Chinese Journal of Chemical Engineering 23 (2015) 1065–1076

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Chinese Journal of Chemical Engineering

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Review

Mixing time in stirred vessels: A review of experimental techniques☆

Gabriel Ascanio ⁎
Center of Applied Sciences and Technological Development, National Autonomous University of Mexico, Circuito Exterior, Ciudad Universitaria, DF 04510 Mexico

a r t i c l e i n f o a b s t r a c t

Article history: Mixing time is defined as the time required for achieving a certain degree of homogeneity of injected tracer in a
Received 13 December 2013 unit operation vessel. It has been used as a key parameter for assessing the performance of a mixing system. From
Received in revised form 2 July 2014 an experimental standpoint, several techniques have been developed for measuring the mixing time. Based on
Accepted 28 October 2014
the disturbances to flow, they can be classified into two groups: non-intrusive and intrusive. However, depending
Available online 3 April 2015
on the type of data generated, they can be also classified into direct measurements and indirect measurements
Keywords:
(Eulerian and Lagrangian). Since the techniques available for measuring mixing times in an agitated tank do
Mixing time not provide the same information, its choice depends on several factors, namely: accuracy, reproducibility,
Stirred vessel suitability, cost, sampling speed, type of data, and processing time. A review of the experimental techniques
Homogeneity reported in the literature in the last 50 years for the measurement of mixing time in stirred vessels under single
and gas–liquid flow conditions with Newtonian and non-Newtonian fluids in the laminar and turbulent regime is
made, and a comparison between these techniques is also presented.
© 2015 The Chemical Industry and Engineering Society of China, and Chemical Industry Press. All rights reserved.

1. Introduction one. Moo-Young et al. [4], the mixing time can be correlated in a di-
mensionless manner as
Mixing time is a key parameter used for analyzing the performance
and the hydrodynamics of a stirred vessel. In general terms, the mixing β
Nθm ¼ α ðReÞ ð2Þ
time is defined as the time required for achieving a certain degree of ho-
mogeneity of tracer inserted in a stirred vessel [1]. From a macromixing
standpoint, the bulk mixing time is the time required to get all points in where α and β are the adjustable parameters and Re is the Reynolds
the vessel uniformly distributed, while the local mixing time is the mea- number,
sure of how fast a material is distributed in a particular region of the
vessel, which depends on the local turbulence.
Therefore, local measurements are time and space dependent, while ρ N D2
Re ¼ ð3Þ
bulk mixing time is based on time dependent measurements (temporal μ
measurements) [2]. Mixing time can be expressed in its nondimension-
al form:
where ρ is the fluid density in kg·m-3, D is the impeller diameter in m
and μ is the fluid dynamic viscosity in Pa·s.
N θm ¼ K ð1Þ
In the case of non-Newtonian fluids, such a number is defined by
where θm is the mixing time in s, N is the impeller speed in revolu-
tions per second and K is a constant which depends on the size, ρ N2−n D2
Re ¼ ð4Þ
geometry of the tank and the flow regime [3]. Constancy of K is k
valid in the laminar and turbulent regimes but not in the transitional

☆ Supported by DGAPA-UNAM through the grant IN-108312.
⁎ Centro de Ciencias Aplicadas y Desarrollo Tecnológico, Universidad Nacional Autónoma
de México, Circuito Exterior, Ciudad Universitaria, DF 04510, Mexico.
E-mail address: gabriel.ascanio@ccadet.unam.mx.
where k and n are the consistency index and the flow behavior index,
respectively, for fluids obeying the Ostwald-de Waele model (power-

law model), in which the rate of deformation has been taken as γ ¼ N.
However, the Reynolds number for non-Newtonian can also be defined
in terms of the effective viscosity, which is a function of the shear rate.
Nowadays, the most used definition of the shear rate in stirred vessels

