W INSTRUCTION Stability Method W7011

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Overview

It is recommended that before starting a complete range of measurements, a simple analysis is carried
out to understand whether the powder being characterised is going to be changed as a result of being
tested.

For example, a friable powder that is prone to attrition (breaking down of particles) under the stresses
imposed during flow, can exhibit different flow properties at the start of the test to those at the end,
due to the changes in particle size and particle shape.

Instability may occur for other reasons also and powders that are cohesive and compressible may
become caked or agglomerated during flow and as a result change their flow properties during a
series of tests.

Therefore, the recommend starting point when measuring a powder for the first time is the Stability
(Rep) program, which runs the powder through a series of identical measurements. If the powder is
stable, then the result from each measurement is similar, however, if the powder changes for any
reason then a trend reflecting this change is usually observed.

Stability (Rep) Test Sequence

The standard Stability Test is a combination of Conditioning and Test cycles, designed to assess if the
powder is going to change as a result of being made to flow. Therefore, unlike other test programs,
this test does not intentionally introduce a variable, such as flow rate or air velocity. Hence, any
change in the flow energy during the test has to be a result of the powder flow properties changing.
The size of this change describes how unstable the powder is and the direction of the change
(increase or decrease in energy) indicates the possible causes.

The structure of the Stability test program is defined below.

Start C Split

C T C T C T C T C T C T C T End

Where

C = Conditioning Cycle

T = Test Cycle

Split = Splitting of vessel to provide precise volume of powder for measurement.

Powder mass is automatically recalculated after splitting.

All test cycles are at 100mm/s blade tipspeed.

Note that graphical data represents the total energy from each downward test traverse only. Whilst
data is recorded during the conditioning cycles, it is not usually analysed graphically.

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Typical Data

Total energy consum ed during test, mJ

Total energy consum ed during test, mJ

Total energy consum ed during test, mJ

1 2 3 4 5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 7

Test number Test number Test number

Stable Unstable Unstable

Energy Test 7
Stability Index, SI =
Energy Test 1

SI ≈ 1 SI > 1 SI < 1

Robust material, not affected Powder affected by being Powder affected by being
by being made to flow. made to flow. Possible made to flow. Possible
causes are: - causes are: -

• De-aeration • Attrition
• Agglomeration • De-agglomeration
• Segregation • Over blending of an
• Moisture uptake additive
• Electrostatic charge • Coating of vessel and
blade by additive

In the event that the powder is unstable, it is recommended that the cause of the instability is
understood.

Some powders may have an SI > 1 due to a de-aeration effect. Others may have a similar trend with
an SI > 1 also, but for a different reason, such as segregation.

Understanding which factors contribute to the trend observed needs to be gained with reference to
what is known about the powder. For example, if the particles are small and the powder bulk
cohesive, then it is possible that the powder may become agglomerated, de-aerated or caked.
However, if it is known that the powder has a wide particle size distribution, it is possible that the
instability is due to segregation, rather than agglomeration.

Small changes (0.9 < SI < 1.1) are normal for most powders and are to be expected. It is
recommended that further work be carried out to understand an unstable characteristic only if the SI is
outside this range.

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For unstable powders, the stabilised energy of test 7 is normally taken as the Basic Flowability
Energy, BFE.

Basic Flowabilit y Energy , BFE = Energy Test 7 ( mJ )

However, if the powder is stable, then the energy of test 1 could be taken and for future tests, the
stability test could be reduced in length.

Other parameters measured during this test program are: -

(Up Energy Cycle 6 + Up Energy Cycle 7 )

Specific Energy, SE = 2 (mJ / g )
Split Mass

Split Mass
Conditioned Bulk Density, CBD = ( g / ml )
Split Volume
Note that Up Energy refers to the energy measured on the upward traverse of the cycle. The
energies in the BFE and SI equations are calculated from the downward traverse of the blade, from
the top of the powder column to the bottom. See Basic Flowability Energy and Specific Energy
definitions for more information.

Test Programs and Accessories

Depending on the sample size available, the following Test Program, Blade and Vessel combination
should be chosen.

Vessel Size Standard Program Name Starting Accessory Vessel

25mm 25mm_1C_Split_Rep_-5 23.5mm Blade 25mm x 25ml Split Vessel

50mm 50mm_1C_Split_Rep_-5 48.0mm Blade 50mm x 160ml Split Vessel

62mm 62mm_1C_Split_Rep_-5 60.0mm Blade 62mm x 240ml Split Vessel

Note: - a Stability program can be combined with a Variable Flow Rate study for a more thorough
analysis (see W7013 - Stability & Variable Flow Rate).

