POWDER FLOW

Prepared by: Dr. Geeta Patel

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Significance for including free-flowing powders
 Powdres are generally considered to be composed of
solid particles of the same or different chemical
compositions having diameters <1000 µm.
 Pharmaceutically, the largest use of powders is to
produce tablets and capsules, in addition to mixing and
compression properties, the flowability of a powder is
of critical importance in production.
 Success or failure in many pharmaceutical operations
can be directly linked to the flow properties of the
powder being processed.
 Flowability is critically important when assessing how
material moves around the plant.
 Industry needs the ability to develop formulations with
tailored flowability, and first step is identifying
suitable techniques for powder characterization.
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Significance for including free-flowing powders
1. Uniform feed from bulk storage container or hoppers
into feed mechanisms of tableting or capsule-filling
machine.
2. Uniform particle packing and a constant
volume/mass ratio which maintains tablet weight
uniformity.
3. Reproducible filling of tablets dies and capsule body,
which improves weight uniformity and uniform
physico-mechanical properties of tablets.
4. Uneven flow leads to excess air entrapment within
powders, which may produce capping or lamination
problems in tablets, also increase particle die-wall
friction, causing lubrication problems, and increase
dust contamination risks during powder transfer.
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Capping tablet (Top) and Laminated
tablet (Right)

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Factors influencing the flow of powders
 Under stress condition powder can flow like a liquids,
they don’t flow if the stresses are to small.
 Many manufacturing problems are attributed to
powder flow, including non-uniformity (segregation)
in blending, under-or0over dosage, inaccurate filling,
and stoppages.
 Storage, handling, production, packing, distribution
and end use can all be negatively affected by common
powder flow problems.
The factors associated with the nature of the particles
and their surface area.
Particle size, particle size distribution & specific area.
Particle shape
Moisture content
Adhesion and cohesion
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Particle size, particle size distribution & specific area
 All matter interacts, as the dimensions of particles
increase, the forces acting on them change.
 With relatively small particles, the flow through an
orifice may be restricted b’cos the cohesive forces
between the particles are of the same magnitude as
gravitational forces.
 Particle size - <100 µm – acted upon primarily by surface
force and >1000 µm – governed by gravitational force –
Balance of interaction forces determines powder
behavior.
 Fine particles (<74 µm) with very high surface area are
more cohesive than coarse particles which are influenced
more by gravitational forces.
 Particles > 250 µm – free flowing, but as the size fall
below 100 µm powders become cohesive and flow
problems are likely to occur.
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Particle size, particle size distribution & specific area
 Very fine particles (<10 µm) - extremely cohesive and
resist flow under gravity, except possibly as large
agglomerates.
 PS has been systemically investigated – flat-bottom
meter.

Particle shape

 Irregular shapes can have markedly different flow

properties due to difference contact areas.
 A group of spheres has minimum interparticle contact
and generally optimum flowability, whereas flakes or
irregular particles have a very high surface area and
poor flow properties.
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Moisture content
 Absorbed moisture in solids can exist either in the
unbound state or as part of crystal structure.
 Its effect directly change surface properties of the
particles.
 It can also affect flow properties indirectly and
permanently through the granules formulation, which
are held together by solid bridges generated by hydration
and dehydration.
 At higher moisture content and higher packing densities
liquid bridges may progress.
 The effect of moisture varies, depending on the degree of
packing or the porosity of the powder bed.
 In a porous and cohesive material, flowability is not
affected by moisture because the moisture can penetrate
to the inside of particle without the formation of liquid
bridge.
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Packing property
A set of particles can be filled into a volume of
space to produce a powder bed which is in static
equilibrium due to he interaction of gravitational
and adhesive/cohesive forces.
The change in bulk volume has been produced by
rearrangement of the packing geometry of the
particles.
In general, such geometric rearrangements result
in a transition from loosely packed to more tightly
pack.
More tightly packed powders require a higher
driving force to produce powder flow than more
loosely packed particles.
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Adhesion and cohesion
Cohesion occurs between like surfaces, such as
component particles of a bulk solid, whereas
adhesion occurs between two unlike surfaces like
between a particle and a hopper wall.
Cohesion and other particle properties affect flow
property of powder. Vander Waals, surface tension
and electrostatic forces are important properties
related with powder flow.
Adhesive/cohesive forces acting between a single
pair of particle and substrate can be accurately
determined using a ultracentrifuge to apply very
high forces strong enough to separate the two
surfaces.
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Figure : Example of (a) free flowing and (b) weakly
cohesive powder blends

