Mixing and Dissolution Times for a Cowles Disk

Agitator in Large-Scale Emulsion Preparation

Thomas L. Rodgers,, Michael Cooke, Flor R. Siperstein, and Adam Kowalski
School of Chemical Engineering and Analytical Science, University of Manchester, M60 1QD,
UK, and Unilever R & D Port Sunlight, Quarry Road East, Wirral, CH63 3JW, UK
E-mail: T.Rodgers@postgrad.manchester.ac.uk

Abstract
Emulsions are often found in formulated products. During the preparation of emulsions, it
is often desirable to dissolve highly viscous fluids, such as surfactants or other additives, into an
aqueous phase. In this work we measure dissolution times for a non-Newtonian highly viscous
surfactant (sodium laureth sulphate) in water using vessels of different diameter (D = 0.9 and
D = 0.15 m) with high shear disk agitators (D/T = 1/3 and 0.62). To monitor the dissolution
times we use a volume averaged conductivity obtained by 3D electrical resistance tomography.
We compare the validity of the method and highlight the difference between dissolution times
for highly viscous fluids and blending times for tracers with the same viscosity as water.

Introduction
Many of the things that make our life more comfortable, safer, and that make us feel better are formulated products. They contain the appropriate quantity of several compounds, mixed, arranged,
University
Unilever

of Manchester
R & D Port Sunlight

Thomas L. Rodgers et al.

Cowles Disk Dissolution

and structured in the correct way to perform a specific application. The performance of a formulated product depends not only on its chemical composition (the ingredient), but also on the
preparation method. A wide range of formulations are emulsion based, such as margarine, creams,
paints, and pharmaceuticals, where a liquid is dispersed as small droplets into an immiscible liquid
that remains as a continuous phase.
Emulsion preparation often requires the addition of an emulsifier agent, such as a surfactant
or protein. The blending and dissolution mechanisms of the emulsifier can affect the properties of
the final product, and understanding such mechanisms is important for the control of the process
and product properties, as well as for the design and scale-up of new processes. These emulsifiers
generally have very different viscosities and densities to the bulk liquid to which they are added,
and the homogenization of such systems can often be very different to blending operations. As both
these processes involve mixing of miscible fluids it is often assumed that this is simply a blending
operation. It is however in reality a two stage process consisting of dissolution (breakdown of the
initial agglomerates) and miscible blending, both of which involve mixing.
Flooding experiment with sodium lauryl sulphate (SLES) clearly suggests that in this system
there is a concentration gradient as there is a phase change, Figure 1. Due to the high viscosity
the SLES can be regarded as a soft solid, thus the surface tension is not important. As the SLES
dissolves into the water it forms a micellar solution with the same viscosity of water.
In this work we compare blending and dissolution rates in agitated vessels for fluids with
different viscosities, and show the factors needed for a general correlation that can be used for the
estimation of blending and dissolution times.
We used Cowles disk style agitators which are commonly used in the preparation of emulsions
due to their ability to produce a high shear rate, which is ideal for drop break-up. 1 They also
have the ability to be used over a large range of emulsion viscosities and handle large viscosity
differences between the dispersed and continuous phases. 2 Nevertheless, little information that
would be necessary for process scale-up, such as blending times and power numbers, are available
in the literature.

Thomas L. Rodgers et al.

Cowles Disk Dissolution

Figure 1: View of 70 wt% SLES in contact with water, showing a thin hexagonal phase boundary
layer. Real image width is 1 m.

Blending Times
The difference between blending and dissolution for the addition of liquid to liquid can be due
to a viscosity, density or surface tension difference between them. This difference can create an
interface between the liquids which has characteristic concentration gradients with diffusion as the
added liquid dissolves into the bulk. However, it is not yet fully understood how this divide can be
quantified and what mechanisms define the difference between blending and dissolution.
Currently there are no correlations which can predict the time taken to produce a homogeneous
mixture when a tracer is added to a bulk solution of a different viscosity.
A large amount of work has been carried out on the blending of liquids with similar physical
properties within the turbulent, transitional, and laminar regimes for Newtonian, shear thinning,
and visco-elastic fluids. 3 It has been shown that the blending time depends on the specific power
input (P/ V ), the tank geometry and the agitator Reynolds number (Re). It has been common place
in the literature to correlate the dimensionless mixing time (95 N) against other dimensionless
values which represent the above variations, i.e. the agitator power number (Po), the impeller to
tank diameter ratio (D/T ), the liquid height to tank diameter ratio (H/T ), and the agitator Reynolds

Thomas L. Rodgers et al.

Cowles Disk Dissolution

number. For blending in the turbulent regime the dimensionless mixing time is independent of the
Reynolds number and has been correlated to equation 1. 3 It is worth commenting here that the
data for this correlation was mainly collected on vessels with H/T 1. Cooke et al.(1988) 4 has
shown that for H/T >> 1 the exponent on H/T increases considerably due to zoning. However,
the correlating equation is of the same form and does not effect the general conclusions drawn.
Therefore, this correlation should be used with caution for large aspect ratios.

95 N = 5.2Po

31

 2   1
D
H 2
T
T

(1)

Equation 1 can be rearranged using the definition of the power number to give equation 2, where

is the liquid density, V is the liquid volume in the tank given by equation 3 where is the
ratio of a dished base height to the tank diameter for a half ellipsoid base (this is very similar to a
torispherical base but simpler to consider, 0 for a flat base to 0.5 for a hemispherical base).


