Professional Documents
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Flowability
James K. Prescott* and Roger A. Barnum
S
everal pharmaceutical processes, propriate test methods to the typical
including blending, transfer, stor- pharmaceutical applications in which
age, feeding, compaction, and flu- interparticle motion occurs and powder
idization, involve powder handling. flowability is of concern, manufacturers
JENIKE & JOHANSON, INC.
(The term powder is used predominantly can decide which test methods best pre-
throughout this article, but these concepts dict the flow behavior that will occur in a
also apply to other bulk solids — fine and given application. (References 1–10, 34,
coarse — such as dust, granulations, and and 36 describe some test methods, in-
granules either as single substances or as cluding the strengths and weaknesses of
multicomponent blends.) The flow of particular testers.)
powder during manufacturing dictates
The term powder flowability is the quality of the product in terms of its Flowability defined
used loosely and has generally weight and content uniformity. Flow also A simple definition of powder flowability
been more closely associated to affects manufacturing efficiency, because is the ability of a powder to flow. By this
the test method used to measure it can determine whether bins can be used definition, flowability is sometimes
it than the significance to the or hand scooping will be required, to what thought of as a one-dimensional charac-
extent product (if any) is scrapped at the teristic of a powder, whereby powders can
process. To the formulator, beginning or end of the run, and the al- be ranked on a sliding scale from free-
flowability is linked to the lowable production rate of product (e.g., flowing to nonflowing. Unfortunately, this
product. To the engineer, blend times and compression speeds). simplistic view lacks the science and un-
flowability relates to the process. During formulation development, the derstanding sufficient to address common
Relating powder flowability flow of a blend may affect excipient se- problems encountered by the formulator
results to actual behavior in the lection and may dictate whether direct and equipment designer.
compression is used or some form of Those who work with powder, whether
production process is the true granulation is required. A full under- in the lab or in production, quickly rec-
reason flowability is measured. standing of powder-flow behavior is es- ognize that powder flow is complex. Flow
This article connects typical sential when addressing segregation prob- behavior is multidimensional and does in
powder handling processes to lems. In extreme cases, the success or fact depend on many powder character-
flow property measurements of failure of a product has hinged on its flow istics. For this reason, no one test could
value to the formulator and the behavior during manufacturing. ever quantify flowability. To address this
Given the importance of powder flow, multivariable problem, some suggest that
process engineer. the pharmaceutical industry still relies all possible test values be considered; oth-
suprisingly heavily on flow properties that ers propose that these values be factored
James K. Prescott is are poorly understood and applied. To be into a single flowability index.
senior project engineer and sure, science currently has little to offer Flowability can never be expressed as a
Roger A. Barnum is about several aspects of powder flow, and single value or index. In fact, flowability is
project engineer at Jenike &
therefore prior experience is required. not an inherent material property at all.
Johanson, Inc., One
Technology Drive, Westford, However, much proven scientific under- Flowability is the result of the combina-
MA 01886, tel. 978.392.0300, standing of bulk powder flow has not been tion of material physical properties that
fax 978.392.9980, e-mail used fully by the pharmaceutical industry. affect material flow and the equipment
jkprescott@jenike.com This article discusses powder flowability used for handling, storing, or processing
*To whom all correspondence in the context of various pharmaceutical the material. Equal consideration must be
should be addressed. production processes. By connecting ap- given to both the material characteristics
60 Pharmaceutical Technology OCTOBER 2000 www.phar maportal.com
one must include both the powder flow precise numerical models and massive
properties and the handling equipment. computational power by current stan-
Flowability is a factor for several dards. Therefore, in working with the
processes in the pharmaceutical industry. technology available to industry today,
These include each of the previously listed processes re-
● powder transfer through comparatively quires appropriate flow property tests to
large equipment such as providing con- characterize and predict the actual flow
sistent flow out of a blender, bin, drum behavior within the equipment.
hopper, Y-branch/chute, press hopper,
or dust collector Powder transfer
● powder storage, which could for example When a raw or in-process material or
Figure 1: An example of a rathole.
