Powder eHandbook

Powder
Processing
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Enhance Safety and Efficiency!

Non-Contact Inventory
Management in Bins & Silos
3DLevelScanner
Accurate Volume
& 3D Mapping

True volume measurement for silos

Works reliably in high levels of dust
Accurate, multiple-point measurement
Measures and maps bin topography
Eliminates climbing for employee safety

NEW! BinMaster RL Level Sensor

RL

Acoustics-based, continuous
level indicator for dusty
environments
Works in powders and
solids including low
dielectric materials
Self-cleaning, minimalmaintenance sensor

BINMaSter level CoNtrolS

www.binmaster.com info@binmaster.com

402-434-9102

2014 BinMaster, Lincoln, NE 68507 uSA

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Table of Contents

Particle Mysteries Take a Powder 7

Insights promise to enhance processing

Scanners take Volume to a New Level 15

Acoustics-based sensors can help accurately measure the volume of powders in vessels

Determine a Coatings Volatile Content 20

Advancements in rapid loss-on-drying techniques significantly reduce testing time

Test Powder Flow with Ease 23

Advances in test methods help better predict flow behavior at elevated temperature and humidity levels

Product Features
Food-Grade Hoses Handle High-Static Applications

Indoor Venting Helps Manage Combustible Dust Explosion Risks 5

MoveMaster Vac Simplifies Vacuum Conveying 11
Flexible Screw Conveyor Extends Conveyor Offerings

13

Food-Grade Hoses Handle High-Static Applications

Hose design helps dissipate static charges to ground.
Kuriyama of Americas new line of Tigerflex Voltbuster food-grade material-handling
hoses have been designed for high-static applications such as the transfer of powders, pellets
and other granular materials.
The hoses design helps dissipate static charges to ground, helping prevent static build-up and reducing the potential for dangerous electrostatic discharges. They have been constructed with static
dissipative plastic materials, allowing for the free flow of static to the hoses embedded grounding
wire. The light-weight design of the hoses can help reduce injuries related to heavier metal hoses.
The Volt Series hose-tube construction includes abrasion-resistant food-grade polyurethane to ensure the purity of
transferred materials. In addition, the grounding wire has been encapsulated in a rigid PVC helix on the exterior of the
hose, eliminating the risk of contaminating the transferred materials. The VLT-SD Series is constructed the same, but has
an FDA polyester fabric reinforcement to handle both suction and higher pressure discharge applications. New 2- and
8-in. ID sizes have been recently added to this product line.
Kuriyama of America, Inc. 847-755-0360 www.kuriyama.com
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Ad Index
BinMaster 2
www.binmaster.com

Brookfield 4
www.brookfieldengineering.com

Beta Raven

Kuriyama of America, Inc.

www.betaraven.com

www.kuriyama.com

Arizona Instrument

10

www.azic.com

Tecweigh 12
www.tecweigh.com

Vac-u-max 14
www.vac-u-max.com

Schenck Process

19

www.schenckprocess.com

Rembe 22
www.rembe.us

Federal Equipment Company

25

www.fedequip.com

Indoor Venting Helps Manage Combustible Dust Explosion Risks

Now includes metal dust explosion protection
The REMBE Q-Rohr-3 family of products is an indoor flameless venting system that
eliminates the need for relocating dust collectors or other enclosures outside. The REMBE QRohr-3 consists of a specialized stainless steel mesh construction and a REMBE rupture disc.
An integrated signaling unit connects to any audible/visual alarm and shutdown to alert plant
personnel, should there be an incident. In an event, flames are extinguished, pressure, noise
and dust are reduced to negligible levels. The system is FM and ATEX approved and NFPA
compliant.
The product line is now approved for use with dusts, gases, hybrid mixtures and metal dusts.
The Q-Rohr-3-6T and Q-Rohr-3-6T-AL are ideal for applications found in pharmaceutical, coatings, steel, iron and other industries. Click here for more info.
For over 40 years, REMBE, GMBH has been and continues to be a leader in the innovation
and manufacture of high-quality explosion protection systems. As the inventor of flameless venting, REMBE, specializes in
combustible dust explosion prevention/protection systems for many applications across a multitude of industries. Download
our free case study guide: http://www.rembe.us/case-studies/documents/BOSS_Booklet_of_Safety_and_Security.pdf
REMBE, INC. 855-821-6230 www.rembe.us
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Particle Mysteries Take a Powder

