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Instrumentation
Types of Flame Atomizer
i) Turbulent flow burner
Similar to conventional Bunsen burner
Nebulization occurs at the flame tip.
Large amount of sample reaches the flame.
Very Noisy.
Path length is shorter lower sensitivity.

This type of burner suffers from fluctuations in

temperature since there is no good mechanism
for homogeneous mixing of fuel & oxidant.

Instrumentation
Types of Flame Atomizer
ii) Laminar flow burner
Have a long narrow burner head that serves as the
samples path (b).
Quiet flames and long path length are obtained
Sample is introduced via aspiration. The nebulizer
control the sample flow, producing a mist
(nebulization occurred before reach the flame).
The mixing chamber assures that the sample mixed
with the oxidant and fuel (e.g. air/acetylene) prior
to entry into the flame.
Instrumentation
Types of Flame Atomizer
ii) Laminar flow burner
Flashback is avoided and very homogeneous mixing
between fuel, oxidant and droplets take place.
The larger droplets condensed &
drain-out of the chamber and the
remaining fine droplets mix with
the combustion gases & enter the
flame.
Only 10% reach the flame & 90%
will condensed out.

Instrumentation Instrumentation
Fuel / Oxidant Mixtures
Turbulent Flow Laminar Flow Fuel / Oxidant Mixtures Temperature, oC
Acetylene (C2H2) / Air 2100 2400
Nebulization occurs at Nebulization occurs Acetylene (C2H2) / O2 3050 3150
the flame tip. before the flame more
Acetylene (C2H2) / N2O 2600 2800
homogenized mixing
Large amount of sample Only 10% of sample The adjustment of the fuel to oxidant ratio & flow rate
reaches the flame. reaches the flame. is very crucial. Although stoichiometric ratios are
Very Noisy. Quiet flame. usually required, optimization is necessary in order to
Path length is shorter Long path length get highest signal. However, in the determination of
Lower sensitivity. Greater sensitivity metals that form stable oxides, a flame with excess
fuel is preferred in order to decrease oxide formation.

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Instrumentation Instrumentation

The solvent firstly must evaporate within the

analytes sample.
Breakdown Destroy any
Then it will atomize the analyte within a short
complexes analyte ions
time period (10-4 s).
It is estimated that
Create atoms (elemental & passes through the path
form) of the element of of the light beam.
interest - Fe0, Cu0, Zn0, etc. This is reflected in a lower sensitivity of flame
methods.

Instrumentation Instrumentation
b) Graphite Furnace / Flameless Atomizer b) Graphite Furnace / Flameless Atomizer
(Electrothermal Atomizer) (Electrothermal Atomizer)
Atomization method mainly for solid samples.
Involves 3 steps:-

Instrumentation Instrumentation
b) Graphite Furnace / Flameless Atomizer
(Electrothermal Atomizer)
Generally it enhanced sensitivity because the
The sample compartment
entire sample is atomized in a short period & the
is really the flame since it
average residence time of the atoms in the
is in the flame that the
optical path is a second or more.
atoms absorb radiation
Require less sample than flame.
from the light source.
Have same temperature range as the flame.
Better sensitivities than flame methods
a longer atom residence time (> 1 s) &
atomized the sample in a short time.

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Instrumentation Instrumentation
Monochromator (wavelength selector) Monochromator (wavelength selector)

Consists of lenses or
mirrors to focus the Isolate analytical lines' photons that passed
radiation entrance & through the flame.
exit slits to restrict Remove scattered light of other wavelengths
unwanted radiation from the flame only a narrow spectral line
& only allows the impinges on the detector.
required radiation
towards the detector.

Instrumentation Instrumentation
Detector and Readout System
The most common detector -

The PMT determines the intensity of photons of

the analytical line exiting the monochromator.
The photomultiplier produces an electrical signal
which is proportional to the intensity of EMR of the
wavelength.
The signal from the detector is transferred to the
computer and the analytical result (output) is seen
on the monitor of the computer.

Sample Preparation
a) Flame Spectroscopic Method
Disadvantage of flame AAS method : require the
sample to be introduced into the excitation source in
the form of solution, most commonly an aqueous.
The sample must be diluted & filtered.
Accuracy of sample preparation
very important.

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Sample Preparation
a) Flame Spectroscopic Method
Others materials of interest, such as soils, animal
tissues, plants, petroleum product & minerals :
must undergo some common methods to obtain
a solution of the analyte in a form ready for
atomization.
Examples : dilute in a strong acid, heat in an oven
& etc.
Sample Preparation
b) Graphite Furnace / Flameless Atomization
(Electrothermal Atomization)
Advantage of GF atomization some of materials can
be atomized directly thus avoiding the solution step.
Liquid samples: e.g blood, petroleum products & organic
solvents can be pipetted directly into the furnace for
ashing and atomization.
Solid samples, such as plant leaves, animal tissues or
some inorganic substances can be weighed directly into
cup-type atomizers for introduction into tube type
furnaces.
However, calibration is usually difficult and required
standard that approximately the sample in composition.
Sample Preparation
d) Cold Vapor Mercury Technique
Mercury atoms exist at room temperature; no
heat required for atomization.
Using reducing agent to produce mercury vapor
in a closed reaction system.
Advantages: sensitivity improved by 100%
sampling & larger sample volume.
Limitation: application limited to mercury.
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Sample Preparation
Some of common methods used for decomposing
& dissolving samples for AAS :
Treatment with hot mineral acid; oxidation with liquid
reagent like H2SO4 / HNO3 / HClO4 (wet ashing).
Combustion in an oxygen bomb or closed container to
avoid loss of analyte.
Ashing at a high temperature.
High temperature fusion with reagents like boric oxide,
sodium carbonate, sodium peroxide or potassium
pyrosulfate.
Microwave digestion.
Hot plate digestion.
Run sample solution through ion exchange column to
remove matric.
Sample Preparation
c) Hydride Generation Technique
Samples are reacted with reducing agent in
acidified aqueous solution.
Sample in volatile form (volatile hydrides),
sample cell need to be heated up to atomized
the analyte.
Advantages: Eliminate matrix related
interference and capable of low detection limit.
Interferences
i) Spectral Interference
- Overlap of analyte signal by other signals from
other species or flame or furnace.
- Example :
Signal for Aluminium - 308.215 nm & 309.27 nm
Signal for Vanadium - 308.211nm
Avoid the interference by observing the
aluminum line at 309.27 nm
- Commonly caused by stable oxides.
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Interferences Typical Industrial Applications

ii) Chemical Interference Pharmaceutical Analysis
- Chemical reactions of other species with analyte.
- Caused by substances that decrease the extent Determination of metallic or metal containing
atomization of analyte. active ingredients- amphetamine, salicylic acid,
- Minimized by high flame temperatures. cocaine using flame AAS or GFAAS.
In traditional Chinese herbal medicines contain
iii) Physical interferences traces of toxic heavy metals such as mercury and
lead in the form of organo-metallic compound.
a. viscosity
b. density
c. surface tension
d. volatility

Typical Industrial Applications Typical Industrial Applications

Chemicals Analysis Forensic Analysis

Paints, Varnishes, Pigments, Fertilizers, Pesticides.
Determination of fertilizers and pesticide inside
foodstuff or wood can be performed.
Determination of toxic elements inside paint,
varnish.
Analysis of the residues remaining on object,
body parts, chemicals.
Examine the weapon, bullets, cartridge.