Powder Pointers Spring 2012 Volume 6 No A

Brought to you by: Material Flow Solutions, Inc.

7010 NW 23rd Way Suite A, Gainesville, FL, 32653 Phone: 352-303-9123 E-mail: [email protected]

Particle Breakage: A Study in Prediction Feature Article:

In This Issue
Particle Breakage: A Study in 1
Creating the particle in Just the Right Size – an Introduction. The Prediction 1
breakage of particles in handling systems is critical in the chemical, Solve Segregation Issues with the
SPECTester 3
energy, and pharmaceutical industries. The desire is to create particles Novel Powder Strength Tester
with a prescribed behavior: for example, a catalyst with a significant Regular Feature: Learning the Trade: 5
Particle Size Distribution
surface area and prescribed particle porosity, yet sufficiently robust to
maintain integrity in unit operations such as fluid bed reactors. Creating Recapture Lost Revenue:
such a catalyst is often a compromise between the porosity and the
particle size degradation. There is a movement in industry to use nano- Solve Segregation Issues
particles to create certain chemical behaviors that add value to everyday A single instrument measures:
products. However, the addition of these small particles into the matrix of • Segregation by Particle Size
other materials can lead to particle design issues where the optimal
• Segregation by Sifting
particle is very porous and, therefore, not sufficiently robust to be handled
• Segregation by Fluidization
by consumers. There is also a movement to create low weight, high
strength materials through novel particle production processes involving • Segregation by Angle of Repose
sintering product mixtures. In this case, the green materials are easily • Segregation by Air Entrainment
broken and must be treated carefully prior to the sintering process to avoid • Segregation by Chemical
breakage. The final product is robust, but the intermediate process steps Composition
require handling products that are friable. In all cases, particle size
degradation is a key flow property that controls the product or process The SPECTester
design.
To design the optimal particle or process, we must first determine the • FAST – 10 to 30 minutes to run an analysis.

expected breakage behavior in a given process or unit operation. It is • Measures a mixture of up to 6 unique
components
critical to understand what causes particle breakage.
• Identifies primary segregation mechanism out
• A particle may be sensitive to breakage by fracture (i.e. a tendency of 4 specific mechanisms

to break in half during an impact or stress-strain event). • Identifies segregation by particle size, sifting,
fluidization, angle of repose, chemical
• A particle may be sensitive to breakage by abrasion (i.e. impact or component and air entrainment
shear events tend to break off corners). • Provides data about component concentration,
• Some particles are sensitive to breakage through fatigue (i.e. particle size differences, product uniformity

repeated stress-strain or impact events eventually cause the • Identifies process design parameters and
quality control issues
particle to fracture). • Results scalable to process conditions –
• Some particles are only sensitive to cutting or tearing in order to mimics actual process conditions
create finer particles. Pinch points and close mechanical tolerance • 50 segregation points measured within a
points can result in particle size degradation of these materials. sample
• Fully automated, reports how much as well as
In addition, the structure of the particle may determine how the particle why the material mixture is segregating
will break. Often a particle is comprised of smaller particles combined to • Touch-screen/pad control
form an agglomerate or extruded structure. In these cases the breakage • Provides uniformity index for sample, and
behavior of both the primary particles, as well as the agglomerated or segregation variance data

