Measurement Techniques To Monitor and ControlFluidization Quality in Fluidized Bed Dryers: AReview

Drying Technology
An International Journal
ISSN: 0737-3937 (Print) 1532-2300 (Online) Journal homepage: http://www.tandfonline.com/loi/ldrt20
Measurement Techniques to Monitor and Control

Fluidization Quality in Fluidized Bed Dryers: A
Review
Mortaza Aghbashlo , Rahmat Sotudeh-Gharebagh , Reza Zarghami , Arun S.
Mujumdar & Navid Mostoufi
To cite this article: Mortaza Aghbashlo , Rahmat Sotudeh-Gharebagh , Reza Zarghami , Arun
S. Mujumdar & Navid Mostoufi (2014) Measurement Techniques to Monitor and Control
Fluidization Quality in Fluidized Bed Dryers: A Review, Drying Technology, 32:9, 1005-1051, DOI:
10.1080/07373937.2014.899250
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Date: 10 January 2016, At: 21:06
Drying Technology, 32: 10051051, 2014

Copyright # 2014 Taylor & Francis Group, LLC
ISSN: 0737-3937 print=1532-2300 online
DOI: 10.1080/07373937.2014.899250
Review Article
Measurement Techniques to Monitor and Control
Fluidization Quality in Fluidized Bed Dryers: A Review
Mortaza Aghbashlo,1 Rahmat Sotudeh-Gharebagh,2 Reza Zarghami,2
Arun S. Mujumdar,3 and Navid Mostou2
Downloaded by [Diego Arroyave] at 21:06 10 January 2016
Department of Agricultural Machinery Engineering, Faculty of Agricultural Engineering and

Technology, University of Tehran, Karaj, Iran
2
Multiphase Systems Research Lab., Oil and Gas Processing Centre of Excellence, School of
Chemical Engineering, College of Engineering, University of Tehran, Tehran, Iran
3
Department of Food Engineering, King Mongkuts University of Technology Thonburi,
Bangkok, Thailand
Fluidized bed dryers (FBD) are commonly employed in many

industries to dry particulate solids. FBDs provide good solids mixing,
high rates of heat and mass transfer, and relative ease of material
handling. For efcient operation, it is important to be able to monitor
and control the uidization regime, particle size distribution (PSD),
moisture content, and bulk density as well as product chemical
properties. This review provides an overview of the trends in the
application of different experimental techniques to monitor and
control the hydrodynamic conditions of FBDs which inuence the
particle physiochemical properties. This review covers a wide range
of measurement techniques, including infrared moisture sensor
(IR), near infrared (NIR) spectroscopy, analysis of pressure uctuations, optical imaging techniques, acoustic emission (AE), electrical
capacitance tomography (ECT), spatial lter velocimetry (SFV),
Raman spectroscopy, focused beam reectance measurement
(FBRM), microwave resonance technology (MRT), triboelectric
probes, positron emission particle tracking (PEPT), and some novel
techniques for monitoring and control of FBDs. The present review
summarizes the use of the diverse techniques and outlines their merits
and limitations. Prospects for future research in this area are also
identied. The measurement techniques can be used for research,
development, and operation of uidized bed equipment used in
non-drying applications as well.
Keywords Bed hydrodynamics; Control; ECT; IR; Moisture
content; NIR; Particle size distribution (PSD); PEPT;
Raman spectroscopy
Correspondence: Rahmat Sotudeh-Gharebagh, Multiphase

Systems Research Lab., Oil and Gas Processing Centre of Excellence, School of Chemical Engineering, College of Engineering,
University of Tehran, P.O. Box 11155-4563, Tehran, Iran; E-mail:
sotudeh@ut.ac.ir
Color versions of one or more of the gures in the article can
be found online at www.tandfonline.com/ldrt.
INTRODUCTION
As widely used drying systems, FBDs have found
many applications in almost all agricultural, biochemical,
chemical, pharmaceutical, food, ceramics, polymer,
dyestuff, and other process industries. FBDs can be utilized
as an efcient dehydration method, not only for moist
particulate and granular products with susceptibility to uidization, but also for removing moisture from suspensions,
solutions, dilute pastes, or sludges in a bed of inert particles.[1,2] Particulate materials are commonly dried by hot
air or superheated steam to a desired level of moisture content. Fluidization provides high rates of heat and mass
transfer, improves uniformity of temperature prole across
the bed, facilitates material handling and solids mixing, permits processing of temperature-sensitive solids, and offers
high thermal efciency of drying process. Generally, FBDs
can be used for drying of particulate materials, agglomerates, granules, coatings, and layers. In uidized bed granulation, coating, and agglomeration, the complexity becomes
even more serious because of a series of transient interconnected phenomena; i.e., binding liquid spraying, particle
agglomeration, and wall deposition. Thus, these processes
are very strict and even impossible to estimate, monitor,
and control during the operation. Moreover, scale-up of
ill-dened processes, such as drying, is well-known to be a
problematic practice of industry and can be expensive
when it goes wrong. Traditionally, FBDs are inspected by
simple methods with easily measurable variables, such as
temperature and humidity of the exhaust air, bed axial
and average temperatures, and variation of pressure drop
and temperature throughout the bed. However, these
measurements provide little insight into the complex hydrodynamic phenomena such as incipient deuidization and
1005
1006
AGHBASHLO ET AL.
physicochemical properties of particles and are, therefore,

ineffective and not useful for real-time monitoring and
good closed-loop process control.[3] Stability of uidization
in FBDs plays an important role in the quality of the
nished product by uniform distribution of the ow of
the drying media, enhancing heat and mass transfer rates
and preventing collapse of the bed. Moisture content, bulk
density, and PSD are other critical parameters, signicantly
affecting the stability of uidization and the quality of
end-products. In some cases, knowledge of the chemical
properties of materials being dried is also very critical. On
the other hand, to develop an automated FBD system for
specied end-product quality and monitoring, real-time
measurement techniques are often integrated with mechanical and instrumental facilities to avoid in-process manual
manipulation.
According to the Food and Drug Administration
(FDA), Process Analytical Technology (PAT) can be
divided into three categories, including at-line, on-line,
and in-line analyzers,[4] as shown in Fig. 1. PAT has been
used to dene a systematic approach for real-time measurements to design, analyze, scale up, and control manufacturing processes through the monitoring of critical quality and
performance properties for primary and in-process materials. At-line analyzers measure the required properties by
taking a sample, isolating it from the environment, and analyzing it in close proximity to the process stream. On-line
analyzers determine the desired characteristics of materials
by directing the sample from the process to measurement
device and returning it to the process stream in most situations. It should be mentioned that in on-line mode the drying uid is commonly circulated in the measuring loop to
keep constant the temperature of the sample. In-line analyzers (intrusive or non-intrusive) are quick measuring devices
or probes to record the sensing data without removing a
sample by direct placing of them into the process stream.[5]
FIG. 1.
Schematic of in-line, online, and at-line product measurements.
In the complex and dynamic environment associated

with FBDs, it becomes necessary to explore technological
and scientic solutions for preventing deuidization and
ensuring mean quality parameters of the particles during
the process. Furthermore, application of monitoring and
control techniques plays an important role in several major
areas in research and industry to optimize and automate the
process, to assure high reproducibility in the end-product
quality, to enhance security aspects of the process, to
minimize the number of failures in batches, and to lower
expenditures of energy and human resources.[3] The aim
of this article is to review and update the usage of various
techniques and instruments available for monitoring and
controlling of uidization and physiochemical characteristics of particles. In particular, this review covers applications of an infrared moisture sensor (IR), near infrared
spectroscopy (NIR), pressure uctuations, optical imaging
techniques, acoustic emission (AE), electrical capacitance
tomography (ECT), spatial lter velocimetry (SFV),
Raman spectroscopy, focused beam reectance measurement (FBRM), microwave resonance technology (MRT),
triboelectric probes, positron emission particle tracking
(PEPT), and some other miscellaneous and innovative strategies for control.
van Ommen and Mudde[6] have reported the use of
different techniques for measuring the voidage distribution
in uidized beds. Burggraeve et al.[4] have reviewed the analytical techniques for monitoring and control of uidized bed
granulators for pharmaceutical application. da Silva et al.[3]
discussed tools for monitoring and control of coating and
granulation processes in uidized beds. Published reviews
have also looked at the application of measurement techniques in uidized beds,[7] process control methods and scale-up
of pharmaceutical wet granulation processes containing
uidized bed granulating,[8] control engineering in drying technology consisting of FBDs,[9] and near infrared spectroscopy
and chemometrics in pharmaceutical technologies including
FBDs.[10] However, this review differs from previous ones
by including all aspects of FBDs utilized for drying itself in
uidized beds as well as drying during uidized bed coating,
granulation, and agglomeration processes and presenting the
most employed techniques for process monitoring, control,
and automation. In addition, advantages and disadvantages
of each technique are mentioned and recommendations
and perspectives are provided for future works.
The diagnostic techniques discussed in this review are
also applicable to other gas-solids contacting devices such
as modied uidized beds, spouted beds, circulating uid
beds, vibrating uid beds, pneumatic conveyors, and various designs of uidized bed reactors as well. An interesting
feature of FBDs is that particle wetness, particularly at
the surface, can affect uidization quality signicantly.
For very high wetness it is possible to cause deuidization,
which affects the performance adversely.
MONITORING OF FLUIDIZATION QUALITY IN DRYERS
MONITORING TECHNIQUES
Conventional Techniques
Traditionally, monitoring particle moisture and process
end-points, the point at which a drying is completed,
in FBDs has been carried out based on measurement of
process variables such as outlet air temperature, outlet air
humidity, inlet and outlet temperature difference, and other
simple measurements of miscellaneous parameters according to the dryer characteristics. Particle size measurement
and tests of the chemical properties of the product are
performed by acquiring samples during the processing
and subsequent analysis using off-line techniques. Fluidization quality was usually identied by visual observation and
evaluation of global hydrodynamic parameters by applying
empirical models. The most important studies regarding the
application of conventional techniques for monitoring of
FBDs are listed in Table 1.
Alden et al.[11] applied the temperature difference techniques using simple psychometric calculation to control the
process end-point in FBD. The end-point of the granulation
process was successfully identied and controlled by a computer program. Watano et al.[12] successfully examined the
uctuations of power consumption in an agitated uidized
bed granulator to monitor granule growth and to determine
the process end-point by computing the coefcient of
variation of the utilized power. In another investigation,
Watano et al.[13] developed a fuzzy controller for controlling the bed height, which was successively measured by
an ultrasonic sensor during uidized bed granulation. The
controller effectively prevented deuidization and channeling by controlling the bed height. Sivashanmugam and
Sundaram[14] developed two different empirical models for
predicting the pressure drop for both dilute and dense phase
ow regimes in FBD for ragi drying with an acceptable
deviation, and presented a correction coefcient for the
dense slugging ow regime. In a similar study, they distinguished the mixed ow behavior up to a certain particle
Reynolds number from the residence time distribution
studies.[15] El-Nans et al.[16] measured minimum spouting
velocity as a function of moisture content for drying of
sludge and found a decrease in the minimum spouting
velocity by progressing of the drying process. Temple and
van Boxtel[17,18] used simple measurements for continuous
and batch tea FBD based on wet material feed rate and
direct feedback of the moisture content and intermediate
exhaust temperature to design a full automated control
system. In addition, this research group has published several papers about design and application of a full automate
control system based on different methods of controller
tuning,[19] a custom-built electronic data logger applied to
combination of experimental ndings with modeling and
simulation results,[20] and an algorithm-employed transient
exhaust air temperature.[21] These strategies appropriately
1007
controlled the drying process better in most cases compared

to the manual control.
Larsen et al.[22] proposed a control strategy based on
in-process thermodynamics calculation using an alternative
thermodynamic factor according to enthalpies of actual and
adiabatic vented drying air during uidized bed coating.
Two separate control loops were suggested in order to
maximize the coating spray rate and keep the process in
mass and energy balance. An inner control loop controlled
the product temperature by the inlet air temperature and an
outer control loop controlled the relative outlet air
humidity and the degree of consumption of the potential
vaporization energy by the spray rate. Devahastin et al.[23]
correlated empirically the size of shrimp, bed height, and
nozzle diameter to the hydrodynamic characteristics of a
jet spouted bed of shrimp using the Buckingham p theorem.
The temperature difference method has shown an appropriate accuracy level in approximating the drying end-point,
in which the uidization activity signicantly affected
detection of the process end-point.[24] Yuzgec et al.[25] satisfactorily employed a model-predictive controller based on
the dynamic recurrent neural networks to predict moisture
content and product activity during bakers yeast drying
using data calculated from heat and mass equations
through dried granules. This methodology gave simulation
results in the short time required for real-time control applications. In a similar work, Koni et al.[26] optimized drying
conditions to maximize product quality while minimizing
the energy consumption by proposing a recurrent neural
network-based algorithm for developing quality and
process models which were solved by a genetic algorithm.
Matero et al.[27] satisfactorily used multi-way methods with
a few process variables to recognize successful batch
granulations from unsuccessful runs and achieved useful
information that can improve comprehension of the FBD.
Traditionally, easy-to-use simple techniques were used to
monitor FBDs. More recently, due to the dynamic and
complex nature of the FBD process, these simple techniques
are found to be unsuitable for some industrial applications
because of their great operator-dependency and often poor
repeatability. In some cases, these techniques can modify
the internal ow of the uidized bed, leading to interference
with the actual process measurements. On the other hand,
heat and mass balance equations commonly used to determine the end-point and estimate the moisture content of
particles in FBD with respect to inlet and outlet drying air
temperatures. However, drying of particles strongly
depends on the humidity of the inlet-air, a small change
of which may result in a considerable error in the predicted
value. Moreover, mechanistic models may fail due to simplifying assumptions and non-consistency between drying
batches.[28] Monitoring of FBDs by traditional techniques
is time-consuming and sometimes causes rejection of the
1008
Intelligent control
based on ultrasonic
height measurement
Watano et al.[13]
Lab-scale top-spray
agitated uidized bed
granulator
Top-spray agitated
uidized bed
granulator
Laboratory-scale FBD
Dryer type(s)
Residence time
To determine the ow
distribution using
pattern
pulse input of tracer
Measuring minimum
spouting velocity
Conventional control
Sivashanmugam
and
Sundaram[15]
El-Nans et al.[16]
Temple and van

Boxtel[17]
To identify some of the

limitations on a
controller in an
industrial FBD based
on modeling results
To characterize the bed

hydrodynamics and
mass transfer
coefcient
Pressure drop
measurement
Sivashanmugam
and
Sundaram[14]
Industrial-scale FBD
Lab-scale spouted FBD
Experimental annular
circulating FBD
To propose the empirical Laboratory-scale

models for calculating
annular circulating
pressure drop at
FBD
different ow regimes
Developing a fuzzy logic

controller for bed
height controlling
during uidized bed
granulating
Power consumption
To analyze the
for granule
granulation process
agitation along with
and progress of
coefcient of
particles
variation
Watano et al.[12]
To control and
instrument the FBD
Application(s)
Temperature
difference technique
Measurement
technique(s)
Alden et al.[11]
Author(s)
Remarks
Drying of Allopurinol and The developed program

lactose mixture granules
based on
obtained with
thermodynamics concept
Providone K30 in water
successfully detected
end-point of granulation
process.
Granulation of mixture
A practical method for the
of lactose and corn
determination of an
starch with
optimum operational
hydroxypropylcellulos
end-point in the tumbling
uidized bed granulation
was developed.
Lactose and cornstarch
Fuzzy logic controller
granulating with
favorably maintained the
hydroxypropylcellulose
bed height at the
predetermined value from
initial to nal stage of
uidized bed granulation.
Drying of Ragi
Two separate models were
suggested for computing
pressure drop for dense
slugging ow and dilute
phase ow regimes with
the average deviation of
10%.
Drying of Ragi particle
The theoretical mean
residence time using
one-dimensional tanks in
series and dispersion
model agreed well with
the experimental data.
Drying of sludge
Increasing the moisture
content of sludge particles
led to an increment in
minimum spouting
velocity.
Tea drying
Wet product feed rate
should be precisely
controlled to maintain
moisture discharge from
dryer at constant value.
Process target(s)
TABLE 1
Most important studies regarding the application conventional for FBDs monitoring
1009
Recoding the
minimum spouting
velocity and
maximum and
steady spouting
pressure drops
Temple et al.[21]
Devahastin
et al.[23]
Custom-made
electronic data
logger and
controller
Temple et al.[20]
Temple et al.[19]
Larsen et al.[22]
Temple and van

