Measuring

Powder
and Granule
Properties to
anticipate
problems
Processing powders in industry
can be a challenging business.

Stable Micro Systems

Measuring Powder and Granule Properties

Some examples of powder forms are shown

The Stable Micro Systems
Powder Flow Analyser
“... countless
different types
of powder..”
A
lmost every manufacturing
industry has to deal with
powders and granules at some
stage during production. Depending on
the nature of your powders, you will
have different testing priorities.
For example, companies that require the
flow of powders through hoppers will be
interested in their caking and
consolidation behaviour, particularly
after a period of storage. Exporters of
panko breadcrumbs will need to know
their fracture behaviour before and after
frying to ensure consistent quality.
Protein powder manufacturers may be
interested in agglomeration properties
and mouthfeel. Cosmetics companies
producing powder compacts such as
eyeshadow and blusher will be motivated
to find an optimum hardness – low
enough for payoff on the brush, high
enough to prevent damage during transit.
in the table below, but countless different
types of powder are manufactured,
transported and used as ingredients for many
different reasons.
With powders accounting for approximately
50% of materials used in industry, this is an
important area of Texture Analysis and
physical testing. Handling and processing
powders, particulates and granules is central
to product processing, but has traditionally
been fraught with problems due to their
unpredictable and irregular behaviour,
specifically with respect to flowability. With
so many raw materials and semi-finished
products in powder form, this sector stands
to gain significant manufacturing and
commercial benefits from improvements in
the assessment of powder flow. Stable Micro
Systems have developed a wide range of tests
to analyse and quantify physical properties
of powders, ranging from the flowability of
powder ingredients to the physical properties
of a final product.

Table 1
Powder Form Food Industry Cosmetics and Pharmaceutical Industrial
Personal Care Industry Materials
Free flowing • Powdered • Titanium • Active • Metal and
powder as an flavouring to dioxide for use ingredients for ceramics
ingredient sell on to in sun cream tabletting powders for
producers of • Mica powder • Dusting for sintering
snack foods medical gloves • Powders for
• Yeast forming
• Powdered egg coatings
white
Free flowing • Flour • Bronzer • Athlete’s foot • Cement
powder as a • Protein powder • Talcum powder powder • Photocopier
final product • Asthma inhalers toner
Compacted • Stock cubes • Eyeshadow • Most tabletted • Ceramic green
powder as a • Pressed • Bath bombs drugs compacts
final product powder
confectionery

1 | Measuring Powder and Granule Properties to anticipate problems

 Learn how to handle your powders

Handling and processing powders production, packing, distribution and end use
Powder handling and processing tends to be can all be negatively affected by common
problematic because powders exhibit powder flow problems like those shown in
properties similar to both solids and liquids. Figure 1. “... powders
Normally, they are surrounded by air and Knowing a powder’s characteristics and the
combine in many ways to change the way the factors which impact on it (see Table 1) is
exhibit
powder behaves. Understanding the flow essential. This allows the optimisation of properties
properties of a powder is important as most formulation and equipment and
powders will be stored in hoppers or silos, or incorporates quality control principles similar to both
transported at some point in the production throughout production, thereby assisting in solids and
process. Many common manufacturing process design, performance evaluation and
problems are attributed to incorrect or poor troubleshooting. Many final products that liquids.”
powder flow, including non-uniformity reach the consumer need some
(segregation) in blending, under- or over- consideration of flowability, too. For
dosage, inaccurate filling and obstructions example, if a product such as artificial
and stoppages. These in turn lead to excessive sweetening powder is being poured from a
rejected material, machine downtime and jar, cakes and lumps will give the product
defective end-products. Storage, handling, an impression of low quality.

