- BY
SUBHASISH DAS
M.PHARM 1ST YEAR
ROLL- 19320712001
REG. NO-121932310012 OF 2012-2013
CLASS ROLL – 13 .
INTRODUCTION
 Atomic absorption spectroscopy was introduced in mid 1950’s by
“Alan Walsh”.
 Most powerful technique to determine trace metals in liquid
quantitatively
 In a sentence “Atomic Absorption Spectroscopy (AAS) “ is a method
of elemental analysis , particularly useful for determination of trace
metals in liquid and is almost independent of the molecular form of
the metal in sample.
MERITS
 The atomic absorption technique is specific
because the atoms of a particular element can only
absorb radiation of their own characteristic
wavelength
 Some element possess higher detection limits by
atomic absorption like Ag , As , Au etc.
 Independent of flame temperature.
THEORY
 Atomic absorption spectroscopy deals with
absorption of specific wave length of radiation by
neutral atoms in the ground state.
 When a light of this wavelength is allowed to pass
through a flame having atoms of the metallic
species , part of the light will be proportional to the
density of the atoms in the flame.
EQUATIONS
 At ,
υ the total amount of light absorbed = ( e2/mc)*Nf
Where,
e = charge on electron.
m = mass of electron.
c = speed of light.
N = total number of atoms that can absorb frequency
ν in the light path.
f = the oscillator strength or ability for each atom to
absorb at frequency ν.
contd..
Contd..
As ,e, m, c are constant equation becomes
Total amount of light absorbed = constant * N * f
GROTRIAN DIAGRAMME
 Walter Robert Wilhelm Grotrian (21/4/1890 - 3/3/ 1954)
was a German astronomer and astrophysicist.
 Grotrian studied the emission line from the solar corona in
the green region of the spectrum; this emission line could not
be attributed to any known chemical element and was
thought to be a new element (which scientists named
"coronium").
 Grotrian and Bengt Edlén from Sweden demonstrated that the
two observed emission lines arise from iron atoms that have
lost about half their 26 electrons .
ATOMIC ABSORPTION TRANSITIONS
EFFECT OF FLAME
TEMPERATURE
e
g
g
=
N
N E
o
u
o
u ex
kT


•Effect of flame temperature: Since flame is at high temperature
might have an effect on fraction of atoms in excited state.
•Boltzmann's equation describes effect of flame temperature:
where
e
g
g
=
N
N
kT
E
o
u
o
u ex

Where,
Nu is the number of atoms in excited state
gu the number of degenerated orbitals on this energy level.
No and go refers to the same figures at ground state.
k is Boltzmann constant and
T is the temperature .
E is energy difference between two orbitals
Therefore, an increase in temperature results in an increase of the
number of excited atoms, which is equivalent to a lowering in
absorption
PRINCIPLE
Light source Light Light
DETECTOR
Gaseous
molecules
Solid/Gas
aerosol
Spray
S
I
G
N
A
L
RECORDER
A light beam is passed through the flame,
Radiation is absorbed, transforming the ground
state atoms to an exited state.
WORKING PRINCIPLE
 Liquid sample → formation of droplet → fine
residue
↓
neutral atom ← Formation of neutral atom
absorbs specific
Wavelength of radiation from hollow cathode lamp.
↓
Measurement of intensity of radiation absorbed by using
photometric detectors.
Atomic Absorption
Instrumentations
INSTRUMENTATION
SINGLE BEAM DOUBLE BEAM
MAJOR PARTS OF
INSTRUMENT
 HOLLOW CATHODE LAMP - The cathode is made up of specific element
or alloys of elements or coating of elements on cathode , as current is
applied between anode & cathode , metal atoms emerge from hollow cup
and collides with filler glass . Due to the collision, number of metal atoms are
excited and emit their characteristic radiation , this is absorbed by neutral
atoms of same element in ground state , occur in the flame , when sample
solution is sprayed. Band width-0.001to 0.01 nm.
CONTD…
 ATOMISER ASSEMBLY–
Assembly used as atomizer and nebulizer.
Premix type Total consumption Graphite furnace
INTERFERENCES
A. PHYSICAL – Due to sample matrix or flame or scattering or similar
alkali halides , termed as Background absorption.
remedy- use background corrector
CONTD..
B. CHEMICAL – In complete dissociation of
compound ,
remedy – 1. use high temperature flame
2. chemical means are applied.
C. IONISATION – Due to too high flame temperature.
remedy – addition of more easily ionisable
element.
D. SCATTERING EFFECTS – Due to presence of
high concentration of interfering element.
remedy – using a continuum source.
APPLICATIONS
 Estimation of trace elements in biological fluid.
