MICROMERITICS Flashcards
MICROMERITICS
came from the greek word ____
micros
MICROMERITICS
micros means
small
- the science and technology of small particles
- cover particles 100nm to 100mm
micromeritics
MICROMERITICS
covers particles ____ to ____
100nm - 100mm
- focuses on particles in the size range of 1nm to ⁓5mm
- has three categories: colloidal dispersions, coarse dispersions, pharmaceutical powders
PHARMACEUTICAL MICROMERITICS
PHARMACEUTICAL MICROMERITICS
focuses on particles in the size range of ____ to ____
1nm to approx 5mm
PHARMACEUTICAL MICROMERITICS
3 categories
colloidal dispersions (& nanoparticles)
coarse dispersions
pharmaceutical powders
PHARMACEUTICAL MICROMERITICS
SIZE:
colloidal dispersions & nanoparticles
< 1,000 nm
PHARMACEUTICAL MICROMERITICS
SIZE:
coarse dispersions
1 - 50um
PHARMACEUTICAL MICROMERITICS
SIZE:
pharmaceutical powders
50um
PHARMACEUTICAL MICROMERITICS
the only dispersion not covered
molecular dispersion
how many micromeritic properties
7
MICROMERITIC PROPERTIES
ANALYTICAL TECHNIQUE:
* laser diffraction
* dynamic light scattering
REOPRTED PARAMETER:
* D-value
SIZE
MICROMERITIC PROPERTIES
ANALYTICAL TECHNIQUE:
* imaging
* scanning electron microscopy
REPORTED PARAMETER:
* high-resolution images
* circularity
SHAPE
MICROMERITIC PROPERTIES
ANALYTICAL TECHNIQUE:
* electrophoretic light scattering
REPORTED PARAMETER:
* zeta potential
CHARGE
MICROMERITIC PROPERTIES
ANALYTICAL TECHNIQUE:
* atomic force microscopy
* rheometry
REPORTED PARAMETER:
* elasticity
* stiffness (Young’s modulus)
MECHANICAL
MICROMERITIC PROPERTIES
ANALYTICAL TECHNIQUE:
* gas adsorption method
REPORTED PARAMETER:
* surface area
* pore size
SURFACE
MICROMERITIC PROPERTIES
ANALYTICAL TECHNIQUE:
* differential sanning calorimetry
REPORTED PARAMETER:
* percentage of crystallinity
INTERNAL MICROSTRUCTURE
MICROMERITIC PROPERTIES
ANALYTICAL TECHNIQUE:
* bulk density
* tapped density
REPORTED PARAMETER:
* hausner ratio
FLOWABILITY & COHESIVENESS
- shape, surface area of each paritcle, size range and number, weight and volume must be considered
- cannot be describe by a single dimension
PARTICLE SIZE
particles cannot be described by a ____
single dimension
PARTICLE SIZE
a size of a spherical particle is characterized by its ____
diameter
PARTICLE SIZE
a size of a non-spherical particle is characterized by its ____
equivalent spherical diameter
PARTICLE SIZE | EQUIVALENT SPHERICAL DIAMETER
- the diameter of a circle that has the same projected area as the particle
- imaginary circle that covers 2 points of the particle
PORJECTED
PARTICLE SIZE
absence of measurable diameter with irregularly shaped particles
equivalent spherical diameter
PARTICLE SIZE
- for non-spherical/asymmetrical particles
- approximate particle size based on diameter of sphere
equivalent spherical diameter
PARTICLE SIZE | EQUIVALENT SPHERICAL DIAMETER
- the diameter of the particle at the point that divides a randomly oriented particle into two equal projected areas
MARTIN’S
PARTICLE SIZE | EQUIVALENT SPHERICAL DIAMETER
commonly used in particle sizing
MARTIN’S
FERET’S
PARTICLE SIZE | EQUIVALENT SPHERICAL DIAMETER
not used in particle sizing because of variations
PROJECTED
PARTICLE SIZE | EQUIVALENT SPHERICAL DIAMETER