Boxtel[18]
To determine the bed

hydrodynamics
To detect the drying

end-point using inlet
and exhaust
temperature
measurement
To control the drying
process based on
thermodynamics
concept
To monitor and control

tea dryer
Experimental jet
spouted FBD
Lab-scale uidized bed

coater with both top
and bottom spraying
techniques
Lab-scale FBD
Experimental FBD
To control and monitor Continuous FBD

the dried product
moisture content based
on two feedback
controllers
Tuning of controllers
Continuous FBD
using different strategy
to precise controlling
of nal product
moisture
Shrimp drying
Sugar spheres and

microcrystalline
cellulose pellets coating
with Eudragit1 NE
30D, Eudragit1 RS
30D, and Aquacoat
ECD1 lm polymers
Developing an algorithm
for automatic end-point
determination
Tea drying
Tea drying
Tea drying
(Continued )
The thermodynamics model

was successfully
incorporated into a new
process control strategy
by calculating the degree
of utilization of the
potential evaporation
energy of the vented air
and the relative humidity
of exhausted drying air.
Three empirical correlations
were developed for
Reynolds number,
maximum pressure drop
and spouting pressure
drop based on the
Buckingham p method as
function shrimp and
dryer characteristics.
Inferential control based on

outlet air temperature
successfully controlled
moisture of outlet
product.
The integrated qualitative
measure and integral
squared error was the best
choice in controller
tuning of FBD under
different operating
condition.
The developed system was
satisfactorily installed in
the majority of related
factories and drying
process was controlled
better than manual
controlling.
The end-point was
successfully determined
by developed algorithm.
1010
[24]
Matero et al.[27]
Koni et al.[26]
Yuzgec et al.[25]
Lipsanen et al.
Author(s)
end-point
Application(s)
Dryer type(s)
Process target(s)
Remarks
Bench-scale uidized bed Granulation of mixture of The temperature difference

granulator
ibuprofen and a-lactose
technique satisfactorily
monohydrate by
identied drying
aqueous solution of
end-point at different
polyvinylpyrrolidone
humidity of drying air.
Industrial-scale FBD
Bakers yeast drying
The presented methodology
Articial intelligent
To predict the moisture
successfully
control based on
content and product
approximated the
activity using a
simple process
moisture content and
dynamic
measurement
product activity and
neural-network-based
accordingly an intelligent
model-predictive
control system suggested
control structure
based on simulation
solved by genetic
results.
algorithm
Intelligent control
To determine and
Large-scale batch FBD
Drying of bakers yeast
The optimal control
based on
control the optimal
algorithm by applying the
neural-networkconditions to maximize
recurrent neural network
based models and
product quality while
models for establishing
modied genetic
minimizing energy
the quality and process
algorithm using
consumption
models, solved through a
process variables
modied genetic
algorithm, was suggested
to promote the
performance of the drying
process of bakers yeast in
batch uidized bed.
The parallel factor analysis
Multi-way models
To distinguish the
Bench-scale top-spray
Granulation of
uidized bed
hydrophobic
PARAFAC2 method
with process
successful batch
granulator
pharmaceutical
provided a good
variables including
granulations from
unsuccessful runs
ingredient, hydrophilic
separation between the
mass temperature,
excipient in a
successful and
inlet air temperature
and outlet air
monohydrate form and
unsuccessful batches
compared with the
temperature
polymeric excipient with
PARAFAC method.
polyvinylpyrrolidone as
binder liquid
Temperature
difference method
Measurement
technique(s)
TABLE 1
Continued
product if the target condition is not met. Conventional

techniques frequently provide time-averaged information
about the bed hydrodynamics and particle properties.
Infrared (IR) and Near Infrared (NIR) Spectroscopy
IR spectroscopy applies the infrared zone of
electromagnetic radiation with longer wavelengths than
those of the visible light, varying from 700 nm to 1 mm,
and a frequency span of approximately 300 GHz up to
430 THz. The IR technique has been commonly utilized
for measuring the moisture in FBDs and is based on certain
IR wavelengths which are absorbed due to the hydrogen of
water molecules as they pass through the particulate
material (in the wave number range 1600 and 1700 cm 1).
NIR spectroscopy is a technique covering the transition
from the visible spectral range to the mid-infrared region
of the electromagnetic spectrum in the wavelength range
of 8002500 nm (wave number range 12,5004000 cm 1),
mainly indicating the vibrations of CH, OH, SH and
NH bands. Absorbance in the NIR region results from
molecular overtone and combination vibrations of the fundamental mid-infrared bands. Thus, the particle size and
moisture content can be tracked effectively using NIR spectroscopy due to the sensitivity of absorbance in this region to
variations in the moisture content, particle size, and chemical state.[3] Pasikatan et al.[29] have illustrated the basic
principles of NIR spectroscopy relevant to particle size
measurement and its dependency on sample preparations,
technique of presentation, reference methods, calibration
development, and validation. Roggo et al.[30] reviewed pharmaceutical applications of NIR spectroscopy chemometrics
in three different subsections, including qualitative analyses
and classications, regression methods and quantitative
applications, and online applications. The chemometric
methods used for analysis of NIR spectra were categorized
into three main approaches: mathematical pretreatments,
classication methods, and regression methods. Their study
also contained an overview of NIR spectroscopy application
to uidized bed granulation and coating to monitor online
the moisture content, chemical compound content,
end-point detection, and coating thickness. De Beer et al.[5]
comprehensively reviewed the use of NIR spectroscopy for
the in-process monitoring of pharmaceutical production
processes with special emphasis on pharmaceutics and dosage forms. A review of the literature, a summary of which
is given in Table 2, shows that a considerable number of
researchers have used NIR for monitoring of physicochemical properties of the product within the FBDs.
Watano et al.[31,32] employed an IR moisture sensor to
monitor moisture content during a uidized bed granulation process and established a fully automated system
by means of a moisture feedback controller and an adaptive
fuzzy controller for controlling the moisture, respectively. A
gain scheduling based on drying capacity was introduced
1011
into a fuzzy control system, which effectively controlled the

moisture content at various inlet air temperatures. Further,
Watano et al.[33] investigated IR absorption with various
powder characteristics, such as water-absorbing potential
and granule size, to create a relationship between granule
water content and the IR absorbance spectra. Generally,
the relationship between moisture content and the IR absorbance should be identied before granulation and drying for
accurate monitoring of the moisture using an IR probe. In
another study, the same research group reported that the
relationship between granule moisture content and the absorbance of IR spectra is not inuenced by the air ow rate of
the purge air for preventing particle adhesion, uidizing air
velocity, agitator rotational speed and spray mist size, while
it is affected signicantly by the uidizing air temperature
and the liquid ow rate at extremely low agitating speed.[34]
Kirsch and Drennen[35] successfully employed NIR spectroscopy in at-line mode to estimate the amount of polymer
coat to tablet core with a maximum standard error of 1.07%.
Inline NIR spectroscopy was also successfully applied for
predicting water uptake and size of particles during the uidized bed drying stage of granulating.[36] A good correlation
was also presented between NIR wavelengths and granule
size.[37] Rantanen et al.[38] proved that the moisture content
of granules during spraying and drying phases can be
approximated using the NIR spectrum with a standard error
of 0.2%. Morris et al.[39] employed a fast drying method by
using a higher inlet air temperature to accelerate the drying
progress without increasing the bed temperature beyond
safe limits towards the end of uidized bed drying of Ibuprofen granules along with real-time monitoring of moisture
using NIR spectroscopy. The NIR absorbance showed a
similar trend with the moisture ratio of the product during
the drying process. In a similar study, Wildfong et al.[44]
showed that NIR spectroscopy can successfully detect the
end-point of the granulation process and determine the
moisture content of the product quite well.
Rantanen et al.[40] employed a four-wavelength NIR sensor for monitoring uidized bed granulation=drying and
utilized three of the recorded spectra for moisture content
determination. In similar works, the same research group
proved that the measurement of water content during
granulation can be accurately carried out by NIR spectroscopy at a wavelength of around 1940 nm.[41,42] They
also studied the effects of different parameters on a fourwavelength NIR probe and compared ANN and PLS
regression for the prediction of the particles moisture
content. It was reported that ANN is more suitable for
approximation of the water content over PLS regression.[43]
Rasanen et al.[45] applied NIR spectroscopy to measure
the moisture content of several materials during drying in
multichamber microscale FBD equipment. Moisture content and drying phase were effectively tracked through three
wavelengths of the NIR region. However, inlet air humidity
1012
To determine the
amount of polymer
coat applied to tablet
cores
Kirsch and
Drennen[35]
NIR spectroscopy
To investigate the effect Lab-scale top-spray

of operating condition
on the accuracy of
granulator
moisture measurement
by IR moisture sensor
Experimental uidized
bed coater
Lab-scale top-spray
granulator
Watano et al.[34] IR moisture sensor
Experimental top-spray
uidized bed
granulator
Dryer type(s)
To investigate the
relationship between
granule moisture
content and IR
absorption
To control the granules

moisture
Application(s)
Watano et al.[33] IR moisture sensor
IR moisture sensor
with feedback
moisture controller
Technique(s)
Real-time monitoring
Experimental agitated
and controlling of
uidized bed
moisture content using
granulator
IR moisture sensor
along with adaptive
fuzzy controller
[31]
Watano et al.[32] Smart control
Watano et al.
Author(s)
Remarks
The granules moisture content

was successfully measured
via IR moisture sensor and
the granule growth was fully
controlled using a moisture
feedback controller.
Mixture of lactose and
Granule moisture content was
cornstarch granulation
effectively controlled at
various drying air
with
Hydroxypropylcellulose
temperatures by introducing
a gain scheduling to
adaptive fuzzy system based
on drying capacity.
Granulation of lactose and The relationship between
cornstarch with
granule moisture content
and absorbance of IR
spectra was profoundly
affected by the
water-absorbing potential of
powder. However, granule
size could affect this
relationship during drying of
wet granules.
The operational condition did
cornstarch granulating
not affect the relationship,
with
except at extremely low
dampening speed, while the
relationship was inuenced
by the uidization air
temperature and liquid ow
rate.
Coating of placebo
The NIR spectroscopy
containing lactose,
satisfactorily predicted the
microcrystalline calluses,
amount of lm applied for
and magnesium stearate
coating.
with ethylcellulose and
as binding solution
Lactose and cornstarch

granulating with
Process target(s)
TABLE 2
Application of NIR spectroscopy for monitoring of FBDs
1013
Multichannel NIR
To monitor the moisture Bench-scale uidized bed
technique with three
content
granulator
statistical
parameters
NIR spectroscopy
Morris et al.[39]
NIR spectroscopy
Rantanen
et al.[42]
To monitor the moisture Bench-scale top-spray

content
uidized bed
granulator
Bench-scale uidized bed

granulator
Multichannel NIR
sensor in
conjunction with
PCA
Rantanen
et al.[41]
To select the NIR
wavelengths for
measuring moisture
content
Four-wavelength NIR To measure the moisture Laboratory uidized bed

sensor
content
granulator
Rantanen
et al.[40]
To monitor the moisture Experimental FBD

content
Bench-scale uidized bed

granulator
Rantanen
et al.[38]
To measure the PSD
NIR spectroscopy
Rantanen and
Yliruusi[37]
To track the granule

Bench-scale top spray
moisture content and
uidized bed
particle size variations
granulator
NIR spectroscopy
Frake et al.[36]
(Continued )
Granulation of magnesium NIR spectroscopy employed

carbonate with
for monitoring particle
Polyvinylpyrrolidone and
growth and moisture
Hydroxypropyl
content with acceptable
methylcellulose
accuracy during uidized
bed granulating.
Granulation of
NIR spectroscopy wavelengths
microcrystalline cellulose
were accurately correlated
with the granule particle
size.
The employed multichannel
Granulation of three
NIR technique satisfactorily
different formulations
estimated the moisture
containing
content of granules during
microcrystalline cellulose,
spraying and drying phases.
lactose monohydrate,
maize starch, mannitol,
verapamil hydrochloride
with polyvinlpyrrolidone
as binder
Ibuprofen-starch
NIR spectroscopy successfully
granulation using
tracked the moisture
Polyvinylpyrrolidone as
variation during uidized
the binder solution
bed granulation.
Granulation of glass
The granule water content
ballotini and
could be trustworthy and
quickly measured using only
with poly[1-(2-oxoa few NIR wavelengths
1-pyrrolidinyl) ethylene]
around the water band.
with gelatin as bending
solution
Granulation of theophylline NIR spectra analyzed with
anhydrate and silicied
PCA accurately detected the
granules moisture content
with
during processing.
solution as binder
Production of granule
The applied NIR spectroscopy
containing mannitol,
set-up with a multichannel
pregelatinized starch, and
detector was a powerful
technique for moisture
solution
measurement during
granulation.
1014
Paul Findlay
et al.[48]
Green et al.[47]
Davis et al.[46]
Rasanen et al.[45]
Wildfong
et al.[44]
Rantanen
et al.[43]
Author(s)
Application(s)
Dryer type(s)
Process target(s)
Four-wavelength NIR To predict the granule