Insights promise to enhance processing
By Sen Ottewell, Editor at Large

Most manufacturers handling powders

certainly would agree that achieving a better understanding of the materials characteristics and how they
change during processing could enhance the efficiency
and safety of their operations. Fortunately, vendors
are making solid progress in demystifying some key
factors affecting powders.
For instance, Freeman Technology, Tewkesbury,
U.K., and Medford, N.J., is looking beyond the physical properties of the particles and treating powder as a
bulk entity. Using its FT4 powder rheometer, the company can evaluate and understand all the parameters
that influence process performance.
Our approach is to simulate the stresses, flow regimes and conditions that a powder may be subjected
to in a process, for example, aeration, moisture absorption and electrostatic charging, and directly quantify
its response, says Jamie Clayton, operations manager.
One project involved dynamic testing to meaningfully quantify differences in flow behavior between
two different samples of sodium nitrite. The aim was
to get the same properties in the second sample as in
the first, commercially available, one.
A combination of dynamic powder testing and
automated imaging showed the process for making the
second sample needed modification to produce coarser
particles with a smoother regular shape (Figure 1).
The results here are not specific for sodium nitrite
and in general could be true for a wide range of different powders. However, our experience tells us that
when working with powders there isnt a one-size-fitsall solution; there is no such thing as a good or bad
powder. The real question is, What is powder flow?
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because the answer will depend on the material in

question, the process concerned and what the formulation scientist or process engineer needs to achieve,
notes Clayton.
For example, the properties of powder necessary
for efficiency in a bulk bag filling process may significantly differ from those required when manufacturing
a pharmaceutical tablet. A common preconception
in both cases is that the most-free-flowing powder is
needed. However, in reality, a free-flowing powder can
introduce its own problems such as dusting, segregation and flooding. So, the key is to identify powders
that best suit a particular process and accurately
quantify their properties.
In some unit operations, such as tableting or
pneumatic conveying for example, a more cohesive
powder may actually be conducive to better results. In
all circumstances though, its important to recognize
that any application will consist of a series of stages
and, in order to achieve efficient processing and a highPARTICLE SIZE ANALYSIS

Figure 1. Dynamic powder testing and automated imaging identified the need
to modify a process to produce coarser particles with a smoother regular shape.
Source: Freeman Technology.

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Thermoplastic Industrial Hoses

Static Dissipative
Food Grade Material
Handling Hoses
Superior Static
Protection!

VOLT

WINNER!

Durable Abrasion
Resistant!
Food Grade!
Light Weight!
BY

VLT-SD

CHEMICAL PROCESSING

TIGERFLEX

EDITION 0114

ISO 9001-2000
REGISTERED Q.M.S.

THE ASSOCIATION FOR HOSE AND

ACCESSORIES DISTRIBUTION

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Made In USA

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INTERLOCKING VERSUS COHESION

Blad

em

ove

men

Stress
transmission
zone

Blad

em

ove

men

Stress
transmission
zone

Figure 2. Efficiently packed large particles transmit blade movement through a much larger stress transmission zone than more cohesive powders.
Source: Freeman Technology.

quality final product, a given powder must be compatible with all stages within the process, he adds.
MOISTURES ROLE

Another recent project focused specifically on controlling the impact of humidity on the powder flow
properties of lactose and microcrystalline cellulose
(MCC). The main driver for this work was not only
to gain a greater understanding of how humidity affects powder flow properties, but also to examine the
general assumption that moisture is always detrimental to powder flow. The results illustrated how small
quantities of adsorbed moisture can actually lead to an
improvement in certain conditions, Clayton explains.
The two materials were selected for study because
they represent powders commonly used in industry
and also exhibit varying degrees of hygroscopicity. The
results demonstrated that even the small quantities of
moisture adsorbed by powders considered to be hydrophobic could significantly impact flow properties.
I think we always knew that assuming moisture
adsorption is always detrimental and that so-called
hydrophobic powders arent affected by humidity was
over-simplistic, but this study allowed us to prove this
and demonstrate how influential even minor changes
in moisture content can be. It was particularly relevant
that some of the greatest changes were seen across a
relative humidity range that would be typical of most
processing environments, he notes.
The effect of humidity on powders can be very
complex; the test results show how properties such as
cohesion can prevail in certain circumstances while
mechanical friction or interlocking can dominate
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when the powder is subjected to different stress levels

