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First Group
A. Khaerunnisa Ha
rdya

nti Arki

Nur Hasanah Jusm
an
Nurhikmah

Atomic
Absorption
Spectrometry
ICP CHEMISTRY A 2011
(AAS)
FMIPA UNM
2013

Sarce Siruru
Hasra Jalil
Contents
•
•
•
•
•

What is AAS
Theory
Instrumentations
Principle of AAS
Applications
What is AAS ?
Atomic absorption spectroscopy is a quantitative
method of analysis that is applicable to many metals
and a few nonmetals.
The technique was introduced in 1955 by Walsh
in Australia (A.Walsh, Spectrochim. Acta, 1955,
7, 108)
The application of
atomic absorption
spectra to chemical
analysis
Concentrations range is
in the low mg/L (ppm)
range.
Theory
A much larger number of the gaseous metal atoms
will normally remain in the ground state.
These ground state atoms are capable of absorbing
radiant energy of their own specific resonance
wavelength.
If light of the resonance wavelength is passed through a
flame containing the atoms in question, then part of the
light will be absorbed.
The extend of absorption will be proportional to the
number of ground state atoms present in the flame.
the gaseous metal atoms

specific resonance wavelength

extend of absorption

the extend of absorption vs the number of ground state atoms
present in the flame.
AAS Instrument
The simple diagram for the AAS
4. T element in the sample
he
will absorb some of the light,
thus reducing its intensity

5. T monochromator
he
isolates the line of
interest

3. A beam of UV light
will be focused on the
sample

1. W set the
e
instrument at certain
wavelength suitable
for a certain element

2. T element
he
in the sample
will be atomized
by heat

6. T detector
he
measures the change
in intensity

7. A computer data system
converts the change in
intensity into an
absorbance
Flame atomization
Processes occurring during atomization
Nebuliser - burner
To convert the test solution to gaseous atoms
Nebuliser --- to produce a mist or aerosol of the
test solution
Vaporising chamber --Fine mist is mixed with the fuel gas and the carrier gas
Larger droplets of liquid fall out from the gas stream and
discharged to waste

Burner head --- The flame path is about 10 –12 cm
1. Nebulizer:
4. T mixture flows
he
immediately into the burner
head.
5. It burns as a smooth,
laminar flame evenly
distributed along a narrow
slot.
1. mixes acetylene (the fuel)
and oxidant
(air or nitrous oxide).

6. L
iquid sample not flowing
into the flame collects in the
waste.

3. T result is a heterogeneous
he
mixture of gases (fuel + oxidant) and
suspended aerosol (finely dispersed
sample).

2. A negative pressure is formed at
the end of the small diameter,
plastic nebulizer tube→
(aspiration).

Note:
W
hen do we use NO2 ?
Elements that are highlighted in pink
are detectable by AAS
Principle of Atomic Absorption
Spectrophotometer

Atomized elements each absorb energy of
a wavelength that is peculiar to that
element. The atomic absorption method
uses as its light source a hollow cathode
lamp which emits light of a wavelength that
is peculiar to each element. Elements
within a solution are heated in a flame or
electrically (2000K to 3000K) and
subsequently determined using the fact
that the degree of absorption will vary with
its concentration.

Light absorption
process of atoms
Principle of Atomic Absorption
Spectrophotometer
Atomic Absorption Spectroscopy, AAS

Excited state E1
Absorption

Ground state E0

Atomic Emission Spectroscopy, AES

Excited state E1

e
e

Emission

Ground state E0

e
Characters of the atomic absorption spectrum
Profile of the absorption line

K0 - maximal absorption
coefficient
Δ ν - half width

ν 0 - central wavelength
The relationship between absorbance
and the concentration of atoms

Beer’s law
I t = I 0ν e

-Kνl

A = log ( I 0ν / I t ) = 0.4343 K ν l
I t - intensity of the transmitted light
I o – intensity of the incident light signal
l – the path length through the flame (cm)
Types of Pretreatment
Dilution
Dilute the sample with purified water, dilute acid, or organic solvents.
Examples: food products (e.g., dairy products), pharmaceuticals, and biological
samples (e.g., blood, urine).

