2. LIST OF CONTENT:
• INTRODUCTION
• INSTRUMENTATION:
-Production of X-rays
-Collimator
-Monochromator
-Detector
• APPLICATIONS
• REFERENCES
3. • It is a novel & non destructive method of
chemical analysis and a variety of x –ray
techniques are available in practice.
• These are : X – ray Absorption
X-ray diffraction
X-ray Fluorescence
4. Definition
The atomic planes of a crystal cause an
incident beam of X-rays to interfere with one
another as they leave the crystal. The
phenomenon is called X-ray diffraction.
6. Bragg’s Law and Diffraction
• How waves reveal the atomic structure of crystals
• How waves reveal the atomic
structure of crystals
N ƛ = 2d sinθ
N = integer
• Diffraction occurs only
when Bragg’s Law is satisfied
Condition for constructive
interference (X-rays 1 & 2)
from planes with spacing d
7. Bragg’s equation is a negative law
If Bragg’s eq. is NOT satisfied no reflection can occur
If Bragg’s eq. is satisfied reflection may occur
Diffraction = Reinforced Coherent Scattering
8. XRD Pattern of NaCl Powder:
Diffraction angle 2θ (degrees
Miller indices: The peak is due to X-ray
diffraction from the {220} planes.
10. Collimator:
• Collimator system is used for achieving a
narrow beam of X-rays.
• X-rays are allowed to pass through collimator.
11. Monochromator:
• Two methods are available:
1)Filter
2)crystal monochromator
Filter: A filter is a window of material that
absorbs undesirable radiation but allows the
radiation of required wavelength to pass.
eg. zirconium filter which is used for
molybdenium radiation.
12. EG: USE OF FILTER TO PRODUCE
MONOCHROMATIC RADIATION
13. • Crystal monochromator :
It is made up of a
suitable crystalline material positioned in the X-
ray beam so that angle of reflecting planes
satisfied the bragg’s equation for required
wavelength.eg flat crystal monochromator.
17. A Modern Automated X-ray
Diffractometer
Detector
Cost: $560K to 1.6M
X-ray Tube
Sample stage
18. Application of X-ray diffraction:
1. Structure of Crystals
• The analytical applications of X-ray diffraction are numerous.
The method is nondestructive and gives information on the
molecular structure of the sample. Perhaps its most important
use has been to measure the size of crystal planes. The patterns
obtained are characteristic of the particulars compounds from
which the crystal was formed.
19. a) X-ray pattern of salt A
b) X-ray pattern of salt B
c) X-ray pattern of a mixture of salt A and B.
21. 2. Polymer Characterisation
• Powder method can be used to determine the degree of
crystalline of the polymer. The non-crystalline portion simply
scatters the X-ray beam to give a continuous background,
while the crystalline portion causes diffraction lines that are
not continuous.
22. 3.Stateof anneal in metals
• A property of metals than can be determined by X-ray
diffraction is the state of anneal.
• Well-annealed metals are in well-ordered crystal form and
give sharp diffraction lines.
• If the metal is subjected to drilling, hammering, or bending, it
becomes fatigued," that is, its crystals become broken and the
X-ray pattern more diffuse.
23. 4. Particle size Determination
• A variety of X-ray techniques may be used to determine the size of particles or
crystallites.
where,
v=the volume or size of an individual crystallite.
V = the total volume of the specimen irradiated
n= the number of spots in a diffraction ring at a
Bragg angle of θ
δθ=the divergence of the X-ray beam and is a
function of the apparatus used.
v = V . δθ . cos θ / 2n
24. Applications of Diffraction Methods to
Complexes.
• Determination of Cis-Trans Isometrism: X-ray diffraction
study has been used to make the distinction between cis and
trans isomers of a complex. An interesting example is the
structure of bis nickel (II) dihydrate.
Nickel chloride Alkaline solution of
ligand
Ni(pia)2.2H2O
25. • Determination of Linkage Isomerism: By X-ray
studies, it becomes possible to identify linkage
isomers of complexes. Sometimes knowledge
of the position of hydrogen atoms is useful.
26. Miscellaneous Application
• Soil classification based on crystallinity
• X-ray diffraction can also be used to assess the weathering and
degradation of natural and synthetic minerals By designed
experiments, the factors responsible for the degradation can be
revealed
• Corrosion products can be studied by this method. When metal
samples are exposed to the atmosphere, they are susceptible to
corrosion.
• Tooth enamel and dentine have been examined by x-ray
diffraction.
27. Application of X-ray Absorption
method
Analysis: Different elements absorb the X-rays to
different degrees. This property has been widely used to
detect broken bones, impurities, segregations, etc.
Widely used in industry and medicine.
28. Other Applications
• This has been used to locate trace elements, such as
barium and iodine in the body
• This has been used to detect below holes or the
segregation of impurities such as oxides in welds and
other joints.
• Also used to measure the volume of liquids in closed
vessels or pipes without opening or breaking the
vessels or pipes.
29. Applicationof x-ray fluorescence
In Agriculture –
• For the determination of trace elements in plants and
foods
• The detection of insecticides on fruit and leaves
• The continuous determination of phosphorus in fertilizer
In medicine
• For determination of chloride in blood serum;
• For the determination of strontium in blood serum and
bone tissue.
30. • In mining and metallurgy
• Other application:
o The determination of additives in motor oil by determining
barium, zinc, phosphorus, calcium, and chloride, and
o The determination of lead or sulfur in gasoline.
o The determination of the elements of the bearings in the used
motor oil, which can be performed by X-ray fluorescence,
o In the rubber industry, the determination of the vulcanizing
element, sulfur, can be done by X-ray fluorescence. This is a means
of ensuring the production of high-quality rubber.
o In space technology, the analysis of new alloys and ceramics can be
carried out by X-ray fluorescence.
31. References:
Text book of Instrumental analysis by skoog,
Holler, and crouch, 2007 Edition from pg.no
2.303 to 2.339.
Pictures and diagram are taken from Google
images.