P
95 = 5.64
V

 1   1
 1
 1 
3
3
2
H 2 H 3
D
3

T
T
T
T
3

(2)



3 H
V= T

4
T
3

(3)

Equation 2, which only applies to the turbulent regime reveals that:

Maintaining constant tank dimensions, agitators of the same diameter have the same mixing
time if they have the same power input,
Increasing the agitator diameter will decrease the mixing time at constant power input,
Increasing the fluid hight will increase the mixing time,
The mixing time is independent of the fluid viscosity at a constant power input,
At a constant power per unit mass the mixing time is slightly longer in a dished base tank
compared to a flat bottom vessel,
4

Thomas L. Rodgers et al.

Cowles Disk Dissolution

When scaling-up at constant power per unit mass and geometry the mixing time will increase
with the tank diameter.
The boundary between the turbulent and the transitional regime can be given by equation 4. 3
Blending in the transitional regime is not independent of the Reynolds number like the turbulent
regime, therefore equation 5 has been proposed. 3 The blending is much slower in the transitional
regime and the variability on equation 5 are much larger than for the turbulent regime, this is due
to the uncertainties in the transitional regime.
1

Po 3 ReT T = 6370

95 N = 33489Po

32

Re

(4)
 2
D
T

(5)

As equation 1 was rearranged in terms of the power, equation 5 can be rearranged to become
equation 6.
 2     2


3
2
 23 P 3
D
95 = 39340.7 1
T3
3
V

(6)

Equation 6 reveals that:

Agitators of the same diameter have the same mixing time if they have the same power input
in the same fluid (if in a Newtonian fluid),
Increasing the agitator diameter will decrease the mixing time at constant power input,
The mixing time is proportional to the fluid viscosity and inversely proportional to the fluid
density at a constant power input,
At a constant power per unit mass the mixing time is longer in a dished base tank compared
to a flat bottom vessel (over 10 % longer for a hemispherical base),
When scaling-up at constant power per unit mass and geometry the mixing time will decrease
with the tank diameter.

Thomas L. Rodgers et al.

Cowles Disk Dissolution

The first two conclusions are the same as in the turbulent regime. The third is different and
shows the dependence of the mixing time on the fluid that is being mixed. The fourth is similar to
the turbulent regime, apart from the effect of a dished base is more pronounced. The fifth is the
opposite to what happens in the turbulent regime, this is due to when scaling up at constant power
per unit mass, the Reynolds number increases and the mixing time is inversely proportional to the
Reynolds number. It is therefore critical to know what regime you are working in when you are
trying to scale a process.
The boundary between the transitional and the laminar regime can be given by equation 7. 3
1

Po 3 ReT L = 183

(7)

Some correlations are available for the calculation of the blending time in the laminar regime, but
these are only for specific agitator systems; e.g. anchor type 5 or ribbon type; 6 or dont offer a
transferable correlation away from the system used. 7
Most of the work upon which the correlations 1 and 5 are based rely on blending of fluids
with similar viscosity. For fluids of different viscosities these correlations will not always be
appropriate, as for some conditions mixing times can be much longer than those predicted. For the
blending of fluids of different viscosities the modified Reynolds number, Re , has been proposed
to characterize the different flow regimes, 8 equation 8.

b
Re = Re
a

b ND2
a

(8)

This has lead to the determination of two possible regions;

Stirrer controlled regime (Re > 100) where the mixing time does not depend on the added liquid properties, the dimensionless mixing time for a given system is constant, and equation 1
predicts the mixing time
Added liquid controlled regime (Re < 100) where the viscosity of the added liquid and the ag6

Thomas L. Rodgers et al.

Cowles Disk Dissolution

itation speed effect the mixing and where the added liquid can maybe said to be dissolving,
rather than simply mixing.
For the blending of fluids of different density the modified Richardson number, Ri , has been
suggested, in a similar manner to the modified Reynolds number, 9 but this also takes into account
the added volume and not just the density difference, equation 9.


Va
Ri = Ri
Vb

(a b ) gHVa
b N 2 D2Vb

(9)

Again two main regions have been defined;

Stirrer controlled regime (Ri < 0.025) where the mixing time does not depend on the added
liquid properties and equation 1 can be used.
Added liquid controlled regime (Ri > 0.05) where the density and volume of the added liquid
and the agitation speed effect the mixing.
The range between Ri = 0.025 0.05 seems to depend on the agitator as different authors have
obtained different critical values. 9,10 This seems to indicate that there are other factors that need to
be taken into account.
There is some evidence 11 that when mixing a tracer of a high viscosity that a smaller agitator
gives a smaller dimensionless mixing time (by several orders of magnitude) when run at the same
power as a larger agitator. This is the converse to what we would expect for blending a brine tracer
into water and from equations 1 and 5.
Table 1 shows a comparison of the pumping rate and the shear rate of a 45 4 blade pitch
blade turbine for two different diameters with equal power input, based on data available in Hemrajani and Tatterson (2004). 12 Although the pumping rate is lower for the smaller agitator, the
shear rate is higher. No matter what concept is used to define the shear in the agitator region, the
smaller agitator produces more shear at an equal P/ V due to its greater speed. Therefore, when
mixing a tracer with high viscosity, where dispersion effects dominate, an agitator that gives a high
7

Thomas L. Rodgers et al.

