Techniques For The

Study Of Crystal
Properties
And
Polymorphism
PRESENTED BY
HARESHKUMAR MULANI
 INTRODUCTION
Every crystal consists of exceedingly small
fundamental structural units that are
repeated indefinitely in all directions.

Hessel conducted investigation of the

possible types of symmetry for a solid figure
bounded by planar surfaces and deduced
that only 32 symmetry groups were possible
for such objects.

These 32 crystallographic point groups are

grouped in to six crystal systems, denoted
triclinic, monoclinic, orthorhombic,
tetragonal, trigonal, hexagonal, and cubic.
Techniques for the study of crystal
properties & polymorphism
I. CRYSTALLOGRAPHY: X- RAY DIFFRACTION
 Single crystal X-ray diffraction
 X-ray powder diffraction
II. MORPHOLOGY: MICROSCOPY
 Polarizing optical microscopy
 Thermal microscopy
III. PHASE TRANSITIONS: THERMAL METHODS
OF ANALYSIS
 Thermogravimetry
 Differential thermal analysis
 Differential scanning calorimetry
WHAT IS X- RAY DIFFRACTION?

When x-rays come in a particular

angle, they reflect off the different
planes of as if they were plane
mirrors.
A reflected x-ray signal is only observed if the
conditions are right for constructive
interference. If the d is the distance between
planes, reflected x-rays are only observed
when 2d SinØ = mλ

That’s known as Bragg’s law

The angles at which you see reflected

x-rays are related to the spacing between
planes of atoms. By measuring the angles at
which you see reflected x-rays, you can
deduce the spacing between planes and
determine the structure of the crystal.
CRYSTALLOGRAPHY: X- RAY
DIFFRACTION

Single crystal X-ray diffraction

X-ray powder diffraction

MORPHOLOGY: MICROSCOPY

Polarizing Optical Microscopy

Thermal Microscopy
PHASE TRANSITIONS: THERMAL
METHODS OF ANALYSIS

Thermal analysis methods are defined as

those techniques in which a property of
analyte is determined as a function of an
externally applied temperature.
Regardless of the observable parameter
measured, the usual practice requires that
the physical property and the sample be
recorded continually and automatically, and
that the sample temperature be alerted at a
predetermined rate.
Measurements of thermal analysis are
conducted for the purpose of evaluating
the physical and chemical changes that
may take place in a heated sample,
requiring that the operator interpret the
events noted in a thermogram.

Thermal reactions can be endothermic

(melting, boiling, sublimation,
vaporization, desolvation, solid-solid
phase transition, chemical degradation,
etc.) or exothermic (crystallization,
oxidative decomposition, etc.) in nature.
 TECHNIQUES OF THERMAL
METHODS OF ANALYSIS
Thermogravimetry

Differential Thermal Analysis (DTA)

Differential Scanning Calorimetry

(DSC)