Solid state characterization by XRD & its applications

Presented by:
Mr. Abhyangshree Mane
M.Pharm (Sem.-I)
Pharmaceutics
Roll no. : 514
Guided by:
Dr. A. M. Avachat
M.Pharm, PhD
(Pharmaceutics)

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 X-ray diffraction.
 History
 Basic principle
 Bragg’s law
 Instrumentation
 Applications
 Case study
 References
AbhyangshreeManeM.Pharm(P'Ceutics)

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Reference- Das R., Ali E., Hamid S.,2014, “Current applications of X-ray powder diffraction: A review”, Rev.
Adv. Mater. Sci., 38, 95-109.

 Short wavelength electromagnetic radiations produced by,
a. Deceleration of high energy electrons.
b. Electronic transitions of electrons in inner orbital of atom.
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 Crystal lattice is defined as an ordinary internal arrangement of
particle in three dimensional space.
Crystal systems:-
1. Cubic
2. Tetragonal
3. Hexagonal
4. Rhombohedral
5. Orthorhombic
6. Monoclinic
7. Triclinic
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 Wavelength of X-rays is of same order
as inter-atomic spacing of crystal.
 Inter-atomic spacing ~2-3 A0 .
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1895 X-rays discovered by Roentgen.
1914 First diffraction pattern of a crystal
made by Knipping and von Laue.
1915 Theory to determine crystal structure
from diffraction pattern developed by
Bragg.
1953 DNA structure solved by Watson and
Crick.
Now Diffraction improved by computer
technology; methods used to determine
atomic structures and in medical
applications
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Adv. Mater. Sci., 38, 95-109.

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Adv. Mater. Sci., 38, 95-109.

Troughs of one wave adds to
tough of another wave & crests
add to crests.
Resulting wave has higher
amplitude.
Troughs of one wave overlaps
crest of another.
Resulting wave has lower
amplitude.
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• Constructive
interference occurs
only when
AB= d Sin θ
AB=BC
n ƛ = 2AB
n ƛ =2d sin θ
X-ray 1
X-ray 2
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Adv. Mater. Sci., 38, 95-109.

 Source ( Production of X-rays).
 Collimator
 Monochromator
• Filter.
• Crystal monochromator.
 Detector
• Photographic methods.
• Counter Method
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Adv. Mater. Sci., 38, 95-109.

X-ray Diffraction Methods
Laue
photographic
Method
Rotating
Crystal
Method
Powder
Diffraction
Method
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 determine orientation of large single crystal.
 Position of crystal is in fixed form.
 Diffracted beam form array of spots, that lies on curves on
film.
 Bragg’s angle is fixed for every set
of plane in crystal
 Types:
a. Transmission method.
b. Back reflection method.
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 Crystal is mounted with an axis normal to a monochromatic
x-ray beam
 A cylindrical film is placed around it.
 Crystal is rotated about the chosen axis.
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Reference- Chauhan A., Chauhan P.,2014, “Powder XRD technique & its applications in science & technology”, J. Anal.
Bioanal. Tech., 5(5), 1-3.

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Crystal structure determination
Degree of crystallinity of polymers
Differentiate between crystalline &
amorphous material
Studying complex material
Determine state of anneal in metals
Reference- Chauhan A., Chauhan P.,2014, “Powder XRD technique & its applications in science & technology”, J. Anal.
Bioanal. Tech., 5(5), 1-3.

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Reference- Phadnis N., Raghuk K., Suryanarayanan R.,1997, “Identification of drugs in pharmaceutical dosage
form by X-ray powder diffractometry”, J. Pharm. Biomed. Anal., 15, 929-943

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Reference-Rajamma A., Sateesha S.,2014, “Preparation & Crystallogaphic analysis of Gliclazide polymorphs”,
Indian Journal of Pharmaceutical Sciences, 34-40.

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 XRD is first aid analytical tool in pharmaceutical industry
for analysis of drug formulation.
 Various XRD applications in pharmaceuticals have shifted
drug design, discovery into novel dimensions.
 The unique feature of the method is it provides information
about solid-state of drug.
 Disadvantage is, only applicable for crystalline material.

11/8/2017 Abhyangshree Mane M. Pharm (P'Ceutics) 26
 Chauhan A., Chauhan P.,2014, “Powder XRD technique & its
applications in science & technology”, J. Anal. Bioanal. Tech.,
5(5), 1-3.
 Das R., Ali E., Hamid S.,2014, “Current applications of X-ray
powder diffraction: A review”, Rev. Adv. Mater. Sci., 38, 95-109.
 Norrman M., Stahl K., 2006, “Characterization of insulin
microcrystals using powder diffraction & multivariate data
analysis”. Journal of applied crystallography, 39, 391-400.
 Phadnis N., Raghuk K., Suryanarayanan R.,1997, “Identification
of drugs in pharmaceutical dosage form by X-ray powder
diffractometry”, J. Pharm. Biomed. Anal., 15, 929-943.

11/8/2017 Abhyangshree Mane M. Pharm (P'Ceutics) 27
 Rajamma A., Sateesha S.,2014, “Preparation & Crystallogaphic
analysis of Gliclazide polymorphs”, Indian Journal of
Pharmaceutical Sciences, 34-40.
 Sarkar M., Perumal O.,2008, “Solid state characterization of
Nevirapine”, Indian Journal of Pharmaceutical sciences, 619-
630.
 Shrigeru T., Giri B., 2011, “ X-ray diffraction as a promising
tool to characterize bone nanocomposite”, Sci. Technol. Adv.
Mater., 12, 1-4.

11/8/2017 28Abhyangshree Mane M. Pharm (P'Ceutics)

Solid state characterization by XRD & its applications

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