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 Surface charges
 Higher the electrostatic charges, poor the flow.
Friction generates electrostatic charges, so minimize
the friction to reduce the electrostatic charges.
 Humidity
 Relative humidity of the air (interstitial as well as head
space) in a storage container, such as a bin or silo, also
affects properties of bulk materials.
 Many bulk materials are hygroscopic and thus the
expose to humid conditions results in increased
moisture content of the bulk. This can leads to an
increased in bulk strength and also to an increase in
angle of repose, flowability and cohesiveness of
granular powder.
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 Temperature
 Temperature also has a sustainable effect on bulk solid
flowability. The most drastic temperature effect is the
freezing of the moisture contained within the granular
materials and on particle surfaces. The resulting ice bonds
weaken the flow.
 However, the temperature from 30  to 40 C does not
usually have a great impact on powder flowability; if there
is the component having melting point exceeds its glass
transition temperature.
 Pressure
 Compacting pressure is also an important factor that
affects the flow properties of bulk solids. The increased
pressure leads to a larger number of larger contact points
between particles thus causing more inter-particle
adhesion and increased compaction produces a significant
increase in critical arching dimensions. 14
Measurement of powder flowability
 It is useful to be able to quantify the type of
behavior of powder.
 Various methods are
- Direct using dynamic or kinetic methods.
- Indirect – measurements on static bed.
Indirect Methods – Angle of Repose (AR)
 It is indirect method used in many branches of
science to quantify powder flowability.
 AR is a characteristic related to interparticulate
friction or resistance to movement b/w particles.
 Many methods may produce different values for
the same powder despite its difficulties, the
method continues to be used in Pharma. industry.
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Measurement of powder flowability
Basic Methods for AR :-
 The AR measured by keeping the powder static
bed condition is called static angle of repose and
the AR if measured by keeping the powder in
motion is called dynamic angle of repose.
 Dynamic AR – is preferred measurement as it is
better correlated with the actual tablet or capsule
manufacturing, in which powder is usually in
motion.
 Static AR can be classified – two experimental
variables
1. The height of the funnel may be fixed relative to the
base or the height may be varied as the pile forms.
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Measurement of powder flowability
2. The base may be of fixed diameter or the diameter of
the powder cone may be allowed to vary as the pile
forms.
Variations in AR Methods
Following variations have been used to some extent
1. Drained AR is determined by allowing an excess
quantity of material. Formation of the cone of
powder on the fixed diameter base allows
determination of the drained AR.
2. Dynamic AR is determined by filling a cylinder
(Flat bottom) and rotating it at a specified speed.
It is the angle (relative to the horizontal plane)
formed by the flowing powder.
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Various Methods for Measurement of AR
1. Funnel Method (Static AR)
 Allow the material to flow through a funnel or
orifice on to a horizontal surface below. The angle
of conical heap so formed can be determined from
simple geometry.

Figure – Fixed Funnel Method

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Measurement of powder flowability

Drawbacks :-
 It’s suitable only for free flowing powders.
 It doesn't give reproducible results, since the
cone shape is distorted by the impact of the
particles.
2. Tilting Box Method (Dynamic AR)
 A sandpaper lined rectangular box is fixed with
the powder and carefully tilted until the contents
begin to slide.
 The repose angle is the angle formed by surface of
the box with the horizontal plane.

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Various Methods for Measurement of AR

Figure – Titling Box Method

3. Rotating Cylinder Method (Dynamic AR)
 A hollow cylinder half-filled with the test powder
with one end sealed by transparent plate.
 Rotate it on horizontal plane, until the powder
surface cascades.
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Various Methods for Measurement of AR

Figure – Rotating Cylinder Method

 The curved wall is lined with sandpaper to
prevent slippage.
 The angle formed by cascading line with the
horizontal plane is the AR.
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Figure : Dynamic angle of repose instrument

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Various Methods for Measurement of AR
4. Drained AR
 It is obtained with flow devices like rectangular
vessel, cubic vessel or cubical box containing
circular disc platform.
 Drained AR is usually larger than the poured AR
for the same powder.
a) Ledge Method :-
 A rectangular vessel (ledge), which contains a
movable or sliding shutter at the bottom side.
 A vessel is filled with the sample to be tested.
 Then the shutter is opened to allow the drainage
of material itself.
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Various Methods for Measurement of AR

Figure – Ledge Method

 The angle formed by material left in the ledge with
horizontal plane is know as drained AR.
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Various Methods for Measurement of AR
b) Crater Method :-
 A cubic vessel, which contains a movable or sliding
shutter at the center of the bottom.
 A vessel is filled with the sample to be tested.
 Then the shutter is opened to allow the drainage
of material itself.