Figure 1: Typical Powder Flow problems Figure 2: Good Powder Flow

Consistent
Ratholing Bridging (arching) Flooding and steady

Measuring Powder and Granule Properties to anticipate problems | 2

Measuring Powder and Granule Properties

Predictable powder flow also enables

“... check how Table 1: Variables affecting powder flow
constituent selection, manufacturing
Powder Variations External factors
new powders Particle size Flow rate
procedures and equipment to be optimised.
This in turn maximises speed of production,
interact with Size distribution Extent of
compaction reduces the risk of stoppages and improves
existing Particle density Vibration blend quality, filling procedures and end
Particle Shape Temperature product quality. As pressure mounts to
constituents.” Surface texture Humidity contain costs, substituting expensive
Cohesivity Electro-static charge constituents with cheaper ones is an
Particle interactions Aeration attractive option. Although these substitutes
Attrition Container surface may be produced to the same specification as
Water content/humidity Container shape
original substances, they may not necessarily
Hardness Outlet diameter
store, convey and process as easily.
Stiffness Storage time
Discovering this after production has started
Thermal properties
incurs downtime and cost.
Critical relative humidity
Compression properties
Ignition properties

When flowability is a necessity

Why Measure the Flowability Traditional instrument-based

of Powder?
Even the most rudimentary methods of
assessing powder flow necessitate the one
resource all technologists lack – time.
However, the benefits to be gained can far
outweigh this immediate concern. For
example, product development teams can
evaluate new constituents and ingredients
and predict their behaviour prior to
commencing large scale production. They can
also check how new powders interact with
existing constituents. This speeds up
development time and minimises trial and
error tactics.
testing
The first, and most common, instrument for
powder flow testing is the Jenike Shear Cell.
Powder is loaded into the cell and then
compressed with a defined weight. After
compression, the operator measures the force
needed to shear through the sample. This
method is commonly used for silo and storage
bin design and eliminates most of the
subjectivity to which earlier test procedures
were prone. However, human involvement in
the loading of the sample can impact on the
results obtained, making them less reliable. In
addition, because minute disturbances – of