(Figure 2). This underscores why a multivariate testing
approach is required to simulate the various stages
within a specific process and understand how the
powder responds.
A further study has looked at factors that influence
blending kinetics, a subject still very poorly understood. Based on work carried out as part of a Ph.D.
research project at the University of Birmingham,
Birmingham, U.K., the study correlated positron
emission tomography (PET) data with flow energy
measurements. The results suggest that dynamic data
may be a reliable predictor of blending behavior and,
consequently, useful for developing and optimizing
blending processes.
While PET primarily is used in academia and isnt
an established industrial tool, Clayton believes it provides a novel comprehensive method for evaluating mixing efficiency to determine optimum parameters such as
speed and mixing time to achieve uniform dispersion.
In this study we see how two different mixtures
require different process equipment settings to achieve
a predefined level of acceptance. These different requirements are likely to be due to the different physical
properties of the constituent powders but after applying a range of powder characterization techniques,
only the FT4 was able to identify and quantify these
differences, he explains.
The company says its reports and white papers
particularly those related to subjects such as caking
or humidity are generating a lot of interest from
process engineers and formulation scientists across a
wide range of industries.
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ONLINE ANALYZER

As a company we have experienced great success

in the pharmaceutical industry where our technology
lends itself well to recent initiatives such as process
analytical technology and quality by design. However,
the FT4 is used across a diverse range of industries
including chemical, food, agriculture, powder coatings
and toners. One of our existing users has recently
demonstrated how minor variations in the raw ingredients and upstream process can have a major impact
on the properties of household detergent tablets,
notes Clayton.
OTHER KEY PARAMETERS

Analyses of particle size and shape present their own

challenges when it comes to understanding how different operating conditions affect various materials. The
main push from its customers is to gain insights for
improving product quality and consistency, notes
Malvern Instruments, Malvern, U.K. Automation can
play a key role in achieving these aims, it stresses.
In one project, the company carried out successful
trials of an online particle size analyzer on an active
pharmaceutical ingredient (API) milling operation at a
commercial site of a major manufacturer.
Like many other API makers, the company used
an iterative process that required numerous offline
analyses of the milled powder to verify it met the
correct product specification. Time consuming and
wasteful, this procedure only can show that the
properties of the batch are acceptable but reveal no
information about manufacturing consistency.
Following the trials, the plant installed an Insitec
online particle analyzer (Figure 3). This is linked to the
mills programmable logic controller by an Insitec PC
to provide a fully integrated system; Malvern software

Figure 3. Device is fully integrated with mill, enabling automated control which
has boosted quality and throughput and cut waste. Source: Malvern Instruments.

handles data exchange. The operator interacts with the

PC via the mills human machine interface and can
input set points for the control loop, remotely start and
stop the analyzer and mill, perform background tests,
and receive particle size results.
The benefits of automating control include improved product quality, increased throughput and less
waste especially in the form of dust. Furthermore,
automation opens up a route to semicontinuous operation and real-time release important long-term
goals in reaching operational excellence.
This system has been used in many milling
campaigns, some in excess of 20 tonnes, with consistent
quality throughout. Together with streamlining operations and ensuring excellent quality, the embedded process analytical technology (PAT) also has enabled this
company to reduce offline sampling lab work by

MoveMaster Vac Simplifies

Vacuum Conveying
System suited for variety of applications
The MoveMaster Vac is a vacuum conveying system ideally suited for
batch dilute phase conveying, direct loss in weight feeder refill, and integrated
volumetric feeding and conveying. It can accommodate rates up to 4,400 lbs/hr
and temperatures to 110F. For more information, visit www.schenckprocess.com/
products/MoveMaster-Vac
Schenck Process 262-413-2441 www.schenckprocess.com
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What Do You Need to Weigh?

Weigh it with

Volumetric Feeders

Weigh Belt Feeders

Bulk Bag Unloaders

Gravimetric Feeders

Sanitary Weigh Belt Feeders

1.800.536.4880
TECWEIGH.COM
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Related Content on ChemicalProcessing.com