Cowles Disk Dissolution

shear rate will perform better. The opposite occurs in blending operations where pumping rate
determines the mixing time.
Table 1: Comparison of pumping rate and shear rate for a 45 4 blade pitch blade turbine. Power
numbers and Flow numbers from Hemrajani and Tatterson (2004). 12

Size
T
2
T
3

T /m
0.91
0.91

1 Value
2 Value

D / m N / rpm Po
P / W NQ Q / m3 s1
0.46
300.0 1.27 3165.0 0.61
0.291
0.30
589.7 1.27 3165.0 0.81
0.225

1/ s1
2.29
3.00

2/ s1
750.0
1474.2

based on ND
based on 150N 12

It has also been noted that at lower speeds tracers of higher viscosity and density can settle
on the bottom of the tank. 13 This means that the mixing time for viscous tracers will be vastly
different for tracers that are lifted by the agitator and those that are not. This critical agitation
speed, NCD , might be predicted by equation 10, 14 where the mean density and viscosity are given
by equations 11 and 12. The very small exponents on the viscosity and surface tension show that
the NCD is fairly insensitive to these physical properties. Note the similarity to the Zwietering
equation (equation 13) 15 with different parameter relating to solids rather than a second liquid.

NCD = S

g0.41 0.41 m0.09 0.045 0.05

D0.725 m0.545

m = a + (1 ) b


b
1.5a
m =
1+
1
a + b
NJS = S

g0.45 0.45 b0.1 0.2 0.13

d p Xp
D0.85 b0.55

(10)

(11)
(12)

(13)

Most previous work has either looked at fluids of similar viscosity in a range of regimes, or
looked at different viscosities with both materials having Newtonian like behaviour. From these
studies two regimes have been seen for solutions of different viscosities, the stirrer controlled
8

Thomas L. Rodgers et al.

Cowles Disk Dissolution

regime and the added liquid controlled regime. This work uses this analysis to examine the mixing
of a viscous shear thinning surfactant when added to water using a typical high shear agitator.

Methods and Materials

Equipment
Two vessels were used in the experiments, a 0.914 m (3 ft) and a 0.152 m (6 inch) diameter vessels.
The 0.914 m vessel is a Perspex cylindrical vessel with a shallow dished base and 4 standard baffles
of width T /10. The cylindrical section is 1.5 m high and is fitted inside a square jacket through
which water can be circulated for temperature control. The square jacket provides distortion free
viewing windows for flow visualisation. The agitator rotational speeds are monitored using a
Ferro-magnetic proximity sensor coupled to a COMPACT MICRO 48 tachometer. The shaft is
continuous and fits into a PTFE bearing located in the centre of the dished base. The agitator
power is measured using a dual torque strain gauge system bonded to the shaft, designed to cancel
out bending moments. The strain gauge is wired to an ASTECH Strain Gauge Bridge fitted with
a telemetry readout, which is connected to a LABVIEW data acquisition unit. The temperature
of the vessel contents is monitored using a Pico PT100 temperature probe inserted through an
analysis block. The analysis block runs all the way up the back of the vessel allowing probes to
be inserted through 3/4 inch BSP tappings. Through another of these ports the inlet tube for the
salt injections into the agitator region was inserted. The vessel is also fitted with 8 rings of 16
equally spaced EIT electrodes in a baffle cage configuration which are connected to a ITS P2000
tomography measurement system. Figure 2 shows a schematic of this vessel.
The agitator used is depicted in Figure 3 (a): this is a 0.305 m diameter Cowles disk with 32
angled teeth (16 up and 16 down) which was rotated clockwise (angled edge first).
The 0.152 m vessel is a geometrically scaled down version of the 0.914 m vessel, without the
square jacket. The two agitators used in this vessel are depicted in Figure 3 (b) and Figure 3 (c):
these are a 0.0956 m diameter Torrance TF/150 saw-tooth disk with 24 angled teeth (12 up and 12
9

Thomas L. Rodgers et al.

Cowles Disk Dissolution

Figure 2: Schematic of the 0.914 m vessel.

down) and a 0.051 m diameter Esco-Labor V4A high shear disk with 12 angled teeth (6 up and 6
down), both were rotated clockwise (angled edge first). These agitators are the closest to Cowles
disks that were available to us at the necessary scale.

(a)

(b)

(c)

Figure 3: Agitators used: (a) 0.305 m Cowles disk (b) 0.0956 m Torrance TF/150 saw-tooth
agitator (c) 0.051 m Esco-Labor V4A high shear disk.

Methods
Experiments were carried out on the 0.914 m tank using both 70 w/w% sodium lauryl sulphate
(SLES) in water (TEXAPON N701 supplied by Unilever, density of 1050 kg m3 ) and a brine
10

Thomas L. Rodgers et al.

