Measuring and

freemantechnology
understanding
Freeman Technology Ltd Freeman Technology, Inc. Freeman Technology China
UIFnPXQSPQFSUJFT
1 Miller Court
Severn Drive
17 Wakefield Drive
Medford
Room 6102, 6/F
21st Century Tower
of powders with
Tewkesbury NJ 08055 No. 210 Century Avenue the FT4 Powder
Gloucestershire USA Pudong New Area
GL20 8DN Shanghai 200120 Rheometer ®
UK P.R.China

Tel: +44 (0) 1684 851 551

Fax:+44 (0) 1684 851 552

info@freemantech.co.uk
www.freemantech.co.uk

D/EZ/d/E

freemantechnology

Freeman Technology® is a registered trademark of Freeman Technology Ltd

Freeman FT4 8pp May15 cover.indd 1 11/05/2015 09:55

 A universal powder tester Proven applications
n
The FT4 Powder Rheometer was originally designed to Dynamic methodology The FT4 has proven application
plication in all powder Intuitive
ntuitive software and
a
The FT4 employs patented technology for measuring the processing industries, including Pharmaceuticals,
Pharmaceu
Fine Chemicals,
cals, Food, Cosmetics, Toners, Metals, flexible
xible
e accessories
accesso
This remains a primary function today, but the instrument,
Ceramics, Plastics, Powder Coatings, Cement and a
accessories and methodologies have been continuously in motion. A precision ‘blade’ is rotated and moved Additive Manufacturing.
developed to the point where the FT4 is now considered a downwards through the powder to establish a precise has
as been written in accordance
ance with CFR21 ParPart 11
universal powder tester. Applications extend
d to: guidelines.
elines. The Powder Rheometer control software
softw is
intuitive
tive and easy to use,, guiding the operator through
throug
 Filling a wizard style interface too ensure sam
sample analysis is
In addition to the patented dynamic methodology, where
uncomplicated.
complicated. d. The Data Analysis package comes
a powder's resistance to flow is measured whilst the  Tablet compression with a site licence allowing
wing data interpretation and
powder is in motion, the FT4 also includes a shear cell for  reporting
eporting to be carried out away ay from the lab, and
an by
measuring the powder's shear strength, a wall friction kit particles resist motion and the harder it is to get the  Wet granulation end point and scale up any number of onsite users. A further app application in the
in order to quantify how the powder shears against the  Flow additive selection and optimisation form of Support Documents
cuments provides on-instrumen
on-instrument,
on-instr
wall of the process equipment (in accordance with ASTM comprehensive support port on all methodologies
methodologies, data
 Humidity effects
standard D7891), and also accessories for measuring Excellent reproducibility is achieved by moving the blade interpretation, calibration and additional
na help that may
 Electrostatic charge be required.
uired
bulk properties, such as density, compressibility and in a precise and repeatable way. The advanced control
 Mixing / Blending
permeability. This range of measurement capabilities systems of the FT4 accurately set the rotational and A full range of accessories is available for the FT4,
 Feeding
makes the FT4 a truly universal powder tester and by far including
ding standard vessel sizes allowing sample
 Segregation
the world's most versatile instrument for measuring and and Tip Speed. volumes in thehe range 10ml to 160ml to be analysed.
understanding powder behaviour.  Attrition In addition, the 1ml Shear
hear Cell can be selected when
w en
 Dry powder inhalers only
nly very limited samples sizes are available. Further
 Caking
accessories es include compaction pistons, shear headheads,
wall friction kits, an aeration control unit and a uniaxia
uniaxial
ia
 Milling
tester. A calibration standard powder is also availab
available,
 Conveying if required. For a full list of available accessories,

An introduction to powders  Wall friction and adhesion

 Hopper design
please contact Freeman
representative.
reeman Technology or your local