 Estimation of Copper ,Zinc, Nickel in food products.
 Estimation of Zinc in Zinc insulin injection
 Estimation of lead in Calcium Carbonate, petrol.
 Estimation of elements in soil ,water, effluents,
ceramic etc.
ELEMENT Λ (nm) ppm
SODIUM 589 0.01
POTASSIUM 766.5 0.01
CALCIUM 442.7 0.05
LEAD 217 0.01
DETECTION LIMIT AND
SENSITIVITY
 The concentration of element present in the sample solution
which produces 1% absorption.
 Sensitivity , expressed in terms of μg/ml for 1% absorption.
 C1%=(C0.1*0.0044)/0.1
Where,
C1% = the concentration give rise to 1% absorption.
C0.1 = the concentration give rise to an absorbance of 0.1
DEMERITS
 A separate lamp for each element to be determined
is required.
 Elements produce oxides in flame may not be
successfully determined quantitatively.
 In aqueous solution , the predominant anions
affects the signal to a negotiable degree.
CONCLUSION
 ATOMIC ABSORPTION SPECTROSCOPY mainly
used to determine trace element in soil samples,
waters, petrol etc ; not just qualitatively, mainly
quantitative determination of metals are done .
 In case of isolation and purification of herbal drugs
or phytochemical form crude form AAS helps as a
support to determine the amount of trace material
present , so as an analytical tool it is very use full.
REFERENCES
1. G. R. Chatwal , S. K. Anand (2010) , Instrumental Methods Of
Chemical Analysis , Himalaya Publishing house , Ch – 13 , Pg. no. -
2.340 – 2.366 .
2 . A. H. Beckett , J. B. Stenlake , (2007) , Practical Pharmaceutical
Chemistry , CBS Publishers & Distributors Pvt. Ltd. , 4th ed. , part two,
Ch – 8 , Pg. no .- 346 – 357. CBS Pubs ISBN : 81-239-0514-9 ,
Athlone ISBN : 0-485-11323-8
3. Hobart H. Williard , Lynne L . Merritt, jr. , John A. Dean , Frank A.
Settle, jr. , Instrumental Methods Of Analysis , (2006), CBS Publishers
& Distributors Pvt. Ltd. , 7th ed. , Ch – 9 , Pg no – 243- 255 , ISBN :
81-239-0943-8
ATOMIC ABSORPTION SPECTROSCOPY

ATOMIC ABSORPTION SPECTROSCOPY

  • 1.
    - BY SUBHASISH DAS M.PHARM1ST YEAR ROLL- 19320712001 REG. NO-121932310012 OF 2012-2013 CLASS ROLL – 13 .
  • 2.
    INTRODUCTION  Atomic absorptionspectroscopy was introduced in mid 1950’s by “Alan Walsh”.  Most powerful technique to determine trace metals in liquid quantitatively  In a sentence “Atomic Absorption Spectroscopy (AAS) “ is a method of elemental analysis , particularly useful for determination of trace metals in liquid and is almost independent of the molecular form of the metal in sample.
  • 3.
    MERITS  The atomicabsorption technique is specific because the atoms of a particular element can only absorb radiation of their own characteristic wavelength  Some element possess higher detection limits by atomic absorption like Ag , As , Au etc.  Independent of flame temperature.
  • 4.
    THEORY  Atomic absorptionspectroscopy deals with absorption of specific wave length of radiation by neutral atoms in the ground state.  When a light of this wavelength is allowed to pass through a flame having atoms of the metallic species , part of the light will be proportional to the density of the atoms in the flame.
  • 5.
    EQUATIONS  At , υthe total amount of light absorbed = ( e2/mc)*Nf Where, e = charge on electron. m = mass of electron. c = speed of light. N = total number of atoms that can absorb frequency ν in the light path. f = the oscillator strength or ability for each atom to absorb at frequency ν. contd..
  • 6.
    Contd.. As ,e, m,c are constant equation becomes Total amount of light absorbed = constant * N * f
  • 7.
    GROTRIAN DIAGRAMME  WalterRobert Wilhelm Grotrian (21/4/1890 - 3/3/ 1954) was a German astronomer and astrophysicist.  Grotrian studied the emission line from the solar corona in the green region of the spectrum; this emission line could not be attributed to any known chemical element and was thought to be a new element (which scientists named "coronium").  Grotrian and Bengt Edlén from Sweden demonstrated that the two observed emission lines arise from iron atoms that have lost about half their 26 electrons .
  • 8.
  • 9.