http://dx.doi.org/10.1016/j.cjche.2014.10.022
1004-9541/© 2015 The Chemical Industry and Engineering Society of China, and Chemical Industry Press. All rights reserved.
1066 G. Ascanio / Chinese Journal of Chemical Engineering 23 (2015) 1065–1076
is the one developed by Metzner and Otto [5], which is calculated from
the power-law model:
μ 1=½n−1
 reviewed by highlighting their advantages and drawbacks along with
γ¼ ¼ ks N
k the most outstanding findings. This review covers single phase and
where the shear rate is proportional to the impeller rotational speed,
being ks the proportionality constant. Based on this approach, the
Reynolds number is defined as
ρ N D2 ρ Nð2−nÞ D2
Re ¼ ¼ :
μ k ks ðn−1Þ
A number of mixing time correlations have been reported in the
literature taking into account the effect of baffles on mixing time
[6–8], as well as the relationship between circulation and mixing
times [9]. In the turbulent regime, the dimensionless mixing time is
independent on the Reynolds number and it can be correlated by empir-
ical expressions involving the size and geometry of the tank as well as
some hydrodynamic parameters [10,11]. Experimental techniques for
measuring mixing time can be classified depending basically on two
different scenarios, namely: (1) level of disturbance to flow and (2)
type of data collected. Based on the first scenario, the techniques are
classified as non-intrusive and intrusive. With respect to the intrusive
techniques, they are based on local and global measurements. Although
they are accurate, its use is limited because the flow pattern is modified
by the presence of probes in the vessel. Mavros [12] reviewed the exper-
imental techniques available for the study of flow patterns in stirred
vessels. Although the aim of his paper was to give a general overview
of intrusive and non-intrusive techniques for the flow visualization in
tanks, some of them can be also applied also for estimating mixing
times.
On the other hand, considering the type of data collected, these tech-
niques are classified as direct measurements or indirect measurements
(Eulerian data or Lagrangian data). In the case of indirect measure-
ments, mixing time is to be inferred from physical measurements of
conductivity or velocity for instance, while direct techniques provide
real time results or at least requiring minimum processing. Table 1 sum-
marizes the classification of experimental techniques as a function of
both scenarios.
Table 1
Classification of measurement techniques of mixing times in stirred vessels
Flow disturbance
Non-intrusive Intrusive
• Colorimetry • Conductometry and pH (probes)
• Electrical resistance tomography
• Positron emission particle tracking
• Planar laser induced fluorescence
• Thermography
Type of data provided
Direct measurement Indirect measurement
Eulerian Lagrangian
• Colorimetry • Thermography • Electrical resistance
• Planar laser induced fluorescence tomography
• Conductometry and pH (probes)
Nere et al. [8] performed a critical review of the literature dealing
with liquid-phase mixing in stirred vessels in the turbulent regime.
Although, the limitations of the techniques employed for measuring
mixing times were described therein, they focused on the effects of
different parameters such as impeller geometry, impeller position on
liquid-phase mixing as well as the mathematical models developed
for analyzing the hydrodynamics in stirred vessels. In this paper, the
experimental techniques reported in the literature over last 50 years
for the measurement of mixing time in stirred vessels have been
ð5Þ
gas–liquid mixing of Newtonian and non-Newtonian fluids in the laminar
and turbulent regimes.
2. Experimental Techniques
2.1. Colorimetry
ð6Þ
From a practical standpoint, colorimetry is by far the most common
technique employed for measuring mixing times in stirred vessels
[13–15]. It is a non-intrusive technique extensively reported in the liter-
ature, which is used not only to determine the time required to achieve
the desired degree of homogenization, but also to visualize qualitatively
flow patterns and to reveal the presence of secondary flows generated
under steady stirring such as well-mixed regions (caverns), islands and
other segregated regions like stagnant of dead flow zones [16–20]. The
technique basically consists of injecting a liquid tracer and observing
how it is dispersed in the fluid contained in stirred vessels. A variant of
this technique is based on the color-decolorization approach by using a
pH sensitive tracer. The reader is referred to Ascanio et al. [18] for a
detailed description of the measuring protocol. Fig. 1 shows an example
of a typical mixing sequence by the colorimetric technique.
Norwood and Metzner [22] reported for the first time the use of an
acid–base neutralization reaction for measuring mixing time in baffled
stirred tanks equipped with turbines operating in the turbulent regime,
which has been extensively adopted in the research. Hari-Prajitno et al.
[23] used also this technique for measuring mixing time under aerated
and unaerated conditions for dual and triple coaxial impeller configura-
tions in the turbulent regime. The decolorization method has not only
been used for measuring mixing time, but also for getting the insight of
flow patterns generated by different impellers such as close-clearance im-
pellers, multiple and coaxial arrangements, inclined impeller, etc. [24–34].
Although colorimetry is a very simple technique to implement,
mixing time estimation depends strongly on the subjectivity of the
human observer. For that reason, complementary techniques based on
image processing have been developed [35–40]. Kouda et al. [35]
dissolved phenolphthalein as pH indicator in bacterial cellulose and
CMC solution, which became dark purple when NaOH being present.
Then, H2SO4 was added at time zero and the images were captured
every 0.5 s. Afterwards, the digital brightness of images was analyzed
by image processing, and the mixing time was determined in terms of
the decolorization ratio (output/reference).
Table 2 summarizes the operating principle, advantages and disad-
vantages of the estimation of mixing time by colorimetry.
2.2. Electrical resistance tomography
Electrical Resistance Tomography (ERT) is a non-intrusive and non-
invasive technique from which cross-sectional images showing the
distribution of electrical conductivity of gas–liquid flows in a stirred ves-
sel from Lagrangian measurements taken at the boundary of the vessel.
It can be used where the continuous phase is conductive and the other
phases have different values of conductivity. A typical ERT setup con-
sists basically of a set of electrodes, the data acquisition system and a
user interface [41]. The array of sensors are usually a series of rings in
which the electrodes are equally spaced around the vessel circumfer-
ence. Electrical measurements are made without affecting the flow in
the vessel. A typical measurement protocol consists of applying the
current to the next electrode pair and the resultant potential differences
on all other electrode pairs are measured. This step is repeated until all
electrode pair combinations have been used. A reconstruction technique
converts the raw peripheral potential difference measurements into a
 G. Ascanio / Chinese Journal of Chemical Engineering 23 (2015) 1065–1076 1067