 Compact hardness and payoff

Powders are complex materials. Often
perceived as just a collection of particles,
they are in fact a complex mixture of solids,
liquids and gases. Unlike the relatively
well understood constituent phases from
which they are derived, powders are
more complicated materials. They are
comprised of: solids in the form of particles;
gas, usually in the form of air between the
particles; and water, either on the surface
of the particle or within its structure. The
behavioural characteristics of these unique
Powder behaviour
Powders exhibit many behavioural
characteristics, which determine how they
application. These characteristics are
often independent of one another, so it is
important to understand and to be able to
is going to be fully characterised.
Powders exhibit the following behavioural
characteristics:
 shape, resulting in changes in powder
through a process, others may bridge,
 Compressibility – some are very stiff,
others observe a large change in density
when consolidated.
 Adhesivity - powders may stick to
process equipment, others slide easily.
 Permeability – the ease with which air
can be transmitted between particles
can be critical during processing and in
 Electrostatic charge – some powders
become electrostatically charged as
a result of handling and processing,
resulting in a change in their behaviour.
 Hydrophobicity – most powders
experience a change in behaviour if
humidity or water content increases, but
to varying extents.
 Particle attrition – if particles are friable
or weak, then mechanical stress Freeman Technology has over 15 5 years’ experience in
sensitivity, agglomeration and the effect of particle size the design of powder characterisation instrumentation
can result in a change in size and reduction / particle shape changes are also available.
and in powder processing applications. So working
behaviour. with Freeman Technology means more than simply
Whether your objective is to optimise a formulation purchasing an instrument. Thanks to our expertise
 Flow rate – powders will behave in a development environment, predict in-process and know-how, we provide FT4 Powder Rheometer
performance, understand batch differences, or to customers around the world with extensive and
ensure the quality of raw materials or intermediates, ongoing consultation and applications support, based
as mixing and blending. the FT4 will provide valuable and unique information on real-world experience.
that will help you address your challenges.

behaviour and often poor in-process
control.
These examples represent just a few of the
ways in which powders can demonstrate
their complex ‘personalities’. Moreover,
these properties are frequently independent
and unrelated, such that two powders
can be equally compressible, but exhibit
permeability.

Powders Solids Liquids Gases

The way these phases They can:  Behave like a single solid entity, deforming elastically and plastically
interact determines the 
behaviour of the powder.  Be compressed like gases

Freeman FT4 8pp May15 cover.indd 3 11/05/2015 09:55


The blade is rotated and moves vertically, as
It becomes easy to see why powders
cannot be described with just one or
two numbers, requiring by contrast the
measurement of a range of parameters to
achieve a thorough understanding. Each
the powder behaves within the process
environment.
For example:
 Does the powder mix properly?
 Does it consolidate into one solid lump if
left in storage or after vibration?
 A further complicating factor is that the
 Does it change its behaviour if exposed
to high humidity?

operation?
For example in relation to:
 Pharmaceutical tablet properties –
powder determines weight variability,
hardness, dissolution and stability.
 Powder coating – whether the powder
uniformly onto the panel, without
agglomerating.
 Chemical manufacturing – is this
powdered raw material too cohesive to
mix well in our process?
in-process performance and the properties
Freeman FT4 8pp May15 text.indd 1
Powder conditioning
Powders have memory, in that their behaviour and
state. If a powder has been consolidated, a proportion of
this stress will be retained after the consolidating load has
been removed. Conversely, if the powder has previously
been aerated, then excess air may exist within the powder.
This variation of stress or aeration occurs as a result of
processing and handling the powder, but also during the
preparation step in any measurement system. In order to
the measured result, the FT4 employs a unique conditioning
process that prepares the sample in a homogeneous way,
creating uniform low stress packing throughout the powder
sample and removing any stress history or excess air prior
to the measurement.
This automatic conditioning step is run before every test
and is paramount if excellent repeatability is to be achieved.
Conditioning reduces operator to operator variability
and ensures that results generated can be accurately
reproduced by a different operator, or on another instrument
in a different lab.
Understanding powder  Elasticity
 Plasticity
behaviour
 Porosity
The particle physical and chemical  Potential for charge
properties determine the behaviour of the
 Hardness / Friability
powder to a large extent, but so too does
the environment in which the powder is  Hygroscopicity
being handled (external variables).  Amorphous content
Particle properties Some of these properties can be measured
The particles alone are complex and rarely directly, whilst others are more challenging.
All will contribute to the way the powder
Particle size distribution has traditionally behaves.
been considered, and it remains important,
but in fact there are many particle properties External variables
the powder, namely: behaviour of the powder will depend on
the environmental conditions to which it is
 Particle size and distribution exposed. If consolidated, its properties will
 Shape be very different to if it is loosely packed or
 Surface texture
even aerated.
 Surface area In each of these images, the physical and
 Density chemical properties of the particles are the
 Cohesivity
different, simply as a result of changing the
 Adhesivity air content and contact stresses between
the particles.
13/05/2015 14:57
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Freeman FT4 8pp May15 text.indd 2 13/05/2015 14:57

 Accuracy
Excluding either Torque or Force signals would result in
misleading data, as the calculated Flow Energy value would not

Due to the rotational nature of the technique, approximately

Using the calculation of Work Done, it is possible to
represent both resistances as a total energy, the energy
required to move the blade through the powder from the
top to the bottom of the powder column. However, as
the blade travels through the powder the values of torque
and force are constantly changing, so it is necessary to
frequently calculate the energy required to move through
the powder over very small distances travelled. This is the
90% of the total resistance is contributed from the Torque
signal, with the remaining 10% from the Force component.
This highlights the importance of measuring Torque as well as
Force when evaluating rheological properties.
Total Flow Energy = Area under curve

Energy Gradient mJ/mm

calculation of Energy Gradient, the energy measured for
each millimetre of blade travel, expressed in mJ/mm.