- the distance between imaginary parallel lines tangent to a radomly oriented particle and perpendicular to the ocular scale
FERET’S
- represents the number of particles in each size present in a given sample
- represented as frequency curve or cumulative percentage over/under a particular size curve
- particles in a group could either be: monodisperse, polydisperse
PARTICLE SIZE DISTRIBUTION
PARTICLE SIZE DISTRIBUTION
collection of particles of uniform size
MONODISPERSE
PARTICLE SIZE DISTRIBUTION
collection of particles of more than one size
POLYDISPERSE
PARTICLE SIZE DISTRIBUTION
is represented as ____ or ____ over/under a particular size curve
frequency curve or cumulative percentage
METHODS OF DETERMINING PARTICLE SIZE DISTRIBUTION
number of particles
optical microscopy
electron microscopy
METHODS OF DETERMINING PARTICLE SIZE DISTRIBUTION
weight of particles
sieving
sedimentation
centrifugation
METHODS OF DETERMINING PARTICLE SIZE DISTRIBUTION
light scattering by particles
photon correlation spectroscopy
METHODS OF DETERMINING PARTICLE SIZE DISTRIBUTION
volume of particles
coulter counter method
particle shape analysis is carried out using ____
imaging techniques
it affects:
* solubility
* packing properties
* flowability
* bulk powder properties
* surface area
PARTICLE SHAPE
carried out using imaging techniques
PARTICLE SHAPE ANALYSIS
PARTICLE SHAPE
measure of deviation from roundness;
- if AR = 1, the particle is a perfect sphere
ASPECT RATIO
PARTICLE SHAPE
expresses the radius of cuvature of the particle corners
- if roundness = 1, the particle is circular
(roundness of corners)
ROUNDNESS
PARTICLE SHAPE
measures the closeness to a perfect sphere
* if sphericity = 1, the particle is sphere
(roundess as a whole)
SPHERICITY
PARTICLE SHAPE
representative of local surface textures between corners
* if roughness decreases, the particle surface has more concavities
ROUGHNESS
SURFACE AREA & SPECIFIC SURFACE
what is the relationship between the asymmetry of the particle to the specific surface
DIRECTLY PROPORTIONAL
defined as the surface area per unit volume or per unit weight
SPECIFIC SURFACE
SURFACE AREA & SPECIFIC SURFACE
what is the relationship of the particle size to the surface area
inversley proportional
materials with high specific area may have cracks and ____ that adsorb gases & vapors into their interstices
PORES
a measure of the air spaces or voids in a material (ɛ)
POROSITY
describes the behavior of a material under load
* elasticity
* stiffness
* rigidity
* hardness
* strength
MECHANICAL PROPERTIES
MECHANICAL PROPERTIES
extent of resistance to deformation (shear modulus, G)
STIFFNESS
MECHANICAL PROPERTIES
resist deformation when exposed to stress and return to its original state (Young’s modulus, Eγ)
ELASTICITY
- the surface charge on a particle has a potential to affect its interaction with other particle
- zeta potential (electrokinetic potential)
- formation of the electrical double layer
ELECTRICAL PROPERTIES
ELECTRICAL PROPERTIES
DIFFUSE LAYER:
ions are diffused more freely ____
around the particle
ELECTRICAL PROPERTIES
hydrodynamic plane of shear is also called
slipping plane
ELECTRICAL PROPERTIES
HYDRODYNAMIC PLANE OF SHEAR:
charges beyond the slipping plane will ____ with the particle as an entity.