Fig. 1. Typical mixing evolution in a stirred tank using colorimetry [21].

Table 2
Operating principle, advantages and disadvantages of colorimetry

Operating principle Advantages Disadvantages

Color change of a solution containing a pH
sensitive tracer
• Direct measurement • Mixing time measurement depends on the human eye subjectivity without
• Simple to implement image processing
• Non-intrusive technique • Temporal resolution with image processing techniques
• No calibration is required • Spatial resolution with high-resolution pictures
• Reveal flow structures • For transparent systems only
• Used under aerated and unaerated conditions • Limited applicability under highly aerated conditions in the turbulent regime
• Accurate when combined with image processing
techniques

two-dimensional electrical conductivity distribution of the measurement
area (tomogram). Such a technique is based mainly on three different
algorithms: linear back projection (LBP), a modified Newton–Raphson
method (MNR) and a parametric model based technique (PM). The
three algorithms use a single point calibration on a set of reference
voltages from a sensor filled with a solution having a known conductivity
[42].
Fig. 2 shows an example of a conductivity map showing the evolu-
tion of the mixing process in the stirred vessel. For that purpose a
color scale is used for showing the variations in conductivity. For this
example, blue regions indicate no mixing, green region partial mixing
and red zone full mixing.
Although, ERT is a relatively new technology developed to get
insight about the hydrodynamics inside stirred vessels, among other
applications, its usefulness in such applications has been already report-
ed [43–57] and validated with Computational Fluid Dynamics (CFD)
[58]. Wang et al. [48,59] reported the use of an ERT system for the
gas–liquid mixing in a stirred vessel for discriminating the differences
of three-dimensional gas hold up variations in the liquid phase viscosity.
Simultaneously, the fluid dynamics was also investigated by following
the spatiotemporal conductivity changes of a fluid tracer injected in
the working liquid. Fig. 3 shows the real time mixing curves of the liquid
for the air-water mixing, which have been plotted from stack of
tomograms obtained in the bottom plane and in the top plane of the
stirred vessel. Looking at both curves, it is observed that the brine tracer
is thoroughly mixed after 19 s and from this point the concentration in
the top and the bottom remains constant, which can be confirmed by
observing the corresponding tomograms.
Although most of the tomographic measurements have been done
using sensors placed outside the tank, Abdullah et al. [60] reported the
use of a series of conductivity electrodes place into the tank to study
the nature of gas–liquid–solid mixing in a gas-induced stirred tank
reactor. Edwards et al. [62] investigated the semibatch precipitation of
aluminum hydroxide by the addition of concentrated sodium hydroxide
(NaOH) to aluminum nitrate in a stirred vessel by using multimodal
tomographic techniques. For that purpose ERT was used to analyze
the mixing performance during precipitation, while positron emission
particle tracking (PEPT) was used to study the flow field in the vessel
as a function of the fill level, power input, etc. They found by PEPT that
mixing time measured with ERT depends on the ratio of the feeding
rate to the bulk velocity in the feed region. PEPT is a useful technique
for studying three-dimensional flow phenomena in opaque systems
[63]. The operating principle is based on a particle tracer labeled with
a radionuclide that decays via beta-plus decay generating two gamma
rays. A PEPT camera detects the two gamma rays and defines a line
along which the annihilation occurred. Fangary et al. [64] used the

Fig. 2. Conductivity maps in a stirred vessel [41].