Work Done = Energy = (Resistance x Distance travelled)

where ‘Resistance’ is the combined Torque and Force

Energy Gradient = Energy per mm of blade travel

Calculating the area under the Energy Gradient curve

provides the Total Flow Energy, representing the powder’s H1 Height H2
Energy Gradient is calculated directly from the
measurements of Torque and Force

Completing the picture

In addition to the dynamic Axial compression
methodology, where the blade is A ‘vented piston’ can be applied to the
top of the powder column in order to
FT4 utilises other accessories and consolidate the
operating modes to fully characterise powder under
your powders. a controlled
and precise
Aeration normal stress.
The Aeration Control Unit is a device
that provides a precise air velocity to
the base of the vessel containing
the powder. A wide range of
velocities is available and the device
communicates automatically via USB Rotational shearing
with the FT4 computer. Shear Cell and Wall Friction Modules
can be attached to the FT4 and used
Air in Air in to measure the shear strength of the
Aeration test Permeability test powder and the wall friction between
the powder and a particular wall
Air can also be introduced whilst the material (in accordance with ASTM D7891).
powder is being consolidated using A controlled normal stress is applied,
the vented piston. For a given air then rotation occurs to induce
velocity and applied consolidating shearing. The greater the resistance,
stress, the air pressure measured at the higher the shear strength.
the bottom of the powder column

powder to transmitting air between

the particles. The more resistant
the bed, the greater the measured
air pressure and the lower the
permeability.

The introduction of air into the base Controlled force

of the powder during a dynamic test (Normal stress)
allows the Aerated Energy to be
Rotation
(Shear stress)
becomes aerated, a property that is
directly related to the cohesive Glass vessel
strength of the powder. containing powder

Freeman FT4 8pp May15 text.indd 3 13/05/2015 14:57

 Methodologies
The FT4 Powder Rheometer is a truly
universal powder tester, with four Bulk

FT4 Universal Powder Tester

Density Compressibility Permeability

as Bulk, Dynamic Flow, Shear, and

Process. Dynamic Flow
Basic Flowability Aeration Consolidation Flow Rate Specific Energy

Shear
Shear Cell Wall Friction

Process
Segregation Attrition Caking Electrostatics Moisture Agglomeration

Basic flowability – measuring the dynamic flow properties of powders in Shear Cell – quantifying a powder's shear strength in accordance with
a conditioned state. ASTM standard D7891. For understanding behaviour in hoppers, and
 Flow additives for use in hopper design exercises. Sample sizes down to 1ml.
 Wet granulation end point 
 Moisture content  Flow function
 Attrition / Segregation  Cohesion
 Physical properties (particle size, shape, surface texture, etc)  Angle of Internal Friction
 Electostatic charging

Wall Friction - measuring the friction acting between a powder and

equipment surfaces in accordance with ASTM standard D7891. Also
required for hopper design.
Aeration – a direct measurement of a powder’s cohesive strength.  Measure friction between powder and surface material
  Hopper, IBC, Punch, Die wall
 Dosing / Mass uniformity  Wall friction angle for hopper design
 Aerosolisation / DPI
 Fluidisation behaviour
 Blending / Mixing
 Segregation potential

Compressibility – determining changes in a powder’s density as a result

of a directly applied consolidating load.
 Transportation
 Storage
 Hoppers
 Kegs
 Processing
 Tablet

compression
 Roller

Consolidation – understanding the effect of direct consolidation or compaction

vibration on powder flow properties.  Screw feeding
 Direct pressure  Extrusion
 Tapped

Understanding the effects of:

 Transport
 Storage
 Processing
 Caking Permeability – measuring the resistance to air flow between particles and
through the powder bed.
 Tablet cappingg / Lamination
 Aerosolisation
n / DPI

