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Lecture 7 (Atomic Absorption Spectroscopy (AAS) ) - Clinical

Atomic absorption spectroscopy involves exciting sample atoms with radiation from a hollow cathode lamp containing the element of interest. Absorption of radiation is measured and follows Beer's law, allowing quantification. Advantages include analysis of almost all elements and high sensitivity. The instrument includes a radiation source, chopper, atomizer such as a flame or graphite furnace, monochromator, and detector. Calibration curves are made from standards to determine unknown concentrations in samples.

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0% found this document useful (0 votes)
41 views12 pages

Lecture 7 (Atomic Absorption Spectroscopy (AAS) ) - Clinical

Atomic absorption spectroscopy involves exciting sample atoms with radiation from a hollow cathode lamp containing the element of interest. Absorption of radiation is measured and follows Beer's law, allowing quantification. Advantages include analysis of almost all elements and high sensitivity. The instrument includes a radiation source, chopper, atomizer such as a flame or graphite furnace, monochromator, and detector. Calibration curves are made from standards to determine unknown concentrations in samples.

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ayaessam392002
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Instrumental Analysis

Clinical pharmacy and therapeutics 1

Instrumental Analysis
CPA2103

Pharmaceutical Chemistry Department

Credit hour: 2
Lecture
12 lectures
Atomic Absorption spectroscopy (AAS)
-In AAS, the temperature of the flame is low enough that the flame it self does not
excite the sample atoms from the ground state but the excitation is done by the use of
external source of radiation which produces one beam of monochromatic light
(resonance wavelength) specific for each element.
-Atomic absorption spectroscopy depends on measuring the amount of light

absorbed at the resonance wavelength as it passes through a cloud of atoms.


-As number of atoms increases, the light absorbed increases in a predictable
way which follows Beer's Lamber's law.
A= Log I0 / I = 0.434 kcb
Where: k = is a coefficient depends on the nature of atoms and the radiations.
c = is the concentration of atoms (sample concentration).
b = is the light path length which depends on the dimensions of the flame
which are standard and constant for each instrument.
❑ Advantages of atomic absorption spectroscopy
It can be used for almost all the elements.
Because about 99.8% of the atoms absorb the radiation, but only about 0.01%
or less of them emit radiation and thus emission will not affect the sensitivity of
the method.
❑ Comparison between atomic and molecular absorption spectra
•Absorption spectra (atomic or molecular) are resulted from absorption of
electromagnetic radiations by the analyte (atoms or molecules) which promotes
the outer most electrons to higher electronic energy levels.
Atomic Absorption spectra Molecular Absorption spectra
(1)The outermost electrons occupy one of the The outermost electrons occupy σ, π, n
atomic orbitals & have its E levels [e.g. electronic E levels in the ground state.
K, L, M, N, S, S.P, S.P.d, s.p.d.f ].

(2)Upon excitation electrons are promoted to Upon excitation electrons are raised to π* or
any permissible higher atomic E level. σ* E levels.

(3) Since there are no bonds, there are no Since there are bonds, there are vibrational &
vibrational or rotational E levels either in rotational E levels in both the ground &
the ground or excited states. excited states.

(4) The spectra are line form The spectra are bands due to the presence of
very close superimposed vibrational &
rotational E levels in the excited state.
(5) The analytical λ is the resonance
wavelength of the analyte (which causes The analytical wavelength is λmax.
the most intense excitation)
* Instrument for Atomic Absorption *
- It consists of:
1- Source of radiation. 2- Chopper.
3- Atomizer. 4- Monochromator.
5- Detector. 6- Read out meter.
A-Source of radiations
• Hollow cathode lamp is used as a source of radiations in AAS which produces
emission lines specific for the element used in construction of its cathode.
•Hydrogen or deuterium lamp can not be used as they produce a much broader
band than that required to be absorbed by the atoms in the flame.
•Each element has its own unique lamp which must be used for its analysis.

❑ Composition of hollow cathode lamp:


-It consists of a tube with a front quartz window that contains a tungsten
anode and a hollow cylindrical cathode made of the element to be determined.
-The glass tube is filled with inert gas (neon or argon) at pressure of 1-5 torr.
❖ How does it work?
1-Applying a low potential between the anode and the cathode leads to
ionization of the inert gas between them.
2-On applying a higher potential, these gaseous ions bombard (hit) the cathode
and eject the metal atoms from it in a process called "sputtering". Collisions
between the sputtered atoms impart energy necessary for their excitation,
when they fall back to the ground state they emit radiation characteristic of the
metal.
3-The shape of the cathode which is hollow cylindrical concentrates the emitted
radiation into a beam which passes through the quartz window to the vaporized
sample.
Drawbacks of the lamp: usually appears when the lamp is operated at
high potential:
1-Increasing the number of free atoms causes self absorbing of the emitted
radiations which leads to decreasing the intensity of the radiations.
2-Doppler broadening: which arises due to high concentration of free atoms
which move with different speeds and thus emit radiations of different
wavelengths () (i.e. broad band light).

B- Chopper
1-It is located in the front of the lamp to fluctuate (modulate) the source
output.
2-It is a circular disc divided into four quarters, two are mirrored and two are
opened.
❖ How does it work?
1-The disc rotates at constant speed, when the mirrored quarters are in front of the
lamp it reflects the radiations.
2-The second time, the opened quarters are in front of the lamp and the radiations
passes to the sample being absorbed and so reaches the detector in the form of pulses
and converted to alternative current (AC).
3- While the radiation from the flame or from atoms excited by the flame will reach the
detector continuously and converted to direct current (DC).
➢ So by using the chopper (modulator of the source output), the detector can
differentiate the fluctuated radiations of the light source from continuous
radiations from the atomizer and that is called “fluctuation of the source
output”.
C- Atomizer
There are two types of atomizer:
1 -Flame atomizer
It is the same as in flame emission spectroscopic technique but the
temperature of the flame is low enough that the flame it self does not excite
the sample atoms from the ground state.
2-Flameless (non flame) atomizer
It is a graphite furnace heated electrically to 6000 °C. Upon heating the
furnace, the sample is ashen (burnt) then atomized by action of the heat.
Advantages of flameless atomizer:
1-Require small sample volume and has high sensitivity.
2-It can be used for liquid and solid samples directly.
3-Heat distribution is uniform and temperature is steady.
4-No need for fuel – oxidant mixtures.
5-No flame noise.

d- Monochromator
Grating which is used to eliminate other resonance lines from the light source
or other radiations from the flame or the sample.
e- Detector: It is photomultiplier tube.
f- Readout meter: Absorbance or transmittance output.
* Applications of Atomic Absorption *

Calibration curve method:


1- Choose a suitable lamp.
2- Prepare a series of standard solutions of reference material/salt of the metal
to be determined.
3- Adjust zero absorbance (while spraying a solvent blank).
4- Measure the absorbance while spraying each of the standard
solutions.
5- Plot conc. Vs. absorbance .
6- Spray the sample & measure its absorbance then get its conc. from the
graph.

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