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Energy Dispersive Spectroscopy,

X-ray Fluorescence,
Optical Emission Spectroscopy
Tech. of Microstructural Analysis
Wahyuaji NP
Energy Dispersive X-Ray
Energy-dispersive X-ray spectroscopy (EDS, EDX, or XEDS),
sometimes called energy dispersive X-ray analysis (EDXA)
or energy dispersive X-ray microanalysis (EDXMA), is an
analytical technique used for the elemental
analysis or chemical characterization of a sample.
It relies on an interaction of some source of X-ray excitation
and a sample. Its characterization capabilities are due in
large part to the fundamental principle that each element
has a unique atomic structure allowing unique set of peaks
on its X-ray emission spectrum.
Energy Dispersive X-Ray
To stimulate the emission of characteristic X-rays from a
specimen, a high-energy beam of charged particles such
as electrons or protons, or a beam of X-rays, is focused into
the sample being studied.
At rest, an atom within the sample contains ground state (or
unexcited) electrons in discrete energy levels or electron
shells bound to the nucleus. The incident beam may excite
an electron in an inner shell, ejecting it from the shell while
creating an electron hole where the electron was.
Energy Dispersive X-Ray
An electron from an outer, higher-energy shell then fills the
hole, and the difference in energy between the higher-
energy shell and the lower energy shell may be released in
the form of an X-ray.
The number and energy of the X-rays emitted from a
specimen can be measured by an energy-dispersive
spectrometer.
As the energies of the X-rays are characteristic of the
difference in energy between the two shells and of the
atomic structure of the emitting element, EDS allows the
elemental composition of the specimen to be measured.
Energy Dispersive X-Ray
Energy Dispersive X-Ray
Energy Dispersive X-Ray
BSE Si K

100m
An oxide grain surrounded
by feldspath and mica

Fe Ti Ca

Lamellar structure of the Fe-Ti phase


X-Ray Fluoroscence
X-ray fluorescence (XRF) is the emission of characteristic
"secondary" (or fluorescent) X-rays from a material that has
been excited by bombarding with high-energy X-rays
or gamma rays. The phenomenon is widely used for
elemental analysis and chemical analysis, particularly in the
investigation of metals, glass, ceramics and building
materials, and for research in geochemistry, forensic
science, archaeology and art objects such as paintings
and murals.
X-Ray Fluoroscence
When materials are exposed to short-wavelength X-rays or
to gamma rays, ionization of their component atoms may
take place.
Ionization consists of the ejection of one or more electrons
from the atom, and may occur if the atom is exposed to
radiation with an energy greater than its ionization
potential.
X-rays and gamma rays can be energetic enough to expel
tightly held electrons from the inner orbitals of the atom.
The removal of an electron in this way makes the electronic
structure of the atom unstable, and electrons in higher
orbitals "fall" into the lower orbital to fill the hole left
behind.
X-Ray Fluoroscence
In falling, energy is released in the form of a photon, the
energy of which is equal to the energy difference of the two
orbitals involved. Thus, the material emits radiation, which
has energy characteristic of the atoms present.
The term fluorescence is applied to phenomena in which the
absorption of radiation of a specific energy results in the re-
emission of radiation of a different energy (generally lower).
Optical Emission Spectroscopy
Optical emission spectrometry involves applying electrical
energy in the form of spark generated between an electrode
and a metal sample, whereby the vaporized atoms are
brought to a high energy state within a so-called discharge
plasma.
Optical Emission Spectroscopy
These excited atoms and ions in the discharge plasma create
a unique emission spectrum specific to each element, as
shown below. Thus, a single element generates numerous
characteristic emission spectral lines.
Optical Emission Spectroscopy
Therefore, the light generated by the discharge can be said
to be a collection of the spectral lines generated by the
elements in the sample.
This light is split by a diffraction grating to extract the
emission spectrum for the target elements.
The intensity of each emission spectrum depends on the
concentration of the element in the sample.
Detectors (photomultiplier tubes) measure the presence or
absence of the spectrum extracted for each element and
the intensity of the spectrum to perform qualitative and
quantitative analysis of the elements.
Optical Emission Spectroscopy
Optical Emission Spectroscopy
In the broader sense, optical emission spectrometry
includes ICP optical emission spectrometry, which uses an
inductively coupled plasma (ICP) as the excitation source.
The terms "optical emission spectrometry" and
"photoelectric optical emission spectrometry," however,
generally refer to optical emission spectrometry using spark
discharge, direct-current arc discharge, or glow discharge for
generating the excitation discharge

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