Cowles Disk Dissolution

solution (100 g table salt dissolved per liter of tap water). The brine solution was added to the
vessel in 100 ml aliquots either on the surface, using a funnel placed less than 1 cm from the
surface in a fixed position 2/3 of the radius from the agitator shaft and between two baffles; or
injected into the outlet flow of the agitator, using a pump. The energy input of both additions was
small compared to that given by the agitator. The SLES was added to produce a final solution of
0.5 w/w% (5.73 kg for H/T = 1.42 (800 l) and 3.93 kg for H/T = 1 (550 l)) to the surface of the
vessel in large lumps (approximately 0.1 m diameter) in under 30 seconds.
Experiments were carried out on the 0.152 m tank using 70 w/w% SLES in water and the brine
solution. The brine solution was added to the vessel in 2 ml aliquots on the surface, using a small
syringe at less than 1 cm from the surface in a fixed position 2/3 of the radius from the agitator
shaft and between two baffles. The SLES was added to produce a final solution of 0.5 w/w% (2.6 g
for H/T = 1.42 (3.7 l) and 1.8 g for H/T = 1 (2.5 l)) to the surface of the vessel either by a syringe
(mouth radius of 1.5 mm) or in a single lump. The SLES was also added in twice the volume for
the double SLES runs. The energy input of the additions was small compared to that given by the
agitator. The experiments were repeated 5 times to produce an average value.
Electrical impedance tomography (EIT) is commonly used to monitor processes which require
good temporal and spacial resolution. It has been used to measure mixing times in industrial single phase and multi-phase systems. 16 The ITS P2000 was chosen for the experiments as it is the
best performing EIT instrument for experiments requiring high temporal resolution and the ability of successfully monitoring homogeneity. 17 Table 2 summarises the data acquisition settings
employed during the experiments. The signal-to-noise ratio (SNR) was checked to ensure that no
voltage measurements were saturating the analogue to digital converter. If this occurs the recorded
voltages read a constant value for the given reading thus making the image reconstruction unreliable for calculating the conductivities inside the vessel. Therefore a SNR over 100 dB should
be avoided. The optimum injection current was found to be 50 mA resulting in a SNR ratio of
approximately 52 dB for water at the start of the experiment.
The turbulent power number was calculated on the 0.914 m vessel using the calibrated dual

11

Thomas L. Rodgers et al.

Cowles Disk Dissolution

Table 2: ITS P2000 data acquisition settings.

Setting
Excitation frequency
Sampling time interval
Samples per frame
Frames per download
Delay cycles
Injection current
Sampling strategy

Value
9.6 kHz
40 ms
1
Equal to the maximum number of frames
3
50 mA
Normal adjacent

strain gauge system mentioned above for the Cowles disk agitator. The power number of the
Torrance agitator was calculated over a range of Reynolds numbers using the same strain gauge
system on a smaller vessel. The low Reynolds number values were produced using different viscosity glucose (Cerestar 01632) syrup solutions (the viscosity was varied by temperature change).
This method was also repeated using the Torrance agitator on the shear thinning 2 w/w% Carbopol
940 solution (BF Goodrich). This allowed calculation of the Metzner-Otto constant as outlined
later.
The viscosity of the solutions were measured using a Haake RV 20 viscometer with a MV2 cup
and bob modality. The shear profile is set so that there is an increase from 0.1 to 450 s1 in steps,
and then decreases back down to 0.1 s1 . Each decade of shear rate has 5 even steps each for 2
minutes, with the 100 to 450 s1 having 3 even steps again each for 2 minutes. The temperature is
controlled using a water circulation jacket.
As both the solutions were power-law fluids, and in fact shear thinning, they can be fitted to
the standard power-law viscosity relationship, equation 14. This gave the values given by Table 3.
As a sense of the magnitude of the viscosities of the solutions, at a shear rate of 1 s1 the viscosity
of the 70 w/w% SLES is 34.1 Pa s and that of the 2 w/w% Carbopol is 180 Pa s.

= kn1

12

(14)

Thomas L. Rodgers et al.

Cowles Disk Dissolution

Table 3: Properties of the non-Newtonian fluids at 25 C.

Solution
70 w/w% SLES
2 w/w% Carbopol

n
k/ (Pa s)n
0.412
34.1
0.134
180

Data Processing
The voltage measurements collected by the ITS P2000 were reconstructed into a true-3D image
using the generalised singular value decomposition (GSVD) method 18 based on a finite element
model comprising 7344 elements. This approach decomposes the image into individual spatial
frequency components and affords the ability to control the number of generalised singular values
incorporated into the solution. The inclusion of a low number of singular values in the solution
yields an image with lower spatial resolution but which is robust to measurement noise. Conversely, the inclusion of a high number of singular values yields an image with potentially higher
spatial resolution which is less robust to measurement noise. The regularisation parameter in the
algorithm was selected frame by frame using the Discrete Picard Condition 19 to produce the results with the most information. The Discrete Picard Condition compares the generalised singular
values (representing the change in the data) with the Picard coefficients (representing the noise
in the data), and gives the value where they are equal. Values of the generalised singular values
greater than the Picard coefficients contain recoverable data and should be utilised, which occurs
if the regularisation parameter is set to this equality.
The values of the conductivity for the 7344 finite elements were combined together using the
root mean squared conductivity to produce an analysis of the mixing time, equation 15.
"

2 #
t,i 0,i
1 N
1
ln [RMS ] = ln
inf,i 0,i 1
2
N i=1

(15)

In equation 15, RMS is the root mean squared conductivity, N is the number of elements, t,i is
the conductivity of element i at the given time step, 0,i is the initial mean conductivity for element
i and inf,i is the final mean conductivity for element i. This approach gives a good calculation of

13

Thomas L. Rodgers et al.

Cowles Disk Dissolution

the mixing time as it weights the answer towards the elements that take the longest to mix.
The vessel can be considered 90 % mixed if the value of RMS drops below 2.3, which is
i
h
equivalent to (1/2) ln (0.9 1)2 . The 90 % mixing time is then the time at which the value never
becomes greater than 2.3 again. The 90 % mixing time is used as there is about 8 % noise on the
final mean conductivity.
As the whole vessel is in the turbulent regime then this time can be scaled to a 95 % mixing
time for comparison with literature correlations by use of equation 16.

