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Characterization of the Residence Time Distribution in

Spray Dryers
a b b
Marcelo G. G. Mazza , Luiz E. B. Brandão & Glória S. Wildhagen
a
Faculdade de Ciências Humanas de Aracruz (FACHA) , Centro Aracruz, Brazil
b
Instituto de Energia Nuclear , Cidade Universitária , Ilha do Fundão, Rio de Janeiro, Brazil
Published online: 06 Feb 2007.

To cite this article: Marcelo G. G. Mazza , Luiz E. B. Brandão & Glória S. Wildhagen (2003) Characterization of the Residence
Time Distribution in Spray Dryers, Drying Technology: An International Journal, 21:3, 525-538, DOI: 10.1081/DRT-120018460

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DRYING TECHNOLOGY
Vol. 21, No. 3, pp. 525–538, 2003

Characterization of the Residence Time

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Distribution in Spray Dryers

Marcelo G. G. Mazza,1 Luiz E. B. Brandão,2 and

Glória S. Wildhagen2,*
1
Faculdade de Ciências Humanas de Aracruz
(FACHA), Centro Aracruz, Brazil
2
Instituto de Energia Nuclear, Cidade Universitária,
Ilha do Fundão, Rio de Janeiro, Brazil

ABSTRACT

In this work it is presented a study on the residence time distribution

(RTD) of particles in a co-current pilot-plant spray dryer operated
with a rotary atomization system. A nuclear technique is applied to
investigate the RTD responses of spray dryers. The methodology is
based on the injection of a radioisotope tracer in the feed stream
followed by the monitoring of its concentration at the outlet stream.
The experiments were performed during the drying of aqueous

*Correspondence: Glória S. Wildhagen, Instituto de Energia Nuclear, Cidade

Universitária, Ilha do Fundão, CP 68550, Rio de Janeiro, RJ 21945-970, Brazil;
E-mail: mazzavivia@predialnet.com.br.

525

DOI: 10.1081/DRT-120018460 0737-3937 (Print); 1532-2300 (Online)

Copyright & 2003 by Marcel Dekker, Inc. www.dekker.com
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526 Mazza, Brandão, and Wildhagen

suspensions of gadolinium oxide. The RTD responses obtained

experimentally presented good reproducibility, indicating that the
technique applied is well suited to investigating fluid-dynamics of
spray dryers. In addition to the experimental investigation, a mathe-
matical model was used to describe the RTD experimental curves.

Key Words: Spray dryer; Residence time distribution; Experiment;

Mathematical modeling.
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1. INTRODUCTION

Spray dryers are employed in the transformation of liquid materials

(solutions, suspensions, and pastes) into solid products with desired
moisture and are used in many sectors of the chemical, pharmaceutical,
and mineral industries.[1] The principle of the process is the atomization
of the fluid feed stream into droplets and their dispersion in a hot gaseous
phase. Due to small size of the droplets, the heat and mass transfer
area per unit volume is considerably high, providing the possibility of
achieving high particle drying rates. The dried particles are recovered by
gravity and through the use of cyclones.[2]
Generally, the time required to dry the process products is calculated
considering the residence time of the particles inside the equipment
similar to the average residence time of the air used in the drying.
However, due to inertial forces and also deposition of the particles on the
internal walls of the equipment, the particles may present residence times
significantly higher than that of the gas, which may result in the thermal
degradation of the product.[3] The proper knowledge of the particles
residence times in the equipment may be helpful during the adjustment
and control of operational variables, minimizing problems related to
product quality. Besides, the knowledge of the RTD function of the
particles is an important issue during the resolution of mathematical
models of spray drying processes based on population balances[4–6] and
for the validation of CFD models.[7–11]
Despite the potential applicability of RTD experiments and
mathematical modeling of RTD responses during design, operation,
and optimization of spray dryers, very few studies in the literature are
concerned to this topic.
Pham and Keey[12] performed a series of exploratory experiments
in order to measure the RTD of droplets of sodium bicarbonate in a
co-current spray dryer. These authors used a solution of sodium
bicarbonate marked with 14C as the tracer. During the experiments the
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RTD in Spray Dryers 527