Bench-scale uidized bed Granulation of anhydrous
sensor in
moisture content
granulator
theophylline with
combination with
Polyvinylpyrrolidone as
partial least square
bending solution
(PLS) and articial
neural network
(ANN)
NIR spectroscopy
To monitor the moisture Experimental FBD
Granulation of
content variation and
Ibuprofen-starch with
Polyvinylpyrrolidone
to detect end-point in
online mode
solution as binder
NIR spectroscopy
To measure moisture
Multichamber
Drying of disodium
content and to detect
microscale FBD
hydrogen phosphates
drying phase in-line
with three different levels
mode
of hydrate water and wet
theophylline granules
NIR spectroscopy
To monitor the
Lab-scale FBD
Granulation of mixture of
with standard
polymorphic
c-glycine and
normal variate
transformations of
glycine during drying
with water as the
phase
granulating liquid
NIR spectroscopy in To monitor the moisture Pilot-scale FBD
Drying of granules
conjunction with
content and to
containing different ratios
PLS
investigate the effects
of the same major
of sampling on method
excipients (lactose
precision
monohydrate and
microcrystalline cellulose)
and different bulk drug
and other minor
excipients
NIR spectroscopy
To monitor the moisture Experimental top-spray Granulation of mixture of
content and particle
uidized bed
acetaminophen or
size for detecting the
granulator
ibuprofen with lactose
end-point of
monohydrate and
granulation process
by povidone as bending
solution
Technique(s)
TABLE 2
Continued
The granulation end-point was

effectively detected using
calibrated NIR spectroscopy
by moisture content and
particle size measurement.
Moisture content of granules

and process end-point was
precisely estimated by NIR
spectroscopy.
NIR spectroscopy was
successful technique in
in-line determination of
product moisture and drying
phase.
successfully applied to
identify the a and c forms of
glycine during granulation
and drying.
Useful information was
obtained regarding the
impact of sampling on
inaccuracy of in-line NIR
spectroscopy method.
The ANN was found to have

more estimative power with
the independent test data
than the PLS.
Remarks
1015
NIR spectroscopy
with multivariate
calibrations
Mark et al.[53]
Peinado et al.[28] NIR spectroscopy and

experimental
moisture
determination along
with PLS
NIR spectroscopy
with PLS and PCA
NIR spectroscopy in
conjunction with
averaging and
clustering of spectra
Granulation of lactose
using de-mineralized
water
The NIR spectrum was

precisely correlated with the
granule moisture content
and particle size.
(Continued )
Drying of pellets containing The NIR spectroscopy

erythromycin dihydrate
detected erythromycin
and microcrystalline
dihydrate transformations
cellulose
to its isomorphic dehydrate
form in the pellets at
temperatures above 45 C.
To control the coating
Custom-fabricated
Coating of mixture of ve The coating thickness was
controlled as well as 3%
thickness
uidized bed coater
pharmaceutical
deviated from the actual
ingredients, including
thickness.
d-mannitol, magnesium
stearate, and corn starch,
using binder solutions of
polyethylene glycol and
hydroxypropyl
methylcellulose
To predict the moisture Industrial-scale uidized Granulating of
The pharmaceutical granule
content, particle size
bed granulator
properties such as moisture
distribution and bulk
with maize starch
content, bulk density, and
density
solution as binder
particle size were excellently
monitored using the NIR
spectroscopy.
To determine the ideal
Experimental FBD
Drying of antibiotic
An automated monitoring
end-point by taking
system based on the
into account product
continuous assessment of
quality, water content
NIR spectroscopy data was
and residual solvent
developed for a uidized-bed
drying process of a
pharmaceutical
intermediate.
To specify the drying
Full commercial-scale
Drying of hydrochloride
The presented methodology
end-point
FBD
salt containing
was effectively applied for
micro-crystalline
in-line determination of
cellulose, sodium starch
product moisture and drying
glycolate and povidone
end-point.
NIR spectroscopy in To identify the moisture Laboratory-scale FBD

conjunction with
principle
size of granules
component analysis
(PCA) and PLS
NIR spectroscopy
To monitor the phase
Microscale FBD
with PCA
transformations
Alcala` et al.[52]
Lee et al.[51]
Romer et al.[50]
Nieuwmeyer
et al.[49]
1016
Hayashi et al.[58] NIR spectroscopy

with PLS
To evaluate the water

content of granules
and to estimate the
constant drying rate.
On- and off-line NIR To predict the residual

spectroscopy along
moisture content
with PLS
Heigl et al.[57]
Lab-scale FBD
Small-scale cold-model
FBD
uidized bed
granulator
Process understanding
and fault diagnosing
Integrating NIR
spectroscopy with
humidity and
temperature data
loggers along with
PLS and PCA
Custom-made
experimental uidized
bed coater
Dryer type(s)
Kona et al.[56]
To quantify the coating

thickness
Application(s)
To monitor the moisture Experimental uidized

content
bed granulator
NIR spectroscopy in
conjunction with
PLS
Technique(s)
Hartung et al.[55] NIR spectroscopy
Lee et al.
[54]
Author(s)
TABLE 2
Continued

successful in monitoring of
granules moisture content.
The coating thickness as a high

quality end-point
designation could be
precisely estimated via
in-line NIR spectroscopy
measurement.
Remarks
Process understanding and

fault diagnosing successfully
carried out by coupling NIR
spectroscopy, humidity, and
temperature data in
conjunction with
multivariate batch modeling.
On- and off-line NIR
spectroscopy was successful
in prediction of moisture
content when compared with
actual moisture content
data. However, online NIR
spectroscopy led to more
precise results than off-line
NIR spectroscopy.
Moisture content of granules
Drying of extruded
was predicted accurately
Riboavin granules
using the PLS model and
obtained by combination
accordingly constant drying
of lactose as the ller,
rate was estimated.
potato starch as the
disintegrating agent, and
hydroxypropyl cellulose
as the binding agent
Coating of mixture of
lactose monohydrate and
with polyethylene glycol
and hydroxypropyl
methylcellulose as coating
materials
Granulating of Enalapril
maleate with lactose
monohydrate, maize
starch, and sodium
hydrogen carbonate
Fexofenadine
hydrochloride,
and lactose monohydrate
blends granulation with
polyvinylpyrolidone as
bending solution
Drying of dibasic calcium
phosphate anhydrous
Process target(s)
had a profound effect on the apparent absorbance of water

and subsequent NIR measurement results. Davis et al.[46]
quantied the polymorphic transformations of c-glycine to
a-glycine during the drying phase of a wet granulation using
NIR spectroscopy. The results were qualitatively conrmed
using X-ray diffraction of the powder. Green et al.[47] carried
out different experiments in FBDs at scales of 65, 300, and
600 L using different sampling schemes (dynamics, owing,
and stationary solids) to better understand and improve
the accuracy of the NIR spectroscopy technique. The process
heterogeneity had an undesirable role in the measurement
accuracy. In another investigation, the NIR spectroscopy
gauge was calibrated for simultaneous real-time monitoring
of particle size and moisture content as well as detecting the
granulation end-point.[48] Their results were in good agreement with ofine analytical measurements for determining
the end-point. Nieuwmeyer et al.[49] discriminated various
stages of the drying process using NIR spectroscopy with a
small relative error compared to Karl-Fischer analysis. The
particle size was also determined with a small prediction
error between nes and granules. NIR spectroscopy and
X-ray diffractometry detected the modication of erythromycin dehydrate solid state to its isomorphic dehydrate form
through FBD based on the moisture content of the pellets at
temperatures greater than 45 C.[50]
Lee et al.[51] introduced NIR spectra averaging and clustering procedures to establish a proper dynamic calibration
model for the measurement of coating thickness. The spectra averaging method for a small number of spectra proved
to be a reasonably good dynamic calibration model with a
high correlation coefcient. However, the PCA-based clustering technique was proposed for a large number of NIR
spectra. Alcala` et al.[52] utilized PCA and PLS as qualitative
and quantitative methods for analyzing NIR spectra to
monitor the uidized bed granulation process of pharmaceutical materials. A good correlation was found between
the absorbed NIR spectra and granule properties. In
another investigation, the absorbed NIR spectra were analyzed by the multivariate statistical method for evaluating
the quality, water content, and residual solvent of antibiotics on FBD. The results were conrmed by ofine measurements such as high performance liquid chromatography
(HPLC), Karl Fischer back-titration method, and gas chromatography (GC).[53]
Peinado et al.[28] developed a PLS model using NIR spectra and experimental moisture measurement for real-time
determination of the end-point in a FBD. Conrmation
tests revealed that the employed strategy was useful in inline
end-point specication. Lee et al.[54] developed excellent
correlations between the coating thickness of pellets predicted by inline NIR monitoring in conjunction with PLS
and two ofine methods, including confocal laser scanning
microscopy and laser diffraction particle size analysis,
during uidized bed coating. Hartung et al.[55] found a good
1017
relationship between water content determined by NIR

spectroscopy and Karl-Fischer titration for Enalapril
maleate formulation during uidized bed granulating.
Kona et al.[56] integrated real-time product moisture
content detection obtained using NIR spectroscopy with
humidity and temperature of the drying bed and established
statistical process monitoring charts (SPMC) by simultaneous application of PLS and PCA techniques for
uidized bed granulation and drying. NIR spectroscopy,
along with humidity and temperature data loggers, appears
to be promising for effective process control and fault determination. Heigl et al.[57] compared the PLS modeling of
online NIR spectra with PLS modeling of ofine NIR spectra according to a reference method (loss-on-drying) for
monitoring the moisture content of dibasic calcium phosphate anhydrous on FBD. The results of ofine NIR
spectroscopy indicated that the amount of withdrawn sample and sampling time interval can cause bias in the moisture content predictions. Hayashi et al.[58] continuously
predicted the water content of granules with negligible error
by employing a PLS model based on the NIR spectra and
loss-on-drying measurements and accordingly distinguished the constant drying regime.
NIR spectroscopy is a real-time, fast, safe, reliable, and
non-intrusive technique which requires no sample preparation, little or no modication to the existing facility,
and minimal or no analyst intervention.[28,39] However, this
technique is formulation-specic and requires calibration
based on reference methods. In this technique, the measuring window sometimes becomes coated with the wet powder, making a moisture measurement impossible or false.
However, the fouling problem of the window of the NIR
measurement can be generally solved by the use of a suitable
air supply system and specialized interfacing in order to
gain reliable data during the drying process.[4] The equipment cost is relatively high and multiple sensors must be
installed to monitor local moisture content or particle size
in a uidized bed.[59] This technique is insensitive to impurities and only the surface moisture of the material can be
determined due to the short wavelength. Absorption spectra
strongly depend on the particles distribution within the
bed, the powder density of the solid material,[60] and sample
temperature. NIR spectroscopy needs black-box multivariate calibration techniques and sophisticated software
for interpretation of very diffuse and non-specic spectral
data.[61] The accuracy of the measurement is confounded
by the alteration in the chemical composition of the solid
during processing and the O-H band interferes with other
bands of interest.[62] On the other hand, scattering and
absorptive attributes of solid product differed because of
modications in the color and surface structure of the particle. Location of the NIR within the bed sensor is a critical
parameter in the measurements and it is useless for monitoring of bed hydrodynamic behavior or assuring of spatial
1018
AGHBASHLO ET AL.
resolution. It is worth mentioning that the NIR imaging system (hyperspectral imaging spectrometer) has been developed
within the last few years with the ability to simultaneously
record spectral and spatial information of particles. This
new system can be a useful tool in the future for real-time
monitoring of particle physiochemical attributes and bed
hydrodynamics. The moisture content affects the measurement in monitoring the particle size,[63] and it gives only statistical characteristics without giving actual information about
particle size.[64] This technique, especially the IR moisture
sensor, is not actually non-intrusive due to its direct effect
on the heat and mass transfer coefcient.
Pressure Fluctuations
Pressure uctuations in a uidized bed are mainly related
to the formation, rise, and collapse or eruption of bubbles,
clusters, and agglomerates.[65] However, transient pressure
uctuations are quite complex and dynamic phenomena
whose exact origin is not yet entirely understood.[66] In
the case of FBDs, variation of the water content of particles
inuences bubble characteristics. Therefore, monitoring
and proper analysis of pressure uctuations can lead to a
more detailed and deeper insight into the process and
possibly generate new ideas for improvement. Real-time
condition monitoring of uidization, particle size, and
moisture content can be obtained by simple measurement
of pressure uctuations. Nevertheless, interpretation and
understanding of pressure signals is complicated due to
their intrinsically non-local nature.[66] It should be mentioned that pressure uctuations measurement is not a novel
technique for monitoring of FBDs. However, various innovative methods, including statistical, frequency domain
(fast Fourier and wavelet), nonlinear (fractal, chaos), and
recurrent plot analyses, have been developed and utilized
in recent years for interpretation of pressure uctuations
of uidized beds.[6771] Recently, several researchers have
attempted to review papers on measurement and analysis
of pressure uctuations in uidized beds. Bi[72] critically
reviewed the complex pressure uctuations phenomenon
in gassolid uidized beds. Sasic et al.[73] reviewed both
modeling and experimental techniques for investigating
the uid-dynamic behavior of gassolid uidized beds using
pressure signals. Van Ommen and Mudde[6] focused on
measurement techniques employed for elucidating the voidage distribution in gas-solid uidized beds. Van Ommen
et al.[66] provided a critical review of time-series analysis
techniques applied for interpreting the pressure signals in
uidized beds. Table 3 summarizes some of the recent
research and the most important results obtained using
pressure uctuations monitoring and analysis of FBDs.
Li et al.[74] found that the addition of smaller particles
increases the frequency and amplitude of pressure uctuations and improves the gassolids contact of soybean in
FBD. Chaplin et al.[75] studied the inuence of inlet air
temperature, initial mass of the wet bed, and pressure sensor

position on bed pressure uctuations as well as bed mass and
PSD by the S-statistic. Chaos theory was applied to interpret
and monitor the bed behavior for measuring the product
state and moisture content.[75] Hydrodynamic changes of
the FBD specied by the S-statistic were profoundly inuenced by the product moisture content. The S-statistic was
sensitive to the PSD only in the dry bed and superior over
the frequency and amplitude analyses in identifying the
hydrodynamic changes of the FBD. Chaplin et al.[76] continued their studies by implementing S-statistic analysis of
pressure uctuations to a lab-scale FBD for online comparison of the S-statistic with entrainment, bed temperature, and
outlet air temperature. The employed methodology was able
to give an early warning of the undesirable hydrodynamic
state by selecting an appropriate reference state. In a similar
work, the S-statistic of the pressure uctuations was not
sensitive to the changes in particle size during uidized
bed granulating of Mannitol.[77] However, two different
regions in the initial stages of granulation and the nal
stages of drying and granules moisture content were
detected by this method. Lopes et al.[78] compared visual
observations along with the statistical and spectral analyses
of data obtained from online pressure uctuations measurements during spouted bed coating. It was shown that statistical analysis is an adequate technique for identication
of the spout instability while the dominant frequency was
not suitable for distinguishing between the uidization
regimes perceived during coating.
Wormsbecker et al.[79,80] investigated the effect of vessel
geometry and uidization regime on hydrodynamics during
drying of placebo pharmaceutical granules. They found
transitions from high to low frequency in pressure uctuations of the conical bed and an increment in the bubbling
frequency of the cylindrical bed resulting from different
particle circulations patterns, both prior to and after uidization of the granule. They also reported a multiple bubbling regime and a coalescence-dominated regime in the
constant rate and falling rate periods, respectively. The simple bed pressure drop and temperature measurements were
able to detect the end-point of the granulation process.[81]
Karimi et al.[65] decomposed the raw pressure uctuations
into 10 sub-signals by wavelet transform and successfully
developed a linear relationship based on the seventh subsignal, corresponding to the macrostructure (large bubbles)
and the supercial air velocity to predict the moisture content of wet rice through FBD. Three various approaches
of signal processing, used to pressure uctuation measurements, including dominant frequency analysis, narrowband standard deviation analysis, and attractor comparison, were compared to extract quantitative information
about the granule size in a uidized bed granulator.[82]
The standard deviation of the narrow band ltered signal
was satisfactorily applied to monitor particle size and
1019
Lopes et al.[78]
Chaplin et al.[77]
Chaplin et al.[76]
Chaplin et al.[75]
Pressure uctuations
with standard
deviation and
power spectra
Li et al.[74]
Dryer type(s)
To study the uidization Lab-scale FBD

velocities, mixing
mechanisms, and
uidization quality
Application(s)
Drying of soybean seeds
Process target(s)
Remarks
(Continued )
Profound improvement was

obtained in gassolids
contacting by introducing
small particles into the bed
of large particles.
S-statistic was superior in
Pressure uctuation in To track the bed
Experimental conical
Drying of wet placebo
identifying the uidized bed
conjunction with
hydrodynamic
lab-scale FBDs
granule containing
state over the standard
chaos analysis
deviation or dominant
(S-statistic)
frequency techniques.
as ller, croscarmellose
sodium as disintegrant,
hydroxypropyl
methylcellulose as binder
and USP water as solvent
Main hydrodynamic
Pressure uctuation
To study the bed
Lab-scale FBD
Drying of granule
variations were specied by
with S-statistic
hydrodynamic
consisting lactose
the S-statistic analysis of
monohydrate (ller),
high-frequency pressure
uctuation data.
(ller), croscarmellose
sodium (disintegrant),
hydroxypropyl
methylcellulose (binder),
and water (solvent)
Pressure uctuation
To monitor the moisture Experimental top-spray Mannitol granulating with Granule moisture changes
analyzed by
content
uidized bed
within the granulator
S-statistic
granulator
as binding solution and
monitored by using the
water as solvent
applied technique without
the need for the direct
measurement of moisture.
Pressure uctuations To monitor the changes Lab-scale coneABS and polystyrene
Statistical method
along with the
that occurred during
cylindrical spout FBD
particles coating by
satisfactorily differentiated
statistic and spectral
particle coating in a
Eudragit L30-D551
the spout uidized bed
analysis
spouted bed by using
based polymeric
instability based on pressure
real-time pressure
suspension
uctuation data.
uctuation
measurement
Technique(s)
Author(s)
TABLE 3
Some of the recent research and the most important results obtained using pressure uctuations monitoring and analysis of FBDs
1020
De Martin
et al.[82]
Karimi et al.[65]
Roy et al.[81]
Wormsbecker
et al.[80]
Wormsbecker
et al.[79]
Author(s)
Application(s)
Dryer type(s)
Process target(s)
Remarks
Pressure uctuation
analysis in
conjunction with
average cycle
frequency and
standard deviation
analyses
To understand the bed