95 = 90

ln [1 0.95]
ln [1 0.9]

(16)

Results and Analysis

Power Numbers and Metzner-Otto Constants
The power of an agitator can be calculated from the definition of the power number or from the
torque. Rearranging these definitions for the torque gives equation 17. In the turbulent regime,
the power number is a constant which means that the torque is proportional to the agitation speed
squared, as shown in Figure 4.
=

Pob D5 2
N
2

(17)

From this method it can be determined that the Power number for the Cowles disk agitator in
the turbulent regime is 0.52 and that of the Torrance agitator is 0.21.
Figure 5 presents the values the power number for the Cowles disk and Torrance agitators over
a range of the Reynolds number. It can be seen that in the laminar regime both agitators have
a constant value of PoRe, which in this case is equal to 65 for the Cowles disk and 55.7 for the
Torrance agitator.
As the addition material is shear-thinning, it is important to know the shear rate so that the

14

Thomas L. Rodgers et al.

Cowles Disk Dissolution

= 0.219N
2
R = 0.999

/Nm

5
4
3

2
1
0
0

10

20

15
2

30

25

-2

N /s

Figure 4: Plot of the torque, , against the agitation speed squared, N 2 , for a Cowles disk agitator
in water. The slope of the line is proportional to the power number, Po.

Torrance Newtonian
Torrance non-Newtonian
Cowles Newtonian
Cowles non-Newtonian

PoRe = 55.7
PoRe = 65

Po

100

Po = 0.52
Po = 0.21

PoRepl = 5.8
PoRepl = 10
0.01
10

10

10

10

Re or Repl
Figure 5: Plot of the Power number against the agitator Reynolds number for the Cowles disk and
Torrance agitators (Figure 3 (a), (b)). Laminar Newtonian and non-Newtonian data for the Cowles
disk are taken from Foucault et al. (2005). 20

15

Thomas L. Rodgers et al.

Cowles Disk Dissolution

apparent viscosity can be calculated. The average shear rate in the agitator region can be given by
the Metzner-Otto constant, Ks , multiplied by the agitation speed, 21 equation 18.

= Ks N

(18)

In the case of a power-law fluid a power-law Reynolds number, Repl , can be defined as equation 19. 22 The Power number for the Cowles disk and Torrance agitators in shear thinning fluids
over a range of power-law Reynolds numbers are shown in Figure 5.

Repl =

N n2 D2
k

(19)

In the laminar regime both agitators also have a constant value of PoRepl , which in this case is
equal to 10 for the Cowles disk and 5.8 for the Torrance agitator. As the true Reynolds number of
the agitators in the laminar regime is given by equation 20, rather than equation 19, then a simple
comparison of the laminar power constants for the non-Newtonian and the Newtonian fluids yields
the Metzner-Otto constant, as in equation 21.

Re =

Ks =

N n2 D2
kKsn1
PoRepl
PoRe

(20)

1
n1

(21)

Using the viscosity parameters for the Carbopol (Table 3) and knowing that the shear thinning
fluid used for the Cowles disk non-Newtonian power measurements by Foucault et al. (2005) 20
was 1.5 w/w% carboxymethyl cellulose solution with k = 60 (Pa s)0.22 and n = 0.22 then the
Metzner-Otto constants can be calculated to be 11 for the Cowles disk and 13.7 for the Torrence
agitator.

16

Thomas L. Rodgers et al.

Cowles Disk Dissolution

Same Viscosity Liquid-Liquid Blending Times

This section describes the blending of a brine tracer over a series of different agitation speeds in the
0.914 and 0.152 m vessels. Figure 6 shows an example of the reconstructed tomograms for a brine
tracer added to the 0.914 m vessel at an agitation rate of 100 rpm. For these three-dimensional
images, the colour scales are constant across all images, the minimum value used is the starting
conductivity of the tap water (0.01 S m1 ) and the maximum value used is the maximum of the
global mean conductivity trajectory (0.0112 S m1 for the 100 rpm run). Four isosurfaces have
been selected, at one-quarter intervals across the conductivity range starting at the first quartile
ending at the maximum of the colour scale, i.e. 25 %, 50 %, 75 % and 100 % of the range. The
opacity of the isosurfaces has been graded such that the lower conductivity isosurfaces are more
transparent than those of higher conductivity, allowing a clear visualisation.
Figure 6 (a) shows the initial homogeneity of the vessel at its initial conductivity of 0.01 S m1
and (b) shows the start of the feed of the higher conductivity brine feed (11.5 S m1 ). Figure 6 (c)
is 4 seconds into the mixing and it can be seen that the high conductivity tracer has moved down
the vessel and out towards the wall due to the flow of the agitator. As the tracer hits the wall it
starts to move up and down the vessel walls forming a highly conducting area at the front of the
vessel, Figure 6 (d).
By 16 seconds into the mixing, Figure 6 (e), the highly conducting area is still at the front the
vessel but starting to tangentially swirl in the direction of the agitator. This shows that the Cowles
disk gives only a small amount of tangential flow, with the main flow from the disk being limited
to the radial direction. After 32 seconds of mixing, Figure 6 (f), the most unmixed areas of the
vessel are towards the back, away from the initial feed position. This is still the case after 60
seconds, Figure 6 (g), but by this time there is only a small area behind the back baffle that has a
significantly different concentration of tracer.
Figure 6 (h) shows the final homogeneous end point of the mixing, showing a conductivity
of about 0.0102 S m1 , it can be seen that the end point is quite homogeneous, with only small
amounts of variation.
17

Thomas L. Rodgers et al.