gas phase was not warmed in order to prevent evaporation of the droplets
and, therefore, simplify the process. The droplets were collected by an
appropriate device to undergo posterior determination of their radiation
content. The results obtained in this work presented fluctuations that
were attributed to errors related to the radiation content determination,
given by the small number of droplets collected in each sample, and also
the instability of the droplets stream.
Taylor[13] studied the gas and particle RTD for two different sizes
countercurrent spray dryers. Gas phase RTD was determined by
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injection of a pulse of hydrocarbon and the measurement of its

concentration in the outlet stream by an organic analyzer. In the
determination of the particle RTD an inorganic salt tracer was used.
The powder output stream was sampled and the tracer concentration
was measured using atomic adsorption spectroscopy. The results were
interpreted using a mixed-flow empirical model, which fitted the
experimental data better than dispersion flow models.
Kieviet and Kerkhof [3] determined the RTD of particles in a
co-current spray dryer during the drying of aqueous maltodextrin solutions.
The tracer used in the experiments was rhodamine, a substance that has
an intense red color that permits the measurement of its concentration
in the dried powder by means of spectrophotometry. The rhodamine
tracer was injected in the feed stream in the form of a pulse of short
duration and its concentration was measured in the dried product samples,
collected within intervals of 2 s, leading to a multitude of absorbance
analyses. The major drawback of this spectrometric technique is that it is
not suitable to problems involving suspensions and pastes, therefore
preventing its usage in many real applications of drying processes.
Ducept et al.[14] performed an experimental RTD of particles study
to validate CFD simulations of a superheated steam spray dryer. The
method is based on conductivity measurement, using a KCl solution.
The experiments were evaluated in two different operational conditions,
leading to distinct RTD responses.
In the present work a nuclear technique is used to determine the
RTD of particles in a spray dryer based on a stimulus-response approach.
A radioactive tracer is injected in the spray dryer feed stream and
is continuously monitored in two specific points along the equipment
by scintillator detectors. The experimental method proposed allows
measurements in real-time, with high sampling frequency, in order to
improve the characterization of the RTD curve and may be applied to
virtually any type of material presented in a solution, suspension, or
paste. In addition to the experimental investigation, a mathematical
model was used to describe the RTD experimental curves.
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528 Mazza, Brandão, and Wildhagen

2. MATERIALS AND EXPERIMENTAL METHOD

2.1. Equipment

The experiments were performed in a pilot-plant spray dryer

(model PSD 52, APV-ANHIDRO Co.) with a drying chamber presenting
a diameter of 1 m and able to evaporate 9.25 kg of water per hour
(Fig. 1). The equipment uses a centrifugal atomization system with a
rotary disc located in the center of the air disperser (Fig. 2). This
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configuration provides a co-current contact between the droplets and

drying hot air. The suspension to be dried was stored in a mixed tank
and was transferred to the rotary atomizer through a peristaltic pump.
The rotary atomizer is capable of operating with rotations per minute as
high as 50,000. The spray of droplets is dispersed into the gas stream
provided by a blower and warmed-up by a set of electric heaters. The
dried material is separated from the gas stream and collected in two parts:
coarse particles are collected by gravity at the bottom of the equipment
and the fine particles are separated by a downstream cyclone (cf. Fig. 1).

2.2. Suspension and Radioactive Tracer

The experiments were performed using an aqueous suspension of

gadolinium oxide. It is important to emphasize that the study of the spray
drying of gadolinium oxide belongs to a extensive research investigation
that aims at obtaining high purity rare-earth elements oxides with
controlled particles morphology.[15]
In order to select an appropriate tracer, the activity of the emitted
gamma radiation and half-life of several substances were taken into
account. An ideal tracer should present a sufficiently high gamma energy
in order to be detected even when dispersed along the radial surface area
of the drying chamber of the spray dryer, and its half-life should be suffi-
ciently small to permit the start-up of the equipment as soon as possible.
Pure lanthanum oxide was the most suited substance for the experiments
because its isotope 140La presents half-life of 40 h and principal gamma
ray emission of 1.59 MeV, which provides perfect experimental detection
of the marked material, as reported by Brandão et al.[16] Furthermore,
the location of lanthanum in the periodic table of elements imparts to
this element physico-chemical properties similar to those found for
gadolinium. Finally, it is important to say that the tracer and product
morphologies are similar, once the particles size distribution (PSD)
influences their residence time in the equipment.
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RTD in Spray Dryers 529

