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INTRODUCTION
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X-ray absorption (or)
radiography
Radiotherapy
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DISCOVERY
X-rays were discovered by W.C.Rontgen is a german
physicist in 1895.
For his work Rontgen awarded the first ever Nobel prize
for physics in 1901
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ORIGIN OF X-RAYS
X-rays are generated when high velocity electrons impinge
on a metal target .
The process of producing X-rays may be visualized in
terms of Bohr’s theory of atomic structure.
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Whenever a fast moving electron impinges on an atom, it
may knock out an electron completely from one of the
inner shells of that atom.
Following the loss of inner-shell electron one of the outer
electrons will fall in to the vacated orbital ,by the emission
of x-rays.
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The energy of the emitted X-ray photon is equal to the
difference in energy between two levels involved.
E = E2-E1
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The frequency of emitted radiation is given by
ϑ= Z² (2∏2me/h3)(1/N12 –1/N22 )
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TYPES OF RADIATION
1) BREHMSSTRAHLUNG (OR) BRAKING RADIATION:
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2) CHARACTERISTIC X-RADIATION:
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X-RAY DIFFRACTION
INTRODUCTION
THEORY
INSTRUMENTATION
METHODS OF X –RAY
DIFFRACTION
APPLICATIONS
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In 1912 von Laue placed a crystal of copper sulphate
between a white x-ray source and photographic plate
The resulting photograph observed here:
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THEORY
ABSORPTION
DIFFRACTION
FLOUROSENCE
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DIFFRACTION
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BRAGG’S LAW
Bragg’s equation is n=2dsinө
Constructive interference occurs only when
n=AB+BC
AB=BC
n=2AB
Sinө=AB/d
n=2dsinө
=2dhklsinөhkl
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IN PHASE OUT OF PHASE
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INSTRUMENTATION
GENERATION OF X-RAYS
DETECTORS COLLIMATOR
MONOCHROMATOR
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GENERATION OF X-RAYS
X-rays are generated when high velocity of electrons
impinge on a metal target.
Approximately 1% of total energy of electron beam is
converted in to x –radiation.
Two type of devices are used for generating x-rays
1) X-ray tube
2) Synchrotron radiation
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X-ray tubes:
Side window tube
End window tube
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Synchrotron radiation
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COLLIMATOR
The x-rays produced by the target material are randomly
directed.
In order to get a narrow beam of x-rays ,they are allowed to
pass through a collimator which consist of two sets of
closely packed metal plates separated by a small gap.
The collimator absorbs all the x-rays except the narrow that
passes between the gap.
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MONOCHROMATORS
Mainly two types:
a)FILTERS: It is a window of material that absorbs
undesirable radiation but allows the radiation of wave to
pass.
e.g. :Zirconium filter
which is used for molybdenum radiation.
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some more examples of beta filters:
b)Crystal monochromators
1)Flat crystal monochromator
2)Curved crystal monochromator
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CRYSTAL MONOCHROMATOR: The beam is split into
component wavelength by the crystal line material such
material is called as Analyzing crystal.
Crystals used in monochromators are sodium chloride,
lithium fluoride, quartz etc.
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DETECTORS
1) photographic method
2)counter methods
a) Geiger - Muller tube method
b) proportional counter
c) scintillation detector
d) solid-state semiconductor detector
e)semi conductor
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PHOTOGRAPHIC METHOD
PRINCIPLE :
By using plane or cylindrical film
Developing the film
D=log Io/I
D is the total energy
Measured by using densitometer
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SCINTILLATION DETECTOR
Its mainly contains a large crystal of
sodium iodide activated with small
amounts of thallium.
They convert incident x-rays in to
visible light which is detected by photo
multiplier tube.
e.g. for crystals :
sodium iodide , anthracene,
naphthalene ,p- terpenol in xylene.
Used for short wavelengths
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PROPORTIONAL COUNTER METHOD:
It is filled with heavier gas like xenon ( or) krypton
it is preferred because it is easily ionized.
More efficiency and sensitive
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GIEGER MULLER COUNTER
PRINCIPLE: Ionization of argon gas which is filled in the
Geiger tube by x-rays.
ADVANTAGES: In expensive
Trouble-free
DISADVANTAGES: only for counting low rates
Efficiency will be less
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SOLID- STATE SEMI CONDUCTOR
DETECTOR:
Electrons produced by x-ray beams are
converted in to conduction bands ,the current
which flows is directly propotional to incident x-
rays.
SEMI CONDUCTOR DETECTOR:
A pure silicon block set up with a thin film
lithium metal placed on to one end.
Semi conductor
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X-RAY DIFFRACTION METHODS
1) SINGLE CRYSTAL DIFFRACTOMETER:
A) LAUE METHOD
a)TRANSMISSON METHOD
b)BACK REFLECTION METHOD
B) BRAGG’S SPECTROPHOTOMETER METHOD
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LAUE METHOD
TRANSMISSION METHOD
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BACK REFLECTION METHOD
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BRAGG’S SPECTROPHOTOMETER
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ROTATING CRYSTAL METHOD
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POWDER CRYSTAL METHOD
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APPLICATIONS
1)STRUCTURE OF CRYSTAL:
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2)POLYMER CHARACTERISATION:
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3)PARTICLE SIZE DETERMINATION:
a)Spot counting method:
b)Broadening of diffraction lines
c)Low-angle scattering
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5)STATE OF ANNEAL IN METALS :
Well annealed metals are in well ordered crystal form and give
sharp diffraction lines.
If the metal breaking is present then the x-ray pattern more
diffuse.
6)MISCELLANEOUS APPLICATIONS:
Soil classification based on crystallinity
Analysis of industrial dusts
Weathering and degradation of naturals and synthetic minerals
Corrosion products can be studied by this method
Tooth enamel and dentine have been examined by X-ray
diffraction.
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PANALITICAL XPERT INSTRUMENT
Features:
X-ray source: Philips high intensity ceramic sealed tube (3kW)
Wavelength: Cu Ka (1.5405 Å)
Incident beam optics: 2 interchangeable fixed slits and one Soller slit.
Diffracted beam optics: fixed slit plus programmable receiving slit,
graphite analyzer
Detectors: sealed proportional counter and X'celerator PSD for high
speed data collection
Sample stage: powder stage, texture cradle with sample translation
Software: Philips X’PERT suite: Data Collector, Graphics & Identify,
Texture
XPERT Powder (I) - for high-speed phase identification
XPERT Thin Film (II) - for thin film, grazing-incidence XRD, texture
measurement
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REFERENCES
Remington 21st edition pg.no.481
Instrumental methods of chemical analysis by
Gurdeep. R. Chatwal ,12th chapter,pg.no.2.303-2.339
Analytical chemistry by Clive Whiston
(x-ray methods)
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THANK YOU
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