3 | Measuring Powder and Granule Properties to anticipate problems


Substitution of ingredients may
affect flowability
any kind – can impact on a sample’s flow rate,
none of the aforementioned test procedures is
suitable for repeated testing. Recent years
have seen intense development activity as
instrument designers strive to provide and
improve truly accurate, repeatable and
objective equipment which can overcome the
shortcomings of earlier test methods.
Using a Powder Flow Analyser
The most convenient way to assess the flow
behaviour of powder is to use a Powder Flow
Analyser (PFA).
Replacing traditional manual pouring
methods, Stable Micro Systems has patented
a helical blade design that controls the flow
of a powder sample. Movement of the sample
is achieved by a blade or rotor, which is
Figure 3
Figure 3a: Figure 3b:
Aeration by rotating Compaction by
and lifting the sample rotating and downward
blade movement
passed through a column of powder
according to vertical and rotational settings
“Tests are set
defined by the user. up quickly and
When the blade is rotated in the direction easily...”
shown in Figure 3a, the sample is lifted or
aerated. This procedure conditions the
powder and eliminates any loading variation
between operators. Figure 3b shows
compaction. It provides a simple quality
control test for variations between batches
and/or sources. Samples being compacted
will resist flow and movement.
Slice compaction, shown in Figure 3c, can
be used to blend and mix samples. This
procedure removes air from the sample and
causes friction between the surfaces of
granules. Users can assess the smoothness of
the contact between the powder and the
blade. These movements can be carried out in Powder Flow Analyser
any combination and in any sequence. A
simple test will involve conditioning, slice
compaction and slice aeration, and blade
shake to remove any powder which has
adhered to the upper blade surfaces.
Exponent software is intrinsic to the Texture
Analyser and Powder Flow Analyser, and
displays data in real time. Tests are set up
quickly and easily and data analysis set to
automatically collect important parameters
from each test in simple or sophisticated ways.
Figure 3c:
Slice compaction is a
less severe form of
compaction
Measuring Powder and Granule Properties to anticipate problems | 4
Measuring Powder and Granule Properties
Several different tests may be performed
“A more using a range of methods on the Powder Flow
cohesive Analyser:
powder will • Caking: This is the tendency of a powder
to form large agglomerates during storage
cling to itself and transportation. The tendency of a powder
to cake is closely related to its cohesiveness.
and to the The strength of the cake will depend on a
blade...” number of factors such as packing efficiency,
particle to particle interactions and humidity.
The caking test gently compacts the powder
column to a user programmed force, then
slices back to the top of the column with
minimum disturbance, before re-compacting.
This is repeated for the programmed number
of cycles and the rotor blade then slices the
compacted cake.
Caking: when you need it Caking: when you don’t want it
Cohesion: When your • Cohesion: Cohesiveness is the tendency for
particles of powder to cling together and
products stick together
agglomerate (form larger clusters of
particles). The PFA measures this cohesion
characteristic by moving the blade in such a
way as to lift the powder. A more cohesive
powder will cling to itself and to the blade,
reducing the force exerted on the base of the
vessel.
• Powder Flow Speed Dependence: Powder
flow properties may change with increasing
or decreasing flow speeds. For example, a
powder may become more resistant to flow
as it is forced to flow faster, or it may become
freer flowing as the flow speed increases. This
5 | Measuring Powder and Granule Properties to anticipate problems
issue can lead to under or over filling as a
result of process changes to meet increased
output demand.
The PFA measures this characteristic by
assessing the work required to move the
blade though the powder at increasing
speeds. An evaluation of the flow stability of
the powder is made by comparing the work
needed to move the blade though the powder
at the start of the test compared to the work
required to move the powder at the same
speed at the end of the test.
• Bridging: As the flow imposed by the PFA
is controlled, powders that flow freely will
exhibit very little resistance transferred
though the powder column in either a
downward or an upward direction.
Conversely, poorly flowing powders exhibit a
substantial amount of force in either
direction. As the blade travels through the
powder column in both compression
(downward) and lifting (upward) directions,
powders resist the advancing blade.
Powders that flow easily will freely cascade
over and around the blade, generating a
smooth graph. If the powder momentarily
bridges, arches or otherwise forms cohesive
bonds, the further progress of the blade will
break those bonds. In granulated products, the
particles can nestle and cause a similar
problem. Force typically increases as the bonds
are made and stressed, followed immediately
by a drop in force as the bonds fail.
Graph displaying ‘bridging’ behaviour
in a powder
The degree of resistance and failure is easily
quantified by measuring the length of a
plotted line (which correlates well with a
line’s jaggedness). The measurement of
bridging is automatically carried out during
the post-test analysis.
• Bulk density: A vessel that splits in two
using a hinge is available to help discard
excess powder (after conditioning) and leave
behind a specified volume. The ability of the
PFA to measure weight allows the automatic
calculation of bulk density.
As with solid objects, density is the ratio
between mass and volume. The structure of
powders is extremely variable, however, so
their density can be easily altered by changes
to their packing. The conditioning cycles on
Split vessel
Split vessel with helical blade
the PFA help to provide a reproducible
measurement of density by treating each
powder sample in a systematic and repeatable
way before each test. During the conditioning
process, filling stresses and differences in
filling techniques are removed by directing the
blade to slice/aerate (lift) through the sample.
This produces a uniform sample, which assists
comparison and result repeatability.
Measuring Consolidation on the
“... automatic
Powder Flow Analyser – Varying
Time/Compaction
calculation of
This test provides the assessment of caking bulk density.”