1068 G. Ascanio / Chinese Journal of Chemical Engineering 23 (2015) 1065–1076
Fig. 3. Liquid phase mixing curves for air–water mixing and the tomograms of the liquid phase mixing of a brine tracer pulse.
Adapted from [48,59].
PEPT technique for determining the flow patterns in water and in
viscous non-Newtonian CMC solutions inside a vessel agitated by axial
flow impellers. Barigou et al. [65] validated the results obtained with
a PEPT system with PIV and LDA in a stirred vessel containing a transpar-
ent fluid. Subsequently, the approach was applied to opaque systems
containing low viscosity and high solid content suspensions obtaining
the spatial distribution of suspended particles of two sizes throughout
the vessel as well as flow fields for liquid and solid phases. Edwards
et al. [62] combined ERT with PEPT to study the hydrodynamics of a
stirred vessel of aluminum hydroxide. In that case the temporal and spa-
tial distribution of fed ionic species provided by ERT was complemented
by flow field information on the feed plume provided by PEPT.
A variant of radioactive tracking consists of injecting a small volume
of a radioactive liquid tracer and monitoring its concentration. This
technique offers some advantages over optical methods such as the
possibility of measuring over a wide temperature range (more than
300 °C) and working with nontransparent vessels [8].
The operating principle as well as the advantages and disadvantages
of ERT technique are summarized in Table 3.
2.3. Planar laser-induced fluorescence
Planar laser-induced fluorescence (pLIF) is a non-intrusive Eulerian
technique suitable for the instantaneous measurement of concentration
maps in liquid flows. Fig. 4 shows a pLIF setup, which consists basically
of the following parts:
• Light source: Typically a Nd:YAG laser (neodymium–doped yttrium
aluminum garnet) or an argon-ion laser. Although a Nd:YAG laser
emits light with a wavelength of 1064 nm, it is also operated in both
continuous or pulsed mode, in which a high-intensity pulse can be
generated at 532 nm or higher harmonics at 355 and 266 nm.
Table 3
Operating principle, advantages and disadvantages of Electrical Resistance Tomography (ERT)
Operating principle
Electrical measurements of conductivity producing cross-sectional images. An image
algorithm converts the raw peripheral potential differences measurements into a
tomogram (two-dimensional electrical conductivity distribution of the measurement
area).
• During the experiments the dye is excited by laser light whose frequen-
cy closely matches the excitation frequency of the dye. It absorbs the
laser light energy at short wavelength and re-emits light at a longer
wavelength that can be detected by a photodetector. The most common
dyes used in pLIF are fluorescein and rhodamine 6G.
• A charge-coupled device camera (CCD) with a narrow-band filter for
capturing fluorescent light only.
Since the dye fluorescence is strongly dependent on the concentra-
tion, the pLIF system must be firstly calibrated. If a dye is chosen for
concentration measurements (fluorescein or rhodamine 6G) the concen-
tration signal (S) is calibrated with the following [61]:
S ¼ f optic AC ðE V c Q λ ÞC ð7Þ
where C is the dye concentration, E is the laser light intensity, Q λ is the
quantum efficiency of the dye (at the laser excitation wavelength), foptic
corresponds to optical factors, V c is the sampling volume, and AC
represents the absorption phenomena integrated on the light path
(L) in the fluid characterized by the absorption index (ε), which is
calculated by
−ε LC
AC ¼ e : ð8Þ
For low concentration experiments, absorption phenomena are neg-
ligible, so that AC = 1, leading to linear relationship between the signal
(S) and (C, E, γ), being γ a constant that characterizes all experimental
parameters. In such conditions, the concentration is accurately mea-
sured as the amount of light received by the detector. Many commercial
LIF systems include a software capable of performing a quick calibration
of concentration, as well as signal corrections and other operations.
Advantage Disadvantage
• Non-intrusive, non-invasive • Expensive technique
• Series of 2-D tomograms at different heights can • Calibration must be made prior to
be used for producing 3-D flow fields. experiments
• Suitable under aerated and unaerated conditions • Time consuming assembly of
• Allows also observing isolated mixing regions setup
• Temporal and spatial resolution • Good skills for interpreting
• For transparent and non-transparent systems measurements
 G. Ascanio / Chinese Journal of Chemical Engineering 23 (2015) 1065–1076 1069

Fig. 4. Basic setup of pLIF.

Adapted from [61].

