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Powder characteristics
Single particle characteristics
Particle systems
Particle size
Definition of diameters
Equivalent sphere
(volume) diameter
Sieve diameter (minimum
mesh size through which
the particle will fall)
Minimum, maximum
diameters
Suspension
Laser
Is ( ) 1 16 4 R 6 n 2 1
2
2
4 2
1 cos
I0
r 2
n 2
Laserlight
Detector
QuickTime and a
TIFF (Uncompressed) decompressor
are needed to see this picture.
Powder characterisation
Intensity
+
0
Scattered intensity as function of
scattering angle for three
individual particles (red < blue <
green)
0
Sum of the scattered intensities
shown on the left.
100%
monodispersed
50%
polydispersed
10%
1
10
100
size (mm)
(Reed, 1995)
dL
Arithmetic mean
Geometric mean
ln d
N i di
N
surface diameter
dS
N d
N
i
2
i
volume diameter
dV
N d
N
i
3
i
N ln d
N
i
Ni
Mi
V di 3
Particle shape
A dimensionless combination of different average diameters of a distribution of
particles is called a shape factor. Shape factors have three functions:
-Proportionality factors between different particle size determination methods
-Conversion factors for expressing results in terms of an equivalent sphere
dimension
-Transformations of the measured particle diameter into particle surface and volume
respectively.
The most common shape factor is the aspect ratio e.g. the ratio between the largest
and the smallest diameter of a particle.
The volume shape factor is defined as:
Vt
Ni di 3
Agglomeration states I
Agglomeration state:
Well dispersed
Particle density I
Density
openporosity(Vop)
closedporosity(Vcp)
Densities:
ultimate density: M/Vs
apparent density: M/(Vs + Vcp)
bulk density: M/(Vs + Vcp + Vop)
M: particle mass (empty pores)
Vs : volume of solid
Pycnometry
This method allows to measure
the apparent density.
(Reed, 1995)
Powder characterisation
Particle density II
The mercury injection porosimeter allows to measure the open
porosity
The volume of mercury (contact angle
with most solids = 140) forced into
the pores of the solid is mesured as
a function of pressure. The pore size
distribution is calculated using the
relationship between applied pressure
and the radius of the pore which can
be filled by this pressure
2 cos
p
r
= wetting angle (140 for most solids)
= surface tension mercury - sample
r = pore radius
(Reed, 1995)
N A VM AM
S
V Mol M s
MeasuringsetupforBET(Bernauer,EmmetandTeller)
measurements.
NA:Avogadrosnumber
VM:adsorbedgasvolume
AM:areaoccupiedbyoneadsorbatemolecule
VMol:volumeofonemolofgasatstandardP,T
Ms:massofthesample
The solid must be free from previously
adsorbed gases and vapours. Evacuation
at 10-4 Torr for several hours is
necessary. It is possible to heat the
solid (100-400c).
Powder characterisation
Powder specifications I
Specifications for three Bayer process aluminas
Powder specifications II
Specifications for three barium titanate powders
Powder segregation I
Powder segregation II
Simulation of particle size segregation during vibration. Interestingly the large
particles move upward = Brazilian nut effect! (http://www.granular.com/POWDER/tour.html)
Langmuir isotherm II
The Langmuir isotherm can be tested in arranging it in a linear form:
KPa KPa
KPa
KPa
KPa
can hardly be determined, but the volume v of gas taken up by the sample can be
measured. The ratio between the volume of the adsorbed gas (v) and the maximum
volume uptake (V) assumed to correspond to a total monolayer coverage is proportional
to the surface coverage.
so
v
P P
1
a a
V
v V KV
AplotofP/vagainstPis
linear.
Theinterceptallowsto
determineKatconstantT.
Microcrystalline cellulose is one of the most useful filler for direct compression.
Cellulose in general consists of an amorphous part and a crystalline part, which
can exist in two
polymorphic forms: cellulose I and cellulose II. UICEL (University of Iowa
cellulose)
is a cellulose II product and can be obtained by mercerization (chemical
treatment with sodium hydroxide) from Avicel PH102, a microcrystalline
cellulose, which contains the cellulose I polymorph. X-ray measurements of the
two substances confirmed the different polymorphic forms and demonstrated a
higher degree of crystallinity for Avicel PH102(73%) than for UICEL (64%).
Cellulose exists in four major crystal modifications, cellulose I, II, III and IV. The
polymorphic forms can be interconverted according to figure 3 mostly by certain
chemical and thermal treatments