Spektroskopi - AAS

Chapter 8
Atomic Absorption Spectroscopy

（ AAS ）
College of Science, BUCT
1
Atomic Absorption Spectroscopy
（ AAS ）
 Introduction
 Elementary Theory
 Instrumentation
 Interferences
 Experimental preliminaries
 Applications
2
Introduction
What is AAS ?
Atomic absorption spectroscopy is

a quantitative method of analysis
that is applicable to many metals.
3
What is AAS ?
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
Alan Walsh 1916-1998
http://www.science.org.au/academy/
memoirs/walsh2.htm#1
4
What is AAS ?
The technique was introduced in 1955

by Walsh in Australia
(A.Walsh, Spectrochim. Acta, 1955, 7,
108)
The first commercial atomic absorption

spectrometer was introduced in 1959
5
What is AAS ?
• An atomic absorption spectrophotometer

consists of a light source, a sample
compartment and a detector.
Sample
Compartment
Light Source Detector
6
What is AAS ?
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. 7
What is AAS ?
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.
8
The relationship between absorbance and
the concentration of atoms
Beer’s law
It = I0νe -Kνl
A = log （ I0ν/ It ） = 0.4343 K l
It - intensity of the transmitted light

Io – intensity of the incident light signal
l – the path length through the flame
(cm) 9
The relationship between absorbance and
the concentration of atoms
2
 2( v  v 0 ) 
Kv  K 0 log   ln 2 
 v 0 
2 ln 2  .e2
K0   fNov
 D  mc
A = 0.4343 K0 l = K1N0v A = KC
10
Instrumentation
Line
source Atomization Monochromator Detector
Nebulizer Read-out
Schematic diagram of a flame spectrophotomer

11
Atomic absorption spectrophotometer
12
Resonance line sources
Emit the specific resonance lines of the atoms in

question
--- Provide the sharp emission lines with a much

smaller half-width than the absorption line
--- Intensity
--- Purity
--- Background
--- Stability
--- Life-time
13
Hollow cathode lamp (HCL)
Cathode--- in the form of a cylinder, made

of the element being studied in the flame
Anode---tungsten
14
A hollow cathode lamp for Aluminum (Al)
15
SpectrAA - AAS
HCL
motorized
Mirror
16
17
Sample atomization techniques
Flame atomization
Electrothermal atomization
Hydride atomization
Cold-Vapor atomization
18
Flame atomization
Processes occurring during atomization
19
Flame atomization
Nebulizer - burner
A typical premix burner

20
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
21
Fuel and oxidant
Auxiliary
flame oxidant
Air- propane Fuel
Air- hydrogen
 Air – acetylene
 Nitrous oxide – acetylene
22
Common fuels and oxidants used in flame
spectroscopy
23
Monochromator
--- diffraction grating
24
Detector
--- photomultiplier
25
Read-out system
--- meter
--- chart recorder
--- digital display
26
Interferences
Spectral interferences
Chemical interferences
Physical interferences
27
----- spectral overlap
（ +, positive analytical error ）

Cu 324.754 nm, Eu 324.753 nm
Al 308.215 nm , V 308.211nm,
Al 309.27 nm
Avoid the interference by observing the

aluminum line at 309.27 nm
28
----- non-absorption line （非吸收线）
----- molecular absorption （ +）

combustion products (the fuel and
oxidant mixture)
Correct by making absorption
measurements while a blank is aspirated
into the flame
29
----- light scatter （ +）
Metal oxide particles with diameters

greater than the wavelength of light
When sample contains organic species
or when organic solvents are used to
dissolve the sample, incomplete
combustion of the organic matrix
leaves carbonaceous particles that are
capable of scattering light
30
----- light scatter （光散射）

（ +）
The interference can be avoided by
variation in analytical variables, such
as flame temperature and fuel-to –
oxidant ratio
Standard addition method
Zeeman background correction
31
----- Formation of compound of low volatility
Ca 2+ ， PO43- Mg2+, Al3+
Increase in flame temperature


 Use of releasing agents (La 3+ )
 Use of protective agents (EDTA)
 Separation
32
----- Ionization
 Adding an excess of an ionization

suppressant (K)
33
Physical interferences
----- viscosity
----- density
----- surface tension
----- volatility
 Matrix matching
34
Experimental preliminaries
Preparation of sample solutions
Optimization of the operating conditions

----- resonance line
----- slit width
----- current of HCL
----- atomization condition
Calibration curve procedure

35
The standard addition technique
36
Sensitivity and detection limit
Sensitivity
----- the concentration of an aqueous

solution of the elements which absorbs
1% of the incident resonance radiation
----- the concentration which gives an

absorbance of 0.0044
37
Sensitivity and detection limit
Detection limit
----- the lowest concentration of an analyte
that can be distinguished with reasonable
confidence from a field blank
D = c × 3σ / A
38
Sensitivity and detection limit (ng/mL)
39
Advantages and disadvantages
High sensitivity
[10-10g (flame), 10-14g (non-flame)]
Good accuracy
(Relative error 0.1 ~ 0.5 % )
High selectivity
Widely used
A resonance line source is required for

each element to be determined
40
The end
41

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Chapter 8

Atomic Absorption Spectroscopy

College of Science, BUCT

Atomic absorption spectroscopy is

The technique was introduced in 1955

Alan Walsh 1916-1998

The technique was introduced in 1955

The first commercial atomic absorption

• An atomic absorption spectrophotometer

Light Source Detector

A much larger number of the gaseous metal

If light of the resonance wavelength is passed

the gaseous metal atoms

specific resonance wavelength

the extend of absorption vs the number of

It - intensity of the transmitted light

Schematic diagram of a flame spectrophotomer

Emit the specific resonance lines of the atoms in

--- Provide the sharp emission lines with a much

Cathode--- in the form of a cylinder, made

Processes occurring during atomization

A typical premix burner

To convert the test solution to gaseous atoms

Nebuliser --- to produce a mist or aerosol of the

Air- propane Fuel

--- diffraction grating

--- chart recorder

--- digital display

----- spectral overlap

（ +, positive analytical error ）

Avoid the interference by observing the

----- non-absorption line （非吸收线）

----- molecular absorption （ +）

----- light scatter （ +）

Metal oxide particles with diameters

----- light scatter （光散射）

----- Formation of compound of low volatility

Ca 2+ ， PO43- Mg2+, Al3+

Increase in flame temperature

 Use of protective agents (EDTA)

 Adding an excess of an ionization

Preparation of sample solutions

Optimization of the operating conditions

Calibration curve procedure

----- the concentration of an aqueous

----- the concentration which gives an

A resonance line source is required for

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