Once the system has been calibrated, the signals are processed by
converting the fluorescence images into concentration or temperature
fields. As the marked fluid flows through the light sheet, the dye is
excited and re-emits light, so that the dye concentration is
S with each other. For that purpose the fluorescence signal of the dye,
C≅ : ð9Þ
γE
This process is repeated for every interrogation zone in the whole
region during a period of time, in such a way that the dye concentration
can be correlated with time and the mixing time can be deducted. This
technique allows simultaneously analyzing flow structures in the tank
[19,66–72]. Distelhoff et al. [67] reported for the first time the use of
pLIF to determine mixing time in a baffled vessel containing water as
working fluid. In this case, the mixing time was defined as the time
required for the dye to be transported from the top of the vessel to the
bottom plus the time required for a further two rotations of the bulk
flow in the circumferential direction. The mixing time was based on
the 99% concentration because large variations were found when
using lower concentration criteria. Arratia and Muzzio [73] reported
the use of the pLIF technique to measure the dye concentration in a
laminar three-dimensional flow in a stirred vessel equipped with
three coaxial impellers. Fig. 5 shows an example of the concentration
fields observed after 90 s, in which the effect of the Reynolds number
on the mixing time is clearly observed. They stated that the tracer
variability decayed exponentially, so that the mixing time can be obtained
once the concentration in the vessel reaches a plateau with a minimum
variability.
Hu et al. [74] developed a technique to quantify the reactive process in
an unbaffled stirred tank using a novel reactive planar laser-induced fluo-
rescence, which consists of visualizing two liquids mixed and reacted
which varies due to the presence of a reacting material (H2O2), was
continuously recorded along the reaction process. Fig. 6 shows an exam-
ple of the concentration evolution, in which the red color corresponds to a
tracer concentration of 100 μg · L-1, while the blue color denotes 0 μg · L-1.
PLIF has been also used to characterize reactive and non-reactive
mixing processes in terms of time θ99 and times τ95 and τ99, respectively
[75]. They reported a time ratio κ99 = θ99/τ99 (99% mixing time to 99%
non-reactive mixing time) ranging from 0.42 to 0.58, which indicates
that reactive mixing is mainly controlled by the corresponding non-
reactive mixing. As in colorimetry, simple digital image processing has
been used with concentration maps obtained with pLIF for determining
mixing times [68,75–77].
The advantages and disadvantages as well as the operating principle
of the planar laser induced fluorescence are summarized in Table 4.
2.4. Thermography
Liquid crystal is an organic material in the amorphous solid form at a
certain temperature and pure liquid beyond the upper limit. Due to its
molecular structure it behaves as a crystal between these two phases.

Fig. 5. Concentration fields observed at 90 s: (a) Re = 40; (b) Re = 60. Concentration scale bar in μg · L-1. Reprinted with permission [73]. Copyright (2004) American Chemical Society.
1070 G. Ascanio / Chinese Journal of Chemical Engineering 23 (2015) 1065–1076

Fig. 6. Normalized concentration fields [74].

When an incident light is selectively scattered liquid crystals are the
basis for temperature measurements. Based on the thermography
principle, Lee et al. [78] and Lee and Yianneskis [79] developed a liquid
crystal thermographic technique for the measurement of mixing time
in a stirred vessel. For that purpose, thermochromic liquid crystals
encapsulated as gelatin-shell micro-spheres having a mean diameter
of 20 μm were injected at the top surface. Since the tracer and the work-
ing fluid had almost the same density the tracer remained suspended.
Fig. 7 shows the hue contours of one-half of the flow field in the vessel
stirred by 2-Rushton turbine array rotating at 540 r · min-1, 200 ms after
the tracer insertion. The tracer was injected at z/T = 1.2 at a higher tem-
perature than the working fluid, and the latter is hued by red color.
The operating principle, advantages and disadvantages of the
thermography technique are summarized in Table 5.
2.5. Conductometry and pH
Physical measurements of conductivity and pH are made using
probes placed at different points into the stirred vessel. Irrespective of
their size, the presence of such probes perturb the flow, so that the mea-
surement of mixing times should be considered as apparent, especially
when using very small vessels. The conductivity technique is based on
the measurement of the electrical conductivity of a solution over the
time [80]. For that purpose a conductivity probe is placed into the
stirred vessel at a specific position. Fig. 8(a) shows a typical setup of a
conductivity measurement system, which consists basically of a con-
ductivity probe and a conductivity meter connected to a personal com-
puter through a data acquisition card.
Basically, there are two types of conductivity probes or cells, namely:
2-electrode cells and 4-electrode cells. The first one is the most common
conductivity probe made of glass with two electrodes made of platinum.
However, this kind of probes is prone to polarization errors due to
the electro-chemical reactions. To overcome this drawback, the 4-
electrode probe is the best option. In such a design, alternating current
is applied to the outer pair of rings and the voltage is measured on the
inner rings avoiding polarization effects since there are no current
flows in the measuring circuit. A typical conductivity probe is composed
by anode and cathode, being the latter made from an inert metal. The
probe is placed into the solution and it is activated when voltage is
supplied. Then electron-carrying (negative) ions move towards the
anode while electron-less (positive) ions move towards the cathode. It
is important to point that conductivity solutions are sensitive to temper-
ature changes, therefore the system must be temperature compensated
or calibrated at the testing temperature.
The conductivity values are then converted into concentration data
versus time scale by using the calibration factor of the conductivity

Table 4
Operating principle, advantage and disadvantage of Planar Laser Induced Fluorescence technique (pLIF)