behaviour after consolidation for varying
periods of time with a specific weight. It
allows the identification of the most
appropriate flow agent for a particular
application and subsequently the
specification of addition levels to contol
clumping and crusting behaviour, and to
maintain free-flowing powders which are
easier to handle and process.
To assess the effects of different degrees of
consolidation a flat compression probe is
attached to the PFA after conditioning, and
Compression test setup
Compression probe used with split vessel Timed Powder Consolidation
the split vessel mentioned earlier is available
to help discard excess powder (after
conditioning) and leave behind a specified
volume for a bulk density measurement
before the compression test. The split vessel
adds an extra benefit of a flat pre-
compression surface once the extra powder
has been discarded, and a constant sample
volume for enhanced repeatability.
Measuring Powder and Granule Properties to anticipate problems | 6
Measuring Powder and Granule Properties
Compaction and Tabletting
Properties of Free Powder
Many industries require the use of powder
compaction during forming processes. Several
parameters may be of interest when a powder
is put under compression, and Stable Micro
Systems offer several testing solutions.
Indexable Powder Compaction Rigs
The simplest test method is the use of an
Indexable Powder Compaction Rig, allowing
low compaction force testing of multiple
powder samples. Two variations are available
that provide indexable testing of 10 samples
up to 50kg, which also serve to increase
usability and efficiency. Cavities that fit a
5mm or 0.5 inch probe are available; the
“... a more Indexable Powder Compaction Rig
free flowing
powder is less
compressible...”
larger volume allows easier sample filling but
the smaller volume may be necessary when
only small sample quantities are available.
Once the first sample is centralised with the
testing probe, subsequent samples can simply
be moved along via a ‘quick-click’
mechanism which aligns the next test ready
to go, increasing sample throughput.
Compaction properties of powders can be
assessed using target force or target distance
modes. Many powder compacts are formed to
a target distance and so this test can be used
to assess the force required to reach this
distance. However, new advances in
tabletting machines allow compression to a
target force (resulting in powder compacts
7 | Measuring Powder and Granule Properties to anticipate problems
with constant porosity). Going to a target
force using this rig will result in a
measurement of the cake’s height.
In addition, by looking at the loading, hold,
and unloading periods of a hold until time
graph (stress relaxation), the information on
compressibility (Carr Index), relaxation,
stiffness and elastic recovery can be
calculated. The loading period involves both
elastic and plastic deformation, the hold
period is generally purely plastic, and the
unloading period is generally purely elastic.
In general, a more free flowing powder is less
compressible (as the powder particles have
already flowed into a more close-packed
state). This corresponds to a small increase in
bulk density with stress and a low
Stress relaxation test result
This graph shows two stress relaxation tests in
the PFA. There is a more significant force
relaxation over the hold period in one sample.
compressibility. A more cohesive powder
tends to show the opposite behaviour and a
high compressibility.
The stress relaxation section of the force-
time curve characterises the viscoelastic
(time-dependent) behaviour of the powder
sample as compacted material undergoes
plastic deformation and moves into void
spaces. This will vary with factors such as the
shape and size of powder particles, the type
of material and the addition of lubricant. The
more viscoelastic the powder, the less spring-
like it is and the more the force will drop
during this hold period. The force usually
drops off quickly at first then tends towards
a plateau.
The initial unloading slope is a measure of compactability characteristics of a new drug
the stiffness of the compact, and the elastic substance alone and in combination with
recovery upon unloading is a function of the some of the common excipients should be
loaded and relaxed column heights. obtained as part of the preformulation
evaluation.
High and Low Tolerance Powder
A High Tolerance Powder Compaction Rig on
Compaction Rigs
the TA.HDplus Texture Analyser can be used
For a more in-depth study of a powder’s
as a compaction simulator on ‘F’ tooling sets
compaction properties using forces closer to
of different dimensions. Using the punch
those used during tabletting operations, there
attached to the load cell, the ejection force
are two additional powder compaction rigs
from the ‘F’ tooling die can also be evaluated.
available. The High Tolerance Powder
To calculate the work of compaction during
Compaction Rig is suited to high force
tabletting, it is necessary to have accurate
applications where the punch/die clearance is
values of force and punch displacement; the
critical; this fixture is auto-aligned using a
Powder Compaction Rigs provide a simple
universal adapter.
and accurate means of measuring these
The Low Tolerance Powder Compaction Rig
properties.
is suited to other powder compaction
applications such as assessing granule Low Tolerance Powder Compaction Rig “... turning to
friability, where the punch/die clearance is
less critical. As with the indexable rigs, advances in
compaction properties of powders can be
assessed using target force or target
tablet
distance modes. technology...”
Pharmaceutical companies are constantly
developing their techniques to maintain or
enhance their product offerings by turning to
advances in tablet technology, with
sophisticated excipients, extended-release
formulations, fast-dissolve tablets and self-
repairing tablets.
Such changes in tablet technology require
rigorous assessment of the effect on physical High Tolerance Powder Compaction Rig
characteristics of the excipients and finished
dosage form. Differing physical properties of
active substances and excipients may lead to
uneven distribution and alteration in drug
delivery to the target site. Testing can be
used to address homogeneity and
performance characteristics of bulk and unit-
solid dosage forms.
Tablet formulations are multicomponent
systems. The ability of such a mixture to form
a good compact is dictated by compressibility
and compactability characteristics of each
component.
Some indication of the compressibility and