hydrodynamic
behavior
Experimental FBD
The potential of using pressure

uctuation measurements to
granule containing
monitor and control
uidization state was
demonstrated.
as ller, croscarmellose
sodium as disintegrant,
hydroxypropyl
methylcellulose as binder,
and USP water as solvent
The dominant frequency
To study the inuence of Cylindrical and conical Drying of granule
Pressure uctuation
decreased during drying in
vessel geometry on the
laboratory-scale batch
containing croscarmellose
analysis with both
the conical bed, while it
hydrodynamic
FBDs
sodium (disintegrant),
time domain
increased during drying in
behavior
lactose monohydrate
(standard deviation
the cylindrical bed.
(ller), microcrystalline
and average cycle
cellulose (ller),
frequency) and
hydroxypropyl
frequency domain
methylcellulose (binder).
(dominant
and water (solvent)
frequency and
power spectra)
analyses
Pressure drop and
To detect the granulation Experimental top-spray Granulation of urea
The bed pressure drop and
temperature
end-point
uidized bed
temperature were
measurement
granulator
successfully authenticated
for identifying the end-point
of uidized bed granulation.
Pressure uctuations To monitor the moisture Experimental FBD
Drying of wetted rice
The original pressure
with time-domain
content and bed
particles
uctuation signal was
and frequency
hydrodynamic
decomposed into 10
domain analyses
subsignals which were more
sensitive to moisture
variations than other
investigated parameters.
Pressure uctuation
To monitor the moisture Lab-scale uidized bed
Granulation of mixture of The particle size and water
with three different
granulator
content were correlated to
techniques of signal
size during uidized
starch with
the data derived with the
processing,
bed granulation
pressure uctuation sensor
including dominant
as binding solution and
by narrow-band standard
frequency analysis,
water as solvent
deviation signal processing
narrow-band
technique.
Technique(s)
TABLE 3
Continued
1021
Dong et al.[85]
Prata et al.[84]
Silva et al.[83]
Pressure uctuations
with statistical
methods
To quantify the bed

hydrodynamics
standard deviation
analysis, and
attractor
comparison tool
Pressure uctuation in To monitor and control
the deuidization
conjunction with
phenomenon in a
Gaussian spectral
uidized bed coating
pressure
process based on
distribution and
pressure uctuation
control of the
data
airow rate and the
coating suspension
ow rate using PI
controllers
Pressure uctuation
To prevent the
measurement for
agglomeration by
process control
pausing the liquid
injection
Experimental FBD

coater equipped with
two-uid nozzle
Experimental uidized
bed coater
Gaussian spectral analysis of

pressure uctuation data
indicated high potential for
applications in uidized bed
coating processes, while the
PI controller successfully
maintained uidization
dynamic in stable state
based on presented analysis.
Microcellulose beads
The developed controller
coating with gum Arabic
effectively controlled
uidized bed coating, while
granules agglomeration was
avoided by stopping the
liquid spraying based on bed
pressure measurements.
Drying of spent liquor
The bed hydrodynamic
mixed with corn bran for
behavior was reasonably
the production of yeast
qualied by measuring the
local bed pressure
uctuations, exhaust air
temperature, and relative
humidity.
Microcrystalline cellulose
coating
1022
AGHBASHLO ET AL.
moisture content during uidized bed drying and granulation

processes. Silva et al.[83] developed PI and PID controllers for
controlling drying air ow rate and spraying liquid to avoid
the deuidization phenomenon during the uidized bed coating, according to the Gaussian spectral analysis of pressure
uctuations. The PI controller showed a good performance
over the PID controller and subsequently the stable uidization conditions were obtained using the PI control system.
Prata et al.[84] designed a single-input=single-output control
strategy based on the bed pressure measurement to prevent
agglomeration of granules by manipulating liquid spraying
during uidized bed coating. Agglomeration was effectively
avoided and homogeneous coating and separated particles
were obtained by the developed control system. Recently,
Dong et al.[85] found that a small variation in the average
pressure drop and the standard deviation can be used for
early warning of the transition of the bed state from channeling to uniform uidization.
Pressure uctuation measurement is sensitive, accurate,
fast, robust, relatively cheap, virtually non-intrusive, and
relatively easy to implement in lab-, pilot-, and industrialscale units, even under harsh conditions. This technique
can be considered to be a truly non-intrusive technique if
the pressure transducer is ush-mounted at the vessel wall
or if differential pressure measurements are applied[75];
thus, distortion of the ow around the point of measurement is avoided.[66] Otherwise, this technique can modify
the local hydrodynamics of the uidized bed and might
not be a reliable means of measurement.[86] This technique
provides information only about global or time-averaged
hydrodynamic behavior of the bed. Therefore, it is useless
for monitoring the local uidization phenomena inside the
bed[87] and ascertaining the location in the bed in which
variations in the dynamic behavior are taking place during
drying.[88] On the other hand, signal processing is an essential tool for extracting information from the recoded pressure uctuations related with the particle physical properties
and the bed hydrodynamics. Unfortunately, few techniques
are available for successful and satisfactory processing of
pressure signals to monitor physical properties of particles
being processed, such as signal energy, average cycle time,
dominant frequency, and attractor comparison tools.
Pressure measurement needs intrusive pressure taps and
the pressure transducer needs to be placed inside the process itself for industrial and experimental applications. This
technique does not provide detailed information about bed
height of uidization media and clear knowledge during
processing of very ne particles. Furthermore, to prevent
fouling of the pressure transducers with ne wet powder,
continuous back-ushing with costly pressurized air or a
mechanical scraper is necessary, which in turn diminishes
the sensitivity of the probe.[89] Pressure uctuations analysis provides statistical information without resolving
specic particle sizes.[64] In addition, identication of the
source of uctuations amongst many simultaneously

occurring phenomena is very difcult due to the extremely
complex local ow structure through the uidized bed.[86]
Optical Imaging Technique
Optical imaging is one of the earliest techniques
employed in the uidized bed drying process for real-time
determination of physical properties of the granule,
including granule size, PSD, and shape,[4] as well as the
uidization regime. This transforms an image captured by
a charge coupled device (CCD) camera into the digital form
and performs some pretreatments on it, such as ltration,
noise reduction, and pattern recognition, in order to obtain
a rened image or to extract useful insights from it.[3] Image
acquisition, preprocessing, segmentation, extraction, and
representation of the characteristic parameters are the main
steps in image processing analysis.[90] Recently, particle
image velocimetry (PIV) has been introduced for determining velocity elds by capturing two images shortly after
each other and computing the distance individual particles
traveled within this time. From the specied time interval
and the recorded movement, the instantaneous velocity
vector eld can be identied in a cross-section of a ow.
As illustrated in Fig. 2, the PIV apparatus contains a
CCD camera, a strobe or laser with an optical arrangement
to conne the physical region illuminated, a synchronizer to
perform as an external trigger for adjusting the CCD
camera and laser and the seeding particles. There are
remarkable applications of the optical imaging technique
in the literature to characterize uidized bed hydrodynamics as well as physical properties of particles, which are
summarized in Table 4.
The rst application of image processing in FBD goes
back to 1995, when Watano and Miyanami[91] developed
a system based on the image processing technique for online
monitoring of PSD and shape of granules in uidized bed
granulation. The particle imaging probe was able to predict
the granule shape precisely, being equivalent to the accuracy of the ofine sieve method. They extended their investigations to more precise controlling of FBD using an image
processing system supplemented with fuzzy rules,[92] a fuzzy
logic controller based on image processing technique,[93]
and an adaptive feedback fuzzy controller based on a
particle image probe and an image processing system.[94]
Saadevandi and Turton[95] found that particle velocity
and bed voidage are functions of both axial and radial
positions using the data obtained by the video imaging
technique. However, the spray rates did not inuence the
particle velocity and voidage measurements. Particle trajectories at different particle loading, jet air velocity, and
position of the Wurster tube were investigated using the
uorescent technique by Karlsson et al.[96] Trajectories of
particles were successfully tracked, even with unexpected
particleparticle collision and particlewall collision.
1023
FIG. 2. Schematic diagram of typical PIV apparatus and its measurement principle.
Narvanen et al.[97] employed a 3D image analysis technique

for determination of particle size within a uidized bed
granulator. Three basic colors, red-green-blue (RGB), were
used to lighten a at granule bed surface from three
different orientations. The PSD obtained by the image processing method satisfactorily corresponded to those of the
sieve analysis. Good agreement was observed between the
results of confocal laser scanning microscopy (CLSM)
and the chemical analysis in determining the coating thickness of microparticles through the uidized bed coater.[98]
It is worth mentioning that the CLSM is a technique for
capturing high-resolution optical images with depth selectivity. The key property of the confocal microscopy is its
capability to capture blur-free images of thick specimens
at different depths, a process known as optical sectioning.
Images are acquired locally and reconstructed with an
appropriate computer program, permitting 3D reconstructions of topologically intricate objects. Mozina et al.[99]
employed digital visual imaging to assess the spherical
diameter, coating thickness, and undesirable agglomeration
of pellets as well as classication and analysis of pellets
within the uidized bed coater. Accuracy, precision, stability, and speed of the developed technique were conrmed
by experimental results. Feasibility of image analysis with
different feature selection approaches for excluding
irrelevant and redundant information was investigated to
monitor the coating thickness of pharmaceutical pellets
during uidized coating.[100] A strong correlation was
found between image features and process parameters.
Wang et al.[101] applied PIV to visualize and classify annular bed ow patterns in the bottom spray uidized bed
coater and accordingly detected three types of ow patterns
within the drying bed. The ow patterns were considerably
inuenced by the coating uniformity, which was determined
by color coating and subsequent tristimulus colorimetry of

inline samples. Liew et al.[102] quantied particle recirculation through the partition column using a high-speedimaging-based visiometric process analyzer and ensemble
correlation PIV. Their results were in good agreement with
the data obtained using an image tracking method.
The optical imagining technique is a real-time, nonintrusive, rapid, low-cost, efcient, repeatable, accurate,
high-resolution, consistent, and objective inspection tool
based on image analysis. Image processing provides reliable
information not only on the PSD, but also direct information on particle sizes. The PIV offers several advantages,
such as simplicity of the experimental set-up and ease of
scale-up procedures, with applicability for non-intrusively
obtaining a complete velocity vector eld.[102] However,
the PIV can only detect close-wall velocity vector elds
and its measurement may be negatively inuenced by wall
effects.[103] The CLSM has also several advantages, including high-resolution blur-free images, easy visualization of
3D structures by stereo pairs, capability of controlling
depth of eld, elimination of background knowledge away
from the focal surface, and the capability of collecting
sequential optical proles from coarse samples.[104] However, image processing necessitates large computational
efforts for data processing due to the very large amounts
of data generated when compared with other monitoring
techniques. Such a disadvantage would be diminished with
further progress in computer technology. On the other
hand, the wavelength of light, the desired eld of inspection,
and the pixel density of the digital camera conne the resolution of the optical imaging. Non-uniform illuminating,
variable solid density in the bed, imperfections or dirt on
the bed wall, background light, and photo-bleaching can
negatively inuence the light intensity and following image
1024
Image processing
technique with
fuzzy logic
controller
Saadevandi and Video imaging

Turton[95]
technique
Watano[94]
To measure the
velocity of particle
and voidage of bed
To measure and
control the
granule growth
To control the granule

size by employing
image processing
technique in
conjunction with
fuzzy logic
Intelligent control
Watano and
Miyanami[93]
To monitor the granule

size distribution and
shape
Application(s)
To control the granule

growth
Image processing
Technique(s)
Watano et al.[92] Image processing in

combination with
fuzzy logic
Watano and
Miyanami[91]
Author(s)
Process target(s)
Remarks
Laboratory-scale topGranulation of lactose and The granule size obtained

spray agitated uidized
cornstarch with
using image processing
bed granulator
technique was agreed well
with data determined by
sieve analysis.
Lab-scale top-spray
Granulation of mixture of The developed system
lactose and cornstarch
accurately controlled the
granulator
granulating with
granule growth at various
operating conditions and
solution
samples attributes.
Dryer type: Lab-scale
Particle size obtained using
cornstarch granulation
image processing technique
granulator
precisely agreed with sieve
analysis and subsequently
the uidized bed granulator
accurately controlled by
fuzzy logic controller.
Lab-scale agitated
Granulation of
Granule growth in uidized
top-spray uidized bed
pharmaceutical powders
bed granulation was directly
granulator
composed of lactose and
and continuously monitored
cornstarch with a solid
using an image processing
binder by spraying
system and also an
puried water
automated control system of
granule growth based on a
fuzzy control system was
presented.
Experimental
Coating of glass particle as Hydrodynamics of uidized
bottom-spray uidized
model material
particles passing through the
bed coater
liquid spray in a semicircular
uidized bed coating device
and the effects of the liquid
spray on particle velocity
and voidage proles in the
spraying zone was exactly
surveyed.
Dryer type(s)
TABLE 4
Application of image processing for monitoring of FBDs
1025
Confocal laser
scanning
microscopy
Image processing
with two different
feature selection
approaches
PIV
High-speed imaging
coupled with
ensemble PIV
Kucheryavski
et al.[100]
Wang et al.[101]
Liew et al.[102]
Mozina et al.[99] Digital visual

imaging
Depypere
et al.[98]
Laboratory-scale
spouted bed coater
with draft tube
Drying of sand particles

coated with
ethyl-cellulose
A uorescent technique was

satisfactorily applied for
detailed studies of the
trajectories of particles in the
fountain region.
Bench-scale uidized bed Theophyllin anhydrate and Particle size measurement was
granulator
a -lactose monohydrate
satisfactorily performed
granulating with 7.5%
using 3D image processing
aqueous solution of
technique and the results
corresponded quite well to
those of off-line sieve
analysis.
To determine the lm
Laboratory-scale
Coating of glass
The applied methodology was
coating thickness and
uidized bed with both
beads,microbeads with
able to predict microcapsule
the top-spray and
subsequent thickness
sodium caseinate, and
coating thickness down to
heterogeneity
bottom-spray
gelatin ASF=A aqueous
11.5 mm.
conguration
solutions
To determine the size
Full-scale uidized bed Pellet coating with solution Pellet size and coating
and shape of pellets, to
coater
consisting the
thickness were effectively
detect the adverse
hypromellose phthalate
determined.
agglomeration of
and dibutyl sebacate in
mixture of acetone and
pellets, and to classify
the pellets
ethanol
To monitor the coating Pilot-scale uidized bed Coating of nonpareil
The angle measure approach
thickness in at-line
coater
sugar=starch pellets
results were found to be
mode
with acetaminophen
more subtle and consistent
(Paracetamol),
than wavelet decomposition
Acryl-EZE1 and
in monitoring coating
Opadry Red
thickness.
To study the annular bed Lab-scale bottom spray Nonpareils coating with
Coat uniformity was
ow patterns and its
uidized bed coater
Hydroxypropyl
profoundly affected by
effect on coating
methylcellulose
annular bed ow patterns
uniformity
identied by PIV.
To monitor the particle Experimental bottom
Coating of sugar pellets
The particle displacement
recirculation within the
spray uidized-bed
with
probability density function
coater
hydroxypropylmethylcelwas consistent with results
partition column and
lulose
of an image tracking
to obtain the particle
displacement
method.
probability density
function
Karlsson et al.[96] High-speed video

