Solids Processing

Online Particle Analysis

In Wet Processes
Discover how laser-diffraction technology can make
these measurements possible, even in tough slurries
David Pugh and Alain Blasco, Malvern Process Systems

any stable processes can

be accurately tracked
and controlled by taking samples every couple
of hours for an offline particle size
analysis in the laboratory. However,
for unstable processes or those where
significant increases in profit can be
generated by closing the loop, online
analysis can be highly beneficial.
Where offline measurements may
miss key events that occur outside of
their once-every-two-hour snapshots,
online analysis records all events
nearly like a film, updating the current status every few seconds.
Online analysis provides a continuous stream of data to the programmable logic controller (PLC) or other control system, and ensures that process
behavior can be fully observed and
acted upon in a timely fashion. For a
number of years, online analysis and
the automated control that it facilitates have provided an alternative to
offline analysis and the manual control that typically accompanies it.
For solids processes, particle size is
frequently the key variable, and therefore online analysis can be highly
beneficial. For dry-solids handling
processes, in industries as diverse as
pharmaceuticals and cement, online
particle size analyzers based on laserdiffraction technology have been used
successfully for many years (see box,
above). These instruments generate
significant cost benefits in the form
of improved process efficiency and enhanced product quality. More recently,
new developments have made online
analysis via laser-diffraction technology accessible for wet processes as

HOW DOES LASER

DIFFRACTION WORK?
When a focused beam of light is shone
through a sample it is scattered by particles present, which interrupt the laser
light beam. Relatively small particles
scatter light at wide angles with low intensity whereas larger particles scatter
light at narrow angles with high intensity. A diffraction pattern a series of
concentric rings of diminishing intensity
can therefore be detected and analyzed, to determine the particle size distribution of the sample (Figure 1).

well. Laser-diffraction particle-size

analyzers can now be used reliably
for a range of wet systems, from emulsions to highly concentrated slurries,
to achieve benefits similar to those enjoyed by dry processors.

Benefits of online analysis

At plants where a switch to online

analysis has been made, it is often
possible to achieve the following:
Control the plant more effectively
during steady-state and transient
operation, either by improving manual control or switching to automatic
control
Fully understand the interactions
between different process parameters and/or carry out systematic
studies to fully optimize the process
(for an example, see box, p. 3)
More consistently manufacture product with the required specification
Minimize certain variable costs
such as those associated with waste
or energy consumption during size
reduction
More rapidly identify process upsets,

FIGURE 1. In laser diffraction, a diffraction pattern a series of concentric

rings of diminishing intensity are
analyzed to determine the particle-size
distribution of the sample

hence minimizing their impact

To achieve such benefits, however,
fully automated particle-size measurement technology must address
the challenges posed by wet process
applications sample extraction and
preparation in particular and incorporate the appropriate techniques
to overcome them.

Why laser diffraction?

A variety of different technologies can

be used for wet-process particle-size
analysis, all of which have different
strengths and weaknesses. Ultrasonic
techniques, recently combined with
gamma-ray transmission and soundvelocity measurement, are attractive
in that they can be used on slurries
that are opaque and electrically nonconducting, but have the drawback
of being highly sensitive to the presence of entrained air bubbles. Optical-image analysis methods are invaluable for the production of particle
shape data and for the detailed analysis of individual particles but, being
based on particle counting, can result

CHEMICAL ENGINEERING WWW.CHE.COM NOVEMBER 2005

55

Solids Processing

Using Online Measurements to Determine the

Effect of Process Parameters

omogenizers are widely used within the food, dairy, cosmetic and pharmaceutical industries to produce emulsions with the required droplet size, and hence,
the desired properties; droplet size impacts directly on product taste, consistency,
performance and stability. With offline analysis this type of study is time consuming and
prone to error as a result of, for example, operator variability and sample stability. With
online analysis, however, the effects of processing variables on droplet size are rapidly
determined and optimal conditions more quickly identified.
This type of systematic study can be carried out during product development or at the
beginning of a production run to optimize the processing response to a change in, for
example, feed-material quality. In either case, the rapid identification of optimal operating conditions and the accompanying development of improved process knowledge,
lead directly to better manual or automatic control, enhanced process efficiency and
variable cost savings.

in highly inaccurate mass or volume

size distributions, especially if only a
limited number of particles has been
taken account of.
Laser diffraction (or low angle laser
light scattering) is an attractive technique in that it rapidly generates consistent, volumetric particle-size analysis without the need for any external
calibration. It is non-destructive and
robust in terms of ambient conditions. Using modern systems, particles
across a broad size range, typically 0.5
to 1,000 mm for wet systems, can be
measured accurately. Its drawback is
that it requires the media to be transparent to some degree.
It is primarily the constraint of necessary transparency that has previously limited the use of online laserdiffraction technology in a range of wet
applications. However, with the development of mathematical algorithms,
which take account of multiple scattering and extend the concentration range
over which laser diffraction can be used,
and more effective sample extraction
and preparation systems, which are
capable of producing a representative
sample stream (from a concentrated
slurry) that is appropriate for analysis,
the applicability of the technique has
been significantly extended.