Figure – Crater Method

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Various Methods for Measurement of AR
 The angle formed by material left in the cubic
vessel with horizontal plane is know as drained
AR.
c) Platform Method :-
 A large container with built-in-platform is used.
 The bottom of the container is provided with a
sliding shutter.
 The container is filled with the sample to be
tested.
 Then the shutter is opened and the material is
allow to flow out at the bottom, leaving an
undisturbed conical heap on the platform.
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Various Methods for Measurement of AR
 This method eliminates wall friction from the
measurement and also avoids cone distortion due
to falling particles.

Figure – Platform Method

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Experimental consideration for AR
 AR is not an intrinsic property of powder, very
much dependent upon type of method.

1. The cone peak of the powder can be distorted by

the impact of powder from above.

2. The nature of base upon which the powder cone

is formed influences the AR. Recommended, cone
be formed on a common base. This can be done
by using a base of fixed diameter with a
protruding outer edge to retain a layer of
powder.

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Pharmacopoeial specifications
Angle of Repose (AR)
 The angle of repose is the constant, three
dimensional angle (relative to the horizontal
base) assumed by a cone like pile of material
formed by any of several methods discuss below.
 If more material is added to the pile, it slides
down the slides until the common friction of the
particles producing a surface at an angle  is in
equilibrium with the gravitational force. The
tangent of the angle of repose is equal to the co-
efficient of friction  between the particles.

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 tan  =  ;  = tan-1 
 Or we can write as:

Where, h = height of the pile

 r = radius of base of pile
  = angle of repose

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Factors affecting angle of repose
 Rough and irregular surface of the particles
give higher angle of repose.
 Decrease in particle size leads to higher
angle of repose.
 Lubricants at low concentration decreases
angle of repose whereas high concentration
increases angle of repose. So, optimum
concentration of lubricants required to
maintain angle of repose for good powder
flow.
 Fines increases angle of repose.
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Angle of Repose (AR)
Table :Types of flow properties and corresponding AR
Flow property Angle of Repose (°)
Excellent 25 to 30
Good 31 to 35
Fair 36 to 40
Passable may hang up 41 to 45
Poor must agitate, vibrate 46 to 55
Very poor 56 to 65
Very, very poor > 66

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Official procedure for density measurement (USP)
 USP recommends two methods
Method-I Measurement in a Graduated Cylinder
Method-II Measurement in a Volumeter
Apparatus:

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Official procedure for density measurement (USP)
Procedure:
 Allow an excess of powder to flow through the
apparatus into the sample receiving cup until its
overflows (using a minimum 25 ml – powder with
square cup, 35 ml – cylindrical cup).
 Carefully scrape excess powder from the top of the
cup (smoothly – spatula).
 Take care to keep the spatula perpendicular to
prevent packing or removal of powder.
 Determine the weight, M of the powder to nearest
0.1%.
 Calculate the bulk density by the formula : M/VO.
In which Vo is the volume in ml of the cup.
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Tapped density measurement (Official)
Procedure:
 Mechanically tapping the measuring cylinder
containing powder.
 After observing the initial volume, the cylinder
mechanically tapped and volume reading are
taken until little further volume change is
observed.
 Tapping is achieved by raising the cylinder and
allowing it to drop under its own weight a
specified distance.
 Two methods.
Method – I : Manual Tapping
Method – II: Tapped density tester (BP)
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Method-I- Tapped density measurement
Procedure:
 Unless otherwise specified, pass a quantity of
material through a 1.0 mm (No. 18).
 Into a dry 250 ml glass graduated cylinder
(readable to 2 ml) weighing 220±44 gm &
mounted on a holder weighing 450±10 gm,
approximately 100 gm of test sample, M, weighed
with 0.1% accuracy.
 If not possible, the amount of the test sample may
be reduced and the volume of the cylinder may be
modified.
 Carefully level the powder without compacting, if
necessary and read the unsettled apparent
volume, Vo.
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Method-I- Tapped density measurement
 Mechanically tap the cylinder, using a suitable
tapped density tester that provides a fixed drop of
14±2 mm at a nominal rate of 300 drops/min.
 Unless otherwise specified, tap the cylinder 500
times, measure tapped volume, Va.
 Repeat the tapping an additional 750 times and
measure tapped volume, Vb.
 If the difference between two volumes is < 2%, Vb
is the final tapped volume, Vf.
 Repeat in increments of 1250 taps, until the
difference between succeeding measurements
<2%.
 Calculate the tapped density – M / Vf (gm/ml).
 Generally replicate determinations.
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Method-II Tapped density tester (BP)
It provides a fixed drop of 3 mm±10 % at a nominal
rate of 250 drops/ min.
Apparatus: Consists of the following components.
1. A settling apparatus, capable of producing 205 ± 15 taps
in 1 min from a height of 3 ± 0.2 mm.
2. The support for the graduate cylinder, with its holder
that has a mass of 450 ± 5 gm.
3. A 250 ml graduate cylinder with a mass of 220 ± 40 gm.
Method : Into a dry cylinder, pour 100 gm (M)
sample. If not possible, select a test sample with an
apparent volume between 50 & 250 ml.
 Secure the cylinder in its holder, read the unsettled
apparent volume (Vo).
 Carry out 10, 500, and 1250 taps and read the
corresponding volumes V10, V500 and V1250.
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Method-II Tapped density tester (BP)
 If the difference b/w V500 and V1250 is greater than 2
ml, carry out another 1250 taps.
Expression of results:
 Apparent volumes: Apparent volume before settling or
bulk volume is Vo in ml and apparent volume after settling
is V1250 and V2500.
 Ability to settle: It is the difference b/w V10 & V500 (ml).
 Apparent densities: Apparent density before settling or
bulk density is M / V0 (gm/ml) and apparent density after
settling or tapped density is M / V1250 or M / V2500 (gm/ml).
Marketed Equipments –
 Tapped density tester from Electrolab–ETD-1020
 Tapped density tester from Quantachrome
 Tapped density tester from Varian

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Hausner’s Ratio (HR)
 It is used to measure both bulk volume and
tapped volume of powder.

 Where,V0 = unsettled apparent volume and Vf =

final tapped volume
 It can also be measured in terms of density.


Where,  tapped = bulk density

 bulk = tapped density
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 Carr’s Compressibility Index (CI)
 This property of powder is also known as
“compressibility’ or “Carr’s consolidation
index.” It is simple, fast and popular method
of predicting powder flow characteristics.
 It is an indirect measure of bulk density,
size, shape, surface area, moisture content
and cohesiveness of material because all of
this can influence observed CI. It is used to
measure bulk volume and tapped volume of
powder.

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 Where,V0 = unsettled apparent volume
Vf = final tapped volume
 It can also be measured in terms of density.

 Where,  tapped = bulk density

 bulk = tapped density

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Pharmacopoeial specifications

Compressibility Index & Hausner ratio

Table : Scale of flowability
Carr’s Index (%) Flow property Hausner ratio
10 Excellent 1 to 1.11
11 to 15 Good 1.12 to 1.18
16 t0 20 Fair 1.19 to 1.25
21 to 25 Passable 1.26 to 1.34
26 to 31 Poor 1.35 to 1.45
32 to 37 Very poor 1.46 to 1.59
> 38 Very, very poor > 1.60

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Flow through an orifice
 Monitoring the flow rate of material through an
orifice has been proposed as a better measure of
powder flowability.
 Flow through an orifice – useful
- for monitoring flow continuously b’cos pulsating
flow patterns have been observed for free flowing
material.
- Changes in flow rate can also be observed.
- Empirical equations have been determined
(opening diameter, particle size and density).
- The flow rate is generally measured as the
mass/flowing time from any types of containers
(cylinders, funnels, hoppers).

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Basic Methods for flow through an orifice
 Flow rate through an orifice can be classified……..
1. The type of container used.
2. The size and shape of the orifice used.
3. The method of measuring powder flow rate. It can be
measured continuously using an electronic balance with
some sort of recording device (computer camera) or in
discrete samples, example – the time taken for 100 gm of
powder or the amount of powder passing in 10 sec.