To follow the trajectory
camera equipped
of single particles in
with an optical lter
the fountain region
with a UV lamp to
excite the
uorescence-marked
particles
Narvanen
3D topographic image Online monitoring of
et al.[97]
processing
particle size
distribution during
uidized bed
granulation
1026
AGHBASHLO ET AL.
attributes. Most imaging techniques are limited to

translucent media and two-dimensional images, apart from
confocal laser scanning imaging, which is suitable for
three-dimensional imaging.[97] Thus, the optical imaging
technique is not usable for large-scale FBDs in which opaque metal chambers are used. Solids moisture content can
affect the reective attributes of the particles, particularly
free surface water, and the captured image quality and
characteristics.
Acoustic Emission (AE)
Many years earlier, human hearing was utilized to
monitor a drying process and the process end-point was
determined by listening to the acoustic signals emitted from
the dryer.[63] An acoustic monitoring technique can be
applied in both active and passive modes. In the active
acoustics mode, an acoustic wave is transmitted into the
object of interest. However, the sound generated by the
process itself can be used as a source of information for condition monitoring of the process in passive mode.[105] In a
gas-solid uidized bed, passive acoustic waves are naturally
released by particle impacts, friction, uid ow and turbulence, particle movement in a limited space, bubble collapse
and eruptions at the surface of the bed, and agglomerates.[65] Changes in the elastic properties of particles inside
a FBD are the basic measurement concept behind AE monitoring. The sound generated during this process can be used
for identifying the uidization regime, estimating the mean
particle size and the PSD, and determining the moisture
content of particles by extracting the desired information
from the signal after calibrating the acoustic signals using
a chemometric technique such as PCA or PLS. The AE
probe monitors passive acoustic signals at frequencies in
and above the human hearing domain. Boyd and Varley[106]
have reviewed the potential application of passive measurement of the AE as a non-intrusive and real-time monitoring
technique in the eld of chemical engineering. As summarized in Table 5, there are many applications of passive AE,
reported in the literature, for monitoring of FBDs.
Tsujimoto et al.[107] used high-frequency (140 kHz)
passive AE of a uidized bed granulator along with an
FFT analyzer and excellently correlated the mean AE
amplitude to the dimensionless excess gas velocity and
dimensionless expanded bed height at various operating
conditions. Positions of acoustic sensors in a pilot-scale
granulator were optimized by Halstensen et al.[108] They
assessed the feasibility of acoustic chemometrics by employing the PLS regression to characterize different aspects of
the granulation process, successfully detected critical conditions, and revealed these situations as early warnings in
an operator-friendly manner.
Naelapaa et al.[109] measured passive AE with two different types of accelerometers, at different positions of the
accelerometers, and two different product containers for
estimating the magnitude of lm applied and percentage

release during top-spray uidized bed coating of potassium
chloride crystals with ethylcellulose. The sound generated
by mechanical vibrations, such as blowers and compressors
used in uidized beds and from electricity, were excluded
from the overall signal to obtain precise results. The type
of acoustic sensor and its position had an important effect
on process monitoring. The best PLS model, provided by
the high-frequency accelerometer, successfully approximated the amount of the lm applied and the percentage
release of potassium chloride with an acceptable correlation
coefcient. The potential application of the passive AE
spectra with the PLS for real-time monitoring of moisture
content was demonstrated by Matero et al.,[27] while the
granule size determination was not successful in all drying
experiments. However, Matero et al.[110] predicted the
end-product granule size distribution by analyzing AE data
using an N-way PLS during the nucleation phase. Karimi
et al.[65] measured passive AE to investigate drying process
stages using frequency domain analysis. The end of constant rate and falling rate stages was successfully detected
by a variation of standard deviation and kurtosis of the
AE signal. In another study, the capability of the passive
AE technique as an early warning method to detect process
deviations was authenticated by ofine analysis of the AE
spectra with the PLS regression.[111] Recently, Ihunegbo
et al.[112] found a good correlation between the actual moisture content of silica gel particles obtained by acoustic
measurements in conjunction with the PLS regression
analysis, indicating the suitability of this technique for
online monitoring of the drying progress and process
end-point detection.
AE monitoring is a non-intrusive, low-cost, easy-toimplement, fast, reliable, non-directional safe technique
which has been employed for online and at-line monitoring
of the FBDs. The acoustic monitoring unit does not require
costly maintenance and modication of existing systems.[112]
This technique also does not need a window for measurement and associated sensors do not have to be placed inside
the process itself, which in turn eliminates the fouling problem. Therefore, it can be successfully implemented when the
original material is adhesive and tends to coat the probe.[63]
However, the sensors location should be carefully chosen in
vicinity to the source because of attenuation of the propagated signal, and signal pollution by improper sound dominating the analysis should be avoided as much as feasible.
Acoustic sensors not only can withstand harsh process conditions (high temperature, high pressure, and corrosive substances), but also can work in situations in which process
changes are not permitted due to potential growth of
bacteria or build-up of material; e.g., in the food and pharmaceutical industries.[113] The AE has the capability of predicting several properties directly from the same acoustic
spectrum, such as early warning of undesired changes,
1027
Passive acoustic
monitoring with
PLS
Passive acoustic
emission with PLS
and PCA
Matero et al.[27]
Passive acoustic with

PLS
Halstensen
et al.[108]
Naelapaa
et al.[109]
Passive acoustic
emission using a
Fast Fourier
Transform (FFT)
analyzer
Technique(s)
Tsujimoto
et al.[107]
Author(s)
granulator
Dryer type(s)
Granulating of particles
made from crystalline
cellulose
Process target(s)
To determine water
content granule size
during granulation
uidized bed
granulator
Production of granule
including hydrophobic
pharmaceutical
excipient in a
monohydrate form and
Semi-industrial
Urea granulation in a
To detect the critical
bottom-spray
uidized bed granulator
situations during
uidized bed
uidized bed
granulator
granulation as early
warnings and to
predict the bed
movement,
concentration of the
liquid feed, reux of
the ne material to
granulator, moisture
content of the
granules, and particle
size average and
variance
Estimate amount of lm Production scale
Potassium chloride
applied and percentage
top-spray uidized bed
crystals coating with
release of potassium
coater
ethylcellulose
chloride during
uidized bed coating
To monitor the
uidization
phenomena
(dimensionless excess
gas velocity and
dimensionless bed
height)
Application(s)
TABLE 5
Recent passive acoustic emission application in FBDs
(Continued )
Potential application of
acoustic emission for
additional control of a
uidized bed coating process
to achieve a controlled
release product was
demonstrated.
Acoustic emissions spectra
analyzed by PLS were
successfully monitored
granule moisture
content,while granule size
was not precisely tracked in
some cases.
AE strongly tracked particle

uidization at different
operating condition,
including different uidizing
gas velocity, bed hold-up,
particle size, moisture
content, and rotational disk
speed.
In-line acoustic signals along
with PLS regression
technique improved
uidized bed granulation
process comprehension.
Remarks
1028
Technique(s)
Application(s)
Acoustic emission
with PLS
Ihunegbo
et al.[112]
Poutiainen
et al.[111]
Passive acoustic
emission in
conjunction with
frequency domain
analysis
Passive acoustic
emission with PLS
Karimi et al.[65]
uidized bed
granulator
Dryer type(s)
To monitor the drying

progress and to
determine the process
end-point
To predict granule size

distribution
Experimental FBD
Top-spray uidized bed

granulator
To study drying and bed Lab-scale FBD

hydrodynamics
Matero et al.[110] Acoustic emission in To determine

conjunction with
end-product granule
N-way PLS method
size distribution
Author(s)
TABLE 5
Continued
Process target(s)
Remarks
Drying of silica gel
Granulation of mixture of
ibuprofen, lactose
monohydrate, and
Off-line analysis of the

acoustic spectra using partial
least squares regression
indicated that AE could be
employed for real-time
tracking of granule size
distribution.
The acoustic chemometrics
was a viable online
technique for tracking the
drying progress and for
identifying the end-point
during drying of particulate
matter.
binder liquid and water as
solvent
Granulation of mixture of The N-way PLS model
obtained from acoustic
hydrophobic
emission satisfactorily
pharmaceutical
determined the granule size
distribution of end-product
excipient in a
based on early stages of the
monohydrate and
process.
bending solution and
water as solvent
Wetted rice drying
Drying stages were
successfully tracked by
acoustic emission signal.
process end-point, clogging of the bottom plate, particle

size, and moisture content, by applying chemometrics
methods.[112] This could be attributed to the fact that the
emitted acoustic signal depends on several parameters, such
as size, moisture content, velocity, density, porosity, and
composition of particles affecting the entire elastic attributes
of granules.[111]
The main drawback of the AE measurement is that the
relationship between signals and the moisture content=size
of granules and uidization state and=or regime is indirect.
It can be quite challenging to interpret the results in order to
extract insight from the signals related to granules and bed
attributes, which hinders the widespread application of
AE monitoring.[97] This problem can be overcome with statistical treatment of data to extract relevant information and
decrease irrelevant information; i.e., interfering parameters.
On the other hand, AE signals are not usually strong and the
sensitivity of the technique may be affected by the uidizing
air ow rate, construction material, and external uncontrollable and unintended interferences,[114] necessitating the preprocessing of the spectra before the actual analysis. The
particle moisture content may undesirably alter the precision of the AE measurement during monitoring of particle
size.[63] The AE technique relies on highly specialized sensors and requires calibration with a reference technique. It
is also worth mentioning that most investigations have been
carried out by passive AE. Therefore, application of active
AE and active ultrasound sensors merits future studies.
Electrical Capacitance Tomography (ECT)
The basic principle of electrical capacitance tomography
(ECT) is to image the varying permittivity distribution of an
insulating medium by measuring the electrical capacitances
outside the boundary of the medium, using collections of
electrodes put around its circumference. The capacitance
between all possible pairs of electrodes can be proportionally correlated to measured electric potentials, electric
currents, and electric charges during applying a known voltage schema to the electrodes.[115] These images are then
reconstructed into tomograms with different methods to
provide information on the electrical properties of the process volume. It must be noted that electrical capacitance
imaging can be obtained in real-time 3D with the recent
introduction of electrical capacitance volume technology
(ECVT).[101] The difference between the dielectric constants
of gas and solid phases inside a FBD can be used to specify
the distribution of these phases and physical attributes of
the product within the dryer. A schematic of the ECT is
shown in Fig. 3. Dyakowski et al.[116] presented a review
on electrical tomography techniques, including ECT and
electrical resistance tomography (ERT) used for investigating, monitoring, and controlling gassolids and liquid
solids systems. Watzenig and Fox[115] comprehensively
reviewed the statistical modeling and inference for ECT.
1029
Several researchers have employed ECT for characterization of uidized bed hydrodynamics, particle moisture
content, and bulk density (Table 6).
Chaplin and Pugsley[88] applied the S-statistic technique
for both reconstructed and non-reconstructed ECT images
to recognize the localized variations in the dynamic behavior of a batch FBD. The S-statistic technique and the visual interpretation of the tomographic data showed that the
variations in the bed hydrodynamics with progressing drying process were most severe at the vicinity of the chamber
walls, while the central region was identied by a more
consistent dynamic behavior. In a similar study, Chaplin
et al.[117] corrected the effect of moisture on the permittivity
of drying pharmaceutical granules based on the leastsquares linear t of the packed bed capacitance to the moisture content and conrmed the ECT results with X-ray tomography. The Bottcher and parallel permittivity models
were more accurate at high and low moisture contents,
respectively.
Wang et al.[118] comprehensively compared the results of
solids concentration and moisture content obtained from
mathematical modeling, CFD simulation, and ECT
measurement. Wang et al.[119] developed a feedback controller based on online ECT measurement to control sample
moisture content on FBD by regulating the air ow rate. It
was shown that the moisture content can be successfully
controlled and the thermal efciency can be slightly
improved by the developed system. Villegas et al.[120] conrmed the results of the lumped-distributed parameter
model by ECT measurement to predict the particle moisture
content, the temperature proles during the drying process,
and the permittivity. The inlet air velocity was manipulated
to design and implement a simple distributed parameter
controller and then it was successfully applied to control a
batch FBD. Amongst different Maxwell permittivity models, the Maxwell series model was able to evaluate precisely
the effective permittivity in the FBD.[121] Measurements by
halogen moisture analyzer conrmed the results of all three
employed approaches. Wang and Yang[121] found that the
capacitance was strongly affected by particle moisture and
excitation frequency. The capacitance was linearly changed
with the moisture content at low water contents, while a
more complex and nonlinear trend was observed at high
moisture contents. However, the effect of reconstruction
models on moisture distribution and hydrodynamics was
obvious at a frequency lower than 1 MHz and high moisture
content of granules on FBD. An algorithm based on
the nite element method (FEM) was developed by
Rimpilainen et al.[122] to reconstruct the 2D image obtained
from ECT measurements. The average moisture content
was precisely predicted by this approach. Threedimensional tomograms, time pipes (constant moisture
surfaces), and normalized moisture curves were used for
identifying the bed hydrodynamics.
1030
AGHBASHLO ET AL.
FIG. 3. Schematic representation of the ECT system.
ECT is the most favored and powerful tool among

tomography technologies for providing pertinent knowledge regarding the physical form, the chemical composition, or the overall status of the manufacturing because
of its non-contact and non-intrusive way of measurement,
small failure probability, easy installation, high-speed-imaging capabilities (typically between 100 and 200 frames per
second), simplicity, suitability for vessels with complex
geometries and different sizes for various sizes and geometries,[101] the fact that it is harmless for human operators
and the environment (no radiation), and its robustness in
hostile environments (high temperature and high pressure).
This technique provides insight into localized changes in the
voidage resulting from the bubbling behavior of the bed
or the hydrodynamic modication at a known location
through the bed.[87] ECT is appropriate for monitoring of
dry or non-conducting media when compared with electrical resistance tomography (ERT), which works well in
wet or conducting systems.[116] However, this technique suffers from several drawbacks, such as poor spatial resolution
(typically 310% of a pipe diameter), long scan time, limited
size of the inspection area, relatively high construction
cost,[123] sensitivity of results to the reconstruction algorithm,[124] and material build-up. The recorded data using
this technique is drastically nonlinear and complex and
therefore considerable computation efforts are required
for image reconstruction. On the other hand, the ECT
provides indirect insights about the particulate phase[125]
and its application is limited to lab-scale FBDs.[126] The
generated electric eld between the pair of electrodes in
the ECT may inuence heat and mass transfer; thus, it is
not always truly non-intrusive. The technique is also
formulation-specic, requiring frequent calibration for each
product.
Spatial Filter Velocimetry (SFV)

SFV determines the chord length and velocity of particles
in an inline manner by registering the shade of crossing particles using a set of optical bers.[3] Photodetectors can determine the frequency of this signal, which is proportionate to
the particle motion. The velocity can be then calculated at

known intervals between two photodetectors. The chord
length can be evaluated by knowing the time of the pulse
signal and velocity of the moving particle. Figure 4 schematically demonstrates the basic optical system of the SFV. It is
worth noting that the advanced version of the SFV,
provided by Parsum GmbH (Chemnitz, Germany), was predominantly applied for monitoring of the FBD. This device
utilizes ber optical spot scanning, with capability of measuring a particle size range of 506000 mm and a particle
velocity range of 0.0150 m=s with a data acquisition rate
up to 20,000 Hz.[127] Several researchers have utilized SFV
for measuring the particle size within FBD (Table 7).
Schmidt-Lehr et al.[128] used SFV successfully for determining granule size growth with high resolution and in
real-time mode. They established a model describing the
relationship between the uidized bed parameters, such as
inlet air temperature, inlet air ow and spray rate, and the
nal particle size in the granulation process. Narvanen
et al.[129] reported good correlation between the particle size
of the sieve analysis and ofine SFV. However, in-line SFV
underestimated and at-line SFV technique overestimated
the nal granule size. In a similar work, a model was
developed based on the SFV measurements in conjunction
with the PLS technique for particle size estimation in a
uidized bed granulator.[130] Huang et al.[131] applied the
Parsum probe for in-line measurement of the particles
formation in granulation batches and evaluated the batch
process performance, batch-to-batch variation, and development of a potential control strategy for the particle size
by multivariate batch modeling. Multivariate=batch statistical process control (MSPC=BSPC) was successfully used
to evaluate batch-to-batch variation with respect to particle
size and to predict the nished product attributes.
Burggraeve et al.[132] investigated the effect of inlet air
temperature during spraying and drying and type of binding solution on the particle properties and conrmed that
the in-line SFV can be used for determination of the particle
development during uidized bed granulation. In another
work, they used the SFV to record in-line PSD and product
temperature for modeling and control of a uidized bed
1031
ECT along with