CP Powder eHandbooks, www.ChemicalProcessing.com/articles/2012/powder-ehandbooks.html
Conveying Changes Direction, www.ChemicalProcessing.com/articles/2012/conveying-changes-direction.html
Dust Removal Gets a Rethink, www.ChemicalProcessing.com/articles/2012/dust-removal-gets-a-rethink.html
Progress with Solids Takes Shape, www.ChemicalProcessing.com/articles/2010/011.html
Effectively Handle Powders, www.ChemicalProcessing.com/articles/2009/095.html
Avoid Blending Blunders, www.ChemicalProcessing.com/articles/2007/154.html
Prevent Fine Powder Flushing, www.ChemicalProcessing.com/articles/2006/018.html
Unlock Better Blending, www.ChemicalProcessing.com/articles/2003/150.html

an amount equivalent to 30% of its initial cost per campaign,

says Alon Vaisman, Westborough, Mass.-based application
development manager for Malvern.
As the technology moves from early adopters to more
mainstream users, Vaisman notes that such PAT solutions
are becoming very widespread in the chemical and other
industries: In my view this has become more of a requirement in the western market where competition is very aggressive and improving quality is a big driver. Whether you
are talking about total quality manufacturing or Six Sigma,
its all about quality control.
In an effort to further improve its online automation, Malvern has launched specialized software to control the analyzer
and peripherals, plus enable integration of the analytical data
into the users control system.
In the future, I think that more of our work will focus on
developing specialized software such as this in order to make
integration easier, he adds.
Looking five years ahead, Vaisman believes the needs of
the biopharmaceutical and nano sectors will spur new online
analytical devices based on technologies now limited to the
laboratory, and there will be a wider variety of online tools
available than is currently the case. He also foresees traditional
manufacturers responding to low-cost competition by opting

for instrumentation that now might be considered too expensive

or not designed for such processes, for example as used in the
food industry, to boost efficiency.
There will also be further improvements in the ease of
process integration. PAT projects are expensive today in terms
of equipment and validation. I hope that an increase in standardization will lead to easier integration and faster validation,
he concludes.
Of course, laboratory-based analytical techniques will
continue to play an important role at many sites far into the
future. So, a major study about how the reliability of analytical instruments and the reproducibility of their results
changes over time by Wyatt Technology, Santa Barbara,
Calif., a maker of light-scattering instrumentation, should
interest many plants. The company focused on results generated by two of its size exclusion chromatography-multi angle
light scattering (SEC-MALS) instruments, which are widely
used when investigating how particle size and distribution
can vary from batch-to-batch in different processes. The
company used data collected from an independent analytical laboratory over a five-year period, an unprecedented
procedure for such instruments, it believes. The findings
found extraordinary reproducibility from day-to-day,
month-to-month, and year-to-year, says Wyatt.

Flexible Screw Conveyor Extends Conveyor Offerings

Conveys product from bulk bag unloaders, bag dump stations and storage vessels
The VAC-U-MAX flexible screw conveyor is designed to compliment
the already extensive range of pneumatic and mechanical conveyors
offered by the VAC-U-MAX Group. The flexible screw conveyor is an
economical method of conveying product from bulk bag unloaders,
bag dump stations and storage vessels. Available in a range of sizes, the
conveyors typically transfer product over distances of up to 40 ft and
rates to 10 tons per hour for materials having a bulk density of 40 pounds
per cubic foot. Typical applications include the refilling of packaging
machine hoppers, metered feed into mix tanks such as lime addition and
gain in weight hopper filling.
Vac-U-Max 800-822-8629 www.vac-u-max.com
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Scanners take Volume to a New Level

Acoustics-based sensors can help accurately measure the volume of powders in vessels
By Jenny Christensen, BinMaster Level Controls

Many devices are available on the market

today for detecting the level of materials in bins,
tanks and silos. However, for calculating whats in
inventory sometimes level data just isnt enough.
To estimate the amount of material on hand and
the dollar value of that inventory, a single measurement point might not contain enough data to provide the accuracy needed. Due to their tendency to
form irregular topography in the silo, this can be
especially true in powders because most dont tend
to flow freely. If inventory volume is based upon
a single measurement from a single point in the
silo, the volume estimate has the potential of being
very inaccurate.
Multiple Points Really Matter

Acoustics-based technology used in sensors referred to as 3DLevelScanners, or generically called

scanners, is very different from other types of sensors. Like the name implies, these devices scan the
material surface to take multiple measurements,
taking into account the high and low spots in the
silo. Scanning the surface also detects conditions
such as cone up or cone down as well as buildup
that may be present along the sidewall of the
vessel. The data from multiple measuring points
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is processed using advanced firmware and algorithms, and when combined with the silos parameters loaded into the software, a highly accurate
volume estimate can be provided. Additional data,
such as the highest, lowest and average level of the
material also is supplied.
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SINGLE MEASUREMENT POINT