Sampling and
sample preparation

For some dilute-stream applications

a laser diffraction instrument can be
simply installed inline for particle size
measurement (Figure 2). One example consists of oil-in-water emulsions
common in oil-rig effluent streams,
which must be directly analyzed for
56

environmental monitoring requirements. Dilute flocculating systems in

the pharmaceutical industry have also
been studied directly using the laserdiffraction method. For other systems,
however, direct analysis is more difficult, a key challenge being the effective design of the process interface
and appropriate sample preparation.
Slurry handling, for instance, is a notoriously difficult issue for the process
industries, particularly at the relatively low flows that can be associated
with sample lines. Thick, hot and sticky
slurries need well-designed sample-extraction systems to avoid the problem
of blocking, and subsequently must be
handled carefully. Mobile calcium-carbonate slurries, for example, can set
solid after the loss of only a small proportion of the diluting solvent.
Studies have shown that for reliable
measurement by laser diffraction, a
minimum of 3060% of the laser light
needs to pass through the sample (depending on the mean size and span
of the particle size distribution); this
typically equates to a solids content of
0.005-0.2% by volume. For many applications, therefore, sample dilution
is an important step. Other conditioning processes may also be required; for
example, additives or ultrasonics may
be required to prevent particle agglomeration, or break up aggregates.
In summary, the main issues needing
careful consideration in the design of
a sample system are as follows:
Reliable extraction of a sample at
the process interface any potential for blockage must be carefully
considered and mitigated
The extent of dilution required, to-

CHEMICAL ENGINEERING WWW.CHE.COM NOVEMBER 2005

gether with the optimum number

of dilution stages investigation
of the effects of dilution on the particles is necessary in the laboratory
before a process solution can be implemented. Factors to be considered
include zeta potential of the particle,
agglomeration effects and the time
delay before these effects take place
in the proposed dilution medium
If a material does tend to aggregate
as a result of changing pH, then the
appropriate solution might require
implementation of additives or the application of ultrasonics to the system
Any tendency of the material to dissolve, as a result of changes in supersaturation, may place limitations
on the dilution of the media
Uninterrupted flow through the
sample system settling and fouling must be avoided
The suitability of either batch or
continuous configurations while
a continuous sampling loop may be
preferred, problems with excessive
diluent or sample usage may result
in the need for a batch system. In
this latter case, line flushing and
cleaning is essential to minimize
operation problems and maintain
data integrity

Sample extraction and dilution

For free-flowing liquid systems, sample extraction from the process can be
achieved using a simple eductor; but
for more-demanding slurries, morecomplex systems are required.
Static sampling with tank dilution. Mineral processors typically need
to sample and analyze high-tonnage,

FIGURE 2. A typical configuration for

an online wet particle-size measurement
system is shown here

FIGURE 3. An effective sample dilution

system needs to dilute the sample representatively, be highly reliable and preferably not require significant manual intervention for maintenance, operation, or
cleaning purposes

concentrated slurry streams with specific gravities in the range of 28. For
many applications in this industry a
two-stage sampling procedure, in combination with dilution in a continuous
stirred tank, has proven highly effective. The particles measured typically
have a diameter of around 101,000
microns in laser diffraction terms
they tend to lie at the coarser end of
the spectrum.
In the first stage of this sampling
process a primary flow of 50170 L/min

luted by mixing it
is removed from the bulk flow,
with water in a diluwhich is typically tens of tons
tion tank. The sample-diper hour, using a static sampler
operating under gravity flow. The sec- lution ratio is typically in the range of
ondary sampling system then cuts a 10100 and residence time within the
representative 0.010.03-L slice from tank around 1 min. The resulting samthe primary flow every 10-30 s by mov- ple is routed to the optical head and
ing the sample line across a stationary analyzed in its entirety. Since the only
cutter. The bulk of the primary flow is material added during the sampling
returned to the process and a represen- process is water, all of the stream can
tative secondary flow of around 0.02 be recycled into the process. The concentration of the sample measured
0.18 L/min is provided for dilution.

