Topic 2 Adsorption and Absorption

Analytical Techniques • Absorption: the incorporation of particles

into the body of another material
Atomic absorption spectroscopy

• Adsorption: the attachment of particles

onto the surface of a material (by forming
secondary interaction between the surface
and the particle)
CHROMATOGRAPHY Chromatography

Spectroscopy
• The use of absorption, emission or scattering
of electromagnetic radiation by atoms of
molecules (or atomic or molecular ion) to
quantitatively or qualitatively study the
atoms or molecules, or the physical processes.
• Absorption: a transition from a lower energy
level to a higher energy level with transfer of
energy from the radiation energy to the atom
or molecule.
• Emission: a transition from a higher energy
level to a lower energy level if energy
transferred to the radiation field.
 Emission of radiation
by atoms and ions
• The metallic elements present in a
compound can be determined simply
by inserting the compound into a non-
luminous Bunsen burner flame;
FLAME TEST
• The metal is identified by observing
the characteristics colour flame
produced by metals.
• The colours arise because
electromagnetic radiation, with
frequencies within the visible range,
is being emitted by the atoms or
ions.
Production of an
Emission & Absorption spectrum
Principle of Flame Test
1. In ground state, valence electrons occupy the
Na+ lowest available energy levels.
2. When the valence electron receives energy in the
form of heat or electricity, it absorbs only the
specific amount of energy required to raise the
valence electrons to one of the available higher
levels (excited state).
Cu2+ 3. But excited electrons are unstable, will immediately
return to lower energy levels, emitting the energy
they have absorbed earlier in the form of light.
4. If this energy emitted falls within the band
energies visible to the eye, it can be seen as
coloured light.
Atomic
Absorption Flame Test
Spectroscopy
8
Atomic Absorption Spectroscopy
Principle of AAS
(AAS) is:
• Common used of modern instrumental technique. 1.Hollow cathode lamp – to produce specific wavelength
• An Australia invention. 2.Atomizer and flame – ions vaporize to elemental state
• Very versatile and sensitive. 3.Monochromator and detector – detect absorption as
• Capable of detecting the type of metals presence absorbance
in an aqueous samples.
[qualitative analysis]
• Also with a calibration graph, the concentrations of
metal in aqueous solutions can be determine.
Typically concentration range in part per million
(ppm) or parts per billion (ppb) level.
[quantitative analysis]

The hollow cathode lamp: The specificity of AAS

• A source of radiation to produce a sharp, intense
and constant light beam with specific wavelength
of the specific metal under analysis.
• What happen in the lamp?
In the lamp, the atoms of the metal are energized
by means of high voltage, valence electrons in the
atoms will absorb specific energy, get excited to
higher energy levels, and upon returning to ground
state, emit radiation of specific frequencies.
• The lamp function:
Produced light / radiation with characteristic /
unique frequency or energy that can absorbed by the
metal ions under analysis only.
• Specific hollow cathode lamp is used.
• The radiation from the hallow cathode lamp has
energy exactly correspond to the electron energy
level gaps for the metal under investigation in an
unknown sample.
• Other metals in the sample cannot absorb the energy
(as other metal have different energy level gap),
therefore will not affect the absorbance reading of
the metal under analysis.
Question:
Manganese in a sample of alloy metal can be analysed
by AAS. Explain why the presence of other metal ions
The atomizer & flame:
does not interfere with the analysis of manganese.
(3m) • Sample must be in aqueous solution. [Metal sample
must be converted into metal aqueous solution by
– Mn lamp produced light / radiation with dissolving/digesting in concentrated acid eg. HNO3]
characteristic / unique / specific frequency or
energy that correspond to the energy level gap of • The solution is sprayed into the flame.
the metal under analysis.
• Atomization take place, where metal ions vaporize
– Only the valence electrons of Mn are able to into its elemental state.
absorb this unique energy / frequency to excite to
a higher energy level. • The light is aligned / directed to pass through the
– Other metal ions require different energy / flame, electrons in metal will be excited by
frequency, as each metal has a different energy absorbing the energy of the light emitted by hollow
level gap and thus not able to absorb this frequency cathode lamp.
/ energy.

Sample
Compartment
The monochromator & detector:

• With monochromator, the metal light that passes

through the flame is selected for analysis,
detected as absorbance (%).
• The amount of metal ion in the sample is
proportional to the amount of light absorbed.
• The higher the absorbance value the higher the Light Source Detector
concentration of the metal ions.
• A calibration curve can be obtained before
sample analysis by analyzing a series of
standard solution of the metal ions.
 Light Path

Distilled
water

Distilled water used for
dilution of sample
(blank sample)
A series of standard
solutions prepared through
dilution of stock solution
Water sample collected or
aqueous solution of a
sample (dilution require)
Sample is vaporized
in the flame (ions
reduced to elemental
state by sbsorbing free
electrons in the flame),
giving coloured flame
Aspirator
tube sucks the
sample into the
flame in the
sample
compartment.

Using AAS for
Qualitative analysis
To determine if a specific metal ion present in the
sample
• Choose a specific hollow cathode lamp (eg. Al lamp)
• Prepare diluted sample solution
• Inject sample solution and take absorbance
reading.
• If there’s a reading, that means the sample contain
that metal ions (eg. Al3+).
• Much better method compare to flame test.
Calibration Graph
Using AAS for
Quantitative analysis
To determine the concentration of metal ions in a
sample
• Choose a specific hollow cathode lamp eg. Al lamp
• Prepare a series of standard solutions (at least 5
different concentrations: eg. 1.0, 2.0, 3.0, 4.0, 5.0
ppm pf Al3+ from a stock solution of Al3+ by doing
dilution using volumetric flask and pipette).
• Take absorbance reading of blank solution
(distilled water used to do dilution: no Al3+, 0 ppm).
Should be zero.
• Take absorbance reading of all the standard
solutions.
• A calibration curve can be obtained by plotting a ppm concentration
graph of absorbance vs concentration of Al3+
solution. (solid and aqueous solution)
• Must be a straight line graph that passed through
zero. Parts per million (ppm)
• Then take the absorbance reading of sample solution. For aqueous solution with very low concentration
• By using the calibration graph plotted earlier, the solutes, eg. salts present in mineral waters or
concentration of Al3+ in the sample can be heavy metal present in rivers or lakes.
determined.
0.6
msolute (in milligram) msolute (in milligram)
0.5 Example: ppm
If the absorbance 1.00 kg of solution 1.00 L of solution
Absorbance

0.4
0.3 reading of sample is 0.35
0.2 Then the concentration
0.1 of Al3+ in the sample is Unit: ppm = mg L-1 (aq)
0 3.5 ppm
0 2 4 6
Concentration, ppm

ppm concentration
AAS question
(solid and aqueous solution)
Parts per million (ppm) AAS is used to analyse a sample of shellfish. From
the result, it was determine that the 100g of
The solid, define as the mass of solute shellfish contained 4.5 mg of zinc express this
(measured in milligrams) present in 1.00 kg of concentration in ppm.
the solid sample.
msolute (in milligram) msolute (in microgram) mzinc (in mg )
ppm C(Zn2+) in shellfish
1.00 kg of sample 1.00 g of sample mshellfish (in kg )
4.5 mg
Unit: ppm = mg/kg = µg/g (solid)
3
100 x 10 kg
45 mg / kg 45 ppm