result in caking tendencies within a vial, product is in bulk form, it must be trans-
drum, bin, or bag after shipping or stor- ferred between pieces of equipment for
and the equipment. The same powder may age time storage, transportation, or processing.
flow well in one hopper but poorly in ● separation of a small quantity of pow- These transfers are usually driven by grav-
another. Likewise, a given hopper may der from the bulk — specifically just be- ity and typically involve dropping prod-
handle one powder well but cause another fore the creation of individual doses such uct from a blender or portable container,
powder to hang up. Therefore, a more ac- as during tableting, encapsulation, and bin, silo, or drum (collectively referred to
curate definition of powder flowability is vial filling, where feed consistency to and as a bin in this article) by opening a valve.
the ability of powder to flow in a desired through the equipment governs the uni- Typically, these steps involve large quan-
manner in a specific piece of equipment. formity of weight of the dose tities of powder with particles in contact
With this definition, the term free flowing, ● blending, in which the quality of the re- with one another, and these contacts may
so commonly used, becomes meaningless sulting blend depends on the type of be changing continuously. The size of the
unless the specific equipment handling the blender used and on the flow behavior equipment involved, particularly the out-
material is specified. of powder during the blend cycle lets and transfer chutes (if used), also is
The specific bulk characteristics and ● compaction processes (e.g., roller com- usually large (e.g., greater than several
properties of a powder that affect flow and paction and tablet compression) inches in diameter).
that can in principle be measured are ● fluidization, whether for assisting flow Several problems can develop as mate-
known as flow properties. Examples of flow or for fluidized-bed processing such as rial flows through the equipment. If the
properties include density (compressibil- granulation and drying powder has cohesive strength, an arch or
ity), cohesive strength, and wall friction. ● purely comparative, physical test meth- rathole may form. An arch is a stable ob-
These flow properties refer to the behav- ods to compare two powders (or two struction that forms within the hopper
ior of the bulk material and arise from the lots or two suppliers). This test method section (i.e., the converging portion of the
collective forces acting on individual par- may be used as a quality control (QC) bin) usually near the bin outlet. Such an
ticles (e.g., van der Waals, electrostatic, check. In this case only, the flow prop- arch supports the rest of the bin’s contents,
surface tension, interlocking, friction). erty measurement may be intended preventing discharge of the remaining
Rumpf and Podczeck provide more in- solely to distinguish between powders, powder. A rathole is a stable pipe or verti-
formation about underlying particle prop- not necessarily providing any specific cal cavity that empties above the bin out-
erties that contribute to flow behavior insight into the behavior of a particular let (see Figure 1). Material is left stranded
(11,12). powder within the equipment. in stagnant zones that usually remain in
Flow property data themselves do not For each of these applications, various place until an external force is applied to
refer to specific equipment that may types of handling equipment can be used. dislodge it. Erratic flow is the result of an
handle the powder and, therefore, should The flow behavior of the same powder obstruction alternating between an arch
not be confused with flowability. Flow between applications may be quite dif- and a rathole.
property data refer to the powder alone. To ferent. For example, a powder that flows Other flow problems related to the state
be clear, the terms powder flow and powder well through a bin may flow poorly at the of aeration or density of the powder can
flow properties should not be used synony- tablet press. Currently, no universal occur during powder discharge. The dis-
mously. Powder flow is an observation and mathematical model exists to predict charge of sufficiently fine powders can cre-
should refer to a description of how mate- powder flow behavior in every situation, ate flooding: When a rathole collapses, the
rial will flow (or did flow) in a given piece nor is such a universal model for powder falling particles entrain air and become
of equipment (e.g., “the powder flow flow anywhere in sight. A promising ap- fluidized. If the solids-handling equip-
through the press hopper was steady, with- proach, but still currently far into the fu- ment cannot handle fluids, powder will
out surging”). Powder flow properties ture for those in industry, is discrete ele- flood through the system uncontrollably.