S-statistic
Technique(s)
Dryer type(s)
To monitor the localized Experimental FBD

changes in dynamic
behavior of bed
occurring during
drying
To examine the inuence Lab-scale FBD
of permittivity models
and number of
iterations on the
reconstruction of
tomograms
Application(s)
To validate a distributed Experimental FBD

parameter model for
predicting the particle
moisture content, the
temperature proles,
and the permittivity
distribution by ECT
measuring and to
design a distributed
parameter controller
Lab-scale FBD
ECT with Landweber To measure the solids
Iteration method
concentration and
and Maxwell
moisture measurement
permittivity models
using ECT and to
for images
compare these results
reconstructing
with mathematical
modeling and
computational uid
dynamics (CFD)
analyses
ECT for developing a To measure and control Lab-scale FBD
closed-loop
the solids moisture
controller
Villegas et al.[120] ECT
Wang et al.[119]
Wang et al.[118]
Chaplin et al.[117] ECT with different

permittivity models
and number of
iterations
Chaplin and
Pugsley[88]
Author(s)
Process target(s)
Local hydrodynamics of batch

uidized bed drying
identied using ECT in
conjunction with S-statistic.
Remarks
Drying of semolina
Semolina drying
(Continued )
ECT successfully employed for

moisture determination in
an FBD and a closed-loop
controller was implemented
by adjusting the air ow
rate.
ECT measurement conrmed
accuracy of the presented
model to predict the
permittivity distribution. In
addition, a distributed
parameter controller was
developed and implemented
to adjust the permittivity
distribution.
Drying of granule including Bottcher and parallel

permittivity models gave the
Croscarmellose sodium
best performance at bed
(disintegrant), Lactose
moistures higher and lower
monohydrate (ller),
than 5 wt%, respectively.
(ller), and
Hydroxypropyl
methylcellulose (binder)
Drying of semolina
The mathematical model,
CFD, and ECT indicate
good potential for
integrating into an online
process control system for a
FBD system.
Lactose monohydrate and

granules drying
TABLE 6
Application of ECT for monitoring of FBDs
1032
Rimpilainen
et al.[122]
Wang and
Yang[121]
Author(s)
Dryer type(s)
To understand the effect Lab-scale FBD

of moisture content,
excitation frequency,
and image
reconstruction models
on ECT measurement
Application(s)
Electrical capacitance To monitor the moisture Lab-scale FBD

tomography (ECT)
content of granules
using Finite
and hydrodynamics of
Element Method
drying chamber
(FEM)-based
reconstruction
algorithm
ECT with different

image
reconstruction
techniques
Technique(s)
TABLE 6
Continued
Remarks
The moisture content and

frequency signicantly
inuenced the capacitance,
loss factor, loss tangent, and
conductance,while
differences between
reconstruction models were
only obvious at higher
moisture content and lower
frequency.
ECT utilized for estimating
Drying of pharmaceutical
average moisture of granules
placebo (microcrystalline
and characterizing bed
cellulose and lactose as
hydrodynamics with respect
ller materials,
to air velocity and moisture
Croscarmellose sodium as
content by tomograms.
disintegrant and
Hydroxypropyl
methyl-cellulose as
binder)
Process target(s)
Drying of semolina
FIG. 4.
Basic optical system of SFV.
granulation process along with the PLS regression

technique.[133] The knowledge achieved using experimental
batches was applied to approximate density and owability
at an early phase of drying. The presented methodology can
be employed to detect early fault detection, to improve
process efciency, and to reduce batch reprocessing time
and=or batch loss.
The main advantages of the SFV technique are real-time
particle size or chord measurement, no need for calibration,
simplicity of signal generation, lack of moving parts,
simplicity and compactness of its set-up, simplicity of the
required hardware, scalability to multiple detector arrays,
ease of use, reasonable commercial cost, high spatial resolution, non-contact nature, and exibility of illumination,
including coherent or incoherent light sources.[134] These
probes can be directly installed on all types of uidized
beds. The SFV can reliably operate even in sticky, damp
environments without assuming the spherical particles at
a standard measurement range spanning between 50 to
6000 mm. However, it is critically important to install these
probes at an appropriate location, commonly the upper
part of the chamber in the process stream, to provide a
representative sampling and detailed measurement and to
prevent window coating. Pressurized air and a mechanical
scraper are usually employed to eliminate the particles
deposition on measurement windows in this probe and to
minimize fouling. To achieve an accurate and reliable
measurement, the data acquisition factors are required to
be optimized according to the dynamics of the process.
On the other hand, this technique underestimates the particles size, since ner particles shift to the upper part of the
bed, leading to a higher concentration of nes.[131] The
number of particles to be registered as the basic population
to estimate a PSD at each time is also a critical parameter
during employing of this technique.
Raman Spectroscopy
Raman spectroscopy is a technique which relies on the
inelastic scattering of electromagnetic radiation created by
energy transfer either from the incident photon to the molecule or from the molecule to the scattered photon, which is
called the Raman effect.[4] Changes in the dipole moment
1033
are responsible for an NIR absorption wavelength, while

molecular polarizability during the vibration is momentous
for the Raman spectroscopy. The Raman spectroscopy
enables identication of the chemical structure of a sample
because of its remarkable chemical specicity in samples
with different forms (solid liquid, slurry, etc.) and to distinguish the compounds presented by measuring molecular
vibrations. Fevotte[135] presented an overview of in situ
Raman spectroscopy for in-line control of pharmaceutical
crystallization and solids elaboration processes. De Beer
et al.[5] aimed at reviewing applications of the Raman spectroscopy to the in-process monitoring of several batch unit
operations during the production of pharmaceutical solid
dosage forms. This technique has been recently applied to
the real-time monitoring and understanding of solid-state
transformations in FBDs (Table 8).
Hausman et al.[62] continuously monitored solid-state
changes of Risedronate during uid bed drying by Raman
spectroscopy in order to relate its spectra with the nal products physical stability. Raman spectroscopy identied the
chemical structure of a risedronate crystal lattice (hydration
state) which was profoundly affected by the nal moisture
of granules. Process end-point and tablet attributes were
successfully determined by direct measurement of the drug
hydration state. Walker et al.[136] applied Raman spectroscopy for in-line determination of the composition of
products inside the uidized bed in 3D as a function of time.
They showed that in situ variation of the structure and composition of the granules=powders within the uidized bed
can be obtained with detailed information by employing
this technique within a relatively short time interval
(120 s). Walker et al.[137] extended their pervious study on
Raman spectroscopy for reducing the time interval of
measurement from 120 s to 10 s. Time-varying composition
of the particle within the uidized bed in 3D was accurately
monitored by this technique.
Raman spectroscopy offers several advantages, including little or no sample preparation, quick data acquisition,
fast response time, remote sampling capability, nondestructive and negligibility of the effect of interfered water
vibrational band on nal results,[137] ability to supply versatile and multivariate information,[5] high exibility,[138]
the manifestation of less complicated and well-resolved
peaks, and the ease of data interpretation. This technique
has the capability of providing online physical=chemical
insights associated with the nal product quality or monitoring solid-state changes within FBDs.
In Raman spectroscopy, the signal intensity is proportional to the concentration of the material in the process
stream, enabling the implementation of quantitative
measurements.[62] Unfortunately, the Raman effect is very
weak, requiring a sensitive and highly optimized instrumentation for suitable detection, which makes it difcult to
measure low concentrations. On the other hand, Raman
1034
Burggraeve
et al.[133]
Burggraeve
et al.[132]
Huang et al.[131]
Narvanen
et al.[130]
Narvanen
et al.[129]
Schmidt-Lehr
et al.[128]
Author(s)
To monitor particle size
Application(s)
granulator
Dryer type(s)
Process target(s)
Remarks
Granulation of mixture of Their probe precisely monitors

granule size suitable for
real-time control of granule
maize starch, starch, and
magnesium stearate using
growth.
polyvinylpyrrolidon
solution as binder
SFV (Parsum probe) To monitor particle size Bench-scale uidized bed Granulation of mixture of SFV was successfully
granulator
theophylline anhydrate
employed in off-line, at-line,
and granule growth at
and a-lactose
and in-line modes to
different water content
monitor particle size.
monohydrate using an
of inlet air, granulation
aqueous binder solution
liquid feed rate, and
of polyvinylpyrrolidone
pause time in liquid
feeding
SFV (Parsum probe) To predict particle size
Lab-scale automated
Granulation of mixture of PLS of SFV data satisfactorily
in conjunction with
top spray uidized bed
theophylline anhydrate
applied for particle size
PLS
granulator
and a -lactose
prediction in uidized bed
monohydrate using
granulator.
aqueous binder solution
SFV (Parsum probe) To characterize
Top spray
Granulating of
Particle size measured using
in conjunction with
particle size
commercial-scale
Biopharmaceutics
the Parsum probe along with
multivariate
uidized bed
Classication System
multivariate approaches in
methods
granulator
(BCS) class 4 compound
in-line mode.
with aqueous solution of
povidone
SFV (Parsum probe) To monitor the
Lab-scale top-spray
Granulation of mixture of In-line SFV technology
showed a good potential for
using different
particle growth
uidized bed
dextrose monohydrate
monitoring of any particle
models including
granulator
and unmodied maize
size changes during
the univariate,
starch with aqueous
granulation.
multivariate PLS,
binder solutions of
and multiway
hydroxypropyl
N-PLS
methycellulose and
Tween 20
SFV (Parsum probe) Modeling and
Lab-scale top-spray
Granulation of dextrose
The employed methodology
in conjunction with
controlling of a
uidized bed
monohydrate and maize
was satisfactorily utilized for
the PLS
uidized bed
granulator
starch mixture with
granules characterization.
granulation process by
Hydroxypropyl
in-line PSD and
Methycellulose as
temperature
binder solution
measurements
SFV (Parsum probe)
Technique(s)
TABLE 7
Application of SFV for real-time particle size measurement in FBDs
1035
TABLE 8
Application of Raman spectroscopy for monitoring of FBDs
Application(s)
Dryer
type(s)
Process
target(s)
Author(s)
Technique(s)
Hausman
et al.[62]
Raman
spectroscopy
To monitor Risedronate
solid-state changes
Walker
et al.[136]
Raman
spectroscopy
To measure composition Lab-scale

of material within the
uidized
uidized bed in three
bed
spatial dimensions as a
granulator
function
of time
Granulation of
standard
Ballotini (glass)
with Lutrol F68
as binder
Walker
et al.[137]
Raman
spectroscopy
To provide three spatial Scientic

dimensions maps of the
uidized
concentration and
bed
chemical structure of
granulator
particles in motion in a
uidized bed
in short time interval
Ballotini
granulation
with Poloxamer
as meltable
pharmaceutical
binder
spectroscopy is not truly non-intrusive because the use of

high-intensity lasers might induce sample heating. The
Raman spectrum can be swamped and hidden due to uorescence interference from impurities or the sample. In
addition, Raman spectroscopy, similar to other spectroscopic techniques used for the online measurement of physiochemical properties, can be costly to implement and may
be subjected to measurement uncertainties originating from
surface physiochemical attributes. It is necessary to generate the calibration sets for each product being produced,
since this technique is also formulation-specic. Raman
spectroscopic monitoring of FBDs typically leads to a considerable amount of spectral data, necessitating the spectral
pretreatment and subsequent chemometric approaches to
illustrate the variation in the data and to extract useful
process information for better process understanding.[5]
Focused Beam Reflectance Measurement (FBRM)
The FBRM operates by projecting a highly focused laser
beam, a continuous beam of monochromatic light, in a
circular path at a high speed (28 m=s), which is produced
by a solid-state laser source. Then, the backscattering time
Lab-scale
FBD
Drying of
Risedronate
sodium
granules
Remarks
Risedronate hydration
state was satisfactorily
monitored using
Raman spectroscopy
for detecting process
end-point by taking
into account the
product quality.
Raman spectroscopy was
applied to present 3D
planes of the
concentration and
chemical composition
of the particles in a
uidized bed within a
relatively short (120 s)
time interval.
Raman spectroscopy
successfully monitored
material composition
and particle
distribution inside
uidized bed with time
interval of 10 s.
from each particle is measured to evaluate the particle

chord length and its distribution (Fig. 5). The backscattered light duration (the measured time of the beam to
cross a particle) is multiplied by the beam velocity to calculate the chord length of the particle. FBRM was developed
for real-time monitoring of particle size and its distribution
in the range of 0.251000 mm at high particle accumulation.[139] Most important researchers have attempted
to utilize FBRM in FBDs to track particle size and its
distribution (Table 9).
The suitability of applying FBRM in uidized bed
granulating was demonstrated by comparing its results with
ofine measurements of laser light scattering and sieve
analysis.[140] Hu et al.[141] found that the chord lengths
obtained by the at-line FBRM technique were equivalent
to those determined by ofine approaches, including
the laser diffraction method and sieve analysis. Recently,
Alshihabi et al.[142] optimized FBRM probe location in
the granulation vessel and identied critical process variables affecting the application of this technique. The data
obtained by FBRM was in agreement with the sieve analysis
with an acceptable correlation coefcient.
1036
AGHBASHLO ET AL.
FIG. 5. Schematic diagram of the focused beam reectance measurement (FBRM) probe technique (upper). Measurement of a particle chord
length using the FBRM technique (lower).
FBRM is easy-to-use, needs minimal maintenance and

calibration, and is applicable for online and insitu determination of particle chord length in FBDs using a special
probe.[143] It can provide information on the number,
nature, shape, and size of particles in the uidized bed
through non-destructive, non-intrusive, and continuous
real-time monitoring of the uidized media. Particle size
measurement by FBRM is not inuenced by the particle
moisture content. However, the FBRM probe is contaminated or fouled by dispersed wet material because of the
intense agitation of wet particles, and this can become
problematic in process analysis without precautionary
system set-ups.[27] It should be noted that pressurized
air and a mechanical scraper have recently been used to protect the probe against fouling. On the other hand, the
main disadvantages of FBRM in a uidized bed is its weak
reliability[111] and the multiple times needed to count particles stuck to the probe window.[143] Moreover, a remarkably
large amount of the sample must be near the probe window
in order to obtain a good measurement[63]; thus, it should be
installed in the dense mass region of the uidized bed.[130]
It can be concluded that the position of the FBRM probe
inside the uidized bed is very likely to affect the magnitude
of the fouling and, hence, the precision of the measurement.
Microwave Resonance Technology (MRT)

