Atomic Absorption Spectr

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ATOMIC

ABSORPTION
SPECTROSCOPY
TARANPREET SINGH
MS12044
Chem. Major
INTRODUCTION
ATOMIC ABSORPTION SPECTROSCOPY
IT IS A QUANTITATIVE METHOD FOR DETERMINING THE
CHEMICAL ELEMENTS IN SAMPLE AND ITS
CONCENTRATION .IT IS APPLICABLE TO MANY METALS
AND SOME NON METALS
The technique was
introduced by Alan
walsh in 1955 At
(CSIRO) Australia .

The first commercial


spectrometer was
introduced in 1959
Atomic Absorption Spectrophotometer
• Atomic absorption spectrophotometer consist of Radiation source ,
Atomizers Monochromator , Detector, Datadisplay or Computer
Schematic diagram of Atomic absorption spectrometer

LINE SOURCE ATOMIZATION MONOCHROMATOR DETECTOR

NEBULIZER READ OUT


Principle of Atomic Absorption
Spectrophotometer
Atomic absorption
spectrophotometer works on the
principle of absorption during
atomization most of gaseous
elements remains in ground state
each elements absorb radiant
energy of their own specific
wavelength . Atoms after absorbing
light make transition to higher
energy states then eventually get
back to its ground state by emitting
light .during absorption the light
that get transmitted from atoms will Light absorption
process of atoms
reach detector . It has linear
relationship that more the
concentration of ground state atoms
more will be the absorption.
Elements that are highlighted in green are
detectable by AAS
RADIATION SOURCE
(HCL - Hollow Cathode Lamp)
(EDL – Electrodeless Discharge Lamp)
Hollow Cathode Lamp (HCL)

• CATHODE – Made of metal that is being studied In the flame


• ANODE - Tungsten
DISADVANTAGE
• FOR EVERY ELEMENT SEPARATE LAMP MUST BE USED
• WORKS ONLY FOR VISIBLE AND U.V REGION
EDL – ELECTRODE LESS DISCHARGE LAMP

• Edl are commercially Available for Sb, As, Bi, Cd, Cs, Pb, Hg, K, Rb, Sn,
Te, etc.
ATOMIZATION TECHNIQUES
• FLAME ATOMIZATION
• ELECTROTHERMAL ATOMIZATION
• HYDRIDE ATOMIZATION
• COLD-VAPOUR ATOMIZATION
LAMINAR FLOW BURNER
Nebulizer
• To convert the analyte solution to gaseous atoms
• Nebulizer – To produce a mist or aerosol of the analyte solution
In vaporizing chamber
Fine mist is mixed with fuel gas and oxidant
Larger droplets of sample falls out from gas stream and discharge into
waste
• Flame path – The path of flame is about 10-12 cm
Common fuel and oxidant
DISADVANTAGE OF FLAME ATOMIZATION
• Low efficiency and low sensitivity
• REASONS OF LOW SAMPLING EFFICIENCY
Large portion of the sample flows down in the waste
The relative time of individual atoms in the optical path in the flame
is brief (≈10-4 s )
• 5-15% of the nebulized sample reaches the flame
• A minimum sample volume of (0.5-1 mL) required for reliable reading
Graphite Furnace techniques
Graphite furnace techniques
• Step involved in it(Process)
Drying Ashing Atomization
HYDRIDE GENERATION METHOD
• FOR METALS LIKE ARSENIC(AS) , ANTIMONY (Te),SELENIUM(Se),BISMUTH(Sb)
Volatile hydride usually be generated by adding acidified aqeous solution of sample to a small
volume of 1% sodium borohydride in a glass vessel. Rxn given below , the volatile hydride then
swept into atomization chamber usually quartz absorption tube that heated to several hundred
degree in a flame or tube where decomposition of the hydride takes place leading to the
formation of atoms of the analyte. The concentration of analyte is then measured by
absorption or emission .

NaBH4 Heat
As (V) AsH3 As0(gas) + H2

[H+] In Flame
Hydride Generation methods
COLD VAPOR TECHNIQUE
• Cold vapor technique is an atomization method for determination of mercury
because it is the only metallic element that has appericiable vapor pressure at room
temperature the determination of mercury In various sample is important because
of toxicity of organic mercury compound . Determination of the mercury is done by
cold vapourisation followed by atomic absorption spectroscopy.so first mercury is
converted to its +2 oxidation state by treatment of sample with an oxidizing
mixture of nitric and sulfuric acid followed by reduction of hg2+ to the metal with
sncl2. the elemental mercury is swept into a long –passs absorption tube by bubling
a stream of inert gas through the reaction mixture.
• The determination is completed by measuring the absorbance at 253.7mm
Cold-vapour technique
MONOCHROMATOR
• Monochromator used to disperse the radiation according to their
wavelength.
• Two types of monochromator
1. Prism
2. Diffraction grating
• Monochromator consist of entrance slit , collimator lens , prism or
diffraction grating ,focusing lens , exit slit
Bunsen Prism Monochromator
Diffraction Grating
MO NO CHR OMATOR S
Detector
• The role of detector is to convert light signal to electrical signal that
can be displayed on computer.
Generally in most of the instruments PMT is used

The detector contains a photoemissive cathode and a series of dynodes. The number
of electrons emitted from the cathode is directly proportional to the intensity of the
light beam. Electrons emitted from the cathode are accelerated to the first dynode
by a 90 volt potential where the electron impact dislodges several additional
electrons which are accelerated to the next dynode by an additional 90V potential.
After nine dynodes (each one at +90V with respect to the one before it), the number
of electrons finally reaching the anode is in the order of ten million for each incident
photon. The current measured at the anode collector is still proportional to the
intensity of the light but it has been amplified over a million times.
Detector(photomultiplier tube)
Applications
• PHARMACEUTICALS
• PETRO-CHEMICAL
• ENVIRONMENTAL SCIENCE
• NANOMATERIALS
• GEOCHEMICAL
• FORENSIC SCIENCE
• CLINICAL ANALYSIS
• FOOD INDUSTRY
Thank

you

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