should refer to test results of the powder ment modeling. However, this approach Even if the powder is contained, its bulk
(e.g.,“at a consolidating pressure of 10 psf, still relies on physical measurements of density can undergo dramatic variations
the unconfined yield strength is 2 psf ”). individual particles and those surfaces once fluidized, negatively affecting down-
When discussing or reporting flowability, with which they interact, and it requires stream equipment. On the other hand,
62 Pharmaceutical Technology OCTOBER 2000 www.phar maportal.com
to correct flow problems. Formulators can
Moving
use these properties during product de-
velopment to predict flow behavior in ex-
isting equipment. Flow properties that are
generally of most interest are described in
the following paragraphs.
Cohesive strength. Consolidation of pow-
Stagnant der may create arching and ratholing
within transfer equipment. These behav-
iors are related to the cohesive strength of
the powder, which is a function of the ap-
plied consolidation pressure. To show the
significance of this property, one could
Funnel flow Mass flow imagine squeezing a material such as wet
sand or snow in one’s hand. The material
Figure 2: Examples of funnel flow and mass flow patterns. may gain sufficient strength to retain its
shape once the hand is opened. In a lab,
cohesive strength can be measured accu-
the flowing channel, often resulting in the rately by a direct shear method. ASTM
formation of a stable rathole. In addition, standard D6128-97 describes the most
funnel flow can increase the extent to which universally accepted method (2).
segregation affects the discharging powder. By measuring the required shear force
In mass flow, all of the powder is in mo- for various vertical loads, one can develop
tion whenever any is withdrawn. Powder a relationship describing the cohesive
from the center as well as from the pe- strength of the powder as a function of
riphery moves toward the outlet. Mass the consolidating pressure (14). This re-
flow provides a first in–first out flow se- lationship, known as a flow function, can
quence, eliminates stagnant powder, pro- be analyzed to determine the minimum
vides a steady discharge with a consistent outlet diameters for bins, press hoppers,
bulk density, and yields a flow that is uni- blender outlets, etc. to prevent arching and
form and well controlled. Mass flow also ratholing (see Figure 4).
reduces the extent to which some types of Other testing methods use the same
segregation affect the powder. Although principles of consolidation and shearing
all of the material is moving, velocity pro- to determine the cohesive strength of a
files may still exist within the hopper (see bulk powder. Annular (ring) shear testers
Figure 3). produce a rotational, rather than a lateral,
Requirements for achieving mass flow displacement between cell halves con-
Figure 3: Model test showing flow profiles in include sizing the outlet large enough to taining material. Because of the unlimited
a hopper. prevent an arch from forming and ensur- travel that can be achieved with this type
ing that the hopper walls are steep and of test cell, the loading and shearing op-
flow-rate limitations also may occur when smooth enough to promote flow along erations are more readily adapted to auto-
fine powders are handled. The expansion them. Several flow properties are relevant mation. Successful use of this test method
of voids during flow can create upward air to making such predictions. These prop- to demonstrate differences in cohesive
pressure gradients at the outlet of dis- erties are based on a continuum theory of strength relating to handling characteris-
charge equipment. During discharge, this powder behavior — namely, that powder tics has been discussed in the industry
gradient acting against gravity reduces or behavior can be described as a gross phe- (15–18).
limits the discharge rate. nomenon, neglecting the interaction of Internal friction. Internal friction values
The occurrence of these flow problems individual particles. The application of are important when characterizing the
is strongly affected by the flow pattern of a this theory using these properties has been flow properties of a powder. Such friction
powder during discharge from a bin. Two proven over the past 40 years in thousands is caused by solid particles flowing against
flow patterns can develop: funnel flow and of installations handling the full spectrum each other and is expressed as an angle of
mass flow (see Figure 2). In funnel flow, an of powders used in industry (13). internal friction. This angle can be mea-
active flow channel forms above the outlet Armed with information about the flow sured using the cohesive strength tests de-
with nonflowing powder at the periphery. properties of a powder, engineers can op- scribed previously.