extruded structure, becomes crucial. It is important to match the breakage • Data can be exported in Excel format
characteristics to the type of action in unit operations behavior. For • Certified CE Compliant
(continued on page 2) (continued on page 5)
Particle Breakage: A Study in Prediction (Continued from page 1) 2
example, a pneumatic conveying system is predominantly driven by impact events. Thus, particles sensitive to
breakage during impact cause significant fines generations in pneumatic systems. A rotary valve maintains close
tolerance between the rotors and the valve housing during operation. Particle breakage in this unit operation will
predominantly depend on stress-strain events. This suggests that measuring particle breakage due to impacts,
stress-strain, and cutting events will provide data to help design processes that resist particle breakage. In this
article we describe some of the method used to determine these key breakage behaviors. They provide an attrition
fingerprint of a particular material and aid engineers to design proper systems to mitigate the breakage.
Impact Degradation. Typically a range of velocities exist in typical operations. Hence, when testing for impact
degradation, it is important to measure breakage at various impact velocities. To measure for impact degradation,
material is placed in a cylindrical container and oscillated at high speed as shown in figure 1. The cylinder moves
relative to the contained material, eventually causing the material to impacts on the opposite end of the container.
Each cycle of oscillation creates two
Impact Box for Measuring Degradation Potential impacts as material is thrown against each
end of the cylinder. During these impacts
the particles interact with the cylinder
wall and other particles within the
cylinder to break due to repeated impacts.
The frequency of the oscillation governs
the impact velocity and the length of time
Figure 1. Schematic of impact degradation box showing ½ of impact cycle. As the dictates the number of repeated impacts.
box move left, the material moves right – relative to the box – and
eventually impacts on the opposite side of the box. This mode of degradation has direct
application to unit operations where
impacts are prevalent. For example, in a pneumatic conveying system the particle bounces off pipe walls as air
currents carry the particles. In a straight section of pipe these impacts are generally glancing blows and the actual
change in impact velocity is small. However, as particles approach an elbow, the trajectory causes more than just a
glancing blow and the change in impact velocity is much greater. If we can estimate the number of impacts in a
typical conveying system as well as the velocity of these impacts, we can determine the particle breakage due to
transport through the system. This system is a series of repeated impacts much like the degradation test. Thus,
data from this type of test can be used to estimate breakage in pneumatic feed systems, and free fall into process
equipment and high velocity blenders where impact is a large fraction of the motion. However, it would be useless
to use this data to describe the breakage that may be present in flowing equipment subject to high stress levels or
excessive strains. Another type of degradation test is required.
Stress-Strain Degradation. In this case, the predominant breaking action is due to fracture or fatigue caused by
large stress or strain conditions. Therefore, we measure the degradation after exposing the material to pure strain
or shear at a known stress condition. The material is placed in a rectangular test cell and allowed to deform as
shown in Figure 2. (continued on page 4)

Powder Pointers Preview Future Topics

Coming Next Quarter – Segregation management To put you at the cutting-edge
Segregation is a primary cause of poor quality product in the chemical and • Eliminating material hang-up
pharmaceutical industries. Powders and granulates segregate for a variety • Blending of powders
of reasons. Understanding segregation of bimodal mixtures is relatively • Robust product design
easy. However, real materials are usually a mixture of more than just two • Making the process work for
components. Interaction of all components in a mixture leads to complex you
segregation behavior that is not intuitively obvious, nor explained by
We encourage and welcome your
popular academic bimodal segregation theories. Knowing why and how
suggestions and special requests for
much segregation is occurring in the system allows formulators and
powder flow topics which you would
engineers to design robust products and processes that increase product
like to see included in future editions
quality, reduce product loss, and increase customer acceptance. Our next
Newsletter will address how to characterize and mitigate multi-component of Powder Pointers.
and multi-mechanism segregation issues. Contact: Susan at 352-379-8879
Novel Powder Strength Tester – Release in 2012 3
The Science of Centrifugal Force. Reactive centrifugal force is the reaction force to centripetal
force. A mass undergoing curved motion, such as a circular motion, constantly accelerates toward
the axis of rotation. This centripetal acceleration is provided by a centripetal force, which is US and
International
Patents
exerted on the mass by some other object. In accordance with Newton’s Third Law of Motion, the Pending

mass exerts and equal and opposite force on the object. This is the reactive centrifugal force. It is
directed away from the center of rotation, and is exerted by the rotating mass on the object
that originates the centripetal acceleration. The concept of reactive centrifugal force, as used
in mechanics and engineering, is referred to as just centrifugal force. (Wikipedia)