Dry Decomposition
Heat the sample to a high temperature (400 to 500°C), Decomposition is possible
in a short time (a few hours) and operation is simple.
Elements with low boiling points (e.g., Hg, As, Se, Te, and Sb) will vaporize

Wet Decomposition
Heat the sample together with acid to a low temperature (approx. 300°C). Suitable for
volatile elements.
A long time is required for the decomposition of organic substances.

Microwave Decomposition
Decompose the sample at high pressure by heating it together with acid to a
temperature in the range 100 to 200°C in a sealed Teflon container.
The decomposition process is sealed; there is little vaporization of elements with low
boiling points; the decomposition time is short; there is little contamination from the
operating environment and the reagent; and only a small amount of acid is required.
Examples: Sediment, soil, dust, ceramics, living organisms, food products, etc.
Characters of the atomic absorption spectrum
Natural broadening
determined by the lifetime of the excited state
and Heisenberg’s uncertainty principle ( 10-5 nm )

Doppler Broadening

( 10-3 nm )

results from the rapid motion of atoms as they emit
or absorb radiation

Collisional Broadening
collisions between atoms and molecules in the gas phase
lead to deactivation of the excited state and thus broadening
the spectral lines
Characters of the atomic absorption spectrum
Doppler Broadening

( 10-3 nm )

results from the rapid motion of atoms as they emit
or absorb radiation
Application of AAS

AAS

Pretreatment (dissolution) is required for solid samples.
Results of Quantitative
Analysis of Cd in Rice
The following 2 methods can be used to analyze unpolished and polished rice decomposed using
acid:

Flame method

Furnace method

Polished rice:
0.118 ppm

0.1 ppm
0.5 ppm
Unpolished rice:
0.070 ppm

Polished rice :
0.118 ppm
Unpolished rice :
0.073 ppm

Air-C2H2

Injected amount: 10 µL
Interference inhibitor: Pd 50ppm 5 µL
Ashing: 400°C; Atomization: 1,800°C
AAS Interferences
AAS Advantages and
Disadvantages'
Advantages
1. High selectivity and sensitivity
2. Fast and simple working
3. Doesn’t need metals separation
Disadvantages
1. Analysis doesn’t simultaneous
2. Fragment have to form ready measure solution
3. Limit types of cathode lamp (expensives)
THANK YOU 
Questions
•
•
•
•

How could atom’s collision
Sample preparation of AAS
The type of sample liquid or gas
Function of AAS of few nonmetals
examples
• What happen to the sample in flame

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AAS Guide to Atomic Absorption Spectrometry

