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
M
any stable processes can
be accurately tracked
and controlled by tak-
ing 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 cur-
rent status every few seconds.
Online analysis provides a continu-
ous stream of data to the programma-
ble logic controller (PLC) or other con-
trol 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 facili-
tates have provided an alternative to
offline analysis and the manual con-
trol that typically accompanies it.
For solids processes, particle size is
frequently the key variable, and there-
fore 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 laser-
diffraction 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 en-
hanced product quality. More recently,
new developments have made online
analysis via laser-diffraction technol-
ogy 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 par-
ticles present, which interrupt the laser
light beam. Relatively small particles
scatter light at wide angles with low in-
tensity whereas larger particles scatter
light at narrow angles with high inten-
sity. A diffraction pattern — a series of
concentric rings of diminishing intensity
— can therefore be detected and ana-
lyzed, to determine the particle size dis-
tribution of the sample (Figure 1).
well. Laser-diffraction particle-size
analyzers can now be used reliably
for a range of wet systems, from emul-
sions to highly concentrated slurries,
to achieve benefits similar to those en-
joyed 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 man-
ual control or switching to automatic
control
• Fully understand the interactions
between different process param-
eters and/or carry out systematic
studies to fully optimize the process
(for an example, see box, p. 3)
• More consistently manufacture prod-
uct 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,
CHEMICAL ENGINEERING WWW.CHE.COM NOVEMBER 2005
FIGURE 1. In laser diffraction, a dif-
fraction 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 mea-
surement technology must address
the challenges posed by wet process
applications — sample extraction and
preparation in particular — and in-
corporate 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 sound-
velocity measurement, are attractive
in that they can be used on slurries
that are opaque and electrically non-
conducting, but have the drawback
of being highly sensitive to the pres-
ence of entrained air bubbles. Opti-
cal-image analysis methods are in-
valuable for the production of particle
shape data and for the detailed analy-
sis of individual particles but, being
based on particle counting, can result
55
 Solids Processing �����

��������������
������������
Using Online Measurements to Determine the
Effect of Process Parameters

H
omogenizers are widely used within the food, dairy, cosmetic and pharmaceu-
tical 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 operat-
ing 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 tech-
nique in that it rapidly generates con-
sistent, volumetric particle-size analy-
sis without the need for any external
calibration. It is non-destructive and
robust in terms of ambient condi-
tions. 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 trans-
parent to some degree.
It is primarily the constraint of nec-
essary transparency that has previ-
ously limited the use of online laser-
diffraction technology in a range of wet
applications. However, with the devel-
opment of mathematical algorithms,
which take account of multiple scatter-
ing 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 exam-
ple consists of oil-in-water emulsions
common in oil-rig effluent streams,
which must be directly analyzed for
56 CHEMICAL ENGINEERING WWW.CHE.COM NOVEMBER 2005
environmental monitoring require-
ments. Dilute flocculating systems in
the pharmaceutical industry have also
been studied directly using the laser-
diffraction method. For other systems,
however, direct analysis is more diffi-
cult, a key challenge being the effec-
tive design of the process interface
and appropriate sample preparation.
Slurry handling, for instance, is a no-
toriously difficult issue for the process
industries, particularly at the rela-
tively low flows that can be associated
with sample lines. Thick, hot and sticky
slurries need well-designed sample-ex-
traction systems to avoid the problem
of blocking, and subsequently must be
handled carefully. Mobile calcium-car-
bonate slurries, for example, can set
solid after the loss of only a small pro-
portion of the diluting solvent.
Studies have shown that for reliable
measurement by laser diffraction, a
minimum of 30–60% of the laser light
needs to pass through the sample (de-
pending 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 ap-
plications, therefore, sample dilution
is an important step. Other condition-
ing processes may also be required; for
example, additives or ultrasonics may
be required to prevent particle ag-
glomeration, 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 poten-
tial for blockage must be carefully
considered and mitigated
• The extent of dilution required, to-
gether with the optimum number
of dilution stages — investigation
of the effects of dilution on the par-
ticles is necessary in the laboratory
before a process solution can be im-
plemented. 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 ap-
plication of ultrasonics to the system
• Any tendency of the material to dis-
solve, as a result of changes in su-
persaturation, may place limitations
on the dilution of the media
• Uninterrupted flow through the
sample system — settling and foul-
ing 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, sam-
ple extraction from the process can be
achieved using a simple eductor; but
for more-demanding slurries, more-
complex systems are required.
Static sampling with tank dilu-
tion. Mineral processors typically need
to sample and analyze high-tonnage,
 ���������
���������

�������

�������
����������

�������‘������

����������� ������‘������
FIGURE 3. An effective sample dilution
system needs to dilute the sample repre-
sentatively, be highly reliable and prefer-
FIGURE 2. A typical configuration for ably not require significant manual inter-
an online wet particle-size measurement vention for maintenance, operation, or
system is shown here cleaning purposes

concentrated slurry streams with spe-
cific gravities in the range of 2–8. For
many applications in this industry a
two-stage sampling procedure, in com-
bination with dilution in a continuous
stirred tank, has proven highly effec-
tive. The particles measured typically
have a diameter of around 10–1,000
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 50–170 L/min
is removed from the bulk flow, luted by mixing it
which is typically tens of tons with water in a dilu-
per hour, using a static sampler tion tank. The sample-di-
operating under gravity flow. The sec- lution ratio is typically in the range of
ondary sampling system then cuts a 10–100 and residence time within the
representative 0.01–0.03-L slice from tank around 1 min. The resulting sam-
the 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 con-
0.18 L/min is provided for dilution. centration of the sample measured
      
