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Thermal and

Microscopy Analysis
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Characterisation
Thermal analysis Microscopy analysis

Crystallographic data Particle properties


Differential Scanning
Calorimetry
Light microscopy

Differential Thermal
Analysis
Hot stage microscopy

Differential Thermal
Gravimetry
Electron microscopy

Thermal Gravimetry
Analysis
Atomic force microscopy

Kuliah Preformulasi 2019


2
Characterisation

Properties of
particles
Manufacturing Properties of Successful Properties of • Size
processes powders formulation
crystal/amorph • Shape
• Surface roughness
material • Surface chemistry
• Movement • Crystallographic
• Blending data
• Manipulation
of solids

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Thermal analysis
DSC DTA

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Thermal analysis
DTG TGA

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Microscopy analysis

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Microscopy analysis

Light Microscopy
• Transmitted light
microscopy
• Reflected light microscopy

Depends on the sample


thickness/transparency

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Microscopy analysis
Hot-stage Microscopy

• Light microscope +
temperature controlled stage
• Visualizing DSC thermogram
• Visualizing TGA thermogram
seen as bubbles release.
• Coupled with cross
polarizing filters to capture
the birefingent of
crystal/polymorphs

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Microscopy analysis

What is
birefringence?
Why some samples
show
birefringence?

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Microscopy analysis
Electron microscopy

• Shorter wavelength than


light microscope
• Electromagnet used to
capture the electron beams
• Transmission electron
microscope
• Scanning electron
microscope

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Microscopy analysis

Atomic force microscopy

• Deflection of a cantilever back


to build up a topographical
image of sample surface

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Particle size
Coulter counter

• Based on the change in conductivity of an


electrolyte as particles in suspension are drawn
through an aperture. Particles assumed as
spherical

Photon correlation spectroscopy

• Dispersed powder in liquid/air placed in a parallel


beam of laser light.

Sieve analysis

Microscopy

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Particle size

Irregular particle
shape’s size measure
Histogram

Limitation: not
representative

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Solid properties
Molecular • Stability
packing • Dissolution rate

• How to process the material


Particle shape • Habit determined by visualization by microscope

Surface • Topography and surface energy


properties • Determined by atomic force microscopy

Particle size
distribution
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