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How to Run a Stability (REP) Test

Decide which Vessel Size to use, based on availability of sample

Select the Test Program

Assemble the Split Vessel

Insert the Blade into the FT4

Enter the Material Information

Fill the Vessel with powder

Attach the Vessel to the FT4

Close the Safety Door

Start the Test

After the first conditioning cycle, the FT4 will Park and a message box will appear.

Follow the instructions to Split the vessel.

Remember to return the Vessel to the closed position.

Close the Safety Door and click OK to continue.

The program will continue automatically.

Once complete, the FT4 will park and the data can be saved.

Any notes that wish to be saved with the test file can be added before saving.

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How to Analyse Data from a Stability (Rep) Test

The standard Stability test is described in the previous pages and is constructed from a series of 7
pairs of conditioning and test cycles.

Below are a few example questions that may arise when analysing the generated data.

1) Why is the powder not stable?

Referring to “Typical Data” on page two above, it can be seen that Stability is quantified by
looking at the change in energy between Test 1 and Test 7.

Unfortunately there is no single factor that causes instability and what may be responsible for
instability in one powder may be of little significance in another material. The clue to
interpreting the result is in analysing what is known about the powder in terms of its physical
properties, for example size distribution, shape, hygroscopicity, particle hardness etc.

For example, if a powder has a wide particle size distribution or is bimodal, it is possible that
segregation could occur during flow, resulting in an unstable powder. However, if the powder
consists of similarly sized, but irregular and friable particles, segregation is less likely and any
instability is more likely a result of attrition of the friable particles, something that is accelerated
by the higher stresses between particles as a function of the irregular shape.

The list below highlights some of the more frequent causes of an SI > 1

• De-aeration

Usually occurs in cohesive powders with low bulk density. The powder bulk contains a
relatively high proportion of air due to the inefficient packing of the particles and when
made to flow, air is squeezed from the bulk and the density increase causing more
particle-particle shearing. The result is an increase in energy over the seven tests and
an SI > 1.

• Agglomeration

Normally occurs in cohesive powders. Agglomerates can form as primary particles are
encouraged to flow relative to one another. Strong cohesive and adhesive forces
promote particle attraction and agglomerates are formed. The increase in density and
“particle” size results in an increasing energy during the Stability test and an SI > 1.

• Segregation

Many powder blends and some bulk materials consist of a wide particle size
distribution. Simply causing the powder to flow can cause the particles to segregate as
a function of size. It is common that large particles migrate to the top of the powder
bulk whilst the smaller ones “sink” to the bottom under gravity (filling voids between
large particles). This segregation effect usually results in an increase in energy during
the Stability test, although it is possible that the energy reduces as the powder
segregates (as other factors like the shape of the two component parts may also
contribute to the flow energy).

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• Moisture Uptake

Powders that are hygroscopic may take on moisture during the test. As a result, the
particles may swell in size and/or the surface frictional forces may increase due to
moisture adhering to the surface of the particles. Both these physical property changes
will cause the energy to increase during the Stability test.

• Electrostatic Charging

For materials that are particularly low in moisture content or chemically prone to
electrostatic charging, forces between the particles may increase during the Stability
test, resulting in higher flow energies. Tribo-charging, which results from rubbing
particles together to generate electrostatic forces of attraction is the most common form
of changes in charge.

The list below highlights some of the more frequent causes of an SI < 1

• Attrition

This is a process of changing the physical size and shape of particles through
mechanical stress. For particles that are friable and brittle, it is likely that the stresses
observed during flow cause the particles to break apart and change in size and shape.
In the majority of cases, the flow energy reduces as particles become smaller and more
rounded and hence a reduction in flow energy is seen during the Stability test, resulting
in an SI < 1. However, it is possible, but less likely that previously smooth or spherical
particles become more angular during attrition and cause an increase in energy and an
SI > 1.

• De-agglomeration

This is a similar effect to Attrition, as described above, however during de-

agglomeration it is the agglomerates that are broken down through mechanical stress
and rarely the primary particles.

• Over blending / continued blending of a flow additive

Many powder blends and bulk materials contain a flow additive in order to enhance flow
properties during handling and processing. Whether the additive is a fumed silica or a
stearate, the objective is to reduce particle – particle friction and improve flowability.
The efficiency of the additive is partly dependant on how uniformly it is distributed within
the powder bulk and in some cases this homogeneity has not been reached during the
blending stage. If the sample being measured in the Stability test had not reach a
homogeneous level during blending, then continued distribution of the additive can
occur during the test, resulting in a reducing flow energy and an SI < 1.