(b) Feed

(c) 4 s

(d) 8 s

(e) 16 s

(f) 32 s

(g) 60 s

(h) 100 s

18

(a) Before

Cowles Disk Dissolution

Figure 6: Tomography images for a surface feed salt tracer in the 0.914 m vessel at 100 rpm with 95 = 84 s (see Figure 7; (a) before
the feed, (b) initial feed point, (c) 4 s into the mixing, (d) 8 s into the mixing, (e) 16 s into the mixing, (f) 32 s into the mixing, (g) 60 s
into mixing, (h) homogeneous end point (100 s).

Thomas L. Rodgers et al.

Cowles Disk Dissolution

Figure 7 shows the evolution of ln [RMS ] over the mixing times for an example of surface
brine blending in the 0.914 m vessel. The pre addition value can be seen to around 0 with small
variation, this corresponds to the inital conductivity of 0.01 S m1 . When the trace is less than
2.3 this corresponds to the final conductivity of about 0.0102 S m1 . It is clear from Figure 7
that the mixing seems to occur in two stages, the first as a decay in the average conductivity, and
the second as secondary loop which reinforces the areas of high conductivity from the first decay.
It can also be clearly seen that the lower agitation speed takes much longer to mix and that the
average conductivity stays above the final value for much longer. Using Figure 7 the mixing time

2
100 rpm
200 rpm
328 rpm
90% mixed

ln(RMS)

-2

-4

-6

-8
0

10

20

30

40

50

60

70

80

time (t) / s
Figure 7: Example traces for the surface brine mixing in the 0.914 m vessel. The arrows show the
time at which the vessel can be considered to be 90 % mixed, the vertical line shows the time of
addition.
can be calculated. The arrows show the time at which the system can be considered mixed and
the vertical line shows the time of addition, this means the mixing time is the difference. Figure 8
shows the mixing times for the brine tracers in the 0.914 and 0.152 m vessels for H/T = 1 and
1.42 and with both a surface and agitator feed for the 0.914 m vessel.
It can be seen from Figure 8 that there is little difference between the mixing time constant
19

Thomas L. Rodgers et al.

Cowles Disk Dissolution

15

0.914m H=1.42T (surface feed)

0.914m H=1.42T (agitator feed)
0.914m H=T
0.152m H=1.42T
0.152m H=T

Nt95Po (D/T) (H/T)

-1/2

20

1/3

10

0 4
10

10

10

Re
Figure 8: Mixing time for brine tracers in the 0.914 m and 0.152 m vessels. The error bars show
the standard deviation of the results, and the horizontal line shows the mixing time constant in the
mixing correlation of Grenville and Nienow (2004) 3 (5.2).
between the two heights in the 0.152 m vessel. Also the mixing time constant is very similar
to the value predicted by Grenville and Nienow(2004). 3 However, the mixing time constant for
the 0.914 m vessel does not seem to be the same for the two liquid heights. For H/T = 1 the
mixing time constant is similar to the value predicted by Grenville and Nienow (2004), 3 though
slightly higher. This is possibly due to the turbulent eddies scaling with agitator size, thus taking
longer for the energy to dissipate into small eddies for the micro mixing with a larger agitator. 23
For H/T = 1.42 the mixing time constant is almost twice that of H/T = 1. This could be due
to poor circulation in the large vessel from the Cowles disk, whereas this is not such a problem
in the smaller vessel. It can also be seen that surface feed takes slightly longer than the agitator
feed. This shows that the flow from the Cowles disk is weakest towards the surface of the vessel,
delaying the homogenation of the fluid in the vessel.

20

Thomas L. Rodgers et al.

Cowles Disk Dissolution

SLES Dissolution
This section describes the dissolution of SLES in the 0.914 and 0.152 m vessels and compares this
with the brine mixing times for different methods of addition at different liquid heights. Figure 9
shows the results for the dissolution times for the SLES addition with a syringe at H/T = 1 and
1.42 and with agitators of D/T = 1/3 and 0.62 in the 0.152 m vessel. It also shows the times for
the addition of SLES in one lump for agitators of D/T = 1/3 and 0.62 in the 0.152 m vessel and
the addition of SLES in lumps for agitator of D/T = 1/3.
4

10

Nt95Po (D/T) (H/T)

-1/2

10

1/3

10

0.914m SLES D/T=1/3

0.152m SLES lump D/T=0.62
0.152m SLES lump D/T=1/3
0.152m SLES syringe D/T=0.62
0.152m SLES syringe D/T=1/3
0.914m brine H=1.42T
0.914m brine H=T
0.152m brine

10

10 2
10

10

10

10

10

Re
Figure 9: Comparison of mixing and dissolution times for salt tracers and SLES in both the 0.914
and 0.152 m vessels. For the 0.152 m brine and the SLES additions, both the liquid heights are
shown together as there is no discernible difference in the results. The black lines act as a guide to
the eye.
It can be seen from Figure 9 that when the SLES is added by syringe changing the liquid
height or the agitator speed does not affect the mixing time constant appreciably. However, the
agitator size does seem to affect the mixing time constant in a way that would not be expected for a

21

Thomas L. Rodgers et al.