Performs Reliably in Heavy Dust

One of the greatest challenges powders present is

the presence of excessive amounts of dust, which
can render some types of sensors inaccurate or unreliable until the dust settles. By operating at very
low frequencies, a scanner isnt bothered by dust
and can perform consistently and reliably regardless of the conditions in the vessel. This technology
has been proven in many different challenging
materials such as alumina powder, carbon black,
detergents, polyethylene powder, silica granules, fly
ash and talc powder.
Self-Cleaning Sensor Minimizes
Maintenance

Figure 1. The RL model detects level in a narrow beam and is ideal

for bins of all size where a single measurement point is adequate.

MULTIPLE MEASUREMENT POINTS

The unique design and materials used to manufacture scanners ensure that the surface resists the
buildup of powders that are suspended in the air
at the top of the vessel. Plus, the acoustic pulses
make a chirping sound that resonates and creates
an almost imperceptible vibration that helps keep
the inside of the scanner clean. This way, the sensor
stays clean and operational without the need for
running an air purge to the top of the vessel,
which can be costly.
Stands Up to Corrosive Materials

When a silo is filled with highly corrosive materials,

its important to outfit the silo with a sensor that can
stand up in the toughest industrial environments.
For this type of specialized application a scanner
that has a HALAR coating on the mechanical parts,
VITON for the o-rings and stainless steel for any
parts exposed to the material will work reliably over
a long period of time. This option is recommended
when the sensor is being used to measure corrosive
materials such as quick lime, sodium chlorite, potassium hydroxide or other materials on the U.S. DOT
Class 8 material list.
Non-Contact Sensor Prevents
Contamination

Figure 2. The S model measures multiple points within a 30

beam angle and is ideal for smaller silos.

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With an acoustic sensor, theres nothing that

comes into contact with the material, making
it very safe to use in powders, granules or other
solids of all types. Theres no risk of equipment being stuck in deep material or becoming
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VOLUME MEASUREMENT

Figure 3. For larger silos, the M model measures multiple points

within a 70 beam angle to accurately calculate volume.

detached and potentially damaging structure or

equipment in the bottom of the silo. Theres no
need to replace probes or cables that can wear
out over time. Eliminating contact with material
helps ensure long life with minimal preventive
maintenance or cost.
Safety Incentives

When inventory monitoring is completely automated, theres no need to climb silos to take measurements. This not only saves time, it eliminates
the risk of falls and the resulting injuries and the
hassles of insurance and paperwork that comes
with accidents. Plants today deal with rigorous
OSHA requirements pertaining to climbing and
entering silos and risk hefty fines when found in
violation. Installing an automated inventory monitoring system allows for material management to
be performed from a personal computer in the
safety of an office.
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Level and Volume Measurement

3DLevelScanners, like most other measurement

devices, come in a variety of models and offer
a wide range of options to tailor the device to
the application. To select the right model for an
application, its extremely important to communicate your expectations of the technology and
how you plan to use the data that you get from
the device. Many plants are focused upon having
a very high level of inventory accuracy. Accuracy
of the scanner is driven by a number of variables,
starting with information about the size of the
vessel, the presence of structure inside it, and the
material thats being measured. The installation
location also is important as scanner technology
measures multiple points, so the device needs to
have a clear view of the material surface.
The most basic model of a scanner is referred
to as an RL, which is short for reliable level.
This model measures material in a narrow beam
directly below the device, penetrating high levels
of dust and performing where other types of level
sensors become unreliable or inaccurate. This
model is most often used when highly reliable level
measurement data is needed on a continual basis.
This model is frequently applied in materials that
are less prone to excessive buildup and in narrow
or smaller silos.
When more than simple level data is needed,
the S model is designed to determine volume based
upon an average level in the bin from multiple
measurements taken within a 30 beam angle. This
model often is used in narrow silos with diameters
up to 16 ft and heights up to 200 ft. This model
can also be used in wider silos, but with diminished accuracy as the 30 beam angle may not
cover the entire material surface.
The M model takes measurements from a
broader 70 beam angle making it appropriate
for larger diameter silos and silos with uneven
material topography. It also generates additional
data including the lowest, highest and average
distances based upon multiple measurements.
Due to its ability to scan the material surface and
take into account irregularities, it can provide a
very high level of volume accuracy from between
one and three percent.
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At the top of the model spectrum is the model MV, which does
everything the M does, plus adds a unique visualization feature.
Using complex algorithms and a lot of processing power, this model
generates a 3D image that indicates where the high and low spots
are in the silo, shows if the cone is up or down, and detects sidewall
buildup. This additional feature can be used to help manage filling
and emptying points as well as detect if maintenance is needed to
clean out buildup. This model is often used in large silos and in
flour-like powders and other types of materials that tend to pile up
unevenly.