Measuring Powder and Granule Properties to anticipate problems | 8

Measuring Powder and Granule Properties
Flowability of Compacted Powder
Unconfined Yield Stress
In industries that handle powders on a regular
basis it is very important to understand how
a powder or granular material responds to
pressure. In storage, the weight of powder in
a container exerts pressure on the particles at
the bottom. If the powder has good flow
behaviour, it will not consolidate and will
flow out of the silo or hopper without sticking
– this is very desirable. The longer a powder
is stored for, the more likely it is to form a
cake in its hopper and refuse to flow without
further assistance.
A good measure of a powder’s flowability is
the force required to cause it to flow. The
methods that have been described so far have
Unconfined Unconfined Yield Stress Rig results
Yield Stress Rig
Graph showing result of loading and hold
period in a stress relaxation test
“If the powder A flow function curve (A) plotted across various
regions of flow behaviour
has good flow
behaviour, it tested a powder sample that has been confined
in a vessel. One example of a simple well-
will not established method (i.e. that does not use a
Powder Flow Analyser) is the measurement of
consolidate...” unconfined yield stress. It can be used to
9 | Measuring Powder and Granule Properties to anticipate problems
analyse the flow behaviour of free-standing
powders and the change in their behaviour
with different consolidation stresses and times.
The measurement is made by filling a chosen
weight of powder sample into a tube and a
compression piston then applies a chosen
consolidation force for a specified time. After
consolidation, the tube is slid upwards above
the consolidation probe and held up via a
support disc before the probe moves back
down to compress the freestanding column
of powder, which “yields”.
Formulae are built into Exponent software
which are able to collect the required
parameters and calculate the unconfined yield
stress. Unconfined yield stress has little
meaning as a measurement in itself as it
depends on the consolidation stress (a powder
more heavily compressed is likely to flow less
freely and have a higher yield stress).
Consequently, the “flow factor” is plotted and
used to compare between samples. The larger
the flow factor, the more easily the powder will
flow after any given consolidation pressure.
Vertical Shear Strength
Another traditional textbook method of
measuring a powder’s bulk resistance to the
initiation of flow is the Powder Vertical Shear
Rig. This also helps to imitate the
consolidation that occurs under the powder’s
own weight when the outlet is shut and the
feeder is switched off. It is when the outlet is
opened and the feeder started again that the
blockages can build up.
The likelihood of a blockage forming depends
on both the properties of the powder and the
conditions surrounding it (humidity,
temperature, stress state, hopper geometry).
The vertical shear test provides a method to
test the commencement of flow of a powder
from a packed state, imitating a filled hopper.
This test can also help to determine the
correct hopper outlet size for reliable flow.
During the test, a known mass of powder is
transferred to the main body of the rig and
 Vertical Shear Strength Rig
Vertical Shear Strength Rig principle
compressed to a known force to create a
uniform cake of powder. A trapdoor below
the powder cake is released, exposing a
circular surface of the cake. A probe slightly
smaller than the hole then pushes a plug of
the powder cake through the bottom of the
rig. The powder is put into an almost perfect
shear state (where the force is parallel with
the powder movement).
Formulae are again built into Exponent
software to calculate the sample’s vertical
shear strength, along with information on the
cake height reached after the hold period,
giving a measure of compressibility.
Measuring Powder and Granule Properties to anticipate problems | 10
Vertical Shear Strength Rig result graph
“Finished
product testing
is essential...”
Testing Finished Products
Being able to measure powder and granule
flow is of prime importance to manufacturers,
but as quality standards continue to rise, few
can afford to stop there. Finished product
testing is essential to ensure correct
performance and safeguard reputation, sales
and market share.
Properties of Hard Compacts
Many final products that reach the customer
are in the form of a hard compact or “cake”.
There will be a range of optimum hardness
and friability for each product that depends
on its intended use. For example, an
eyeshadow compact that is too hard will not
yield any product on the brush, but a product
too soft may fracture during transit. Likewise,
tablets designed to be broken in half with the
hands must be strong enough to withstand
transit, but not so strong that they cannot
easily be broken by an elderly or infirm
person. There are several ways to test a
Measuring Powder and Granule Properties.