The SSSpinTester Revolutionizes the Chemical and Pharma Industries

In Pharmaceuticals. All drugs must be “packaged” somehow with excipients in order to be
marketable. Material bulk properties MUST be measured at some point in the development process to
quantify drug formulations for use in tablet press, tablet fill, and segregation modeling. The SSSpinTester can be
used to measure bulk properties of pharmaceutical powders at formulation time. In the
formulation step of drug development, only a few grams of material are created due to very high
cost of production. The SSSpinTester is the only instrument that can measure material bulk
properties (strength) during the formulation step in drug development—the amount of sample
required by other testers prohibits measuring these properties until much later in the process.
Having this data sooner rather than later narrows the R&D path, speeding time to market for new products by at
least as six to eight months. Optimization and characterization of products can now be done at the formulation
stage. Low pressure measurements simulate filling of dies—characterization and quality control can now be
achieved on a capsule-to-capsule, tablet-to-tablet basis.
How it works. The SSSpinTester uses the science of centrifugal force to measure the unconfined yield strength of
fine powders by first consolidating material using centrifugal force and then causing the compacted material to
yield using centrifugal force. Using state-of-the-art technology, it allows measurement at forces as
small as 0.2 KPa and as large as 6000 KPa (ASTM standard base limestone). We no longer must
rely on inherently inaccurate extrapolation for answers. Current methods of measuring strength of a
powdered material require at least 50 gram of sample—and some as much as 300 gram—usually
hard to come by in the pharmaceutical and chemical industries. If you can generate sufficient sample
to run a particle size analysis, you’ve got a sample of sufficient quantity to measure strength with the SSSpinTester.
In Chemicals: Measured values of material strength under stress are critical to proper design and utilization of
both process system equipment and product characterization. Material properties of fine powders often change
with exposure to fluctuating environmental conditions. This is particularly true in the chemical industry. The
single sample SSSpinTester analysis can be conducted in under ten minutes, making it an essential tool from the
formulation process, all the way through end-product quality assurance.
Using the Tester. Material sample size is based on the parameters of the testing cell: a conical frustum with a top
aperture 0.25 inches and 0.20 inches deep. Depending on sample density, this translates into a bulk weight
between 0.01 and 1.00 grams material to conduct the single test necessary to determine the
unconfined yield strength. Materials tested to date include ASTM standard limestone reference
powder, herbiceuticals, household cleanser, time-release allergy compound, sodium sulfate, lactose
monohydrate, multiple spices and mixtures, powdered drink mix, light-weight polyethylene
powders, pigment powder, tungsten/lead mixture, calcium carbonate, titanium dioxide, infant
formula, sodium citrate dehydrate, fabric care compound, gelatin, cosmetics, vitamins, talc, sleep
aid compound, and more.
Specific Machine Features:
• Quantifies the strength of fine powders in as • Requires ONLY ~0.05 grams of material to run a full
little as 15 minutes. strength analysis.
• 16x18 inch footprint makes the tester easy to • Testing range from 0.2 to 6000 KPa.
accommodate in any testing lab. • Ships with pre-programmed computer and test cells
Particle Breakage: A Study in Prediction (Continued from page 2) 4
This deformation induces nearly perfect shear and causes the particle to experience strain at a controlled stress
condition. As the test cell osculates between a square and a rhombus shape, we can measure breakage at a
prescribed stress level for several total strains. It is obvious that this degradation date would be useless when
applied to transfer in pneumatic transfer systems. However, it exactly describes the breakage that may occur in
silos, screw feeders, rotary valves, low shear mixers and other process equipment that moves material slowly.
Relating Test Data to the Process. Consider bran cereal Shear Box for Measuring Degradation Potential
that has been subjected to stress-strain events. We use the F F F F F

difference in cumulative particle size between the

unstrained and strained materials as a measure of particle
breakage (Figure 3). This is expressed as a difference in
cumulative particle size as indicated in Figure 4. Note that
the peak in Figure 4 corresponds to the greatest difference Figure 2. Schematic of stress strain degradation test
between the two cumulative curves before and after
subjecting the cereal to stress-strain events. After computing similar degradation profiles for other stress and strain
conditions, this information can be used to determine the degradation of a material in a particular process geometry.
For example, consider the bin below that is 20 foot in diameter with a 40 foot tall cylindrical section and necks
down to a 2-foot diameter outlet (Figure 5). We have shown the typical stress and strain profile that would exist in
this storage bin. A series of stress-strain degradation tests could be conducted to cover the range of stress level as
well as strain levels in this bin, and that data could be used to compute the expected particle breakage in this bin.