The resonance frequency and the resonance bandwidth
of the microwave eld, produced by the induction of
electromagnetic waves with frequencies ranging from
300 MHz to 300 GHz and wave lengths varying from
1.0 mm to 1.0 m, are affected during interacting with solid
products and water molecules. Thus, by measuring the shift
in microwave frequency and resonance attenuation simultaneously, moisture content and density of particles can
be determined without inuencing each other. Figure 6
illustrates the principle of the determination of the product
moisture by MRT. Okamura[144] reviewed the development
of sensors for moisture content measurements by the microwave technique, particularly from the subsurface sensing
point of view for online applications. Table 10 summarizes
recent applications of MRT for monitoring moisture
content and powder density in FBDs.
Buschmuller et al.[145] successfully developed and
employed an MRT probe for successive in-line monitoring
of moisture content of particles through the uidized bed
granulator. Lourenc o et al.[146] employed the in-line MRT
in conjunction with different multivariate data analyses to
determine moisture, temperature, and density of granules
in an industrial uidized bed granulator and dryer using
only historical process data and a few off-line particle size
measurements. They found good correlation between
MRT timely measurements and particle size of the nal
granules based on the PLS regression approach. Chen
et al.[126] studied the effect of different drying air temperatures and mass ow rates on moisture content of granules
and found that MRT can be successfully used for the process
end-point tracing, in particular at low moisture contents.
MRT is a non-contact, non-chemical, and very fast technique to determine moisture and density of particles in a
uidized media. It is insensitive to environmental conditions (like vapor and dust), less sensitive to material
build-up, safe at the low power levels used in measurements,
and has low maintenance requirements.. This technique
provides more representative moisture data continuously
since the measurement is not limited to surface moisture
and is independent from density or product load, color,
and surface structure of solids. The technique does not need
sample withdrawal and provides in-process results because
of its fast acquisition and processing times.[147] A chemometric method is not required if one-target information is
needed, making it more appropriate for monitoring
situations where sophisticated chemometric software and
expert chemometricians are not available.[147] However,
multivariate data analysis techniques should be applied in
order to extract multiple-target information from a large
data set. Moreover, this technique is not always actually
non-intrusive, since the emitted microwave might slightly
accelerate heat and mass transfer during drying, and its
probe has a few intrusive parts. The technique requires
1037
TABLE 9
Application of FBRM in FBDs
Author(s)
Technique(s)
Scheibli[140]
FBRM
Hu et al.[141] FBRM
Alshihabi
et al.[142]
FBRM
Application(s)
Dryer type(s)
To monitor particle
Lab-scale
size distribution at
top-spray
different condition
uidized
of granulation
bed
process and probe
granulator
positions
To investigate granule Bench-scale
growth
top-spray
uidized
bed
granulator
To monitor
granulation growth
kinetics
Bench-scale
uidized
bed
granulator
more expensive electronic components due to the requirement of applying high frequency, and it must be calibrated
separately for different materials. It is difcult or even
infeasible to attain an appropriate spatial resolution
because of the relatively long wavelengths.
Triboelectric Probe
Triboelectrication is dened as a process of charge
exchange between a certain metal surface and the particle
on which a moving particle comes into contact with the
metal surface and friction takes place.[148] The polarity
and strength of the charge is considerably affected by the
type of material, surface roughness, temperature, strain,
and other properties. A triboelectric current can arise from
this charge transfer, namely triboelectric effect or triboelectric charging, when the metal surface is grounded.[148] Intensity and uctuations of the triboelectric current are affected
by several parameters, including concentration of particulate material, size, surface roughness, and velocity of moving particles, geometric characteristics of the particle-metal
surface collisions, material work function and eventual preexisting charge, and the moisture content of particles.[149]
Thus, the triboelectric probe can be effectively applied in
FBDs for identifying the particle moisture and the uidization regime. A typical diagram of the triboelectric probe and
its measuring principle is illustrated in Fig. 7. A survey of
the literature shows that there are few references of using
triboelectric probes to monitor FBDs (Table 11).
Process target(s)
Remarks
Granulation of
Probe position and
polyethylene
process conditions
oxide with
signicantly affected
Polyvinylpyrrolidone
the precision of
(PVP) solution as a
measurement.
binder
Granulation of
Granule formation
pharmaceutical
kinetics was measured
ingredient with
using the handy at-line
microcrystalline
FBRM technique with
cellulose as a ller in
an acceptable accuracy.
the formulation and
binder solution
Granulation of mixture Mean particle size of
of paracetamol and
granules by sieve
microcrystalline
analysis was acceptably
cellulose by binder
correlated with mean
chord length of FBRM.
solution of
Portoghese et al.[149] utilized a triboelectric probe to

detect the local moisture in uidized solids during liquid
injection and the following drying stage at various supercial gas velocities and amounts of the injected liquid. In
another study, the triboelectric probe was used for accurate
real-time measurement of moisture content in gassolid
uidized beds by calibrating with a reliable Karl-Fischer
titration method. Triboelectric signals analyzed by
W-statistic were very sensitive to moisture content below
100 ppm and showed a good agreement with the sample
moisture content with a high correlation coefcient.[59]
Brennan et al.[89] applied the triboelectric probe to diagnose
the minimum bubbling velocity and to monitor drying of
moist particles in a vibrated FBD. This methodology was
useful in determining minimum bubbling velocity and tracing sample moisture content in the drying process.
Triboelectric probes has several benets, including
accuracy, high temperature tolerance, lab-scale or
commercial-scale application, quick measurement,[148] simplicity, sensitivity, low cost, and suitability for qualitative
measurements. However, this technique can only be applied
to detect the end-point of the drying process due to its
acceptable sensitivity in the low moisture content range.[126]
Moreover, the precision of the triboelectric probe is eclipsed
by its blindness for high concentrations and dependency
on ow speed and humidity. This technique cannot be used
behind electric precipitators, and signal processing and
verication is required to obtain reliable information. The
1038
AGHBASHLO ET AL.
FIG. 6. Fundamental of the measurement of particle moisture by the

microwave resonance probe: (a) absorption of microwaves by water
molecules; (b) frequency shift of microwaves by particulates; (c) correlation of the signals to a reference sensor in the center.
position of the triboelectric probes has an important role in

their measurement accuracy, and they do not provide information about the hydrodynamic of drying bed.[122] In
addition, it is necessary to install the triboelectric probe
inside the product bowl, which is not always feasible. As
such, these probes may change the hydrodynamics of the
bed and cannot be considered as a real non-intrusive
approach. Wet powder deposition on the probe can inuence its sensitivity towards the end of the drying process.
Positron Emission Particle Tracking (PEPT)
The PEPT technique employs a positron-emitting tracer
particle into the object of interest. According to the decay
of the isotope, positrons are released and immediately
annihilated with local electrons, generating a pair of collinear back-to-back gamma photons. Using a number of
successively detected c-ray pairs, the location of the tracer
can be found in three dimensions using the triangulation

method.[98] The schematic of PEPT principles is illustrated
in Fig. 8 and is explained comprehensively by Parker
et al.[150] Table 12 summarizes recent application of the
PEPT for monitoring of FBDs.
Schaafsma et al.[151] used a resin bead as the tracer during
uidized bed granulation of lactose to investigate the particle
ow pattern and granule segregation. PEPT experiments
generally agreed well with the segregation experiments, even
when using a different material for the tracer. Depypere
et al.[98] found that the PEPT is a powerful technique in the
visualization of particle motion in a tapered laboratory-scale
FBD. The uidization pattern in a tapered uidized bed was
far from being random. Moreover, this technique can provide quantitative information regarding the bed height and
particle circulation time and size of the coating zone.
The PEPT, as a non-intrusive and real-time measurement technique, can be used to investigate and quantify
particle recirculation within the uidized bed and make
possible direct monitoring of particle pulses. The main
advantage of PEPT measurements is the ability to track
the movement of a tracer in an opaque system without
the need for pre-calibration at high temporal and spatial
resolution due to involving the penetrative c-rays, making
the technique suitable for actual process equipment.[98]
However, major disadvantages of this technique are the
complicated experimental set-up, harder scale-up procedures, limited size of the inspection zone, high initial cost,
and radiation hazards, all of which hinder its widespread
application. In some cases, bed particles cannot be used
as the tracer since the size of the tracer has to be relatively
large to give sufcient activity for monitoring.[152] Thus,
this technique is not a reliable method for monitoring drying processes in which the physiochemical properties, particularly the bulk density of particles, undergo instantaneous
changes with the progress of the drying time.
Miscellaneous Approaches
Two innovative techniques for monitoring different
aspects of FBDs are listed in Table 13. The tracing techniques for measuring cycle time distribution (CTD) of particulate materials can be categorized by the nature of the tracer
and divided into the following four groups: (1) radioactive
tracer; (2) radio transmitter tracer; (3) ferromagnetic tracer;
and (4) magnetic tracer. Traditionally, the radioactive tracer
and radio transmitter tracer have been used in both spouted
and uidized beds[155160] and in both liquid and gas uidized beds.[161,162] However, few works have been published
using ferromagnetic and magnetic tracers.[153,163] Cheng and
Turton[153] reported a linear correlation between the mean
and standard deviation of the CTD over a wide range of uidized bed operating conditions using a magnetic tracer. The
variation in the CTD inuenced the amount of material
deposited on a particle during the batch-coating operation.
1039
TABLE 10
Application of MRT in FBDs
Author(s)
Technique(s)
Application(s) Dryer type(s)
Buschmuller MRT
et al.[145]
To measure
Lab-scale
the moisture
FBD
content of
granules
Lourenc o
et al.[146]
To determine Industrial
scale
the
moisture,
uidized
temperature
bed
and density
granulator
of granules
Chen
et al.[126]
MRT along
with PLS,
PCA and
multivariate
batch
control
charts
MRT
To measure
the granule
moisture
Industrial
FBD
X-ray densitometry is a special kind of nuclear densitometry approach. This technique employs attenuation of photons
produced by a radiation source to determine the density of
material, or volume fraction of solids, along a given measurement path. Wormsbecker et al.[154] investigated the effect of
FIG. 7.
Process target(s)
Remarks
There were close correlations

Drying of placebo
between moisture content of
(containing
the granules determined by the
microcrystalline
microwave resonance probe and
cellulose and
two off-line approaches; i.e.,
a-lactose
loss on drying by infrared light
monohydrate and
disposal and Karl Fischer
povidone 90 as
titration.
binder) and verum
(containing API
cellulose and
povidone 90 as
binder) granules
Granulation of one
There was an acceptable
API and two
agreement between MRT
excipients with an
and particle size of the nal
aqueous solution
granules through a PLS
as binder
regression model.
Drying of granules
including the
Cornstarch,
Maltodextrin,
Microcrystalline
cellulose and water
The MRT provided more subtle

ndings when the granule
moisture was below 25%
(wet basis).
the type of distributor and moisture content of particles

on the uidization regime. The ability of the 1D X-ray
densitometry imaging was authenticated for determining
solids concentration by standard deviation analysis of
high-frequency solids concentration information. Also,
The typical diagram of electrical circuit for the triboelectric probe.
1040
AGHBASHLO ET AL.
TABLE 11
Application of triboelectric probes for monitoring of FBDs
Author(s)
Technique(s)
Application(s)
Dryer
type(s)
Process
target(s)
Injection of
propanolwater
solutions on
glass beads
followed by
drying
Granulation of
glass beads
and silica sand
Portoghese
et al.[149]
Triboelectric
probes
along with
W-statistic
To measure the
solid moisture
content
Experimental
top-spray
FBD with a
rectangular
cross-section
Portoghese
et al.[59]
Triboelectric
probe
with moving
average
Triboelectric
probes with
time-averages,
Fourier analysis
and Holder
exponent signal
processing
method
To monitor the
moisture
content of
solid
To identify the
minimum
bubbling
velocities and
to monitor the
drying
progress
Lab-scale
uidized bed
granulator
Brennan
et al.[89]
FIG. 8.
Schematic diagram of PEPT principle.
Lab-scale
vibrated
FBD
Drying of
ceramic
microspheres
and FCC
Catalyst
Remarks
Triboelectric probe
successfully utilized
for measurements of
solid moisture
resulting from liquid
injection into
uidized beds.
Solid moisture content
was successfully
correlated with
triboelectric signal.
The minimum bubbling
velocities and drying
kinetics were
effectively tracked by
triboelectric probes.
solids concentration was signicantly affected by drying

variables.
The magnetic tracing technique is a non-intrusive,
mobile, and inexpensive monitoring method for continuous
tracking of a single particle in closed media with capability
for measuring the particle alignment and circulation. This
technique also has several other advantages, such as its lack
of need for external energy supply, good resistance versus
interferences, applicability in industrial-scale equipment,
long-time stability, its resistance to pollution, applicability
in non-transparent systems, and the minimal required computational effort. However, this technique has a relatively
low spatial resolution with applicability to only quasistationary external magnetic elds. On the other hand,
the technique is based on tracing of only one comparatively
big magnet particle, limiting its widespread application in
drying processes in which bulk density and moisture content of particles successively vary.[124]
X-ray densimetery is a non-intrusive measurement technique applicable to transparent systems; it eliminates the
potential ow eld distortions by applying intrusive sensors and enables researchers to visualize and quantify opaque uid ow characteristics with a high spatial resolution.
However, the temporal resolution is poor, meaning that
this technique is appropriate only for providing timeaveraged phase distributions.[124] In addition, the limited
size of the inspection area, relative high capital investment,
1041
TABLE 12
Recent application of PEPT for monitoring of FBDs
Author(s)
Technique(s)
Schaafsma
et al.[151]
PEPT
Depypere
et al.[98]
PEPT
Application(s)
Dryer type(s)
Process target(s)
Remarks
To study the
particle ow
pattern and
granule
segregation
Experimental
top-spray uid
bed granulator
PEPT was successfully

employed for
specifying the granule
segregation.
To visualize and
quantify the
features of
the powder
movement
Lab-scale topspray uidized

bed coater
Granulation of
a-lactose
mono-hydrate by
spraying uniform
droplets of a PVP
solution
Coating of glass
microbeads,
sucrose=starch
beads
(nonpareils),
cellulose as core
materials and
sodium caseinate or
gelatin hydrolysate
as coating material
and potential radiation hazard hinder the widespread

application of this technique.
Integrated Approaches
Several researchers have combined different diagnostic
techniques presented in previous sections, or other novel
techniques, for further understanding and precise monitoring of FBDs. Table 14 summarizes some of the recent integrated studies and the most important results obtained
using these approaches.
Better understanding of
the bed
hydrodynamic was
achieved through
monitoring the bed
height, particle
circulation time,
velocity prole,
and residence time
distribution in a
tapered uidized bed.
NIR and Raman spectroscopies were successfully used in

FBD to detect the conversion point of the theophylline
monohydrate to the anhydrate form.[164] Results of in-line
measurements were also conrmed by off-line techniques
such as X-ray powder diffraction and water content
analysis. In a similar study, Bogomolov et al.[138] found that
interpreting a combination of Raman and NIR data can
lead to a synergic improvement in the moisture prediction.
The coating thickness was appropriately determined by
NIR and Raman spectra individually. However, their
TABLE 13
Some miscellaneous approaches applied for monitoring of FBDs
Author(s)
Cheng and
Turton[153]
Technique(s)
Magnetic
tracer
Application(s)
Dryer type(s)
To measure mean and Lab-scale bottom

variance of the
spray uidized
particle cycle time
bed coater
distribution
Wormsbecker X-ray
To study bed
et al.[154]
densitometry
hydrodynamics in
imaging
perforated,
punched, and
porous plate
distributors during
drying of wet and
dry granules
Lab-scale FBD
Process target(s)
Coating of
Nu-Pareil
particles
Drying of wet
placebo
granule
Remarks
The magnetic tracer
particle was
successfully applied
to measure the
particle circulation
rate.
Type of distributors
and moisture state of
granules considerably
inuenced the
time-averaged solids
concentration
proles.
1042
Technique(s)
NIR spectroscopy
sand Raman
spectroscopy with
PLS
ECT, high-frequency
pressure
uctuations,
and RPT
FBRM, NIR
spectroscopy, and
passive acoustic
emission
measurements
NIR spectroscopy and

