Carr indices, attrition and abrasion yield again.

With free flowing material

Handling of powders and granular resistance in a rotating drum or the shearing of the material is easily
materials is of great importance to repeated impact tester and dustiness performed. With cohesiveness
industry. In 80% of the industry these by a rotating drum according to materials the initiation of flow is more
materials are involved. In the chemical Heubach or EN 15051 methodologies. difficult. Jenike’s method is the most
industry alone, half of the products common method to measure powder
and at least 75% of the raw materials Dr Schleuniger flow properties after steady-state
are in the form of powders and The tablet hardness tester measures flowing. The methods apply the history
granular solids. the crush strength axial or radial of a to the powder by consolidation after
single pellet and tablet, directly in which the resulting strength is
In any particulate process, the physical Newtons (N), Strong Cobbs (Sc), measured. In this way the situation in a
characteristics of powder and granular Kiloponds (Kp), or Pounds Apothecary silo or hopper is simulated, in which
material e.g. cohesiveness, density, (Lb), in a hardness range of 0 – 400 N. the powder undergoes a certain history
compressibility, particle size distributi- A motorized test jaw drives continuous of shear and consolidation in the top
on, particle shape and humidity have forward increasing the pressure giving it strength when it reaches the
an effect on the flowability and applied to the pellet, tablet, capsule, bottom of the silo or hopper.
floodability of the bulk material. etc. The pressure is monitored and at With the Jenike tester internal friction
Also, solid particles and granules wear the moment of breakage the reduction and wall friction on various wall
down during production, handling and in resistance recognized with the surfaces can be measured. A sample is
transport. The forces particles undergo highest value just before as breakage placed in a shear cell of specific
are broadly classified into impact strength. dimensions. The specimen is pre-
forces, compressive forces and consolidated by twisting the cell cover
abrasive forces. Compressive forces Robotic Compression Tester according while applying a compressive load
tend to occur in hoppers, conveying to Pitchumani normal to the cover; subsequently with
systems, silos and on truck or rail The Robotic Compression Tester (RCT) a normal load to the cover the
where the particles are compressed by measures the maximum crushing force specimen is presheared until a steady
their own weight. of individual particles or granules. The state and finally by shearing in
Compressive forces can cause fragmen- crushing force of particles with size horizontal direction under a reduced
tation of particles, a process whereby a ranging from 500 µm to ≈ 4000 µm can load until the shear force goes through
particle splits into smaller parts, usually a maximum value.
be measured. About 40 up to 200
large in number and including a range The rotational split level shear tester
particles are placed on a smooth finely
of sizes of daughter particles this designed by Peschl rotates the
polishes stainless steel plate and the
sometimes results in the release of powder over itself producing a torque
coordinates of each particle and size
enclosed material. Abrasion causes from which the shear stress can
determined by a CCD camera.
dust and segregation has an impact on be calculated.
Consecutively all particles at the known
the quality of the powder material. Consolidation pressures up to 16, 30
coordinates are crushed and the
required force measured with a quartz and 50 kPa, respectively are applica-
A range of different techniques is ble by Jenike, up to 2.5 kPa by Peschl
available for characterizing bulk force transducer. The highly sensitive
transducer is suitable for measuring and for the Brookfield 0.6 - 4.85 kPa
powder behavior and testing. Single
quasi-static and dynamic tensile and with the large ring cell and 1.6 - 13.3
pellet crush strength for radial and
kPa with the small ring cell.
axial crush of pellets and tablets, Delft compressive forces ranging from a few
mN to 80 N. The data points, (maximum shear vs
robotic compression technique for
load) result in a yield locus with two
particles and granules, shear testing
according to Jenike, Peschl or Schulze, Jenike, Peschl Shear or Ring Shear Mohr circles. Several sets of Mohr
Delft compact strength test after (Brookfield) Testing circles result in a flow function which
uniaxial compaction, powder After storage of powder the intention is visualizes the powder flow behavior
characteristics using Hosokawa for usually to make the powder flow or and as such can be used to compare

