Minerals Engineering 132 (2019) 142–148

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Minerals Engineering
journal homepage: www.elsevier.com/locate/mineng

Short communication

Modeling the effect of air flow, impeller speed, frother dosages, and salt T
concentrations on the bubbles size using response surface methodology
María P. Arancibia-Bravoa,b, Freddy A. Lucaya, Jean Lópezc, Luís A. Cisternasa,
⁎

a
Departamento de Ingeniería Química y Procesos de Minerales, Universidad de Antofagasta, Avenida Angamos 601, Antofagasta, Chile
b
Csiro-Chile International Center of Excellence, 2827 Apoquindo Street, 12th floor, Las Condes, Santiago, Chile
c
Departamento de Ingeniería en Minas, Universidad de Antofagasta, Avenida Angamos 601, Antofagasta, Chile

ARTICLE INFO ABSTRACT

Keywords: The size of bubbles plays an important role in the performance of a flotation system in mineral processing. The
Bubbles size inorganic salt studied in this work, stabilizes the interfacial air-liquid films which inhibit bubble coalescence and
Salinity therefore the bubble size. In this work, the response surface methodology (RSM) was adopted to study, at
Response surface methodology laboratory-scale tests, the influence of various process parameters such as air flow, impeller speed, frother do-
Box–Benhken design
sages, and salt concentrations on the bubble size. The significance of these parameters was identified by using
the analysis of variance (ANOVA). The resulting correlations were capable of predicting bubble sizes which were
in excellent agreement with experimental data. Several saline solutions were used including a synthetic sea
water solution, NaCl, KCl, and MgSO4.

1. Introduction bubble sizes smaller than 1 mm is recommended in the cleaning stages,

The use of seawater (SW) in froth flotation is a complex process
which requires further studies to better understand the phenomena of
the three-phase system (Jeldres et al., 2017). Sodium chloride is the
most important component of seawater comprising 77.7% of the salts,
but calcium, potassium, sulfate, and magnesium play important roles
(Cisternas and Gálvez, 2017). These ions can have positive effects on
mineral flotation by increasing the kinetics of the minerals (Smith and
Heyes, 2012) through decreasing the coalescence of the bubbles (Quinn
et al., 2007), generating similar effects of the frother (Kracht and Finch,
2009), or increasing the synergy between SW and the frother (Castro
et al., 2013).
The stability of the foam depends on the variables directly influ-
encing the form and size of the bubbles, which are the air flow rate (see
Fig. 1 as an example), impeller speed, reagents dosages (see Fig. 2 as an
example), and water quality (see Fig. 3 as an example) where it is
shown that D32 depends on the dose of foaming, aeration when it is in
saline solutions with doses over 5 ppm of frother and Jg of 0.5. Due to
the above, the air flow, agitation, and doses of frother affect the con-
stant kinetics and the recovery in water flotation (Gorain et al., 1999;
Heiskanen, 2000). In the case of frother agents, better performance has
been demonstrated in saline water for the foam phase although in the
presence of solids (over 20%) a decrease in performance has been ob-
served (Ramos et al., 2013). If better flotation selectivity is sought,
which can be achieved with salinity bellow 0.4 M (Bournival et al.,
2012; Kracht and Rebolledo, 2013). The actual effect of salinity on the
size of the bubbles has been evaluated so far by experimental tests that
varied one factor-at-a-time and kept the other input factors constant
(Sovechles et al., 2016). This experimental approach does not address
the uncertainty of whether the interaction between these factors in-
fluences the D32 or if it is only the salinity that generates these reduc-
tions in the size of the bubbles.
This work aimed to identify which input factor or factor interactions
generated the most significant effect on the bubble size (D32 ) under
different operational conditions: air flow, XA ; impeller speed, XI ;
frother dosages, XF ; and salt concentrations, XS . Furthermore, we
looked for simple models for the bubble size as a function of the im-
portant input factors. Four solutions were studied: synthetic sea water
(SSW), NaCl, KCl, and MgSO4.
2. Methodology
The Box–Benhken design (BBD) (Box and Hunter, 1957) was used to
design the experiments for identifying the input factors that affect the
bubble size, and replicas of the central point were used to obtain an
independent estimation of the experimental error. To determine the
salinity, the concentration of seawater was considered as the upper
limit. It is important to note that the concentration of seawater

⁎
Corresponding author. Mobile: +56 991384556.
E-mail address: luis.cisternas@uantof.cl (L.A. Cisternas).