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Figure 1. Diagram of the experimental set-up. 1—Drying chamber;

2—Suspension feeding tube; 3—Rotary atomizer; 4—Air duct; 5—Temperature
sensor; 6—Electrical heaters; 7—Drying chamber lateral port; 8—Air blower;
9—Scintillator detector; 10—Valve; 11—Product collecting device; 12—
Peristaltic pump; 13—Cyclone; 14—Control panel.
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530 Mazza, Brandão, and Wildhagen

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Figure 2. Diagram of the air and suspension feeding system. 1—Rotary atomizer;
2—Feed pipe; 3—Drying air.

Table 1. Morphology of particles.

Morphology of particles Gd2O3 La2O3

D(v, 0.5) (mm) 4.33 4.49

D(v, 0.1) (mm) 0.32 0.29
D(v, 0.9) (mm) 17.51 45.77

Both tracer and dried product were analyzed according to their PSD
in a laser diffraction Malvern Mastersizer Micro Plus (model MAF 5001).
Table 1 presents the PSD results obtained, where D(v, 0.5) is the diameter
that divides the particle distribution into two equal parts, and D(v, 0.1)
and D(v, 0.9) represent the diameters below which it is found 10% and
90% of the sample volume, respectively. It is observed that both tracer
and dried product present similar average diameters and that the
140
La oxide PSD is larger than that obtained for gadolinium oxide.

2.3. Methodology for the RTD Determination

The methodology used in the experimental determination of the RTD

consists of injecting a pulse of radioactive tracer in the suspension feed
stream of the spray dryer followed by the monitoring of its concentration
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RTD in Spray Dryers 531

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Figure 3. Diagram of the alternative injection system of tracer suspension.

signal at the outlet stream. The injection was carried out using a syringe
located at the atomizer inlet in the form of a pulse of approximately 3 s.
In each experiment, 10 mL of tracer with approximately 20 mCi was
injected.
An alternative injection system was used to verify the effect of the
pressure exerted by the syringe. In order to perform such comparison,
a set of experiments was performed with tracer injected in the drying
chamber at the same conditions of the suspension. Figure 3 illustrates
this alternative method. Through the manipulation of the two upstream
on-off valves it was possible to alternate the suction point of the peristal-
tic pump from the suspension tank to the reservoir containing the tracer,
also kept in an aqueous suspension. The tracer suspension was colored
using an inert dye in order to identify the exact moment of introduction
and time duration of the pulse in the equipment.
The tracer dynamics along the equipment was monitored by two
scintillator detectors NaI (3
300 Ortec—Integral Line) coupled with
photomultipliers located at the upper part of the drying chamber, below
the atomizer, and at the discharge cone, both placed 15 cm distant from
the equipment external wall (cf. Fig. 1). In order to minimize electronic
noise interference on the tracer signal recorded by the system, each set
detector/photomultiplier was covered by a copper sheet of 0.3 cm
thickness and shielded by a lead conic collimator of 5.0 cm thickness.
The signal of each detector was processed by a monochannel analyzer
system and converted through an analog/digital interface to be acquired
and stored in real-time in a computer.
The response obtained from the technique presented above is the
temporal profile of the radiation counting rate, C(t), which is proportional
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532 Mazza, Brandão, and Wildhagen

to the dynamic evolution of the outlet stream tracer concentration.

The residence time distribution function is given by the following equation:
CðtÞ
EðtÞ ¼ R 1 , ð1Þ
0 CðtÞ dt

where C(t) is the radiation counting rate as a function of time.[17,18] E(t) dt

represents the fraction of tracer elements that have spent a time between
t and t þ dt inside the spray dryer.
It is important to emphasize that the amount of radiation collected
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by the scintillator detectors varies according to the concentration of

140
La present in the tracer sample, therefore generating response curves
with different amplitudes. Thus, it is more convenient to represent the
RTD function in a dimensionless form:
Eð
Þ ¼
EðtÞ, ð2Þ
where
is the dimensionless time given by:
t

¼ , ð3Þ


and
is the particles average residence time in the drying chamber and
is given by the following expression that represents the first moment of
the distribution:
Z1