Operating principle Advantage Disadvantage

The flow region to be analyzed is illuminated with a laser sheet and
a fluorescent tracer is fed. Such tracer absorbs the laser light
energy and re-emits light at a longer wavelength that can be
detected by a photodetector.
• Direct measurement • Calibration is required prior to the experiments
• Use in reacting and non-reacting flows • Expensive technique (cameras and laser)
• Non-intrusive • For transparent systems
• Instantaneous visualization with high temporal • For semi-opaque fluids when using high power laser
and spatial resolution • Not suitable under highly aerated conditions
• Different flow field variables can be obtained
(concentration, density, temperature)
• Allows visualizing 2-D isolated mixing regions
• For unaerated and low aerated conditions
 G. Ascanio / Chinese Journal of Chemical Engineering 23 (2015) 1065–1076 1071

Fig. 7. Hue contours of the flow field observed with two-Rushton turbines 200 ms after
tracer injection [79].

probe. In such a case, the initial concentration should be measured and

the mixing time requires the final concentration, where the following
Fig. 8. (a) Stirred vessel equipped with a conductivity measurement system; (b) tracer
expression must be small enough:
concentration fluctuating with time [3].

C ðt Þ−C ð0Þ
Ci ¼
C ð∞Þ−C ð0Þ
where C(0) is the initial tracer concentration, C(∞) is the final tracer
concentration and C(t) is the tracer concentration at a certain time.
Fig. 8(b) shows a typical plot of concentration fluctuations of tracer as
a function of time. As stated by Tatterson [3], the amplitude of the con-
centration fluctuations decays exponentially with e−K a t , where Ka is a
constant determined for various impellers and geometries. The data
can be replotted in terms of probe log variance as a function of time
[78]. Under these conditions, the mixing time can be determined once
the concentration fluctuations are smaller than 5%, which is known as
the 95% mixing time (θ95).
Holmes et al. [81] reported for the first time the use of the conductiv-
ity technique to perform a study of mixing effectiveness in a baffled
stirred vessel. Using a conductivity cell around the impeller, the average
time required for a fluid element to complete one circulation around the
tank, which can be used for estimating the mixing time. Bouwmans et al.
[82] found that the probe position does not have any effect on the
ð11Þ mixing time measurement in the turbulent regime. Although the con-
ductivity technique has been used as an intrusive technique, Giona
et al. [83] reported the use of impedance probes attached to the baffles
and another one mounted on the shaft, so that the flow in the tank
was not perturbed.
Most of the studies reporting the effect of different parameters on
the measurement of mixing time coincide that the mixing time in the
laminar and turbulent regime is strongly dependent on the following
parameters [84–98]:
 
D NQ V a Δρ
Nθm ¼ f ; ; ; ð13Þ
T Np V ρ
where D is the diameter of the impeller, T is the tank diameter, NQ/Np is
the pumping effectiveness of the impeller, Va is the volume of the tracer
added, V is the volume of the liquid in the vessel and ρ is the density.
The use of the conductivity technique has been also used for deter-
mining mixing times in several applications such as gas dispersion
[92,99], steel converters [100], quality of mixing on animal cell culture