NOT MOVE
ELECTRICAL PROPERTIES
HYDRODYNAMIC PLANE OF SHEAR:
ions within this boundary will ____ with particle as one entity
MOVE
ELECTRICAL PROPERTIES
STERN LAYER:
the particle will attract ions of the ____ charge
OPPOSITE
ELECTRICAL PROPERTIES
STERN LAYER:
positive ions will ____ to the surface. these ions are tightly bound immediately around the surface
MOVE CLOSER
- the choice of sutiable sizing technique for measuring PSD depends on the expected size range of the particle
- has three categories:
- single particle counting
- fractionation
- ensemble averaging
PARTICLE SIZING TECHNIQUES
PARTICLE SIZING TECHNIQUES
the choice of sutiable sizing technique for measuring PSD depends on the ____ of the particle
expected size range
means to verify and supplement the information gained from the first technique with a complemenetary second and possibly a third technique that used different mechanism to measure particle size
ORTHOGONAL
- used to confirm measurements made by an unrelated method
- confirmation of an initial test with a different method
ORTHOGONAL MEASUREMENTS
IMAGING ANALYSIS
- direct measurement of microstructural features and intermolecular forces at nanoscale level
- high resolution, atomic-resolution method – topographical image
ATOMIC FORCE MICROSCOPY
IMAGING ANALYSIS
provides measurements on surface textures
TOPOGRAPHICAL IMAGE
IMAGING ANALYSIS
- high resolution direct technique for characterizing particles from about 1 microns to several mm
- typically used in conjunction with ensemble-based particle sizing method such as laser diffraction
AUTOMATED STATIC & DYNAMIC IMAGE ANALYSIS
IMAGING ANALYSIS
Automated Static & Dynamic Image Analysis is typically used in conjunction with ensemble-based particle sizing method such as ____
LASER DIFFRACTION
IMAGING ANALYSIS | AUTOMATED STATIC & DYNAMIC IMAGE ANALYSIS
- uses microscope to capture image of the stationary particles
- size and shape measurements
STATIC
IMAGING ANALYSIS | AUTOMATED STATIC & DYNAMIC IMAGE ANALYSIS
- uses microscope to capture image of particles flowing
- ideal for bulk solids
DYNAMIC
IMAGING ANALYSIS | AUTOMATED STATIC & DYNAMIC IMAGE ANALYSIS
dynamic image analysis is ideal for ____
bulk solids
- photon correlation spectroscopy (PCS); quasi-electric light scattering (QELS)
- measures particle size in the submicron range below 1nm
- measurement with light-scattering of dynamic
DYNAMIC LIGHT SCATTERING
- small amount of sample is required
- analysis is rapid
- does not require highly specialized personnel
- noninvasive
DYNAMIC LIGHT SCATTERING
an ensemble technique - the diameter obtained is that of a sphere that has translational diffusion coefficient as the particle being measured
(means that size is larger than what is measured in EM)
DYNAMIC LIGHT SCATTERING
- used for particles ranging from hundreds of nanometers up to several millimeters
- measured PSD by measuring the angular variation in the intensity of light scattered as a laser beam passes through a dispersed particle sample
LASER DIFFRACTION
LASER DIFFRACTION
what is the relationship between particle size and the angle of diffraction
DIRECTLY PROPORTIONAL
- one of the oldest method; method of choice for coarser powders
- this method utilizes a series of standard sieves stacked over one another then subjected to standardized period of agitation and the weight retaned on eahc sieve is accurately determined
SIEVING
SIEVEING
it is a method of choice for what type of powders
COARSER POWDERS
METHODS FOR DETERMINING SURFACE AREA
can be computed from ____ obtained
PSD
- the amount of gas or liquid solute that is adsorbed onto the powder to form monolayer
- depends on the rate at which gas or liquid permeates a bed of powder
METHODS FOR DETERMINING SURFACE AREA
METHODS FOR DETERMINING SURFACE AREA
- amount of a gas or liquid solute that is adsorbed onto the sample of powder to form a monolayer is a direct function of the surface area of the sample
ADOSORPTION METHOD
METHODS FOR DETERMINING SURFACE AREA | ADSOPRTION METHOD
insturment used to calculate surface area and pore structure
QUANTASORB
METHODS FOR DETERMINING SURFACE AREA | ADSORPTION METHOD
what is the relationship between the amount of quantasorb and the surface area
directly proportional
METHODS FOR DETERMINING SURFACE AREA
- the rate at which a gas or liquid permeates a bed of powder is related to the surface area exposed to the permeant
AIR PERMEABILITY METHOD
METHODS FOR DETERMINING SURFACE AREA | AIR PERMEABILITY METHOD
instrument used to calculate surface area and pore structure