  • 1. First Group A. Khaerunnisa Ha rdya nti Arki Nur Hasanah Jusm an Nurhikmah Atomic Absorption Spectrometry ICP CHEMISTRY A 2011 (AAS) FMIPA UNM 2013 Sarce Siruru Hasra Jalil
  • 3. What is AAS ? Atomic absorption spectroscopy is a quantitative method of analysis that is applicable to many metals and a few nonmetals. The technique was introduced in 1955 by Walsh in Australia (A.Walsh, Spectrochim. Acta, 1955, 7, 108) The application of atomic absorption spectra to chemical analysis Concentrations range is in the low mg/L (ppm) range.
  • 4. Theory A much larger number of the gaseous metal atoms will normally remain in the ground state. These ground state atoms are capable of absorbing radiant energy of their own specific resonance wavelength. If light of the resonance wavelength is passed through a flame containing the atoms in question, then part of the light will be absorbed. The extend of absorption will be proportional to the number of ground state atoms present in the flame.
  • 5. the gaseous metal atoms specific resonance wavelength extend of absorption the extend of absorption vs the number of ground state atoms present in the flame.
  • 7. The simple diagram for the AAS 4. T element in the sample he will absorb some of the light, thus reducing its intensity 5. T monochromator he isolates the line of interest 3. A beam of UV light will be focused on the sample 1. W set the e instrument at certain wavelength suitable for a certain element 2. T element he in the sample will be atomized by heat 6. T detector he measures the change in intensity 7. A computer data system converts the change in intensity into an absorbance
  • 9. Nebuliser - burner To convert the test solution to gaseous atoms Nebuliser --- to produce a mist or aerosol of the test solution Vaporising chamber --Fine mist is mixed with the fuel gas and the carrier gas Larger droplets of liquid fall out from the gas stream and discharged to waste Burner head --- The flame path is about 10 –12 cm
  • 10. 1. Nebulizer: 4. T mixture flows he immediately into the burner head. 5. It burns as a smooth, laminar flame evenly distributed along a narrow slot. 1. mixes acetylene (the fuel) and oxidant (air or nitrous oxide). 6. L iquid sample not flowing into the flame collects in the waste. 3. T result is a heterogeneous he mixture of gases (fuel + oxidant) and suspended aerosol (finely dispersed sample). 2. A negative pressure is formed at the end of the small diameter, plastic nebulizer tube→ (aspiration). Note: W hen do we use NO2 ?
  • 11. Elements that are highlighted in pink are detectable by AAS
  • 12. Principle of Atomic Absorption Spectrophotometer Atomized elements each absorb energy of a wavelength that is peculiar to that element. The atomic absorption method uses as its light source a hollow cathode lamp which emits light of a wavelength that is peculiar to each element. Elements within a solution are heated in a flame or electrically (2000K to 3000K) and subsequently determined using the fact that the degree of absorption will vary with its concentration. Light absorption process of atoms
  • 13. Principle of Atomic Absorption Spectrophotometer Atomic Absorption Spectroscopy, AAS Excited state E1 Absorption Ground state E0 Atomic Emission Spectroscopy, AES Excited state E1 e e Emission Ground state E0 e
  • 14. Characters of the atomic absorption spectrum Profile of the absorption line K0 - maximal absorption coefficient Δ ν - half width ν 0 - central wavelength
  • 15. The relationship between absorbance and the concentration of atoms Beer’s law I t = I 0ν e -Kνl A = log ( I 0ν / I t ) = 0.4343 K ν l I t - intensity of the transmitted light I o – intensity of the incident light signal l – the path length through the flame (cm)
  • 16. Types of Pretreatment Dilution Dilute the sample with purified water, dilute acid, or organic solvents. Examples: food products (e.g., dairy products), pharmaceuticals, and biological samples (e.g., blood, urine). Dry Decomposition Heat the sample to a high temperature (400 to 500°C), Decomposition is possible in a short time (a few hours) and operation is simple. Elements with low boiling points (e.g., Hg, As, Se, Te, and Sb) will vaporize Wet Decomposition Heat the sample together with acid to a low temperature (approx. 300°C). Suitable for volatile elements. A long time is required for the decomposition of organic substances. Microwave Decomposition Decompose the sample at high pressure by heating it together with acid to a temperature in the range 100 to 200°C in a sealed Teflon container. The decomposition process is sealed; there is little vaporization of elements with low boiling points; the decomposition time is short; there is little contamination from the operating environment and the reagent; and only a small amount of acid is required. Examples: Sediment, soil, dust, ceramics, living organisms, food products, etc.
  • 17. Characters of the atomic absorption spectrum Natural broadening determined by the lifetime of the excited state and Heisenberg’s uncertainty principle ( 10-5 nm ) Doppler Broadening ( 10-3 nm ) results from the rapid motion of atoms as they emit or absorb radiation Collisional Broadening collisions between atoms and molecules in the gas phase lead to deactivation of the excited state and thus broadening the spectral lines
  • 18. Characters of the atomic absorption spectrum Doppler Broadening ( 10-3 nm ) results from the rapid motion of atoms as they emit or absorb radiation
  • 19. Application of AAS AAS Pretreatment (dissolution) is required for solid samples.
  • 20. Results of Quantitative Analysis of Cd in Rice The following 2 methods can be used to analyze unpolished and polished rice decomposed using acid: Flame method Furnace method Polished rice: 0.118 ppm 0.1 ppm 0.5 ppm Unpolished rice: 0.070 ppm Polished rice : 0.118 ppm Unpolished rice : 0.073 ppm Air-C2H2 Injected amount: 10 µL Interference inhibitor: Pd 50ppm 5 µL Ashing: 400°C; Atomization: 1,800°C
  • 22. AAS Advantages and Disadvantages' Advantages 1. High selectivity and sensitivity 2. Fast and simple working 3. Doesn’t need metals separation Disadvantages 1. Analysis doesn’t simultaneous 2. Fragment have to form ready measure solution 3. Limit types of cathode lamp (expensives)
  • 24. Questions • • • • How could atom’s collision Sample preparation of AAS The type of sample liquid or gas Function of AAS of few nonmetals examples • What happen to the sample in flame