lithium is used as an internal standard The sample solution(Li) is sucked by atomiser. Emitted radiation is collected by mirror through filters which has 2 parts One is due to Li and the other is due to presence of element to be measured which are received by amplifiers until to detectors and is recorded

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Applications of flame photometry

Qualitative analysis I. To detect elements such as Na, K, Li, Mg, B, etc Quantitative Analysis I. Standard addition method

To determine very low concentration of the element present in the sample. To estimate elements which are rarely analysed Simultaneous multielement analysis
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II.

Internal standard method

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Interferences in flame photometry

A. B. C. D. E. F. Special interference Ionisation interference Chemical interference Cation Anion interference Cation cation interference Oxide formation interference
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Special Interferences
It occurs when emission of species in flame occurs at same wave length as the compound being measured Eg:- Solution of Ca and Na in flame where sodium is to be measured at 5889A but the sodium was more due to presence of another species. This can be overcome by using extraction method or by using calibration curves.

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Ionisation Interference
This interference occurs mostly in metal ion. If its occurs in sodium it can be overcome by adding potassium, but it undergo ionisation so it can be enhanced by sodium atom emission
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Cation anion Interference

It affect the intensity of radiation results in analytical error Eg:- Ca in presence of phosphate ion

Cation cation Interference It decrease the signal intensity of element present in sample Eg: Al with Ca and Mg.
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References
Instrumental Methods of Chemical analysis By Gurdeep Chatwal Pg 2.367 - 2.388 Spectroscopy By B. K. Sharma Pg 421-454
Text book of Pharmaceutical Analysis By Ravishankar Pg 26.1 26.13

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