Table 5
Operating principle, advantages and disadvantages of thermography

Operating principle Advantage Disadvantage

It is based on the change of color of thermochromic liquid
crystals when they are subjected to different temperatures.
• Liquid crystals exhibit a rapid and reversible
response to dynamic temperature changes
• Wide range of temperatures
• Affordable setup
• Non-intrusive
• Temporal and spatial resolution
• Use of sophisticated image processing software
• Data processing is time consuming
• Used in transparent liquids and transparent tanks
• Invasive technique
• Mixing time must be inferred from Eulerian data
• Limited applicability under highly aerated conditions
1072 G. Ascanio / Chinese Journal of Chemical Engineering 23 (2015) 1065–1076
[71], blending of fluids having different densities [101], gassed condi-
tions [102,105], etc.
On the other hand, Nagata [6] described a method based on local
measurements of pH for the determination of mixing times in stirred
vessels. Following that approach, Poulsen and Iversen [103] developed
a system based on the signal of two pH sensors placed at the bottom
and top of a stirred reactor and a conventional stimulus–response
technique, in which the tracer signal was the difference between two
pH measurements, so that the effect of the position of the probes in
the tank was minimized and the initial and final values of the tracer
became zero being easier the determination of mixing times. Fig. 9
compares the determination of mixing time based on the measurement
of pH at the top (pH1) and at the bottom (pH2) of the vessel and the
difference between the two pH probe measurements (ΔpH). As mixing
time is slightly shorter when using the difference of the two signals, the
position of each probe in that case does not play an important role.
Fig. 9. pH signal as a function of time: Signals from each probe (upper plot); difference
between the two probes (lower plot).
Adapted from [103].
Vallejos et al. [104] developed a confocal optical to study mixing
times in a stirred reactor, whose results were validated by measuring
pH at a specific position. Van der Gulik et al. [106] reported also the
use of the pulse-response technique for the measurement of mixing
time in a horizontal stirred reactor. For that purpose, they perform the
measurements outside the tank by circulating the reactor contents
through a spectrophotometer placed in an external loop.
The advantages, disadvantages and the operating principle of the
technique based on the use of probes (conductivity and pH) are summa-
rized in Table 6.
3. Empirical Correlations
From the findings reported previously, mixing time can be predicted
as a function of the operating conditions. The mixing time correlations
in Table 7 have been selected from mixing studies using different
Table 6
Operating principle, advantages and disadvantages of probes
Operating principle Advantage
Physical measurement of conductivity, pH, etc. using • Affordable setup
probes placed at different positions in the stirred • Simple to implement
vessel. • Direct measurements
• For transparent and opaque liquids
• Suitable for unaerated and aerated conditions
measurement techniques as well as different conditions, namely: flow
regime, type of impeller, baffle and fluid rheology. From such a table it
is observed that the mixing time under the laminar regime correlates
well with the hydrodynamic characteristics, mainly on the agitation
regime or the power drawn by the impeller, which is true when mixing
viscous fluids with close clearance impellers such as helical ribbon
impellers. However, in the turbulent regime under ungassed conditions,
mixing times is not only dependent on the agitation regime and the
power consumption (Np = 2πNTm/ρN3D5), but also on the tank geom-
etry. Looking at the ratio of impeller size (D) to tank size (T), it is
observed than bigger impellers are more effective than small impellers
in the turbulent regime. However, in the same flow regime but under
gassed conditions, mixing time correlates with a number of parameters,
additionally to the latter case, the gas flow rate and the volume of liquid,
among other parameters. In this case, the mixing time is strongly
dependent on the ratio of the impeller size to the tank size being the ex-
ponent of the order of 2. On the other hand, the gas flow rate does not
play a significant role on the mixing time.
4. Comparison Between Techniques
The selection of a specific technique for the measurement of mixing
time in stirred vessels is dependent of several factors such as the
following:
• Accuracy and reproducibility
• Type of information generated
• Suitability
• Costs
• Assembly of the experimental setup
• Calibration
• Sampling speed and data processing time
In general terms, the accuracy provided by techniques involving the
use of tracers is higher compared to physical methods. Colorimetry is by
far the simplest technique in which a color tracer is only needed; how-
ever, its accuracy and reproducibility is strongly dependent on the
subjectivity of human observer. This drawback can be overcome by
combining the technique with image processing methods. In that case,
higher resolution images will provide better results, but the cost will
increase and the data processing time could be longer. On the other
hand, sophisticated techniques such as electrical resistance tomography
(ERT) are very accurate methods for the measurement of mixing time.
In such a case, the initial investment for acquiring those systems should
be considered, as well as the time for assembling the experimental
setup and the data processing time.
In regard to the type of information generated, it is important to
point out that experimental techniques providing Eulerian or Lagrang-
ian data do not give a direct measurement of mixing time, so the infor-
mation obtained from these techniques must be related to the mixing
efficiency.
Other techniques, such as positron emission particle tracking (PEPT),
computer automated radioactive particle tracking (CARPT), particle
image velocimetry (PIV), and laser Doppler anemometry (LDA) have
been developed for visualization purposes. However, mixing times can
Disadvantage
• Invasive and intrusive technique
• Measurements of mixing times depend on the position of probes
• Require calibration
• Measurement system to be compensate for temperature changes
• Limited temporal and spatial resolution
 G. Ascanio / Chinese Journal of Chemical Engineering 23 (2015) 1065–1076 1073

Table 7
Mixing time correlations for stirred vessels

Correlation Geometry Fluid Ref. Measurement technique

Laminar regime (ungassed)

θm = 896 × 103 Kp−1.69 Helical ribbon Viscous Newtonian [107] Conductometry
½1þ30 ðNR =NG Þ−2=3  Triaxe® agitator Viscous Newtonian [36] Colorimetry
θm ¼ NG

Turbulent regime (ungassed)

−2 Single impeller Non-Newtonian shear-thinning [10] Conductometry
N θ95 ¼ 5:2 Np−1=3 DT
H/T = 1
Baffled tank



D −2 H b Single axial or radial impeller Low viscosity [56] Electrical resistance
N θ95 ¼ 5:2 Np−1=3 T T
H/T = 2 Newtonian tomography
Baffled
θ95 ¼ 1:20 ðEi εd Þ−1=3 H 2=3 J−1
J 2=3
Multiple axial and radial impellers Low viscosity Newtonian [108] Conductometry
H/T N 1
Unbaffled tank

Turbulent regime (gassed)