SELF-CLEANING SENSORS

Other Measures to Improve Accuracy

If a bin is very wide or large, two or more scanners can

be combined into a multiple-scanner system. By adding a
controller that synchronizes the measurements from all of
the scanners on a silo, the MVL model is able to provide very
high volume accuracy in some of the largest silos. The number of scanners needed on the silo is determined by how large
the silo is and the desired level of accuracy. The MVL also
can generate a 3D visualization of the material surface from
the measurements taken from all scanners. If visualization
is not a requirement, an ML model supplies the same level
of accuracy without the visual, making it more economical
choice when budgets are tight.
Silos can be challenging structures to measure and often
they come with some surprises that need a little work
around. For example, sometimes there is structure in the top
of the silo, so a measurement device might try to measure the
structure instead of the material. Neck extensions have been
designed for scanners that allow them to clear structure and
see beyond it to get an accurate measurement of the material.
Angled mounting flanges are designed to keep the device level,
while angled mounting adaptors can be used when its necessary to aim the device in a problematic silo.
Although they have only been in the North American market
for about five years, acoustic sensors have already revolutionized
inventory management by adding the ability to accurately estimate
the volume in a silo without ever leaving the safety of an office.
The data derived from these devices improves operations in so
many ways by allowing for timely replenishment and purchasing,
reducing safety stock, and making inventory valuation far more accurate. For plant personnel, the scanner has been a game changer,
keeping personnel safe from climbing silos and making them more
efficient. Scanners truly have taken volume to a new level.
JENNY CHRISTENSEN, MBA, is vice president of marketing, for
BinMaster. She can be reached at jchristensen@garnerindustries.com.

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(a)

(b)

(c)
Figure 5. The scanner on a powder silo is covered
with dust (a). Inside of the silo, the outside of the
unit also is coated with dust (b). However, the selfcleaning sensors inside the unit are clean and fully
functional (c).

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Determine a Coatings Volatile Content

Advancements in rapid loss-on-drying techniques significantly reduce testing time
By James A. Moore, Arizona Instrument LLC

For 40,000 years people have been using

paints and coatings for decoration, protection and camouf lage in daily life. Early paints
contained naturally occurring dyes and used egg
yolks, linseed oil, waxes or other natural binders
to help it adhere to surfaces. Changes have been
made since early formulation, but the paints and
coatings industry was revolutionized following
World War II when toxic components, such as
lead and mercury, began to be removed.
Today synthetic polymers, resins and solvents
are used for paint production. These materials
outperform their historic predecessors, showing
an increased resiliency for weathering effects such
as acid exposure, extreme heating and cooling,
and water exposure from rain or snow.
Paint is a three component material made of
a pigment, a vehicle and carrier. High quality
paints are made from high quality materials, and
manufactures need to test materials to ensure
that consumers will be happy with the products
they purchase. To ensure they have the right
blend of components, a manufacturer will run
loss-on-drying assays, which examine the amount
of material that will volatilize once it is heated.
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Traditional Testing Methods

ASTM International has dedicated method

D2369 for determining volatile content of coatings using an oven method test. First approved
in 1965, this method effectively determines the
volatile content, but is not able to take advantage of new technology that reduces testing and
throughput times, which would allow manufacturers to improve the efficiency of their metrology process and allow them to reduce product
manufacturing times. Additionally, this method
isnt able to provide real-time results for analysis,
which would be helpful to immediately diagnose
possible manufacturing problems.
Rapid Loss-On-Drying

Because of technological advancements in traditional loss-on-drying techniques, ASTM International

adopted method D7232 in 2006. This method is
designed to produce the same result obtained from
testing using method D2369, but reduces testing
time from 2+ hours to minutes. In addition, the
Computrac MAX 4000XL analyzer provides insitu measurements, giving metrologists the ability to
diagnose manufacturing problems immediately.
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Test Method Results

CLEAR ACRYLIC RESIN

MAX 4000XL
(% Solids)