FISHER SUBSIEVE SIZER
FUNDAMENTAL properties of powders
particle size distribution
surface area
powders may be:
* free-flowing
* cohesive/sticky
FLOW PROPERTIES & FLOWABILITY
FLOW PROPERTIES & FLOWABILITY
- characterized by dustibility
- example: lycopodium - 100% dustibility
FREE-FLOWING
FLOW PROPERTIES & FLOWABILITY
Free-flowing is characterized by
DUSTIBILITY
FLOW PROPERTIES & FLOWABILITY
dustibility of lycopodium
100%
- the maximum angle possible between the surface of a pile of powder and the horizontal plane
the lower the θ, the bettwer the flow
ANGLE OF REPOSE
ANGLE OF REPOSE
what is the relationship of the angle of repose to the flowability of the sample
directly proportional
ANGLE OF REPOSE
the lower the θ, the ____ the flow
better
ANGLE OF REPOSE
θ
theta in degree
- the granular materials are poured from a funnel at a certain height onto a selected base with known roughness properties
- the funnel is either fixed or raised slowly while the conical chape of the material heap is forming to minimize the effect of the falling particles
FIXE FUNNEL METHOD
PORE SIZE & POROSITY (VOIDS OR SPACES)
what do you call the voids in between powder particles
INTERPARTICULATE VOIDS
PORE SIZE & POROSITY (VOIDS OR SPACES)
the voids within a specific particle
INTRAPARTICULATE VOIDS
DESNITIES OF PARTICLES
density of material itself is exclusive of inter- and intraparticular voids
TRUE DENSITY
DESNITIES OF PARTICLES
density of material itself including intraparticular voids
GRANULAR DENSITY
DESNITIES OF PARTICLES
density of material itself inclusive of inter- and intraparticular voids
BULK DENSITY
DESNITIES OF PARTICLES
- aka compressed bulk density
- obtained after compacting by tapping or vibration
TAPPED DENSITY
DESNITIES OF PARTICLES
tapped density is also called
compressed bulk density
DETERMINATION OF BULK DENSITY
Method I
graduated cylinder
DETERMINATION OF BULK DENSITY
Method II
SCOTT VOLUMETER
DETERMINATION OF BULK DENSITY
ρ
rho
DETERMINATION OF BULK DENSITY
what is the relationship between the bulk density and the interparticulate voids
directly proportional
DETERMINATION OF BULK DENSITY
what is the relationship between the tapped density and the interparticulate voids
inversely proportional
mechanical tapping is achieved by raising the cylinder and allowing it to drop under its own weight
DETERMINATION OF TAPPED DENSITY
DETERMINATION OF TAPPED DENSITY
is achieved by raising the cylinder and allowing it to drop under its own weight
MECHANICAL TAPPING
Carr reported that the more a material is compacted in a compaction or tap bulk density test, the poorer are its flow properties
COMPRESSIBILITY (CARR’S) INDEX
COMPRESSIBILITY (CARR’S) INDEX
who reported that the more a material is compacted in a compaction or tap bulk density test, the poorer are its flow properties
Carr
COMPRESSIBILITY (CARR’S) INDEX
what is the relationship between the compressibility index and the flow property
directly proprotional
- a set of particles can be filled into a volume of space to produce a powder bed, which is in static equilibrium owing to the interaction of gravitational and adhesive/cohesive forces
- by slight vibration of the bed, particles can be mobilized and at static equilibrium, they occupy a different spatial voume than before
PACKING GEOMETRY
PACKING GEOMETRY
a set of particles can be filled into a volume of space to produce a ____, which is in static equilibrium owing to the interaction of gravitational and adhesive/cohesive forces
powder bed
PACKING GEOMETRY
a set of particles can be filled into a volume of space to produce a powder bed, which is in ____ owing to the interaction of gravitational and adhesive/cohesive forces
STATIC EQUILIBRIUM
PACKING GEOMETRY
a set of particles can be filled into a volume of space to produce a powder bed, which is in static equilibrium owing to the interaction of ____ and ____ forces
GRAVITATIONAL & ADHESIVE/COHESIVE FORCES
PACKING GEOMETRY
by ____ of the bed, particles can be mobilized and at static equilibrium, they occupy a different spatial voume than before
SLIGHT VIBRATION
PACKING GEOMETRY
by slight vibration of the bed, particles can be ____
MOBILIZED
PACKING GEOMETRY
at ____, they occupy a different spatial voume than before
STATIC EQUILIBRIUM
PACKING GEOMETRY
static equilibrium, they occupy a ____ than before
DIFFERENT SPATIAL VOLUME
PACKING GEOMETRY
- loosest packing
- porosity = 48%
CUBIC
PACKING GEOMETRY
POROSITY:
cubic
48%
PACKING GEOMETRY
- closest packing
- porosity = 26%
RHOMBOHEDRAL
PACKING GEOMETRY
POROSITY:
rhombohedral
26%