The secondary-flow sample is di- can be controlled by altering either

������������� Another Vision

��������� in process simulation
State of the art solutions
with dedicated support
• Unique time-tested thermodynamic package
• Best in class numerical methods
• Tailored and open solutions
• CAPE Open compliant software
• Comprehensive unit operation libraries
• User data integration capabilities
• Easy to learn and use solutions
• Process engineering support by experts
• Unmatched customer service quality
• Hundreds successful implementations
• Affordable pricing

����������������������������������
��������

�����������������������������������
�����������������������������������������
�������������������������������������
��������������������������������������������
�������������������������������������
���������
����������������������������������������
����������������������������
�������������������������
������������������������
������������������
������������������������
��������������������
Software & Services Solutions for Process Modeling,
Simulation and Optimization
General steady-state process simulation - Simulation of nitric acid plants and nitrous
vapors absorption columns - Simulation of batch distillation columns and of batch
chemical reactors - Pure component and mixtures thermodynamic properties and
fluid phase equilibrium calculations - Optimization and management of energy production
plant - Process data management - Application consulting - Custom software development

Tel: +33(0)562 882 430 - Fax: +33(0)562 882 439 - email: info@prosim.net - www.prosim.net
���������������������������������������������������������������
Circle 32 on p. 33 or go to adlinks.che.com/4822-32 Circle 33 on p. 33 or go to adlinks.che.com/4822-33
CHEMICAL ENGINEERING WWW.CHE.COM NOVEMBER 2005 57
 �����

�������������������
�����
Solids Processing
����

the secondary-sample cutting fre- ���� FIGURE 4. These

quency or the dilution ratio, allowing
the approach to be tailored to a range
of different applications. Overall mea-
surement 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 ef-
fectively replicate continuous online
measurement. For example, at a clay
producing facility, an analyzer was re-
quired to measure the particle size of
material leaving a ball mill. The slurry
to be characterized was hot, sticky, and
concentrated, with relatively fine par-
ticles — around 10 microns. Continu-
ous sample extraction posed a signifi-
cant challenge, and sample dilution
was also required.
����
���� ���� �����
���������������������
A rotating sphere with a central 8-ml
cylindrical channel was used to success-
fully 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 5–8 with water;
the relatively low dilution factor of this
initial stage prevents dilution shock.
For further dilution, a two-stage ver-
sion 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
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 ef-
fective 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 fur-
ther identical dilution stages.
At each stage, the throat, which ef-

DOUBLE WALL
PLASTIC STORAGE TANKS
All-in-one Design,
Saves Valuable Floor
Space.
Elliminates the Need for
Containment Pallets. �������������������������������
���������������������������
50 GALLON TANK ������������������������������
DESIGNED TO FIT
THROUGH A 28” ���������������������������
DOORWAY/OPENING! ������������������������
�
Choose From 12 ���������������������������������
Sizes in 50 - 6,000 Shown with optional pump
���������������������������������
Gallon Capacities ����������������������������
���������������������������������
������������������������������
������������������������������
Sales office open 8AM - 8 PM EST INDUSTRIES, INC.
1 8 0 0 2 7 5 2 4 3 6 c h e m t a i n e r. c o m
• • •

Circle 34 on p. 33 or go to adlinks.che.com/4822-34

58 CHEMICAL ENGINEERING WWW.CHE.COM NOVEMBER 2005

 Solids Processing
fectively forms a venturi mixer, ensures
rapid intermixing with the clean dilu-
ent, thereby delivering a homogeneous
sample to later dilution stages and ul-
timately the analyzer. The diameter of
nozzle used in the design dictates the
dilution ratio, which can be controlled
in the range of 2:1–5:1. The unit is suit-
able for particles with a maximum di-
ameter no greater than 150 microns.
The key test of any diluter is the con-
sistency of particle-size measurements
taken at different dilutions. Figure 4
shows data for a talcum slurry mea-
sured using the diluter shown in Figure
3. The extent of dilution has no impact
on particle size, confirming the repre-
sentative nature of the dilution process
and the effectiveness of the design.
By combination of this diluter de-
sign and the rotating sampler, a con-
tinuous online analysis system for ball
mill monitoring at the clay production
facility has been achieved. The system
operates continuously, day and night,
������������
60 CHEMICAL ENGINEERING WWW.CHE.COM NOVEMBER 2005
producing a measurement every 30
sec. Currently, the data produced are
used to more optimally respond to
changes in feed quality and to moni-
tor 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 ef-
ficiency, and therefore regular change-
out 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. ■ interface solutions as well as working to enhance
Edited by Rebekkah Marshall
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 Univer-
sity 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 Instru-
ments in Boston, Mass. Since returning to Mal-
vern 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 Mal-
vern Instruments Ltd. (Email:
Alain.Blasco@malvern.
co.uk). Alain joined Malvern
Instruments SA (France) in
the 1990’s, working first in
customer support, and later
designing new products in
response to specific customer
requirements. He has first-
hand experience of online solutions. A founder
member of Malvern’s process department, Alain
now contributes to the development of process-
the performance of measurement sensors.
���������������������