This is a first in–last out flow sequence. As timize the selection of transfer equipment. Wall friction. Used in a continuum
the level of powder decreases, layers of non- These same properties can be used as a model, wall friction (particles sliding along
flowing powder may or may not slide into basis for retrofitting existing equipment a surface) is expressed as the wall friction
64 Pharmaceutical Technology OCTOBER 2000 www.phar maportal.com
sliding to the normal force to accurately determine capacities for pro-
applied to the wall material cessing, storage, and transfer equipment
Unconfined yield strength
flow can be used in industry to to calculate the time required for fine pow-
308
measure bulk density. These ders to settle or deaerate in the equipment
methods incorporate vari- and to design efficient drying or purging
208
Mass ous-sized containers that are systems (discussed later in this article).
flow measured for volume after Once these properties have been deter-
108
being loosely filled with a mined for a powder, they can be used to
08 known mass of material and analyze existing equipment to prevent or
08 108 208 308 408 508 then are measured again solve handling problems (14,21). For in-
Hopper angle from vertical (uc) after vibration or tapping. stance, ratholing within a portable con-
USP 24/NF 19 describes one tainer or feed hopper could possibly be
Figure 6: Example of a mass flow angle design for a conical frequently used approach prevented by selecting a wall surface fin-
hopper. for measuring the bulk ish that provides mass flow at the existing
(loose) and tapped density hopper angle or by changing the hopper
angle or the coefficient of sliding friction. (20). Although such methods can offer design. An insert can be properly designed
As the coefficient of sliding friction in- some repeatability with respect to the con- to activate flow in a hopper that would
creases, the hopper or chute walls must be ditions under which measurements are otherwise be too shallow to provide mass
steeper for a powder to flow along them. taken, they don’t represent the actual com- flow. Arching can be eliminated by in-
The friction coefficient can be measured paction behavior a powder may undergo creasing the outlet size of a hopper to
by sliding a sample of powder in a test cell during bulk transfer operations. greater than the minimum requirement
across a stationary wall surface using a In a more complete approach, one can determined from the cohesive-strength
shear tester (2,14). Figure 5 shows one assess the degree to which a powder com- test. Problems achieving weight control
arrangement of a test cell. In this case, a pacts as a function of the applied pressure also can be eliminated by the use of mass
coupon of the wall material being evalu- (13,14). Results often are expressed as a flow, which provides a uniform bulk den-
ated is held in place on the frame of the straight line on a log-log plot (see Figure sity at the outlet that is nearly indepen-
machine, with a cell of powder placed 7). In the literature discussing bulk solids, dent of the material level. If limiting dis-
above. The coefficient of sliding friction is the slope of this line typically is called com- charge rates occur, an analysis of the
the ratio of the shear force required for pressibility. The resulting data can be used handling system can provide guidelines
66 Pharmaceutical Technology OCTOBER 2000 www.phar maportal.com
der as a function of the consolidating
pressure after storage at rest then is
1
developed (14).
This new time-dependent flow function
can be analyzed to determine the mini-
mum outlet diameters for converging
geometries to prevent arching and rathol-
Bulk density, g/cm3
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80 Pharmaceutical Technology OCTOBER 2000 www.phar maportal.com
height was designed and installed. The bled and consistent tablet weights were Conclusion
existing press hopper, incidentally, was achieved. Powder flow was improved Too often, the measurement of powder
sufficiently steep and smooth to provide without changing the powder flow prop- flowability does not take into considera-
mass flow. With the new bin, mass flow erties. In this case, all other comparative tion the specific equipment used to handle
eliminated ratholing and hence the need measures of flowability such as angle of the powder. Only with an understanding
for the operator to poke the material. Fur- repose, compressibility, or flow funnel of the root causes of the problems that can
ther, the steady flow to the press hopper times would not have provided any in- occur or are occurring can test methods be
allowed uniform feed onto the dies. With- sight into the true cause of the problem selected to diagnose and then avoid these
out modifications to the press or the for- nor how to solve it. situations.
mulation, the press speed was nearly dou-
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Continued on page 236
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