 Compression
 Pneumatic
transfer

Freeman FT4 8pp May15 text.indd 4 13/05/2015 14:57

 A universal powder tester Proven applications
n
The FT4 Powder Rheometer was originally designed to Dynamic methodology The FT4 has proven application
plication in all powder Intuitive
ntuitive software and
a
The FT4 employs patented technology for measuring the processing industries, including Pharmaceuticals,
Pharmaceu
Fine Chemicals,
cals, Food, Cosmetics, Toners, Metals, flexible
xible
e accessories
accesso
This remains a primary function today, but the instrument,
Ceramics, Plastics, Powder Coatings, Cement and a
accessories and methodologies have been continuously in motion. A precision ‘blade’ is rotated and moved Additive Manufacturing.
developed to the point where the FT4 is now considered a downwards through the powder to establish a precise has
as been written in accordance
ance with CFR21 ParPart 11
universal powder tester. Applications extend
d to: guidelines.
elines. The Powder Rheometer control software
softw is
intuitive
tive and easy to use,, guiding the operator through
throug
 Filling a wizard style interface too ensure sam
sample analysis is
In addition to the patented dynamic methodology, where
uncomplicated.
complicated. d. The Data Analysis package comes
a powder's resistance to flow is measured whilst the  Tablet compression with a site licence allowing
wing data interpretation and
powder is in motion, the FT4 also includes a shear cell for  reporting
eporting to be carried out away ay from the lab, and
an by
measuring the powder's shear strength, a wall friction kit particles resist motion and the harder it is to get the  Wet granulation end point and scale up any number of onsite users. A further app application in the
in order to quantify how the powder shears against the  Flow additive selection and optimisation form of Support Documents
cuments provides on-instrumen
on-instrument,
on-instr
wall of the process equipment (in accordance with ASTM comprehensive support port on all methodologies
methodologies, data
 Humidity effects
standard D7891), and also accessories for measuring Excellent reproducibility is achieved by moving the blade interpretation, calibration and additional
na help that may
 Electrostatic charge be required.
uired
bulk properties, such as density, compressibility and in a precise and repeatable way. The advanced control
 Mixing / Blending
permeability. This range of measurement capabilities systems of the FT4 accurately set the rotational and A full range of accessories is available for the FT4,
 Feeding
makes the FT4 a truly universal powder tester and by far including
ding standard vessel sizes allowing sample
 Segregation
the world's most versatile instrument for measuring and and Tip Speed. volumes in thehe range 10ml to 160ml to be analysed.
understanding powder behaviour.  Attrition In addition, the 1ml Shear
hear Cell can be selected when
w en
 Dry powder inhalers only
nly very limited samples sizes are available. Further
 Caking
accessories es include compaction pistons, shear headheads,
wall friction kits, an aeration control unit and a uniaxia
uniaxial
ia
 Milling
tester. A calibration standard powder is also availab
available,
 Conveying if required. For a full list of available accessories,

An introduction to powders  Wall friction and adhesion

 Hopper design
please contact Freeman
representative.
reeman Technology or your local

 Compact hardness and payoff

Powders are complex materials. Often
perceived as just a collection of particles,
they are in fact a complex mixture of solids,
liquids and gases. Unlike the relatively
well understood constituent phases from
which they are derived, powders are
more complicated materials. They are
comprised of: solids in the form of particles;
gas, usually in the form of air between the
particles; and water, either on the surface
of the particle or within its structure. The
behavioural characteristics of these unique
Powder behaviour
Powders exhibit many behavioural
characteristics, which determine how they
application. These characteristics are
often independent of one another, so it is
important to understand and to be able to
is going to be fully characterised.
Powders exhibit the following behavioural
characteristics:
 shape, resulting in changes in powder
through a process, others may bridge,
 Compressibility – some are very stiff,
others observe a large change in density
when consolidated.
 Adhesivity - powders may stick to
process equipment, others slide easily.
 Permeability – the ease with which air
can be transmitted between particles
can be critical during processing and in
 Electrostatic charge – some powders
become electrostatically charged as
a result of handling and processing,
resulting in a change in their behaviour.
 Hydrophobicity – most powders
experience a change in behaviour if
humidity or water content increases, but
to varying extents.
 Particle attrition – if particles are friable
or weak, then mechanical stress Freeman Technology has over 15 5 years’ experience in
sensitivity, agglomeration and the effect of particle size the design of powder characterisation instrumentation
can result in a change in size and reduction / particle shape changes are also available.
and in powder processing applications. So working
behaviour. with Freeman Technology means more than simply
Whether your objective is to optimise a formulation purchasing an instrument. Thanks to our expertise
 Flow rate – powders will behave in a development environment, predict in-process and know-how, we provide FT4 Powder Rheometer
performance, understand batch differences, or to customers around the world with extensive and
ensure the quality of raw materials or intermediates, ongoing consultation and applications support, based
as mixing and blending. the FT4 will provide valuable and unique information on real-world experience.
that will help you address your challenges.

behaviour and often poor in-process
control.
These examples represent just a few of the
ways in which powders can demonstrate
their complex ‘personalities’. Moreover,
these properties are frequently independent
and unrelated, such that two powders
can be equally compressible, but exhibit
permeability.