SOLIDS-
SOLIDS-SOLUTIONS.COM

The flow characteristics of various
powders upon to a certain stress. The
flow function is categorized into 5
different categories: free flowing, easy
flowing, cohesive, very cohesive and
non-flowing. Also the effective angle of
internal friction, the exit opening and
angle of a hopper or silo can be
calculated.
Compact Strength Tester according to
Van der Kraan
The technique measures the strength
of consolidated powder after uniaxial
compaction. The force at failure is
measured as a function of the surface
ratio and is suitable for processes
which don’t involve steady state
shearing as for storage of powders in
silos but for problems in powder
technology for which the construction
of the flow function is not
representative like caking behavior,
tabletting at low stresses, storage in big
bags, trains, mixers or storage in any
container in which the compaction of
the powder is governed mainly by its
own weight.
Hosokawa Powder Characteristics
Tester (Carr Indices)
Bulk powders are characterised by
seven mechanical measurements and
three supporting measurements. This
provides a numerical evaluation of the
characteristics of a powder by deter-
mining the flowability and floodability
at the transition points when
transferred from a static to a dynamic
state. The measured values are
assigned to indices based on
standardised analysis of about 3000
different bulk materials by R.L. Carr.
The ‘Angle of repose’
measurement characterises the
flowability of a material.
‘Compressibility’ testing indicates the
difference between the aerated and
the packed density of material, with
low compression indicating good
flowability.
‘Angle of spatula’ indicates the relative
angle of internal friction of the bulk
powder.
The ‘Angle of fall’ alters the angle of
Delft Solids Solutions B.V. • Molenweer 2 B • 2291 NR Wateringen • The Netherlands • +31 174 271 460 • info@solids-solutions.com
Bulk Powder Behavior
gradient of the cone or heap of materi- handling of powders, granules, tablets,
al by applying vibration. etc. These emissions tend to generate
‘Dispersibility’ indicates the fugacity, human diseases or cause other
dusting and flushing characteristics of environmental effects..In the Heubach
the powder. assessment of the dustiness potential,
‘Angle of difference’ is the difference handling and conveying is simulated by
between the angle of repose and the the rotation of the drum in which the
angle of fall, a large value indicates that sample has been placed. The dust
the material has the characteristics of released from dropping materials is
flushing. conducted by an air flow to a sampling
Supporting measurements are ‘Aerated section where it is preseparated
bulk density’, ‘Packed bulk density’ and aerodynamically and the airborne
‘Uniformity’. particles are deposited onto a filter.
The particulates are quantified or can
Attrition and Abrasion be used for further analyses.
Rotating drum Stauber-Heubach is an adaptation of
The test method covers the attrition Heubach and is focused on the dusting
and abrasion resistance of tablets, potential of feed premixes and
extrudates, spheres and irregularly additives.
shaped particles of 1.6 mm up to 19 EN 15051 is the general standard
mm. A sample is rotated for a set specifying apparatuses and reference
methods for the production of dust
period of time in a cylindrical drum
having a single baffle. The fines from bulk materials and the
produced by attrition and abrasion are measurement of the inhalable,
determined by sieving through a thoracic and respirable fractions of
standard sieve. The values obtained are dust.
significant principally in relation to
Segregation
values for other materials.
Segregation can affect final product
quality e.g. tablet-to tablet variation of
Repeated Impact Tester according to the active ingredient in pharmaceuti-
Pithumani cals. Tendencies of powders and dry
The Repeated Impact Tester (RIT) bulk solids for segregation are
basically consists of a box filled with an simulated by means of the fluidization
amount of particles or granules. mechanism or the sifting segregation
mechanism. In fluidization segregation
A motor is driving a shaft which is
(ASTM D 6941), controlled fluidization
connected with a plate confined
between two steel rods. On the plate a is used to potentially cause vertical
segregation, fine particles will
box with a sample is mounted. The
accumulate near the top and large
plate is allowed to slide over the steel
and or dense particles will settle to the
rods by two linear ball splines, only in
vertical direction. The confined motion bottom. Sifting segregation is
prevents acceleration in the horizontal investigated by a controlled emptying
direction and only forces in the normal of a first hopper into a second hopper
direction are transferred. After the test (ASTM D 6940). Subsequently, the
second hopper with the potentially
only the mass of half the original
particle size is determined as function segregated material is emptied thereby
collecting different fractions. The
of the number of collisions in the RIT.
difference in properties of the variously
collected fractions is an indication for
Dustiness according to Heubach, Stau- segregation and can be evaluated by
ber-Heubach and EN 15051-2 and -3 particle size distribution and skeletal
Heubach according to DIN 55992 is the density, but also by other possible
European standardized method for the differences e.g. color, reactivity or
determination of dust generated by the concentration of a certain component.