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Atomization Techniques in

Atomic Spectroscopy
CH301 LECTURE
• In previous lectures we learnt about two major
atomization process in atomic spectroscopy:
1. Flame
2. Plasma

In this lecture you will learn about three other


atomization technique used in conjunction with AAS
mostly:
• Graphite Furnace AAS
• Hydride Generation AAS (HG-AAS)
• Cold vapor AAS (CV-AAS)
Graphite Furnace
Atomisation Process
Drying
• Sample is heated for 20-30 seconds at 110-
125°C to evaporate any solvent or volatile
matrix components.

Ashing
• Performed at an intermediate temperature
to prevent loss of analyte
Atomization

• Temperature of furnace unit raised


instantaneously to bring about the
dissociation of residues into free atoms ( 2000
- 3000 K) that are responsible for absorption
ADVANTAGES
• provide a reducing environment for easily
oxidized elements
• small sample sizes
• solid and liquid samples
• higher sensitivity
• samples placed directly in the graphite
furnace
 Low amounts of noise from the furnace
 Lower detection limits for many elements (10-
10 to 10-13 g of analyte)

• Sample solution is not wasted


Disadvantages
 Much more time consuming
 More severe matrix effects
 Lower precision
 Analytical range is low compared to flame &
plasma atomization
• Analysis is usually limited to metals
Hydride Generation
• Versatile technique for the determination of number
of elements that forms volatile hydrides e.g. arsenic,
antimony, bismuth, germanium, lead, selenium,
tellurium and tin.

• The method involves a reduction of the element from


a higher oxidation state to its lower state (usually –II or
–III), which appears as volatile hydride.
• Common reluctant used is sodium tetrahydroborate.
HG-AAS
Optical Cell – fused silica
glass thermally stable at high
temp.

Acidity of sample plays a critical role.


Alkaline samples differentiate between Se(VI) and Se(IV)
because Se(VI) is not reducible by NaBH4
Cold Vapor - AAS
• Mostly used for mercury analysis
• Sample solution containing mercury is mixed
with a reducing agent (stannous chloride) to
form elemental Hg vapor.
• Inert gas carries Hg vapor to drying tube that
dehumidifies the gaseous mixture.
• Dry vapor enters the optical cell
• Hg HCL delivers a stable source of emission at
253.7 nm

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