¼ tEðtÞ dt: ð4Þ
0

The experimental RTD responses were described according to the

mathematical model of continuous stirred tanks in series. The number
of tanks in series necessary to describe the experimental RTD curve was
determined from the first and second moments of the distribution. In
dimensionless form, the theoretical RTD function for tanks in series is
given by:
nðn
Þn1 n

Eð
Þ ¼ e , ð5Þ
ðn  1Þ!
where n is the number of tanks in series, defined as the inverse of the
dimensionless variance:
2 2,t 
2

¼ : ð6Þ

2
In Eq. (6), m2,t represents the second moment of the distribution and is
defined by the following expression:
Z1
2,t ¼ t2 EðtÞ dt: ð7Þ
0
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RTD in Spray Dryers 533

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Figure 4. Experimental and theoretical RTD curves of the particles for

experiment 01.

3. RESULTS AND DISCUSSION

Figures 4 to 7 present the results of the technique describe above

during the drying of an aqueous suspension of gadolinium oxide present-
ing 35% w/w of solids concentration and a feed flow rate of 70 mL/min.
The air temperature at the spray dryer inlet was maintained at 240 C
with a mass flow rate of 148 kg/h. The speed used in the atomizer was
46,000 rpm. In each experimental run, approximately 20 mCi of radioac-
tive tracer suspension (
10 mL) were injected in the spray dryer. The
tracer concentration at the outlet stream was recorded within
intervals of 50 ms. Figures 4–6 present the particles experimental and
theoretical RTD responses for the experiments performed using the
syringe tracer injection technique. The experimental responses were
described according to the mathematical model of continuous stirred
tanks in series presented above (cf. Eq. (5)). The experimental results
presented very good reproducibility with an estimated average residence
time of 72.5 s and standard deviation of 3.8 s. The number of continuous
stirred tanks in series that better described the experimental responses
was 1.99 with a standard deviation of 0.09.
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534 Mazza, Brandão, and Wildhagen

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Figure 5. Experimental and theoretical RTD curves of the particles for

experiment 02.

Figure 6. Experimental and theoretical RTD curves of the particles for

experiment 03.
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RTD in Spray Dryers 535

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Figure 7. Experimental and theoretical RTD curves of the particles for

experiment 04.

The experimental RTD curves of particles obtained in this work was

considerably different from that observed for the gas phase, that presented
an average residence time of 20 s in disagreement with the common sense
in the literature. In spite of using different equipment configurations, this
difference was also observed by Kievet and Kerkhof.[3]
Figure 7 presents the results obtained for the experiment performed
using the alternative injection system of tracer suspension. The calculated
average residence was of 71.6 s and was described by 1.86 tanks in series.
Considering 95% of confidence interval and that the experimental data are
normally distributed,[19] the average residence time and number of tanks in
series for the experiment using the alternative method lay within the con-
fidence intervals found for the previous experiments. This result indicates
that both injection techniques lead to similar results. The relatively enhanced
level of noise found for this experiment was due to a background signal
increase, and is not related to the modification of the injection technique.

4. CONCLUSIONS

Experiments were performed in order to characterize the residence

time distribution of particles in a pilot-plant spray dryer during the drying
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536 Mazza, Brandão, and Wildhagen

of an aqueous suspension of gadolinium oxide. A nuclear technique based

on a stimulus-response methodology was proposed using radioisotope
140
La as radioactive tracer. The experimental RTD curves presented
very good reproducibility, indicating that this technique is perfectly
suited for this sort of equipment. This work enhances that particles and
gas can present significant different average residence times, as previously
reported by Kieviet and Kerkhof.[3]
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NOMENCLATURE

E Residence time distribution function

C Outlet stream tracer concentration signal (cpm)
n Number of tanks in series
t Time (s)

Greek Characters

Dimensionless time

Average residence time of the particles (s)
m2,t Second moment of the distribution

ACKNOWLEDGMENT

The authors would like to thank CNPQ—Conselho Brasileiro de

Desenvolvimento Cientı́fico e Tecnológico (Brazil) for providing
scholarship to M. G. G. Mazza.

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538 Mazza, Brandão, and Wildhagen

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