In this slide contains principle working of XRD and there applications. Presented by: J Lokdeep Reddy. (Department of pharmaceutics), RIPER, anantapur.

1. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721
A seminar as part of curricular requirement for first year
M.Pharm first semester
Presented by
J.Lokdeep Reddy
[Reg.No.20L81S0305]
Under the guidance of
Dr.CH.pavan kumar.,M.Pharm.Ph.D
Associate professor and Head
Department of Pharmaceutics

2. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 2
• Introduction to XRD
Principle of XRD
Working of XRD
• Introduction of preformulations
• Use of XRD in preformulation studies
• References
Contents

3. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 3
• X-ray diffraction is a method of X-ray crystallography,in which a
beam of X-rays strikes a sample[crystalline solid],land on a piece of
film or other detector to produce scattered beams.
• It is a powerful non-destructive technique for characterizing
crystalline materials that provide detail information about the
crystallographic structure ,chemical composition and physical
properties of materials .
Introduction to XRD

4. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 4
• X-rays used for diffraction are electromagnetic waves with short
wavelength in the range 0.05-0.25nm.
• To produce X-rays for diffraction purpose,a voltage of about 35-50kV
is necessary and applied between a cathode and an anode target
metal,both are continued in a vaccum.
• When the tungsten filament of the cathode is heated,electrons are
released by thermionic emission and accelerated through the
vaccum by the large voltage difference between anode and cathode.

5. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721
• Principle:An X-ray irradiation produce a highly specific diffraction
pattern from a crystal of material.
• An X-ray diffraction pattern from the crystal is formed a series of
dots of varying intensity with fixed angular and recorded on
photographic film.
• It is powerful tool for particle size analysis.
X-RAY DIFFRACTION IN PREFORMULATION

6. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721
• When beam of nonhomogenous X-ray is allow to pass through the
crystal,X-ray beam is diffracted and it is recorded by means of
photographic plate.
• Diffraction is due to crystal which acts as 3 dimensional diffraction
grating towards X-ray.
• Random orientation of crystal lattice in the powder causes the X-ray
to scatter in a responsible pattern of peak intensities.
• The diffraction pattern is characteristic of a specific crystalline lattice
for a given compound.
Working of XRD:

7. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 7

8. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 8
• Preformulation is the stage of development during which the
physiochemical properties of the drug substance are characterized
and established.
• Preformulation can be considered as a critical decision making tool
during development and drug discovery.
Objectives:To determine its kinetics and stability.
• To establish its compatibility with common excipients.
• It provides insights into how drug products should be processed and
sroredto ensure their quality.
Introduction to preformulation studies

9. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 9
A:physical characteristics
1.organoleptic properties:
colour,odour,taste of the new drug be determined.
2.Bulk characteristics:
a.Solid state characteristics b. Flow properties
c.Densities d.Compressibility
e.Crystallinity f.Polymorphism
g.Hygroscopicity
3. Solubility Analysis:
a.Ionization constant b.Partiton coefficient
c.Solubulization d.Thermal effect
e.Common ion effect f.Dissolution
Preformulation parameters

10. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 10
4.Stability Analysis a.Solution state stability.
b.Solid state stability.
c.Drug –Excipient compatability
B.Chemical characteristics
1.Hydrolysis
2.Oxidation
3.Photolysis
4.Racemization
5.Polymerization
6.Isomerization

11. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 11
• To determine the structure of crystals.
• To determine the polymer characterization.
• To state of anneal in metals.
• Used in particle size determination.
• Determination of cis trans isomerisim.
• Determination of linkage isomerisim.
Uses of XRD in preformulation studies

12. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 12
Structure of crystals

13. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 13

14. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 14
XRD Pattern of Nacl powder

15. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 15
• It is a rapid and powerful technique for identifying unknown
minerals and materials .
• It only requires preparation of a minimal sample for analysis.
• The data obtained by this is relatively straight forward.
Limitations of XRD:
• It has size limitations.
• It ia much more accurate for measuring large crystalline structures
rather than small ones.
• Small structures that are present only in trace amounts will often go
and detected by XRD method.
Advantages of XRD:

16. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 16
• D.K sharma , 17th edition 1997-19998, Instrumental methods of
chemical analysis, GOEL publishing house.page no:329-359.
• A.skoog, f.James holles, Timothy A.Niemen.page no:277-298,
Principles of instrumental analysis.
• Gurudeep R.chatwal,sham k.annad,Himalays publications page
no:2.303-2.332, Instrumental methods of chemical analysis.
• H.Kaur pg no:727-729,737, Instrumental methods of chemical
analysis.
References:

17. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 17