Coating 1

Convection
Oven

74.644

Mean

74.404

0.111

Standard
Deviation

0.400

14:17

Test time

2 hours

Testing and Results

BROWN ACRYLIC RESIN

MAX 4000XL
(% Solids)

Coating 2

48.429

Mean

48.198

0.261

Standard
Deviation

0.377

10:01

Test time

2 hours

MAX 4000XL
(% Solids)

Top Coat

Convection
Oven

60.317

Mean

60.028

0.111

Standard
Deviation

0.035

7:20

Test time

2 hours

Table 1. Statistical analysis of three different materials show newer test methods, such as
the MAX 4000XL, can reduce testing times when compared to a convection oven.

TIME
Result

660

616

0
572

0
528

484

20

440

10

396

40

352

15

308

60

264

20

220

80

176

25

132

100

88

30

% OF SOLIDS

120

Rate

James A. Moore is research chemist for Arizona Instrument LLC. He can be reached at sales@azic.com.

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Figure 1. Real time measurements of volatile content and the rate of loss over time.

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RATE OF LOSS

DETERMINATION OF SOLIDS FOR BROWN ACRYLIC RESIN

Conclusion

For testing paints and coatings, rapid losson-drying methods prove to be more desirable than traditional testing methods. Both
testing methods were able to provide similar
results, but the MAX 4000XL was able to
reduce testing times when compared to the
convection oven, and gives a complete profile
of the materials as they are being analyzed.
This technology can be used to reduce manufacturing throughput times, and provide
quality improvement with more information
should formulation problems arise.

Convection
Oven

FINISH COAT WITH ADDITIVES

44

For this experiment three different materials

(Table 1) were tested using ASTM method
D2369 and D7232. For method D2369 a
convection oven was used, and for D7232 a
Computrac MAX 4000XL instrument was
used. Between sample tests using the MAX
4000XL, the coatings and pigment were
shaken in their containers. A f lat pan with
paper was used for each test and the materials
were placed onto the pan using a 5mL plastic
syringe.
The data from the table shows that the
two methods provide similar results. However, the MAX 4000XL showed a significantly
tighter testing result range for two of the
three sets of testing.
Figure 1 shows the resin begins to volatilize around 100 seconds, suggesting that the
idle temperature is cool enough to prevent
the material from evaporating prior to data
collection. Also, the tail of the rate graph
shows that the material has lost all volatile
content and the test is allowed to end. This
is a typical graph for all three materials that
were examined.

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Test Powder Flow with Ease

Advances in test methods help better predict flow behavior at elevated temperature and humidity levels
By Dr. Erik Miller and Michael Olson, Solutia/Eastman Chemical Co., and Vinnie Hebert, Brookfield Engineering Laboratories

One of the more difficult characterization tests for bulk solids involves testing at higher temperature and humidity levels.
Many materials are susceptible to an increase in temperature
and humidity levels, which could cause their flow properties
to change. A material that was flowing easily at lower ambient temperature and humidity levels could now jam the feeder
system when these levels rise. Too often, the way to address this
flow problem involves a hit or miss proposition by merely adding in some flow aid compound, increasing the amount until
flow improves, and hopefully before too much is added to affect
the base material. Another solution is to fully alter process
conditions, which can be a very costly modification.
This unscientific method is fairly common practice in industry. Part of the reason is the absence of an established characterization test for evaluating powders at elevated temperature
and humidity levels. However, a test method does exist using
a shear cell instrument modified to run at higher temperatures
and humidity levels.
Shear Cell Basics

The shear cell has been utilized for defining powder flow
properties accurately for many years. Its concept is well-defined
in ASTM D6128 and accepted in the bulk solids industry. The
initial design of the cylindrical Jenike shear cell has evolved to
the annular Walker shear cell, which generates powder flow
data much more rapidly.
With an annular shear cell (Figure 1), powder is sheared
against itself at defined consolidation stresses to simulate the
conditions when powder particles move downward in a bin

under influence of gravity. This annular configuration ensures

the shearing action is uniform across the sample of powder.
Information from this test is then utilized to create data for defining standard flow behavior properties such as flow function
and bulk density. Mathematical calculations provide additional
information on arching dimension and rat-hole diameter.
The flow function test provides a quantitative measure for
flowability, far superior in usefulness compared to something like
a subjective cup test or angle of repose measurement, which
are, surprisingly, accepted and still used within many industries.
Temperature and Humidity: The Problem

