Approved by AICTE, PCI & Affiliated to ANU

Recognized by Department of Technical Education, Govt of A.P.

Certified By ISO 9001:2008

www.chalapathipharmacy.in
INTRODUCTION

X –RAYS: The X-ray region of electromagnetic spectrum

consists of shortest wavelength in the region of about 0.1 to
100AO
 For analytical purposes ,the range of 0.7 to 2.0AOis mostly
used.

3
X-ray absorption (or)
radiography

X-ray diffraction (or)

crystallography
CLASSIFICATION
OF X-RAY
X-ray fluorescence
METHODS
method

Radiotherapy

4
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

5
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.

6
 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.

7
 The energy of the emitted X-ray photon is equal to the
difference in energy between two levels involved.

E = E2-E1

 E2 and E1 are the final and initial energies which are

emitted from L and K shells respectively
 If the vacancy produced in the K-shell is filled by the
electron from L-shell, the radiation is called Kὰ .
 Electron from M-shell it is called Kβ.

8
 The frequency of emitted radiation is given by

ϑ= Z² (2∏2me/h3)(1/N12 –1/N22 )

Z = Atomic number of an atom

m = mass of the electron
e = charge of the electron
h = plank's constant
N1 , N2 =1 & 2 for K&L shell

9
TYPES OF RADIATION
1) BREHMSSTRAHLUNG (OR) BRAKING RADIATION:

10
2) CHARACTERISTIC X-RADIATION:

11
X-RAY DIFFRACTION
INTRODUCTION

THEORY

INSTRUMENTATION

METHODS OF X –RAY
DIFFRACTION

APPLICATIONS

12
 In 1912 von Laue placed a crystal of copper sulphate
between a white x-ray source and photographic plate
 The resulting photograph observed here:

13
THEORY

ABSORPTION

DIFFRACTION

FLOUROSENCE

14
DIFFRACTION

15
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

16
IN PHASE OUT OF PHASE

17
INSTRUMENTATION
GENERATION OF X-RAYS

DETECTORS COLLIMATOR

MONOCHROMATOR

18
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

19
 X-ray tubes:
Side window tube
End window tube

20
 Synchrotron radiation

 Synchrotron radiation is emitted by electron and positrons

travelling at near light speed in circular storage ring.
 Powerful sources which are thousands to millions of times
more intense than x-ray tubes.

21
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.

22
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.

23
some more examples of beta filters:

TARGET ß-FILTERS THICKNESS %LOSS IN K∞

ELEMENT INTENSITY
Co Fe 0.012 39
Cu Ni 0.015 45
Fe Mn 0.011 38
Mo Zr 0.081 57
Ni Co 0.013 42

b)Crystal monochromators
1)Flat crystal monochromator
2)Curved crystal monochromator

24
 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.

25
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

26
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

 USES: For diffraction studies

For quantitative measurement
 DIS ADVENTAGES: Time consuming

27
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

28
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

29
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

30
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

31
X-RAY DIFFRACTION METHODS
1) SINGLE CRYSTAL DIFFRACTOMETER:

A) LAUE METHOD
a)TRANSMISSON METHOD
b)BACK REFLECTION METHOD
B) BRAGG’S SPECTROPHOTOMETER METHOD

2)POWDER CRYSTAL DIFFRACTOMETER

32
LAUE METHOD
TRANSMISSION METHOD

33
BACK REFLECTION METHOD

34
BRAGG’S SPECTROPHOTOMETER

35
ROTATING CRYSTAL METHOD

36
POWDER CRYSTAL METHOD

37
38
APPLICATIONS
1)STRUCTURE OF CRYSTAL:

39
2)POLYMER CHARACTERISATION:

40
3)PARTICLE SIZE DETERMINATION:
a)Spot counting method:
b)Broadening of diffraction lines
c)Low-angle scattering

4)APPLICATIONS OF DIFFRACTION METHODS TO

COMPLEXES:
a)Determination of cis-trans isomer
b)Determination of linkage isomer

41
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.

42
43
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
44
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)

45
THANK YOU

46