Raman
spectroscopic and
their combination
with PLS regression
analysis
An acoustic emission
sensor, a ash
topography particle
size analyzer, and
multi-point NIR
probes
Author(s)
Aaltonen
et al.[164]
Pugsley et al.[87]
Tok et al.[63]
Bogomolov
et al.[138]
Leskinen
et al.[165]
To characterize the
granule size
distribution and
moisture content of
granules
To characterize the
coating thickness and
the moisture content
Monitoring uidized
bed drying of
pharmaceutical
granules by electrical
capacitance
tomography,
high-frequency
pressure uctuations,
and radioactive
particle tracking
To detect the
granulation regimes
To monitor the
solid-state transitions
Application(s)
Custom-made
modular top-spray
uidized bed
granulator
Pilot-scale bottomspray uidized bed

coater
Pilot-scale uidized
bed granulator
Conical lab-scale
FBDs
Lab-scale FBD
Dryer type(s)
Granulation of CelletsR,
protease granules,
and caffeine
Drying of granules
containing a-lactose
monohydrate and
microcrystalline
cellulose and
as binding solution
Coating of nonpareil
sugar=starch pellets
with acetaminophen
(Paracetamol),
Acryl-EZE1, and
Opadry Red

granule
Drying of theophylline
monohydrate granules
Process target(s)
TABLE 14
Integrated approaches for monitoring of FBDs
All three employed approaches

were able to identify the
three granulation regimes or
rate processes (wetting and
nucleation, consolidation
and growth, breakage) with
different level of sensitivity.
The coating thickness and
moisture content of pellets
were predicted using the
individual NIR spectroscopy
and Raman spectra and
their combination using
PLS.
The accurate particle size
measurement was obtained
using both the topographic
camera prototype and the
AE signal. Moreover, three
granulation phases,
including the mixing,
agglomeration, and drying,
were successfully detected by
multi-point NIR (eight
probes) and AE methods.
The conversion of the

monohydrate to the
anhydrate form was directly
specied and tracked in
real-time mode.
FBD hydrodynamic was
satisfactorily investigated
using the ECT, RPT, and
pressure uctuations.
Remarks
1043
Passive AE and
vibration
measurements and
pressure uctuation
in conjunction with
various statistical,
frequency, fractal,
and chaos
techniques
Diode laser
stroboscopy (DLS)
and particle
tracking
velocimetry (PTV)
Briens and
Bojarra[166]
Photometric stereo
imaging and Raman
spectroscopy
SFV, FBRM, and

NIR spectroscopy
Burggraeve
et al.[114]
Burggraeve
et al.[168]
Ehlers et al.[167]
Passive acoustic
emission, vibration
measurements, and
pressure uctuation
measurements
Vervloet
et al.[113]
To predict and control

bulk and tapped
densities of nished
To detect the droplet by

diode laser
stroboscopy and to
determine the droplet
size and speed by
particle tracking
velocimetry
To measure the particle
size distributions and
to detect the
solid-state
transformations
during uidized bed
drying
To compare the
potential of both
passive AE and
vibration
measurements to
monitor gradual
process changes with
pressure uctuation
measurements
end-point and to
provide the
additional
information about
the process
Laboratory top-spray
uidized bed
granulator
Lab-scale FBD
Lab-scale uidized
bed granulator
Lab-scale FBD
Lab-scale FBD
Granulation of dextrose
monohydrate and
unmodied maize
Drying of pellet
formulated by mixture
of anhydrous
theophylline and
microcrystalline
cellulose
Glass beads as model

material

granules drying
(mixture of lactose
monohydrate, corn
starch, and
polyvinylpyrrolidone)
Drying of wetted
pharmaceutical
placebo granule
(Continued )
At-line use of photometric

stereo imaging for
measuring the particle size
distribution and brightness
value variations occurring
during pellet drying was
examined in a successful
fashion. Differences between
the Raman spectra
demonstrated
transformation of
theophylline monohydrate
to anhydrate.
Real-time monitoring of
nished granules attributes
was carried out through
The DLS and PTV systems

were satisfactorily used to
specify spray characteristics
and to monitor and estimate
nozzle performance.
The vibration emission

measurements indicated a
potential criterion to
support drying end-point
identication during wet
pharmaceutical granules
drying.
Passive AE and vibration

measurement in conjunction
with a state-space data
analysis method detect
changes in process
hydrodynamics, equivalent
to pressure uctuation
analysis.
1044
Kukec et al.[169]
Author(s)
FBRM and SFV
Technique(s)
product using in-line
measurement in
conjunction with
statistical methods
and to develop a
process control
strategy for a
top-spray uidized
bed granulation
process.
To study the granule
growth kinetics
Application(s)
Lab-scale uidized
bed granulator
Dryer type(s)
TABLE 14
Continued
Similar trends with slightly

different values observed for
the granule growth using
both in-process FBRM and
SFV as affected by binder
content, inlet air
temperature and product
end-point temperature.
Comparable trends in
end-granule particle size
were obtained when
comparing different both
in-process FBRM and SFV,
at-line SFV and off-line
Alpine air jet sieve and
vibrating sieve shaker
particle size measurements.
coupling particle size (SFV)

and moisture (NIR)
measurements and
end-product density was
certied in the established
feed-forward control
procedure.
starch mixture with

Tween 20 and
hydroxypropylmethylcellulose as aqueous
binder solution
Granulation of
carvedilol as model
drug with lactose and
microcrystalline
cellulose as llers and
poloxamer 188 as
meltable binder
Remarks
Process target(s)
combination did not lead to a better performance in this

state. Pugsley et al.[87] applied ECT, high-frequency pressure uctuations, and RPT to improve the fundamental
understanding of gas and solid ow structures in an FBD
and developing monitoring and control apparatus. The
S-statistic was found to be sensitive to changes in the bed
hydrodynamics resulting from the granule moisture evaporation and the corresponding reduction in interparticle
capillary forces. ECT images showed a centralized gas ow
in the beginning of the drying process, which was followed
by a breaking apart of the centralized gas ow as the granule was dried. The RPT results showed that the mixing of
the larger granule fractions was poor at the initial state of
the drying process and then particle mixing improved
towards the end of the drying process.
Tok et al.[63] used three different techniquesFBRM,
NIR, and passive AEto monitor the granulation process.
All three techniques were suitable in discerning granulation
regimes or rate processes (wetting and nucleation, consolidation and growth, breakage) at different levels of sensitivity. However, fouling of the measurement window in
the NIR and FBRM techniques may lead to a slight inconsistency in the result. Three different techniques, including
AE, ash topography particle size measurement, and
multi-point NIR, were used by Leskinen et al.[165] to monitor the uidized beds. Acquired topographic images by ash
topography were employed for particle size determination.
Their results of the in-line measurement agreed well with
the off-line sieve analysis. Vervloet et al.[113] studied capability of the AE and vibration measurements to monitor
the bed hydrodynamics using two types of microphones
and an accelerometer, respectively. The results obtained
by a microphone and the accelerometer, in conjunction with
the S-statistic analysis, were successfully used to track gradual process changes as pressure uctuation measurements
did. It is worth mentioning that the vibration signals originate from the particle-wall collision, as well as formation,
movement, coalescence, break-up, and eruption of bubbles
within the bed. Thus, various vibration signals are generated from particles of different size or density. These signals
can provide useful information regarding bubble characteristics or cluster characteristics.[170] Vibration signature
analysis is widely used for condition monitoring and subsequent fault diagnosis and its severity in mechanical engineering as it ascertains important insights about the defect
development within machines. This technique has been
extensively used for identifying the bed hydrodynamics in
liquid-solid and gas-solid uidized beds.[170173] However,
application of this technique in FBD has been limited to a
few studies in conjunction with other techniques.[113,166]
Application of passive AE measurement for detecting the
drying end-point was unsuccessful during drying of wet
pharmaceutical granules in a uidized bed.[166] However,
the results can be applied to process control to adjust the
1045
uidization gas velocity. In contrast with the passive AE

measurement, the bed vibration measurements showed
a good potential to approximate the drying end-point.[166]
Ehlers et al.[167] investigated the effect of liquid-spraying
nozzle distance from the particle bed, atomization pressure,
relative humidity, inlet air ow rate, and inlet air temperature on size and velocity of droplets by two innovative
procedures, diode laser stroboscopy (DLS) and particle
tracking velocimetry (PTV). They found that these techniques are useful and rapid in determining spray characteristics and in monitoring and predicting the nozzle
performance. The DLS uses a powerful and fast (less than
1 ms) stroboscobic light source for accomplishing highspeed imaging. The short time interval of the lighting pulse
created by light-emitting diodes and semiconductor lasers
was applied to freeze the movement of the target, while
the exposure time of the camera can be relatively long.[174]
The low-image-density PIV was based on measuring the
displacement of particles in the uidized beds over the
known time interval to obtain instantaneous velocities of
suspended particles by illuminating the ow with a uniform
sheet of light and acquiring the images.[175]
Burggraeve et al.[114] satisfactorily examined the use of
at-line photometric stereo imaging during spheronization
and uidized bed drying for determining the PSD and
brightness value measurements with Raman spectroscopy
for detecting solid-state transformations. Photometric
stereo is referred to as a technique in the machine vision
technology for shape estimation (the surface normal and
the surface reectance) of an object by perceiving it under
various illumination sources.
Burggraeve et al.[168] developed a feed-forward control
strategy for the uidized bed granulation process based
on real-time collected process and product information
obtained by SFV, FBRM, and NIR spectroscopy. The
end-product granule characteristics (bulk and tapped
densities) were effectively predicted by a PLS model.
Moreover, real-time moisture content of granules was
estimated using a quantitative PLS model of the NIR data.
Kukec et al.[169] observed similar particle growth trends
at different critical formulation=process parameters from
in-process FBRM and SFV probes, which were in close
correlation with the product temperature. In-line and
at-line SFV measurements showed an excellent potential
for continuous process monitoring in the pilot and
production scales.
Integrating different techniques can provide detailed
process-relevant information and more representative
results with greater reliability of the measurements.
However, the main disadvantages of integrated approaches
are their difculty with timely signal interpretation,
complexity of the set-up, intricacy of required hardware,
high cost, complexity of application in industrial-scale
equipment, and difculty of use.
1046
AGHBASHLO ET AL.
Vibration measurement is a real-time and non-intrusive

technique that requires no measurement tap drilled in the
apparatus, is durable in harsh process conditions, low cost,
easy to implement, rapid, reliable, non-directional, and
intrinsically safe. However, the noise level of the collected
signal is high, the signal can be easily polluted due to background vibrations from other equipment,[113] and the sensors must be located in close contact with the apparatus
as much as possible.
Radioactive particle tracking is a non-intrusive monitoring tool which works quite well in non-transparent particulate media. It provides local-dependent information and has
an ability to monitor the movement of particles with different sizes, shapes, and densities. However, this technique is
time-consuming and expensive, with a limited size of its
interrogation area. The hazards presented by radiation
and changes in the physiochemical attributes of the particle
through the bed are other problems of this technique.
Photometric stereo imaging and ash topography particle size analysis are novel and patented optical imaging
approaches for producing full 3D-structured, ultra-highresolution, blur-free topographic digital images from the
particles surface. Another novel technique, diode laser
stroboscopy, is a high-speed video imaging technique for
monitoring high-speed phenomena (frame rate is several
kHz) with high resolution.[174] Some problems associated
with optical imaging techniques are minimized in these
approaches. However, the price is the limiting factor for
application of these techniques in both the lab and for commercial use.
CONCLUSIONS AND FUTURE TRENDS
Different kinds of non-intrusive techniques have been
employed for monitoring and automating of FBDs, and
these as well as their benets and drawbacks have been
reviewed in this work. Non-intrusive techniques have a
unique niche in real-time and continuous monitoring of
the particles properties, identifying of the uidization
regime, and controlling of the ongoing uidized bed drying
process. These procedures have provided useful insight into
a variety of complex uidized bed drying systems and processes. The interest in non-contact and non-destructive
monitoring of FBDs is growing due to the need for
high-quality reproducible end products, reduction in batch
failure, demand for reducing labor and energy costs, and
demand for safe and accurate automated production equipment. However, the major obstacle for the application of
advanced non-intrusive techniques for monitoring FBDs
is the capital cost. It is necessary to develop a cost-effective,
inexpensive, multipurpose monitoring technique that is
especially applicable to FBDs.
It is clear that there is no perfect technique for monitoring and controlling FBDs. Generally, pressure uctuation,
acoustic emission, and vibration signature analysis present
the least expensive and the easiest options for monitoring

bed hydrodynamics and identifying the process end-point.
It is worth noting that the vibration signature analysis has
great potential to nd applications in drying technology.
However, the positioning of sensors and the method of
processing the signal must be chosen appropriately to
obtain accurate insight. Optical imaging, FBRM, and
SFT techniques offer the best opportunity for particle size
measurement. Nevertheless, the position of the window
and fouling problems must be solved before employing
these techniques. Other innovative approaches, including
ultrasound attenuation, optical visualization by means of
an optical microscope, and laser diffraction, have also presented good potential for monitoring the PSD in FBDs.
NIR spectroscopy, MRT, and ECT techniques have shown
the highest applicability for measuring the moisture content
of particles. However, a reference method needs to be used
for calibration of the instrument. Raman spectroscopy is
the best technique for characterizing the dehydration state
of a particle during drying.
In recent years, biosensors have been applied successfully
for real-time measurements of organoleptic properties of
food materials during processing, as these techniques
permit rapid, non-intrusive, and non-destructive measurements without sampling and preparation. Thus, biosensors
have potential for detecting volatile components and they
can be easily used for monitoring the chemical state of
particulate materials, especially food. More recently, an
emerging generation of innovative smart particles has been
reported in the literature, in which micro-electro-mechanical systems (MEMS) are used to obtain information on
the processes and streams. Such a tool, positioned in a uidized bed, coupled with automatic manipulation of drying
conditions, can be considered for monitoring real-time
bed hydrodynamics and dried material quality assurance
in FBDs. The obvious deciency or gap in non-intrusive
monitoring of FBDs is that different techniques work well
for measuring a specic property; this means researchers
need to employ complex and expensive integrated techniques. It is worth noting that the results given by integrated
approaches are very accurate and more complete than
single-technique measurements. Thus, it is believed that
by employing several techniques concurrently, a clearer
relationship between the recorded signal and particle
properties is obtained. It will be important to develop more
informative techniques or interpretation techniques in order
to overcome any shortcomings of this approach. Otherwise,
multivariable monitoring and control systems should be
employed for in-process tracking and control of the uidization regime and particle physiochemical characteristics.
Increased attention is being paid to the development of
articial intelligence approaches for better modeling and
control of complex dynamic systems. It seems that the
combination of multivariable or multipurpose monitoring
techniques through articial intelligence paradigms may be

one of the interesting elds for future researchers.
FUNDING
The authors would like to extend their appreciation for
nancial support provided by the National Elites Foundation of Iran and the Iran National Science Foundation
(Grant no. G011).
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Measurement Techniques To Monitor and ControlFluidization Quality in Fluidized Bed Dryers: AReview

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Drying Technology

ISSN: 0737-3937 (Print) 1532-2300 (Online) Journal homepage: http://www.tandfonline.com/loi/ldrt20

Measurement Techniques to Monitor and Control

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Date: 10 January 2016, At: 21:06

Drying Technology, 32: 10051051, 2014

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Department of Agricultural Machinery Engineering, Faculty of Agricultural Engineering and

Fluidized bed dryers (FBD) are commonly employed in many

Correspondence: Rahmat Sotudeh-Gharebagh, Multiphase

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physicochemical properties of particles and are, therefore,

Schematic of in-line, online, and at-line product measurements.

In the complex and dynamic environment associated

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MONITORING OF FLUIDIZATION QUALITY IN DRYERS

controlled the drying process better in most cases compared

Temple and van

To identify some of the

To characterize the bed

Lab-scale spouted FBD

To propose the empirical Laboratory-scale

Developing a fuzzy logic

Drying of Allopurinol and The developed program

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Temple and van

To determine the bed

To detect the drying

To monitor and control

Lab-scale uidized bed

To control and monitor Continuous FBD

Sugar spheres and

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The thermodynamics model

Inferential control based on

Bench-scale uidized bed Granulation of mixture of The temperature difference

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MONITORING OF FLUIDIZATION QUALITY IN DRYERS

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product if the target condition is not met. Conventional

into a fuzzy control system, which effectively controlled the

To investigate the effect Lab-scale top-spray

Watano et al.[34] IR moisture sensor

To control the granules

Watano et al.[33] IR moisture sensor

Watano et al.[32] Smart control

The granules moisture content

Lactose and cornstarch

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To monitor the moisture Bench-scale top-spray

Bench-scale uidized bed

Four-wavelength NIR To measure the moisture Laboratory uidized bed

To monitor the moisture Experimental FBD

Bench-scale uidized bed

To measure the PSD

To track the granule

Granulation of magnesium NIR spectroscopy employed