Many bulk solids are sensitive to heat and humidity. As these

levels rise, either in the feeder system or via outside conditions,
flow problems crop up. As the powder gains strength, jams and
poor flow conditions begin to appear. Costly downtime and a
loss of product are incurred while a search is made for a solution
to the flow problems. Certainly, it would be much more cost
effective to have the product defined at different temperature
and humidity levels.
Solutia Inc., a subsidiary of Eastman Chemical Company,
had just such a problem. Solutias product line includes a range
of high performance PVB interlayers for automotive and architectural glazing applications. With manufacturing operations
located around the world, the same PVB resin can encounter a
varying process environment caused by geography and seasonal
weather. Even within the same plant, the large scale of the operation can see the material moving from a cool climate-controlled
pre-processing area, through a nearly tropical, hot operating area

ANNUAL SHEAR CELL

(a)

(b)

(c)

Figure 1: Components of an annual shear cell include the powder trough (a) vane lid (b) configured for uniform shearing action. A filling accessory
(c) can help to fill the trough with the powder sample.

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POWDER FLOW TESTER

PVB RESIN RESULTS

Figure 2: The Brookfield powder flow tester utilizes shear cell methodology and intuitive software to display flow data.

Figure 3: Flow function curves generated on the modified Brookfield PFT

shear cell. The data are all for one type of PVB resin, at various temperature
(C) and humidity (%RH) conditions.

just upstream of the extruder. The matter is further complicated

by the need to run a variety of resin types for different products. Clearly, the ability to quantitatively characterize all resin
products across the known range of operating conditions was not
only beneficial for Solutia, but a critical step in the continuous
optimization of processing conditions and equipment.

conditions is summarized by the flow function curves in

Figure 3.
PVB resin, the main ingredient in a very strong yet flexible
sheet product, isnt a free flowing material, and becomes less so
with increasing temperature. For one particular resin, the flow
function changed from easy flowing to very cohesive, spanning
three flow regimes purely as a function of a 20C temperature
change. An unexpected result of this test was the relative independence of this resins flow function to increasing humidity
level. It was hypothesized that elevated humidity levels would
compound the effects of higher temperature. However, results
showed that this was not the case; temperature was the driving
factor for flow function behavior. This one example shows the
value that the modified PFT was able to provide. Knowing that
humidity wasnt a strong influence on performance allowed
R&D to concentrate on controlling temperature alone.

Temperature and Humidity: The Solution

After looking at various instruments for testing powders,

Solutia settled on Brookfield Engineerings powder flow tester
(PFT) (Figure 2), which utilizes shear cell methodology and
intuitive software to display flow data. However, the PFT is
rated for environmental conditions of 0C40C at 20%80%
relative humidity (RH). While the temperature range was
adequate, Solutia needed to ramp humidity levels to 95% RH.
They approached Brookfield with the issue.
Solutia planned to place the entire tester inside of a steady
state environmental chamber (Blue M CEO-916) to allow for
testing at defined temperature and humidity levels necessary
to characterize their product. The problem is that at levels of
humidity past 80%, moisture would begin to form inside of
the PFT instrument and cause the electronics to fail.
Working in concert with Brookfield, the solution was to
fully seal the exterior housing of the instrument and add two
purge fittings: inlet and outlet. These purge fittings would be
used to pump cool air through the instrument while running a
test at elevated temperature and humidity levels before processing begins. Brookfield initially tested the modified instrument
and then turned it over to Solutia for more robust testing in
their environmental chamber on their products.
Data Results

One example of an interesting and somewhat unexpected finding provided by the ability to test at defined environmental
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Conclusion

When testing powder flow behavior at higher temperature and

humidity levels, a solution does exist. The described method
utilizing a modified Brookfield PFT has been running successfully at Solutia for almost two years. The data gathered has
been valuable to ongoing process development.
Thanks to close cooperation between Solutia and Brookfield to address temperature and humidity level problems, a
powder test method and solution for enhanced equipment
design were developed jointly. This version of the PFT is now
available to the general powder processing industry where similar temperature and humidity issues may require attention.
Dr. Erik Miller is advanced mechanical engineer at Solutia/Eastman
Chemical Co. He can be reached at eemill1@eastman.com. Vinnie Hebert is senior sales engineer at Brookfield Engineering Laboratories, Inc.
Contact him at v_hebert@brookfieldengineering.com.

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