Penetration test Determination of Hardness A vast range of powders and granules

with a wide range of problems

powder compact, but the best method for any

particular product depends on its form.

Penetration
Hardness or cake strength can be determined
by means of a penetration test, attaching a
“This enables cylindrical or needle probe to the Texture
manufacturers Analyser. Results from this test provide the
force required to penetrate the sample within Don’t let your flow properties
to optimise a given distance (e.g. 1mm). Test comparisons control your fill weight
their tablet may highlight a need for weaker or stronger
binding ingredients depending on the balance
formulations...” of characteristics desired.

Bilayer Tablet Shear Rig

When it comes to tablet manufacture, bilayer
systems typically contain an immediate-
release component in one layer and the
extended-release component in the other
layer. The development and production of
quality bilayer tablets is not without issues
such as layer separation.

Bilayer Tablet Shear Rig Bilayer Tablet Shear Rig result The Bilayer Tablet Shear Rig provides the
means to assess this problem. The bilayer
tablet fits into the central cavity of a
guillotine-type blade and is then compressed
until the two components of the tablet are
sheared apart. The shear force and distance to
failure are measured. Visual characterisation
of the fracture surface is necessary to quantify
the percentage of each fracture failure mode.
This enables manufacturers to optimise their
tablet formulations for adhesion of the two
tablet components.

11 | Measuring Powder and Granule Properties to anticipate problems

Properties of Powder and Granule
Particles
In many cases, the properties of the powder
particles or granules themselves are of
interest. There are two main ways that these
can be tested – in a ‘bulk’ test in the Granule
Compaction Rig, or by testing a single particle
at a time during a cylinder compression test.
Granule testing is important to provide an
indicator of the tabletting potential of some
materials, or a measure of friability or
compaction strength of granules.
Granule Compaction Rig
This test allows the granule hardness and
compressibility to be assessed. Where granules
are irregular in form, the testing of single
Granule Compaction Rig
Granule Compaction result
Measuring Powder and Granule Properties to anticipate problems | 12
granules is discouraged as repeatability is
compromised. In this instance, the testing of a
fixed area of sample creates an averaging effect
and improves the repeatability of the results.
The Granule Compaction Rig provides a
circular testing area into which the sample is
contained before compression with a cylinder
probe of similar diameter to the testing area.
Normally, the maximum force and energy
(area under the curve) are taken and used as
an indication of hardness. The higher the
force and energy required to compress, the
more difficult it will be to form the granules
into tablets.
Cylinder Compression Test
This test can provide a means of measuring
the progressive swelling of granules under
Single Granule Compaction “... the testing
of a fixed area
of sample
creates an
averaging
effect...”
water, or can be used simply to compress (and
possibly fracture) an individual granule. If the
probe height is calibrated before the test, the
height of the granule can be recorded, which
is useful when granule dimensions are of
importance. A large number of tests must be
made to have a realistic set of measurements
as granules often vary in their geometry.
However, this type of test is very quick to
perform.
 Measuring Powder and Granule Properties
“...our expertise...
is unparalleled.”
© 2018 Stable Micro Systems
13 | Measuring Powder and Granule Properties to anticipate problems
Stable Micro Systems offers a wide range
of fixtures to accompany its market-leading
and highly customisable texture analysers,
presenting powder and granule
manufacturers with the opportunity to
produce perfectly textured products.
We can also design and manufacture probes
or fixtures for the Texture Analyser that are
bespoke to your sample and its specific
measurement. Once your measurement is
performed, our expertise in its graphical
interpretation is unparalleled.
Not only can we develop the most suitable
and accurate method for the testing of your
sample; we can also prepare analysis
procedures that obtain the desired parameters
from your curve and drop them into a
spreadsheet or report designed around your
requirements.
To find out more about any of these test
methods, contact Stable Micro Systems today.
Stable Micro Systems
Vienna Court, Lammas Road, Godalming, Surrey GU7 1YL, UK
Tel: *44 1483 427345
Fax: *44 1483 427600
Email: sales@stablemicrosystems.com
app.support@stablemicrosystems.com
tech.support@stablemicrosystems.com
Web: www.stablemicrosystems.com