T
13=6
 Q 1=12  N2 D4
1=15 Different type of impeller Low viscosity Newtonian [102] pH and conductometry
Nθm ¼ 20:41 aHþTT D
W
D NV
s
gWV 2=3 unbaffled tank
−1=3 −1 H
2:43 Four coaxial radial or axial impellers Low viscosity Newtonian [105] Conductometry
θm ¼ 3:3 NpG N D
θ95 = 12.5 Q−0.34 H−0.56 R1.93 Gas nozzles placed at the bottom of the vessel Low viscosity Newtonian [92] Conductometry
θm = A [1 − exp(−B Re)] Blade gas-entrainment impellers Low viscosity Newtonian [60] Electrical resistance
tomography

be indirectly inferred by following a sophisticated protocol. For instance,
García-Cortés et al. [109] reported the use of LDA data, from which
Eulerian information is generated and the mixing time can be deducted
by means of a mass balance as follows:
1. Radial profiles of the mean velocity (vr) in the vicinity of the impeller
were obtained.
2. The pumping capacity (Qp) was calculated by integrating the mean
radial velocity along the blade height times the cross sectional area.
3. The renewal time (tR) was determined as the ratio of the pumping
capacity to the volume of liquid, which is equivalent to the circula-
tion time (θm).
4. The mixing time was found to be proportional to the renewal time:
VL
θm ¼ m ¼ m tR
Qp
where m is the number of time the discharge liquid circulates in the
vessel, which is a function of the tank diameter, the impeller geome-
try and the impeller blade number.
On the other hand, the Lagrangian approach follows a fluid particle
over time as it moves through the flow field, then the mixing time can
be determined from the flow number or the circulation time. Nienow
[110] found that macromixing mixing time correlates well with the
flow number, which is defined as the pumping capacity (Q p) divided
by ND3, being N the impeller rotational speed and D the impeller diam-
eter. The circulation time (θc) is here defined as the ratio of volume of
liquid (V) to the pumping capacity.
In regard to the suitability, most of the techniques, especially those
based on flow visualization (e.g. colorimetry, pLIF) allow determining
not only mixing times but also obtaining 2-D and 3-D flow patterns in
transparent vessels and fluids, which is a limitation at industrial scales.
This drawback can be alleviated using other techniques like ERT, which
can be applied to opaque systems. On the other hand, the use of probes
can provide also information about the hydrodynamics with opaque
fluids. Techniques involving the use of probes for the measurement of
physical properties are in general affordable systems and easy to be
implemented; however, since the measurements are local, a map show-
ing the distribution of physical values could result in a time consuming
and costly process. From a physical standpoint, the use of probes can
disturb the flow, being this effect stronger when using small tanks.
Both calibration and data processing time are also important issues
to consider when selecting a measurement technique for mixing
times. Particularly, pLIF is a technique requiring calibration before use
and sophisticated software is required for data processing. However,
such a technique provides reliable information about flow patterns,
which can be further used for the accurate estimation of mixing time.
Besides calibration, some measurement techniques are sensitive to
temperature; therefore they need to be compensated for these changes
(e.g. pLIF).
On the other hand, techniques based on probes provide almost real
time measurements. For instance, the measurements of conductivity
or pH can be easily correlated with mixing time in a stirred vessel if
the probes are connected to a data acquisition system and then such
data is processed to determine the mixing time. However, response
time should be also considered, especially when using probes for the
ð14Þ
measurement of conductivity or pH.
Mixing time has not only been determined by using experimental
techniques but also by numerical simulation [111–113]. All the
techniques here described are useful methods also for validating
mixing time predicted with numerical simulations, such as the one
reported by Coroneo et al. [111], who performed simulations of fluid
mixing in a single phase of a stirred vessel with different levels of spatial
discretization by finding good agreement when comparing their results
with pLIF results.
To summarize, besides the investment costs, the ideal experimental
technique would be the one which does not disturb the flow, it can be
applied over a temperature range, it can be used with opaque and trans-
parent fluids and nontransparent tanks, and it can provide accurate and
reproducible results.
5. Conclusions
The experimental techniques developed in the last 50 years for mea-
suring mixing times in stirred vessels have been reviewed and the most
outstanding works reporting these techniques have been described. The
applicability and limitations of all techniques as well as a comparison
between them in terms of the accuracy, type of information generated,
cost and processing time, among others, have also been described.
Techniques such as colorimetry and pLIF have been supplemented in
the last years with digital image processing resulting in more robust
and accurate measurement methods. On the other hand, relatively
new techniques based on radioactive tracking like positron emission
1074 G. Ascanio / Chinese Journal of Chemical Engineering 23 (2015) 1065–1076

particle tracking have emerged to provide information not only on τ99 99% non-reactive mixing time, s
the homogeneity level in the tank, but also on the flow fields in non- ω angular speed, rad·s−1
transparent systems.
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