Cowles Disk Dissolution

mixing mechanism dominated process, i.e the larger agitator seems to mix slower than the smaller
agitator. This demonstrates that when the SLES is in small pieces, as introduced by the syringe,
the dissolution of these pieces controls the mixing process as the mixing time constant is around
10 times higher than the brine mixing in the same vessel.
If the SLES is added as one lump then the mixing time constant is no longer constant with
agitation speed and seems to be affected by the agitator size, which suggests that it is not a mixing
mechanism. Also the smaller agitator gives a faster dissolution time, especially at lower agitation
rates, which would not be expected for a mixing process. This suggests that the dissolution is the
dominant effect and that increasing the agitation rate helps to increase this. At the higher agitation
rates the larger agitator produces mixing times which are almost as quick as the syringe addition
times.
Figure 9 also shows the dissolution time constant for the SLES addition into the 0.914 m vessel.
It can be seen that the dissolution time constant is greatly affected by the agitation rate, decreasing
by an order of magnitude when the agitation rate is increased by a factor of 3. We suggest that
the large lumps of SLES added are difficult to break up with the low shear rates of the slower
agitation speeds. Also the lower agitation rates have problems suspending the larger lumps of
SLES meaning that some sit on the base of the vessel diminishing the dissolution rates even more.
For dissolution of the SLES the change in liquid height does not affect the dissolution time as
the blending time is at least an order of magnitude less than the dissolution time, therefore the bulk
can almost be taken as perfectly mixed from the view point of the SLES.

Effect of the Modified Reynolds Number

One of the main issues with SLES, and other surfactants, is that the viscosity of the material varies
with the shear rate that it experiences. This means that an average value of the SLES viscosity can
be calculated for each agitation speed inside of the vessels if the shear rate is known within the
vessel. However, calculation of the shear rate in an agitated vessel is not a clear concept, especially
as it varies throughout the vessel.
22

Thomas L. Rodgers et al.

Cowles Disk Dissolution

In the turbulent regime, the turbulent stress can be calculated throughout the vessel which
could be used with a rheological equation to calculate the local viscosity of the material throughout
the vessel. This would provide a very complicated view of the process and would be difficult to
correlate as what average viscosity do you take. However, from observation of the breakup process,
the main breakup of the SLES occurs in the agitator region and little occurs elsewhere in the vessel.
This leads to the thought of using a local viscosity in the agitator region as this is where the main
processes happens. Figure 10(a) shows the 70 w/w% SLES approaching the agitator but with no
real break up, whereas Figure 10(b) shows the SLES right in the agitator region, with small pieces
being sheared from it. This is typical of the whole process and reveals that this is not an emulsion.

(a) Before contact

(b) At contact

Figure 10: Images of SLES in the agitator region. (a) SLES approaching the agitator, (b) Small
pieces of SLES being sheared from the main lump in the agitator region (within circle).

A convenient and commonly used method for determining the average viscosity in this agitator
region is by means of the Metzner-Otto equation, equation 18, and a rheological equation, equation 14. The Metzner-Otto constants are determined from measurements in the laminar regime and
are only strictly applicable in this regime. However, this approach is valid as the substance which
the Metzner-Otto constant is used on (SLES) gives a laminar Reynolds number and both the power
and mixing are independent of viscosity in the fully turbulent regime (i.e. the bulk water).
The modified Reynolds number (Re ) is calculated from equation 8 using this viscosity. This
now allows the dissolution times to be plotted against the modified Reynolds number as shown by
Figure 11. From Figure 11 it can be seen that the trends do not change from Figure 9. The slope
23

Thomas L. Rodgers et al.

Cowles Disk Dissolution

0.914m SLES D/T=1/3

0.152m SLES lump D/T=0.62
0.152m SLES lump D/T=1/3
0.152m SLES syringe D/T=0.62
0.152m SLES syringe D/T=1/3
0.914m brine H=1.42T
0.914m brine H=T
0.152m brine

10

Nt95Po (D/T) (H/T)

-1/2

10

1/3

10

10

10 0
10

10

10

Re

10

Figure 11: Comparison of mixing and dissolution times for salt tracers and SLES in both the 6 inch
and 3 ft vessels against the modified Reynolds number, shown with best fit lines. For the 0.152 m
brine and the SLES additions, both the liquid heights are shown together as there is no discernible
difference in the results.

24

Thomas L. Rodgers et al.

Cowles Disk Dissolution

of the curve in Figure 11 seem to scale well the agitator size. The equations of the SLES added
as lumps to a concentration of 0.5 w/w% all fit to the general equation 22 with values given in
Table 4.

 2   1 #
2
H
D
Nt95 Po
= A0 ReA1
T
T

"

1
3

(22)

A1 represents the slope of the curve in Figure 11 and its dependence with the diameter of the
Table 4: Constants for equation 22.
D/m
A0
0.0508
820.30
0.0956
5212.22
0.3048 2.99 1011

A1
-0.58
-0.97
-4.43

agitator is given by equation 23. A0 varies exponentially with the agitator diameter, as described
by equation 24. The fact that these two equations are dependant on the agitator diameter and not
the ratio of agitator to tank diameter shows the dependency of scale on this operation.

A1 = 0.35 15.57D

(23)

A0 = 6.4185e80.04D

(24)

Being able to predict the values of A0 and A1 allows the dissolution time constant to be predicted.

Effect of Tracer Volume

Figure 12 shows that the mixing time is different when the volume of SLES added is larger. When
added from the syringe the mixing time constant is independent of Re, but higher than that of
the 0.5 w/w% solution. Also if the SLES is added as a single lump, the mixing time constant
is similar between the 1 and 0.5 w/w% solutions for high agitation speeds, but diverges as the
agitation speed decreases. This could be an indication that the SLES is dissolving; because the
concentration difference is less between the 1 w/w% solution and the added SLES giving a lower
mass transfer rate, which is exacerbated if the SLES is added in a lump at a low agitation speed.
25

Thomas L. Rodgers et al.