Powders Solids Liquids Gases

The way these phases They can:  Behave like a single solid entity, deforming elastically and plastically
interact determines the 
behaviour of the powder.  Be compressed like gases

Freeman FT4 8pp May15 cover.indd 3 11/05/2015 09:55

 FT4 Specifications

SYSTEM:- ENVIRONMENTAL CONDITIONS: -

FT4 Powder Rheometer intended for use in a laboratory Humidity range 20-80% non-condensing
environment for measuring the rheological properties of Temperature range (operating) 10˚C to 40˚C
powders, pastes and semi-solids. Temperature range (storage) 0˚C to 50˚C
Complies with the following EMC specifications and ASTM
International standards: VESSELS: -

 EN61000-3-2:2001 Precision bore, borosilicate glass tube.

 EN61000-3-3: 1995 Standard sizes:-
 EN61326: 1997 + A2:2001 25mm x 10ml Split Vessel
 ASTM D7891 25mm x 25ml Split Vessel
Certificates of conformity available on request. 25mm x 35ml Vessel
50mm x 85ml Split Vessel
PERFORMANCE: -
50mm x 160ml Split Vessel
50mm x 260ml Vessel
Force +/- 50N maximum
0.0001N resolution 62mm x 137ml Split Vessel
Torque +/- 900mNm maximum 62mm x 240ml Split Vessel
0.02mNm resolution 62mm x 400ml Vessel
Vertical travel 185mm
Rotor speed 120 rpm maximum
Axial speed 30 mm/sec maximum BLADES: -
Residual energy level in air < 2mJ
Hardened stainless steel.
Standard sizes:-
COMPUTER SPECIFICATION: - 23.5mm diameter x 6mm wide
48.0mm diameter x 10mm wide
The instrument incorporates an integrated high specification 60.0mm diameter x 10mm wide
processor and operates on a Microsoft Windows Embedded
operating system. It has built in networking capability and a
universal serial bus to provide serial daisy chaining of all CALIBRATION KIT: -
automated accessories.
Force, torque, height, carriage velocity and spindle speed are
CONSTRUCTION: - configured for calibration.

Working zone: 316 stainless steel Calibration fixtures, weights and height gauges are supplied as part of the
Contact parts: 316 stainless steel calibration kit.

Borosilicate glass
A calibration log is automatically kept of the current and all
Delrin and Peek plastics
previous calibrations.

DIMENSIONS: -
ACCESSORIES: -

Main instrument 306 x 306 x 760mm high

25mm Accessories Kit
50mm Accessories Kit
WEIGHTS: -
62mm Accessories Kit
Aeration Control Kit
Main instrument 22kg net 24mm Shear Cell
48mm Shear Cell
24mm Wall Friction Kit
POWER REQUIREMENTS: - 48mm Wall Friction Kit
1ml Shear Cell
Supply voltage range: 90 to 264VAC
Input current range: 1.6A at 120VAC
0.8A at 230VAC SOFTWARE: -
Input frequency range: 47Hz to 63Hz
All Control and Data Acquisition Software is supplied and
configured with the instrument and includes Microsoft Office
 Measuring and
freemantechnology
understanding
Freeman Technology Ltd Freeman Technology, Inc. Freeman Technology China
UIFnPXQSPQFSUJFT
1 Miller Court
Severn Drive
POWakefield
17 Box 2022Drive
Wayne
Medford
Room 6102, 6/F
21st Century Tower
of powders with
Tewkesbury Southeastern
NJ 08055 No. 210 Century Avenue the FT4 Powder
Gloucestershire PA 19399
USA Pudong New Area
GL20 8DN USA Shanghai 200120 Rheometer ®
UK P.R.China

Tel: +44 (0) 1684 851 551

Fax:+44 (0) 1684 851 552

info@freemantech.co.uk
www.freemantech.co.uk

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0687465556/7 www.
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D/EZ/d/E

freemantechnology

Freeman Technology® is a registered trademark of Freeman Technology Ltd

Freeman FT4 8pp May15 cover.indd 1 21/08/2015 13:49