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Chapter Five-Atomic Spectros

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5 views23 pages

Chapter Five-Atomic Spectros

Uploaded by

Zekarias Geneto
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Chapter five: Atomic spectroscopy

OUTLINE

AT the end of this session, you will be able to


describe:
• Basic principle of Atomic spectroscopy

• Types of atomic spectrophotometric techniques

• Instrumentation

• Applications
Introduction
 Atomic spectroscopy is used for the qualitative and
quantitative determination of elements.
 Atomic spectroscopy deals with the absorption, emission, or
fluorescence by atom or elementary ions.
 Two regions of the spectrum yield atomic information
- The UV-visible and the X-ray.
- Atomic spectra are mostly in UV (sometime in visible) regions
 Atomic spectroscopic methods normally are classified
according to the type of spectral process involved and the
method of atomization used.
 As atoms have no rotational or vibrational energy, transitions
occur only between electronic levels and bandwidths in atomic
spectra are very narrow ( line spectrum ) .
Principle
 The elements present in the sample are converted to gaseous
free atoms by a process called atomization using either flame
or electrical means . Then , these free atoms can be treated in
several ways :
1. It can be excited by the flame itself and their ultraviolet/visible
emission can be measured . The flame is both ,the atomization
and the excitation mean . This technique is called Flame Atomic
Emission Spectrophotometry (FAES ) .
Cont.…
2. It can be atomized and excited by an electrical mean and their
ultraviolet/visible emission can be measured. These techniques are
termed Induced coupled plasma ( ICP ) and Arc Spark emission.
3. The free atoms in the flame can be irradiated using
ultraviolet/visible source and their ultraviolet/visible emission
( fluorescence ) can be measured (atomization by flame or
electrical mean while excitation by radiation) . This technique is
named Atomic Fluorescence Spectroscopy ( AFS ) .
Cont.….
4. The analyte is atomized by either the flame or electrical mean
and the absorption of ultraviolet/visible radiation from a radiation
source is measured (atomization by flame or electrical mean ,
then irradiation using radiation source)
• This method is called Atomic Absorption
Spectrophotometry ( AAS)
Instrumentation of AAS
 An atomic absorption spectrophotometer consists of the
following components:
1. Light source.: A hollow cathode lamp coated with the
element being analysed.
2. Flame: is usually air/acetylene, providing a temperature ca
2500°C. Nitrous oxide/acetylene may be used to produce
temperatures up to 3000°C, which are required to volatilise salts
of elements such as aluminium or calcium.
Cont.…
3. Monochromator: is used to narrow down the width of the
band of radiation being examined and is thus set to monitor the
wavelength being emitted by the hollow cathode lamp.
This cuts out interference by radiation emitted from the flame,
from the filler gas in the hollow cathode lamp and from other
elements in the sample.
4. Detector. The detector is a photosensitive cell.
Cont.….

• Schematic diagram of an atomic absorption


spectrophotometer
Application
 AAS is used in a number of limit tests for metallic
impurities,
• e.g. magnesium and strontium in calcium acetate,
• palladium in carbenicillin sodium and lead in bismuth
subgallate.
Cont.…
 It is also used to assay metals in a number of other preparations:

• zinc in zinc insulin suspension and tetracosactrin zinc injection;


• copper and iron in ascorbic acid;
• zinc in acetylcysteine; lead in bismuth subcarbonate;
• silver in cisplatinum;
• lead in oxprenolol; aluminium in albumin solution and calcium,
magnesium, mercury and zinc in water used for diluting haemodialysis
solutions.
Atomic emission spectrophotometry
(AES)
 In AES, Atoms are thermally excited so that they
emit light and the radiation emitted is measured.
 Instrumentation
An atomic emission spectrophotometer is composed of the
following components:
1. Flame. The sample containing the metal is volatilised in a
natural gas/compressed air flame at 2000°C.
Cont.…
(ii) Monochromator/Filter. The radiation emitted by the excited
atoms is passed through a filter, or a monochromator in more
expensive instruments. Thus a narrow band of emitted radiation
is selected and interfering sources of radiation such as the flame
and other components in the sample are screened out.
(iii) Detector. The intensity of the selected radiation is then
measured using a photosensitive cell.
Cont..

• Schematic diagram of an atomic emission spectrophotometer


Application of AES
• Quantification of alkali metals in alkali metal salts, infusion
and dialysis solutions.
• Determination of metallic impurities in some of the other
inorganic salts used in preparing these solutions.
Other elemental analysis techniques

 Induced coupled plasma ( ICP ) and Arc Spark emission

• If high enough temperatures can be reached, any element can


be excited to a level where it will produce emission of
radiation. Such high temperatures can be achieved by using
plasma emission.
• A schematic diagram of an inductively coupled plasma (ICP)
‘torch’ is shown in Figure .
Cont.…..

• Schematic diagram of an ICP torch


Cont.…
• In ICP, High temperatures are achieved by heating argon with
high-intensity radiofrequency radiation. At such high
temperatures all elements will emit radiation as they are
excited and then return to the ground state.
• In order to derive spectral information from the process, an
efficient monochromator and computer processing of the data
are required in order to unscramble the large number of lines
that are derived from a particular sample.
Application
• ICP has been used to determine a complex of the metal ion
dysprosium, which is used as a magnetic resonance imaging

contrast agent, in serum.

• Recently an ICP method was developed for the analysis of the


calcium salt of an investigational drug.
Atomic fluorescence spectrometry

• Atomic fluorescence spectrometry (AFS) differs from atomic


emission spectrometry only in that the atoms are excited by
photons, rather than thermally.
• General AFS instruments use a changeable light source
specific for the element being analyzed.
• The fluorescence signal is directly proportional to the exciting
light intensity; Boosted discharge hollow cathode lamps are
generally considered as are the preferred sources for AFS.
Cont.…

• The emitted fluorescence radiation is collected at


90◦ to the excitation beam and focused on to the
detector.
• Low-resolution high-throughput monochromators /

changeable interference filters are commonly used.

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