Figure 3. Typical degradation due to stress-strain events at a Figure 4. Cumulative degradation at a stress of 414 psf and a
prescribed stress and total strain: stress of 414 psf strain of 52 in/in
and a strain of 52 in/in

Figure 6 shows the expected particle size degradation for the bin configuration shown in Figure 5. In the zero
strain zone, crushing occurs. In the hopper section, the high stress and low stain region shows a rapid increase in
particle breakage followed by a slow increase in particle breakage in the low stress and high strain section. This
behavior suggests that taking steps to retrofit this bin and minimize stress levels will mitigate particle breakage.

Crushing

High Stress
low strain

Low stress
high strain

Figure 6. Typical degradation profile

Figure 5. Typical stress and strain profile in bin
in bin (400 mm particles)

Examining a degradation problem from this mechanistic viewpoint allows engineers to design a solution to address
troublesome particle breakage issues. This approach saves time and money and allows minimal down time to make
process changes. The key pieces of information needed are a correct description of the degradation behavior of
your material and knowledge of stress-strain profiles in the unit operation. Similar analyses can be carried out for
screw feeders, belt feeders, rotary valves, blenders, transition points, pneumatic conveying systems, blow pots, and
stock piles. Measuring the degradation due to impact and stress-strain events is a valuable characterization tool.
Mitigate Segregation with the SPECTester (Continued from page 1) 5

Segregation, also called

Data is presented numerically and graphically
separation, of granular
and powder materials is
one of the three main
causes of process
failure with systems
that handle powder
materials. It is a global
problem, affecting all
industries: conservative
estimates suggest that
30% of all unscheduled
process downtimes are due to segregation and quality issues. The
SPECTester’s spectrophotometer acquires data to analyze the segregation
potential of a material mixture by scanning spectral reflectance of the top
layer (edge) of the material pile in the testing hopper. It compares that
gathered data to the previously acquired spectras of the individual ingredients
in the mixture by de-convoluting the data to identify the presence and
concentration of the various components and their locations in the hopper.
The SPECTester will measure up to 50 squares along the pile edge, with a
matrix of up to 49 points within each square. Concentration data identifies the
magnitude of the segregation. Using state-of-the-art spectroscopic technology, the innovative SPECTester
measures samples containing up to six unique components and reports how much, as well as why, your material is
segregating. Fully automated, the SPECTester identifies: component concentrations, particle size differences,
differences in chemical composition, product uniformity, and up to four specific segregation mechanisms.

Learning the Trade – Particle Size Distribution

Knowing and understanding key material properties is power to characterize bulk material flow behavior. We will
empower you quarterly as we discuss one of these fundamental flow properties and its industrial application.
Particle-Size Distribution (PSD). The particle-size distribution of a powder or
granular material defines the relative amounts of particles in a sample mixture,
sorted according to size.
Particle size is an important parameter that can be used for product and process
design scale up. There are many methods available for measuring particle size.
Some of the most widely used include, but are not limited to: optical techniques,
laser diffraction, sieving, settlement, and electro-sensing. Often particle-size
distribution is the primary factor in understanding how a bulk material will
segregate, blend, dissolve, and fluidize. It is one of the process variables that
engineers have moderately good control over. It is related to bulk unconfined
yield strength and can be used to predict cohesive flow properties if the structure
and surface characteristics of a particle assembly are known. Thus, we can predict cohesive flow problems with
knowledge of particle size distribution, moisture content, particle surface energies, and shape changes.
At Material Flow Solutions, our particle analysis method also allows us to characterize particle shape and bulk
granularity. These techniques can be extended to look at the structure of individual particles or agglomerates and
determine if the agglomerate structure is robust. Particle size is the key parameter used to determine the attrition in
a process or characteristics of a particular material. We measure material particle size with both standard and
proprietary optical methods in order to recommend optimal process parameters so your product will be what you
want it to be – the first time.
All Bran® pictures courtesy of: http://www.mrbreakfast.com/cereal_detail.asp?id=6