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13/3/2017

Overview of AAS - Flame

Detector

Flame

Signal Processor &


Output Device
Liquid Sample

Principle of Atomic Absorption


Introduction
Spectroscopy
Atomic absorption spectroscopy is a quantitative is an analytical method based on the absorption
method of analysis that is applicable to many of UV or visible light by gaseous atoms.
metals. It makes use of the absorption of light The sample becomes atomized by injecting a
by these elements in order to measure their solution into a flame (flame AAS) or by heating a
concentrations. dried sample in a graphite furnace.
Atoms : cannot rotate or vibrate as a molecule
does only electronic transitions within the
atom can take place when energy is absorbed.
In atomic spectroscopy, the absorption and
emission methods deal with free atoms.

Principle of Atomic Absorption


Atomic Absorption Spectroscopy
Spectroscopy
AAS is a quantitative methods of analysis based Advantages of AAS
on the absorption of light by atoms at the free
atomic state. Able to distinguish one element from
The absorption measurements followed the another in a complex sample.
Principle of Beers - Lambert law. Used for qualitative & quantitative determination
of 70 to 80 elements.
Able to perform simultaneous
= abc multi-element analysis.
Analyte is usually measured in
A = absorbance of analyte
a = absorptivity ppm ppb
ppt

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Classification of Atomic
Absorption vs. Emission
Spectroscopy
Every element has a specific number of electrons
Atomic Absorption amount of radiation associated with its nucleus.
absorbed by ground state atoms created in the The normal & most stable orbital configuration of
flame. an atom is known as the .
Atomic Emission amount of radiation emitted If energy is applied to an atom, the energy will be
to return to the ground state. absorbed & an outer electron will be promoted to
Atomic Fluorescence amounts of radiation a less stable configuration known as the
which emit the same wavelength that was .
absorbed (external lamp or laser) or fall to the
lower state and emit longer wavelength.

Absorption vs. Emission


Since the excited state is unstable, the atom will The ground state atom absorbs light energy of a
immediately return to the ground state, releasing specific wavelength as it enters the excited state.
light energy. By measuring the amount of light absorbed a
Atomic absorption instruments are capable of quantitative determination of the amount of analyte
measuring both atomic absorption and atomic
emission. can be made.

The atomic absorption process

Example : Absorption & Emission of


Hydrogen
Involved excitation & decay processes. Since the
Hydrogen Absorption Spectrum
excited state is unstable, the atoms spontaneously
return to the ground state & emit light.

If an atom jumped > 1 energy


energy
DE
n=1
levels because absorbed Hydrogen Emission Spectrum
high E, the process of
n=2
n=3
returning to its ground
state may take several steps,
- i.e. to the nearest low
energy level first, then down
to the next level.

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Instrumentation : Performance
Instrumentation Checking
The basic design in AAS includes a radiation
source, chopper, atomizer (burner),
monochromator, detector & data system.
Single & double beam instruments are available,
however, double beam AAS are more sensitive &
accurate.

Instrumentation : Performance Instrumentation : Performance


Checking Checking
Reasons for knowing the C.C value : Calculation of Characteristic
Concentration Value
To determine whether all instrumental
conditions are optimized.
To determine whether the instrument is
performing up to specification by measuring
the absorbance of known concentration and
compare the result to the expected value.
CC value of the prepared standard solution will be
To predict the absorbance range & determine
compared with the expected CC value. Percentage
the concentration range which will produce difference of within 20% is considered
optimum absorbance levels. acceptable.

Instrumentation Instrumentation

Since samples are usually liquid or solids, the Single-Beam AAS


analyte atoms or ions must be vaporized in a flame
or graphite furnace.
The atoms absorb ultraviolet or visible light &
make transition to higher electronic energy level
(excited state).
The analyte concentration is determined from the
amount of absorption. The light source (hollow cathode lamp / electrodeless
discharge lamp) emits a spectrum that specific to the
element of which it is made, which is focused through
the sample cell into the monochromator.

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Instrumentation Instrumentation
Double-Beam AAS Basic Component AAS

Light
source

Light source from the lamp is divided into a sample Atomizer


beam & a reference beam. In this system, the
readout represents ratio of the sample & reference
beams. Stability is enhanced.

Instrumentation Instrumentation
Basic Component AAS 5 Basic Components
Light source - emits the spectrum of the element of
interest.
An absorption cell - in which atoms of the sample
are produced (flame, graphite furnace).
Monochromator for light dispersion.
Detector which measures the light intensity and
amplifies the signal.
A readout device : A display that shows the reading
after it has been processed by the instrument
electronics.

Instrumentation Instrumentation
Light Sources for Atomic Absorption a) Hollow Cathode Lamp (HCL)
Necessary to use a narrow-line source which HCL is an excellent, bright, stable line source for
emits a narrow-line spectra of the element of most elements.
interest. Hollow cylindrical cathode is made of element
Narrow-line sources provide high intensity & of interest.
make atomic absorption a specific analytical The tube is filled with argon or neon.
technique.
Main sources used are:

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Instrumentation Instrumentation
Hollow Cathode Lamp b) Electrodeless Discharge Lamp (EDL)
To improve the limitations of the HCL.
A high voltage is impressed across the electrodes, cause the More intense & brighter, more stable, more
gas atoms to be ionized at the anode. sensitive offer better precision & lower detection
Positive ions are accelerated toward the negative cathode. limits for some elements.
When they bombard the cathode, they cause some of the
metal to sputter and become vaporized. Using the RF generator to create the RF field.
The vaporized metal is excited to higher electronic levels by RF will vaporize & excite the
continued collision with the high-energy gas ions. atoms inside the bulb, causing
When the electrons return to the ground state, the them to emit their
characteristic lines that metallic element are emitted. characteristic spectrum.
Sharp line of light came out from the lamp when the electrons
(in the metal) return to the ground state and emit photon of light.

Instrumentation Instrumentation
Chopper Chopper
Used to fluctuate the source output.
Is a circular disc with four quarters :
mirror
open
The disc rotates at high constant speed,
when the mirrored quarter in-front of the lamp,
it reflects the radiation.
When the open quarter is in-front of the lamp,
the radiation will pass.

Instrumentation Instrumentation
Atomizer a) Flame Atomizer
component used for atomization of analyte.
Atomization : Conversion of the liquid
is separation of particles into individual molecules sample to a fine spray.
& breaking molecules into atoms.
To convert our sample to free atoms Solid atoms are mixed with
Two approaches are used: the gaseous fuel.
Flame atomizer
Graphite furnace
Solid atoms are converted to
a vapor in the flame.

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Instrumentation Instrumentation
a) Flame Atomizer
Use flame to convert liquid sample to free atoms.
Three types of particles that exist in the flame: Mg : atomized by longer exposure
- Atoms - Ions - Molecules to flame, but is eventually
oxidized.
Flame Structure Ag : slow to oxidize, the
Interzonal region = the hottest part number of atoms increases
& the best for atomic absorption. with flame height.
Fuel rich flames are the best for Cr : oxidizes readily, highest
atoms because the likelihood of concentration of atoms at
oxidation of the atoms is reduced. the base of the flame.
Oxidation occur at secondary zone