• Coating of the blade and vessel

Powders that contain flow additives and flow enhancing materials like magnesium
stearate are prone to contaminating any surface they come into contact with. In many
cases, such as tablet manufacture, the primary reason for the addition of magnesium
stearate is to reduce the friction coefficient between the tablet and the die wall during
tablet ejection. It is therefore no surprise that when a material that contains magnesium
stearate is made to flow in the Powder Rheometer test vessel, it coats the blade and
vessel walls resulting in reduced friction properties and lower energy. In fact, the rate
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at which the energy reduces and the overall reduction in energy during the Stability test
can provide information about how effective the additive is and whether an optimum
amount has been identified.

2) How to interpret Basic Flowability Energy, BFE (mJ)

The Basic Flowability Energy is defined as the energy required to promote flow in a conditioned
and stable powder. It is usually taken as Test 7 of the Stability Test. It is dependant on many
physical properties such as particle size, shape density etc. A detailed explanation of the BFE
can be found in document W7030 Basic Flowability Energy.

3) How to interpret Specific Energy, SE (mJ/g)

The Specific Energy is a dynamic measurement, similar to the BFE. However, the major
difference is that the energy is derived when the blade is moving upwards, from the bottom of
the powder to the top. A detailed explanation of the SE can be found in W7031 Specific
Energy.

4) How to interpret Conditioned Bulk Density, CBD (g/ml)

The Conditioned Bulk Density is a density measurement of the powder when in its conditioned
state. For further information see W7007 Density.

5) How to interpret erratic or unconventional data

The data below shows two powders that have each been measured using the Stability test. In
both cases, the overall stability (as defined by the SI) is fairly close to unity (SI = 1) and the
BFE’s (energy of test 7) are similar.

However, what is obvious about these two data sets is that the profile of Figure 1 is much
smoother than that of Figure 2, and therefore there is clearly some behavioural differences
between these two materials that is not being described by the SI or the BFE.
Total energy consumed during test, mJ
Total energy consumed during test, mJ

1 2 3 4 5 6 7 1 2 3 4 5 6 7

Test number Test number

Figure 1 Figure 2

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Unlike the smooth nature of the energy profile in Figure 1, suggesting the powder is behaving
in a similar way during each of the 7 tests, Figure 2 shows that the flow properties for this
powder are changing from test to test.

As described previously, the conditioning process is designed to create a homogenised

packing state and uniformity in the powder, however, if the material is particularly cohesive or
adhesive then large agglomerates can readily form simply as a result of inducing flow in the
powder.

Therefore the cause of this instability is the continuous formation and breaking down of
relatively large agglomerates and as a result, the material is rarely the “same” in each of the
test cycles. This erratic behaviour is most common with very cohesive or “sticky” powders.

6) What happens if the powder does not stabilise during the Stability test?

The standard Stability program is a combination of 7 conditioning and test cycles. Most
powders will stabilise during this sequence, however sometimes it will be necessary to extend
the length of the stability program to accurately characterise a powder that takes longer to
reach stability.

Figure 3 below shows data from a stability test where the powder sample has become stable
as described by the similar energies of tests 4 to 7.

This is not the case for the powder in Figure 4, which continues to decrease in energy and
shows no sign of stabilising by test 7.
Total energy consumed during test, mJ

Total energy consumed during test, mJ

Total energy consumed during test, mJ

1 2 3 4 5 6 7 1 2 3 4 5 6 7 1 2 3 4 5 6 7 8 9 10 11 12

Test number Test number Test number

Figure 3 Figure 4 Figure 5

Therefore, in order to fully quantify the instability of the powder in Figure 4, it is necessary to
extend the number of cycles in the Stability test. This can be done by editing the standard
Stability test program using the Program Editor.

As a first step, it is recommended that the standard program is increased in length from 7 to 12
cycles. If necessary, the program can extended further if the powder does not reach stability
using the 12 cycle program.

Figure 5 above shows the results of the increased stability program. Here the data shows that
stability was reached by test 9, although test cycles 10 and 11 were needed to confirm stability
had been reached.

A powder is considered stable when a minimum of 3 test cycles produce similar energies. For
powders that have a smooth profile, 2 consecutive similar energies may be considered enough
to conclude stability has been reached.

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