Coating nozzle characterization using
the Malvern Spraytec
Mansoor Ansari and Frantisek Stepanek – Imperial College, London
Introduction
The spraying of liquids is an integral
part of fluidized-bed coating and
granulation. Examples of products
prepared by these processes include
detergents, fertilizers, various instant
food and beverage formulations and
many specialty chemicals and
pharmaceutical products.
In the coating process, a spray of fine
droplets is generally preferred for
even distribution of the liquid onto the
mass of the solid particles (or
granules), as larger drops may lead to
over-wetting and unwanted
agglomeration. In the granulation
process different sizes of binder
droplets provide different conditions of
nuclei formation and granule growth
and thus may significantly influence
the granulation end point. The
characterization of liquid sprays is
therefore an essential pre-requisite for
process optimization and
troubleshooting.
Nozzle Characterization
Techniques
The droplet size distribution delivered
by the nozzles used in coating
processes is dictated by the
properties of the coating liquid
(density, viscosity, surface tension),
the liquid flow rate through the nozzle,
the nozzle geometry and, in the case
of a twin-fluid nozzle, the flow-rate or
pressure of the secondary gas supply.
Although order-of-magnitude
estimates of the mean droplet size
can be made from established
correlations, in general the most
practical and reliable way to
determine droplet size distributions is
to measure them experimentally
1 Spraytec application note
100
0.25 bar
0.5 bar
1.0 bar
80
1.5 bar
2.0 bar
Cumlative Volume (%)
60
40
20
0
0.1 1 10 100 1000
Droplet Size / Microns
Figure 1: Change in droplet size as a function of atomization pressure for de-
ionised water at a fixed flow rate of 10 ml/min.
under the conditions of interest for the stream into a fine spray. It is used in a
nozzle of interest. There exists a wide desktop fluid bed granulator for the
variety of nozzle characterization spraying of various binder liquids,
techniques; these include collection including aqueous solutions of
based methods, imaging analysis and polymers. The behavior of the nozzle
techniques using laser light scattering for different atomization conditions
or absorption. Of those available, and different liquids has been
laser diffraction provides a flexible investigated.
and rapid approach for the
assessment of the delivered droplet Spray Characterization
size, providing advantages in terms of
the ease of set-up and the ability to Different spray profiles were
carry out real-time measurements characterized by systematically
regarding the evolution of the spray varying the air pressures from 0.25 to
plume. 2.0 bar and liquid flow rates from 5 to
20 ml/min in order to determine the
In this study Malvern Spraytec has droplet size distribution for the
been used to measure the droplet operating conditions of interest. The
size of the spray produced by a lab droplet size distributions presented
scale twin-fluid nozzle (Schlick below were measured in the axis of
970S1). This nozzle utilizes the kinetic the spray plume, approximately 50
energy of high-pressure gas (air in mm from the nozzle exit (it is well
this case) to break up the liquid known that droplet size variation can
MRK726-01
occur as a function of position in the Results size distribution shifts to smaller
spray plume). droplet sizes. This relates to the
Figure 1 shows the droplet size increased shear observed within the
The overall atomization performance distributions reported by the Spraytec atomization zone at higher pressures.
was determined for operation of the for the atomization of de-ionised Even so, the nozzle does produce
nozzle using de-ionised water and a water. The flow rate of de-ionised large droplets, even at high air
typical binder used in pharmaceutical water through the nozzle was kept pressures, as shown in the results
granulation, in this case a 5% constant at 10 ml/min whilst the obtained at 2 bar pressure.
aqueous solution of polyvinyl supplied gas pressure was varied. As
pyrrolidone (PVP). the pressure increases the droplet For different processes there may be
a requirement to increase the mass
100
5 ml/min flow of liquid through the nozzle in
10 ml/min order to reduce coating times or
15 ml/min
20 ml/mim
increase coating thickness. Figure 2
80
shows how the flow rate of de-ionised
water through the nozzle affects the
spray plume properties at a fixed
Cumlative Volume (%)

60 atomization pressure of 0.5 bar. The

size distribution was found to increase
in proportion to the liquid flow rate,
40 tracking the change in the available
atomization energy per unit volume of
liquid.
20
Similar observations were noted when
the above experiments were repeated
with a 5% PVP solution, at selected
0 gas pressures and liquid flow rates
0.1 1 10 100 1000
(Figures 3 and 4). In Figure 3, the size
Droplet Size / Microns
distribution observed at 0.25 bar
pressure was found to be bimodal.
Figure 2: Change in droplet size as a function of flow rate for de-ionised water This is probably due to viscous forces
at a fixed atomization pressure of 0.5bar. in the PVP solution that impart a
100 resistance against droplet formation at
0.25 bar lower air pressures. This bimodality
0.5 bar
1.0 bar
progressively disappears as the
80
1.5 bar pressure, and therefore the
atomization energy, is increased.
The same explanation could describe
Cumlative Volume (%)

60 the bi-modal distribution observed at

15 ml/min in Figure 4. An air pressure
of 0.5 bar seems in-adequate to
40 produce a uniform PVP spray. Only
when the liquid flow rate is decreased,
or the atomization pressure
20
increased, is a uniform size
distribution observed.

0 Spray Development
0.1 1 10 100 1000 The variable nature of the PVP spray
Droplet Size / Microns
plume observed at low pressures is

Figure 3: Change in droplet size as a function of atomization pressure for the

5% PVP solution at a fixed flow rate of 10 ml/min.

2 Spraytec application note MRK726-01

confirmed by examining the changes
in the measured droplet size as a
function of time during operation of
the atomizer. This is shown in Figure 100
5 ml/min
5 for the atomization of the 5% PVP 10 ml/min
solution at a pressure of 0.5bar and a 15 ml/min
flow rate of 10 ml/min. As can be 80
seen, significant changes in the
measured Dv90 are observed over

Cumlative Volume (%)

time (Coef. Of Variation = 15%), 60
representing significant fluctuations in
the coarse droplet fraction. This
suggests that liquid break-up is 40
relatively uncontrolled in this situation
as the atomization energy available is
low. At higher atomization pressures
20
the variation in the Dv90 is
considerably less (Coef. Of Variation
= 1.5% at 1.5bar for the 5% PVP
0
solution), representing a more uniform
0.1 1 10 100 1000
spray plume (Figure 6). Droplet Size / Microns

Conclusions Figure 4: Change in droplet size as a function of atomization pressure for

The measurement of the droplet size the 5% PVP solution at a fixed atomization pressure of 0.5 bar.
distribution produced by a twin-fluid
spray nozzle has been demonstrated.
The results obtained show that the
size can be regulated by adjusting
200
gas pressure and liquid flow rate. In
Dv10
addition to these process parameters, Dv50
the physical properties (e.g., viscosity) Dv90
of the spraying liquid also play an
important role in defining droplet size 150

and its distribution.

Size / Microns

The Spraytec system provides a

reliable and rapid way for spray 100
characterization. The system is
therefore a valuable tool in designing,
optimizing and troubleshooting of
coating and granulation processes.
50

0
0 10 20 30 40 50 60
Time / sec

Figure 5: Change in droplet size as a function of time for the 5% PVP

solution at liquid flow rate of 10 ml/min and a gas pressure of 0.5 bar.

3 Spraytec application note MRK726-01

 50
Dv10
Dv50
Dv90

40
Size / Microns

30

20

10
0 10 20 30 40 50 60
Time / sec

Figure 6: Change in droplet size as a function of time for the 5% PVP solution at
liquid flow rate of 10 ml/min and a gas pressure of 1.5 bar.

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4 Spraytec application note MRK726-01