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FFT 6107: FOOD ANALYSIS AND INSTRUMENTATION

(ATOMIC ABSORBANCE SPECTROSCOPY)

Prof. Eddy Owaga

[email protected]
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Lecture overview : AAS

• Introduction
• Principle of analysis
• Instrumentation
• Applications

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Elements that are highlighted in pink are detectable by AAS

What is AAS?

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Atomic Spectroscopy

• determination of mineral type and concentration by atomic

spectroscopy is more sensitive, specific, and quicker than
traditional wet chemistry methods.

• For this reason it has largely replaced traditional methods in

laboratories that can afford it or that routinely analyze for minerals.

Lecture overview : AAS

• Introduction
• Principle of analysis
• Instrumentation
• Applications

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Atomic Absorption Spectroscopy (AAS)

• AAS is an analytical method that is based on the absorption of UV-visible

radiation by free atoms in the gaseous state.

• food sample to be analyzed is normally ashed and then dissolved in an aqueous

solution. The solution is placed in the instrument where it is heated to vaporize
and atomize the minerals.

• A beam of radiation is passed through the atomized sample, and the absorption
of radiation is measured at specific wavelengths corresponding to the mineral of
interest.

• Information about the type and concentration of minerals present is obtained by

measuring the location and intensity of the peaks in the absorption spectra.

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Atomic Absorption Spectroscopy

• The analyte concentration is determined from the
amount of absorption.

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Atomic Absorption Spectroscopy

• The analyte concentration is determined from the

amount of absorption.

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Principle of AAS
• AAS is commonly used for metal/elements analysis

• A solution of a metal compound is sprayed into a flame and vaporises

• The metal atoms absorb light of a specific frequency, and the amount of light
absorbed is a direct measure of the number of atoms of the metal in the
solution
• The analyte concentration is determined from the amount of absorption
(Beer’s law)

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This absorption intensity will be proportional to the

concentration of the atom in the ground state. Mathematically
the total amount of light absorbed may be given by the following
equation.

At the lambda wavelength the total amount of

light absorbed = (πe2 / mc).Nf

Where, e= charge of electron

M= mass of electron
C= speed of light
N=total number of atom that can absorb at specific
wavelength.

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PRINCIPLE OF AAS
Liquid sample

flame

Formation of
droplets

Fine residue

Formation of Neutral atoms

Neutral atoms absorb specific wavelength of

radiation from hollow cathode lamp

Measurement of intensity of radiation absorbed by the

neutral atoms using a detector

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PROCESS OF ATOMIC ABSORPTION

Lecture overview : AAS

• Introduction
• Principle of analysis
• Instrumentation
• Applications

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AAS instrumentation

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AAS- Hollow cathode lamp (HCL) is the light source

HCL

Motorized
Mirror

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Hollow cathode lamp (HCL)

Cathode -- in the form of a cylinder, made of the element being studied in

the flame
Anode -- tungsten
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Hollow Cathode Lamp

Quartz window

Pyrex body

Anode

Cathode

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1. A large voltage across the anode and cathode will cause the
inert gas to ionize.

2. The inert gas ions will then be accelerated into the cathode,
sputtering off atoms from the cathode.

3. Both the inert gas and the sputtered cathode atoms will in
turn be excited by collisions with each other.

4. When these excited atoms decay to lower energy levels they

emit a few spectral lines characteristic of the element of
interest.

5. The light is emitted directionally through the lamp's window,

a window made of a glass transparent in the UV and visible
wavelengths.

6. The light can then be detected and a spectrum can be

determined.

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A hollow cathode lamp for Aluminum (Al)

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• The shape of the cathode which is hollow cylindrical

concentrates the emitted radiation into a beam which passes
through a quartz window all the way to the vaporized sample.

• atoms of different elements absorb characteristic

wavelengths of light.
• Aim: Analyzing a sample to see if it contains a particular
element means using light from that element /quantity

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Atomization process

Nebulizer converts the

solution into a spray

Flame (or Plasma) causes the solvent to evaporate,

leaving dry aerosol particles, then volatilizes the particles,
producing atomic, molecular and ionic species

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Nebulizer - burner

To convert the test solution to gaseous atoms

1. Nebulizer --- to produce a mist or aerosol of the

test solution

2. 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

3. Burner head --- The flame path is about 10 –12 cm

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Nebulizer – burner process

4. The mixture flows

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). 3. The result is a heterogeneous 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).

6. Liquid sample not flowing

into the flame collects in the
waste.
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Common fuels and oxidants used in flame

spectroscopy

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Temperature Profile

Temperature profile in degrees Celsius for a natural gas-air flame

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During combustion, atoms of the element of

Interest in the sample are reduced to
free,
unexcited ground state atoms, which absorb
light at characteristic wavelengths.

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Stage 1: Drying at about 100°C to remove water

Stage 2: Ashing (300-500°C) to remove organic constituents

Stage 3: Atomisation (2000-2900°C) to liberate the elements as

gaseous atoms

Stage 4: Removal of remaining inorganic matter at the

maximum operating temperature about (3000°C)

drying ashing atomization

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Monochromator

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Photomultiplier Tube

Light Photocathode
e-
Dynode
Dynode
Dynode

Current

Convert light energy to electrical energy

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Lecture overview : AAS

• Introduction
• Principle of analysis
• Instrumentation
• Applications

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Application of AAS

AAS

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AAS Advantages and Disadvantages'

Advantages
1. High selectivity and sensitivity
2. Fast and simple working
3. Doesn’t need metals separation

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Advantages

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

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Advantages of AAS

 Highly specific in nature – atom of a particular element can

only absorb radiation of their own characteristic wavelength
other elements cannot be interfered in the study. Ex: light of a
particular wavelength can easily be absorbed by specific
element to which it is characteristic.
 Variation in flame temperature shows relatively less effect in
AAS than FES.
 High sensitive.

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Advantages of AAS
• Solutions, slurries and solid samples can be analysed.
• Much more efficient atomization
• Greater sensitivity
• Smaller quantities of sample (typically 5 – 50 μL)
• Provides a reducing environment for easily oxidized
Elements

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Limitations of AAS
 Need of separate lamp for each element to be determined is
main limitation of AAS.
 This technique cannot be used very successfully for the
elements which produce oxides in the flame. Ex: Al, Ti, W,
Mo, Si.
 In aqueous solution, the predominant anion effect interfere
the signal to a significant level.
 AAS is applicable to analysis of metals only.
 presence of incompletely absorbed background emission
from the source and scattered light from the optical system.
As background becomes more intense relative to the
absorption of the analyte, the precision of the measurement
decreases dramatically

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• Expensive
• Low precision
• Low sample throughput
• Requires high level of operator skill
• Sample must be in solution or at least volatile
• Individual source lamps required for each element
• Analysis not done simultaneously
• Fragment have to form ready measure solution
• Limit types of cathode lamp (expensive)

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Take away overview : AAS

• Introduction
• Principle of analysis
• Instrumentation
• Applications

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