    EFFECT OF FLAME TEMPERATURE e g g = N NE o u o u ex kT   •Effect of flame temperature: Since flame is at high temperature might have an effect on fraction of atoms in excited state. •Boltzmann's equation describes effect of flame temperature: where
  • 10.
    e g g = N N kT E o u o u ex  Where, Nu isthe number of atoms in excited state gu the number of degenerated orbitals on this energy level. No and go refers to the same figures at ground state. k is Boltzmann constant and T is the temperature . E is energy difference between two orbitals Therefore, an increase in temperature results in an increase of the number of excited atoms, which is equivalent to a lowering in absorption
  • 11.
    PRINCIPLE Light source LightLight DETECTOR Gaseous molecules Solid/Gas aerosol Spray S I G N A L RECORDER
  • 12.
    A light beamis passed through the flame, Radiation is absorbed, transforming the ground state atoms to an exited state.
  • 13.
    WORKING PRINCIPLE  Liquidsample → formation of droplet → fine residue ↓ neutral atom ← Formation of neutral atom absorbs specific Wavelength of radiation from hollow cathode lamp. ↓ Measurement of intensity of radiation absorbed by using photometric detectors.
  • 14.
  • 15.
  • 16.
    MAJOR PARTS OF INSTRUMENT HOLLOW CATHODE LAMP - The cathode is made up of specific element or alloys of elements or coating of elements on cathode , as current is applied between anode & cathode , metal atoms emerge from hollow cup and collides with filler glass . Due to the collision, number of metal atoms are excited and emit their characteristic radiation , this is absorbed by neutral atoms of same element in ground state , occur in the flame , when sample solution is sprayed. Band width-0.001to 0.01 nm.
  • 17.
    CONTD…  ATOMISER ASSEMBLY– Assemblyused as atomizer and nebulizer. Premix type Total consumption Graphite furnace
  • 18.
    INTERFERENCES A. PHYSICAL –Due to sample matrix or flame or scattering or similar alkali halides , termed as Background absorption. remedy- use background corrector
  • 19.
    CONTD.. B. CHEMICAL –In complete dissociation of compound , remedy – 1. use high temperature flame 2. chemical means are applied. C. IONISATION – Due to too high flame temperature. remedy – addition of more easily ionisable element. D. SCATTERING EFFECTS – Due to presence of high concentration of interfering element. remedy – using a continuum source.
  • 20.
    APPLICATIONS  Estimation oftrace elements in biological fluid.  Estimation of Copper ,Zinc, Nickel in food products.  Estimation of Zinc in Zinc insulin injection  Estimation of lead in Calcium Carbonate, petrol.  Estimation of elements in soil ,water, effluents, ceramic etc. ELEMENT Λ (nm) ppm SODIUM 589 0.01 POTASSIUM 766.5 0.01 CALCIUM 442.7 0.05 LEAD 217 0.01
  • 21.
    DETECTION LIMIT AND SENSITIVITY The concentration of element present in the sample solution which produces 1% absorption.  Sensitivity , expressed in terms of μg/ml for 1% absorption.  C1%=(C0.1*0.0044)/0.1 Where, C1% = the concentration give rise to 1% absorption. C0.1 = the concentration give rise to an absorbance of 0.1
  • 22.
    DEMERITS  A separatelamp for each element to be determined is required.  Elements produce oxides in flame may not be successfully determined quantitatively.  In aqueous solution , the predominant anions affects the signal to a negotiable degree.
  • 23.
    CONCLUSION  ATOMIC ABSORPTIONSPECTROSCOPY mainly used to determine trace element in soil samples, waters, petrol etc ; not just qualitatively, mainly quantitative determination of metals are done .  In case of isolation and purification of herbal drugs or phytochemical form crude form AAS helps as a support to determine the amount of trace material present , so as an analytical tool it is very use full.
  • 24.
    REFERENCES 1. G. R.Chatwal , S. K. Anand (2010) , Instrumental Methods Of Chemical Analysis , Himalaya Publishing house , Ch – 13 , Pg. no. - 2.340 – 2.366 . 2 . A. H. Beckett , J. B. Stenlake , (2007) , Practical Pharmaceutical Chemistry , CBS Publishers & Distributors Pvt. Ltd. , 4th ed. , part two, Ch – 8 , Pg. no .- 346 – 357. CBS Pubs ISBN : 81-239-0514-9 , Athlone ISBN : 0-485-11323-8 3. Hobart H. Williard , Lynne L . Merritt, jr. , John A. Dean , Frank A. Settle, jr. , Instrumental Methods Of Analysis , (2006), CBS Publishers & Distributors Pvt. Ltd. , 7th ed. , Ch – 9 , Pg no – 243- 255 , ISBN : 81-239-0943-8