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Funnel method for flow rate measurement (BP)
Apparatus: The funnel with or without stem, with
different angles and orifice diameters are used. The
funnel is maintained upright. The assembly must be
protected from vibrations.

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Funnel method for flow rate measurement (BP)
Method:
 Introduce a test sample weighed with 0.5% accuracy in
to a dry funnel,
 The bottom opening of which has been blocked by
suitable means, without compacting the sample.
 Unblock the bottom opening of the funnel and measure
the time required for entire sample to flow out.
Expression of results: The flowability is expressed in
seconds per 100 gm of sample.
Variations in methods – Either mass flow rate or volume
flow rate can be determined, but it biases the results in
favor of high-density materials.
 A vibrator is occasionally attached to facilitate flow
from container; however this appears to complicate
prediction of the results.
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Direct method for powder flow measurement

Hopper flow rate:

 The simplest techniques, to measure the rate at which
powder discharges from a hopper.
 The shutter is placed over the hopper outlet and the
hopper is filled with powder.
 The shutter is then removed and the time taken for te
powder to discharge completely is recorded.
 By dividing the discharged powder mass by time, a flow
rate is obtained.
 Hopper or discharge tube outlets should be selected to
provide a good model for a particular flow application.
 Example – If a powder discharges well from a hopper
into a tablet machine feed frame, but does not flow
reproducibly into the tablet die.
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Recording flowmeter
A recording flowmeter is essentially similar to
the previous method except that powder is
allowed to discharge from hopper or container
on to a balance.
 In case of analogue balances a chart recorder is
used to produce a permanent record of the
increase in powder mass with time.
 Recording flowmeters allow mass flow rates to
be determined and also provide a means of
quantifying uniformity of flow.
A. Hosokawa powder characteristics tester
B. Aero-flow
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Improvement of powder flowability
A. Alteration of particle size & size distribution
 Coarse particles are less cohesive than fine particles
and an optimum size for free flow exists.
 The flowability problem can be solved by removing
a proportion of the fine particle fraction or by
increasing the proportion of coarser particles.
B. Alteration of particle Shape and texture
 Spherical particles – better flow properties than more
irregular particles.
 Spray-drying can be used (spray dried lactose).
 Temp cycling crystallization.
 Very rough surface will be more cohesive and greater
tendency to interlock than smooth-surfaced particles.
 Both controlled by crystallization and granulation.

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Improvement of powder flowability

C. Alteration of surface forces

 Reduction of electrostatic charges can be achieved
by reducing frictional contacts or altering process
conditions.
 Electrostatic charges can be prevented ordicharged
by efficient earth connections.
 Moisture content – as absorbed surface moisture
films tend to increase bulk density and reduce
porosity.
 In cases where moisture content is excessive,
powder should be dried and if hygroscopic – stored
properly.

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Improvement of powder flowability
D. Flow enhancers or flow promoters:Glidants
 Small amount of glidant is often used.
 Like talc, corn starch, silicon dioxide and colloidal
silica (Cab-O-Sil, Aerosil).
Praposed mechanism for glidant action
 Distribution of glidant in the host particles.
 Dispersion of static charges from the host paticles
surface.
 Preferential adsorption of gases and moisture.
 Physical separation of particles and subsequent
reduction in Van-der walls interaction.
 Reduce friction between granules and surface
roughness is minimized.
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Improvement of powder flowability
E. Alteration of process conditions
Use of vibration-assisted hoppers
 In cases where the powder arch strength within a bin
or hopper is greater than the stresses in it, due to
gravitational effects, powder flow will be broken up or
prohibited.
 The poor powder flow may result because of either
rate holing or arching/bridging that may take place.

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Improvement of powder flowability
 Powder flow can be encouraged by adding stresses
due to gravitational interactions by vibrating the
hopper mechanically.
Use of force feeders
 The powder discharge irregularly or flood out can
be improved by fitting vibrating baffles, known as
live-bottom feeders, at the base of the conical
section within a hopper.
 Force feeders are usually made up of a single or two
counter-rotating paddles at the base of the hopper
just above the die table in place of feed frame.
 The paddles presumably act by preventing powder
arching over dies, improve die filling at high speeds.
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