The secondary-flow sample is di- can be controlled by altering either

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CHEMICAL ENGINEERING WWW.CHE.COM NOVEMBER 2005

57

Solids Processing
the secondary-sample cutting frequency or the dilution ratio, allowing
the approach to be tailored to a range
of different applications. Overall measurement time using this approach is
around 2 min.
Rotating sampler/diluent powered
diluter. A rotating-type sampler
similar in design to a four-way valve
can be used to extract slugs of flow
from a process stream if a continuous
sample stream cannot be successfully
taken. The resulting system can effectively replicate continuous online
measurement. For example, at a clay
producing facility, an analyzer was required to measure the particle size of
material leaving a ball mill. The slurry
to be characterized was hot, sticky, and
concentrated, with relatively fine particles around 10 microns. Continuous sample extraction posed a significant challenge, and sample dilution
was also required.

A rotating sphere with a central 8-ml

cylindrical channel was used to successfully extract a sample. As the sphere
rotated, a slug of slurry was removed
from the process, and then washed
through the sampler with water. This
water began the dilution process and
cleaned the rotating sphere to prevent
blockages. The initial sample was fed
into the pre-diluter tank, where it was
diluted by a factor of 58 with water;
the relatively low dilution factor of this
initial stage prevents dilution shock.
For further dilution, a two-stage version of a diluent-powered, commercially
available diluter was used to let down
the sample, firstly by a factor of two and
then by a factor of five. The initial stage
prepared the sample for more intense

FIGURE 4. These
data correspond
to a talcum slurry
diluted using the
unit illustrated in
Figure 3

dilution and eliminated the dependency

of dilution factor on the distance from
the sample line.
Figure 3 shows a schematic of a
five-stage version of the diluter. An effective sample dilution system needs
to dilute the sample representatively,
be reliable, and preferably not require
significant manual intervention for
maintenance, operation or cleaning
purposes. This diluter is mechanically
relatively simple and trouble-free,
with has no moving parts. The throat
and tip of the unit are designed such
that the diluent entrains a slurry
sample into the central tube. Diluted
sample flows through the tube to further identical dilution stages.
At each stage, the throat, which ef-

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CHEMICAL ENGINEERING WWW.CHE.COM NOVEMBER 2005

Solids Processing
fectively forms a venturi mixer, ensures
rapid intermixing with the clean diluent, thereby delivering a homogeneous
sample to later dilution stages and ultimately the analyzer. The diameter of
nozzle used in the design dictates the
dilution ratio, which can be controlled
in the range of 2:15:1. The unit is suitable for particles with a maximum diameter no greater than 150 microns.
The key test of any diluter is the consistency of particle-size measurements
taken at different dilutions. Figure 4
shows data for a talcum slurry measured using the diluter shown in Figure
3. The extent of dilution has no impact
on particle size, confirming the representative nature of the dilution process
and the effectiveness of the design.
By combination of this diluter design and the rotating sampler, a continuous online analysis system for ball
mill monitoring at the clay production
facility has been achieved. The system
operates continuously, day and night,

producing a measurement every 30

sec. Currently, the data produced are
used to more optimally respond to
changes in feed quality and to monitor the performance of the milling
media in order to determine when
fresh material is required. (The balls
used to promote milling wear out over
a period of weeks, reducing milling efficiency, and therefore regular changeout is required.) A long term aim for
the facility is automated mill control,
which is now a real possibility.
For alternative applications, the
size of bore, number of rotations of the
sampler, volume to which the sample
is initially diluted, and number of
stages of the main diluter, could all
be altered to control the concentration
of solids at the optical head and meet
the requirements of the process. This
approach is therefore applicable to a
wide range of processes with hard to

handle slurries.
Edited by Rebekkah Marshall

60

CHEMICAL ENGINEERING WWW.CHE.COM NOVEMBER 2005

Authors
David Pugh is European
manager for Malvern Process
Systems, a division of Malvern
Instruments Ltd. (Enigma
Business Park, Grovewood
Rd, Malvern, Worcestershire,
WR14 1XZ, U.K.; Phone: +44
(0) 1684 892456; Fax: +44 (0)
1684 892789; Email: David.
Pugh@malvern.co.uk). He has
a B.S.ChE from the University of Aston in Birmingham.
He joined Malvern Instruments Ltd. in 1990 as
sales manager in Europe for laboratory particle
sizers, before working as business development
manager in the U.S. office of Malvern Instruments in Boston, Mass. Since returning to Malvern UK six years ago, he has been in charge of
sales within the European process market.
Alain Blasco is technical
manager for Malvern Process
Systems, a division of Malvern Instruments Ltd. (Email:
Alain.Blasco@malvern.
co.uk). Alain joined Malvern
Instruments SA (France) in
the 1990s, working first in
customer support, and later
designing new products in
response to specific customer
requirements. He has firsthand experience of online solutions. A founder
member of Malverns process department, Alain
now contributes to the development of processinterface solutions as well as working to enhance
the performance of measurement sensors.