Cowles Disk Dissolution

10

Nt95Po (D/T) (H/T)

-1/2

double lump
single lump
double syringe
single syringe

1/3

10

10

10

10

Re

10

Figure 12: Comparison of dissolution times for SLES additions of different volumes in the 0.152 m
vessel against the modified Reynolds number, shown with best fit lines (D/T = 1/3).

26

Thomas L. Rodgers et al.

Cowles Disk Dissolution

Also, there is more SLES to dissolve.

The use of the modified Reynolds number does not take into account the volume of the tracer,
which can be seen from the different trends in Figure 12. The modified Richardson number however does involve a volume term, and in fact a liquid height term as well. This means it might
be an important parameter in trying to predict the dissolution for a change in the tracer volume.
Figure 13 shows the variation of the modified Fourier number in the 0.152 m vessel for both liquid
heights and both added tracer amounts. The modified Fourier number represents a dimensionless
form of the mixing time and is given by equation 25.

a b
Fo = Fo
b a

a 95
a T 2

(25)

It can be seen from Figure 13 that the use of the Richardson number seems to collapse the lump

1000

Fo

100

single lump D/T=1/3

double lump D/T=1/3
single lump D/T=0.62
single syringe D/T=1/3
double syringe D/T=1/3
single syringe D/T=0.62
double syringe D/T=0.62

10

0.1
1e-05

0.0001

0.001

Ri

0.01

0.1

Figure 13: Comparison of dissolution times for SLES additions of different volumes in the 0.152 m
vessel against the modified Richardson number.
addition and the syringe addition into two separate trends independent of tracer volume, agitator
27

Thomas L. Rodgers et al.

Cowles Disk Dissolution

size and liquid height. This shows that a volume term is needed in the correlation, and the modified
Richardson number could be this term. The two lines could be collapsed on to each other by looked
at the surface area to volume ratio, like in equation 26. For low agitation speeds the value of
seems to need to be about 1, where as at high agitation speeds the value of needs to be much less
than 1. This fits with the idea that the higher shear rates of higher agitation speeds split the lumps
up more creating less effect of the lump size.
Fo

 s 
V

Ria

(26)

Discussion and Conclusions

Experiments have been undertaken in 0.914 and 0.152 m diameter vessels to look at the mixing
and dissolution times of brine and high viscosity material. Mixing times in the turbulent regime
for materials of similar viscosities can already be predicted for many different agitators, and this
work shows that the correlation can also be used for high shear disk agitators, however, with some
caution for larger vessels. Materials with large viscosity differences however take much longer
to mix which needs to be understood to help development of processes. The time taken for high
viscosity fluids to mix seems to be dependent on the operating conditions and the scale of operation.
Previous work with similar viscosity liquids has shown that for agitators of different D/T
increasing this value decreases the mixing time, however this work shows that for high viscosity
differences this is not the case with smaller values of D/T giving smaller dissolution times. It has
also been shown for 0.5 w/w% SLES that the dissolution time scales with the modified Reynolds
number according to equation 27.
Nt95 Re(0.3515.57D)

28

(27)

Thomas L. Rodgers et al.

Cowles Disk Dissolution

It has also been shown that the volume of the tracer has an effect on the dissolution time of SLES,
with it having a greater effect at low agitation speeds for one lump. This helps to show that the
main effect is a dissolution effect and not a mixing effect. It has also been shown that the modified
Richardson number can take the dissolution times of the SLES of different volumes and collapse
these to one trend, producing equation 28, where the value of varies with agitation speed.
Fo

 s 
V

Ria

(28)

Nomenclature
D Agitator diameter

d p Particle diameter

m
= 9.81 m s2

g Acceleration due to gravity

H Liquid height

m
(Pa s)n

n Consistency index
Ks Metzner-Otto constant

s1

N Agitation speed
N Number of readings

n Power-law index

NCD Critical dispersion agitation speed

s1

NJS Just suspended agitation speed

s1

P Power

W
m3 s1

Q Flow

m2

s Surface area
T Vessel diameter

t Time

s
m3

V Volume

29

Thomas L. Rodgers et al.

Cowles Disk Dissolution

X p Percent weight solids per weight of liquid

Ratio of dished base height to tank diameter

Torque

Nm

Shear rate

s1

Viscosity

Pa s

Volume fraction of dispersed phase

Density

kg m3

Conductivity

S m1

Surface tension

N m1

RMS Root mean squared conductivity

S m1

95 95 % mixing time

Fo Modified Fourier number , see equation (25)

= b 95 /b T 2

Fo Fourier number

= Q/ND3

NQ Flow number

= P/ N 3 D5

Po Agitator power number

Re Modified agitator Reynolds number , see equation (8)

= N n2 D2 /k

Repl Power-law Reynolds number

= ND2 /

Re Agitator Reynolds number

Ri Modified Richardson number , see equation (9)

= (a b ) gH/b N 2 D2

Ri Richardson number
SNR Signal to noise ratio

dB

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Cowles Disk Dissolution

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Acknowledgement
Tom Rodgers would like to thank The University of Manchesters EPSRC CTA (Collaborative
Training Account) and Unilever for financial support during his PhD. The authors would like to
thank the SCEAS workshop staff who helped with equipment modifications and construction.

33