https://doi.org/10.1016/j.mineng.2018.12.001
Received 6 February 2018; Received in revised form 21 October 2018; Accepted 1 December 2018
0892-6875/ © 2018 Elsevier Ltd. All rights reserved.
M.P. Arancibia-Bravo et al.
Fig. 1. Impact of gas rate (Jg), on number frequency bubble diameter (Db)
(Nesset et al., 2006).
Fig. 2. The effect on bubble size (D32), of increasing tip speed at various frother
concentrations and gas rate (Jg), (Finch et al, 2008).
Fig. 3. Sauter mean bubble diameter vs MIBC concentration for the seawater
ion solutions tested (Sovechles et al., 2016).
considers concentrations over the critical coalescence concentration
(CCC). Regarding the concentration of the foam, concentrations were
considered under CCC as the interest was in evaluating the effect of the
concentration of the foam in seawater and values over the CCC would
not have allowed us to see the effect of salinity on the bubble size.
2.1. Materials and equipment
An AEROFROTH 70 frother (equivalent to MIBC) was provided by
Solvay-Chile. Marine Salt Solutions (SSW) were prepared using the
following reagents: sodium chloride (> 99%), potassium chloride
(> 99%), and heptahydrate magnesium sulfate (> 98%). These
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Minerals Engineering 132 (2019) 142–148
Fig. 4. The mechanism for capturing bubbles in operation includes the capture
of the bubble view, the mechanical flotation cell and the auxiliary equipment.
reagents were provided by Merck. These salts were chosen as they have
been used in scientific studies related to marine biodiversity to emulate
seawater. The standards suggested by Rodríguez et al. (1986) were
followed with 26.41 NaCl, 0.88 KCl and 7.7 g/L MgSO4 corresponding
to a concentration of 3.5% w/v. The MIBC was selected as it is a
commonly used frother in the industry that operates with seawater. For
the experiments, a Metso D-12 laboratory flotation machine with a
volume cell of 3.5 L was used. A Nikon brand camera model D-6000 and
auxiliary accessories were used (Borjas, 2008) to photograph the bub-
bles.
2.2. Methodology of bubbles capture
Fig. 4 shows the procedure for bubbles capture using the bubble
collection device used for the development of this work following the
designs and examples developed at the Mc Gill University by Finch
et al. (2008). All saline solutions used were prepared with distillate
water 30 min prior to each test. For each test, the solution was put in
the flotation cell, then the froth was added, and the solution was con-
ditioned for 5 min at 900 rpm without air. To ensure that the solutions
were not contaminated with external agents, their preparation was
carried out independently for each test in reactors that were thoroughly
cleaned using distilled water. The same treatment was carried out both
with the flotation cell and with the bubble collection device. The sur-
factant only came into contact with the flotation cell when each test
was started.
To validate our bubble size measurement procedure, our results
were compared with the results delivered by Finch et al. (2008). Fig. 5
shows that the results were practically the same. These tests were done
in triplicate. At least 3000 bubbles were measured per test to ensure the
robustness of the results; this value was greater than those used by
Quinn et al. (2014).
Later, the pump (peristaltic model Masterflex L/S) was activated,
and the bubble viewer capture was filled with the solution. Finally, the
air flow was activated at a suction flow of 2.3 L/s, and the capture of
bubbles started until a total of 250 images had been completed. Each
test was batched and without overflow to guarantee that the salinity
and foaming concentrations were always the same in the system under
environmental conditions (average value of 1 atm and 20 °C).
M.P. Arancibia-Bravo et al. Minerals Engineering 132 (2019) 142–148

(a) Finch et al., 2008 versus our measurement. (b) Correlation between bubbles sizer devices.
Fig. 5. Comparison between bubble collection devices.

Table 1 used are detailed in Table 1. The values of the input factors for the 27
Factors and their levels for BBD experiments. trials are given in Table 2. The bubble size was modeled using a second
Factors Coded variable level order polynomial as shown in Eq. (1). This model is the usual model
used in response surface methodology.
Low Center High
k k k k
−1 0 1 2
y= 0 + i Xi + ij Xi + ij Xi Xj + e0
XA: Air flow, cm/s 0.34 0.51 0.68 i=1 i=1 i=1 j =1 (1)
XI: Impeller speed, rpm 800 900 1000
XF: Frother, ppm 4 7 10
XS: Sea salt solution, M 0.054 0.297 0.54 2.4. Bubble size measurement

A processing program (ImageJ) was used to analyze the images to

2.3. Mathematical modeling
The Box–Benhken experimental design was used to minimize the
number of experiments. For the four input factors (air flow, XA ; impeller
speed, XI ; frother dosages, XF ; salt concentrations, XS ), a series of 27
trials with three central points were obtained. The input factor ranges
determine the size distribution of the bubbles. The bubble diameter was
calculated using an expression that determines the projected diameter
as a function of the projected area of the bubble, as shown in Eqs. (2)
and (3) (Nesset et al., 2006; Gomez and Finch, 2007):
Da = 4Ap / (2)

Table 2
Summary of BBD experimental results on bubbles size.
Run order Actual level of variables Bubble size per saline solution, D32

XA XI XF XS MSS NaCl KCl MgSO4

cm/s rpm ppm M mm mm mm mm

1 0.51 900 7 0.297 0.84 0.88 0.85 0.86

2 0.51 800 7 0.054 2.71 2.25 2.98 3.10
3 0.68 1000 7 0.297 0.84 0.85 0.82 0.81
4 0.34 800 7 0.297 1.01 0.85 0.88 0.84
5 0.68 900 10 0.297 1.18 1.19 0.89 0.87
6 0.51 1000 7 0.054 2.83 2.32 3.08 2.89
7 0.68 900 7 0.054 3.10 2.93 3.00 2.68
8 0.34 1000 7 0.297 0.78 0.85 0.85 0.75
9 0.68 900 7 0.540 0.84 0.86 0.86 0.85
10 0.51 1000 4 0.297 0.81 0.86 0.82 0.85
11 0.51 900 10 0.540 0.82 0.73 0.86 0.84
12 0.68 900 4 0.297 1.01 0.92 0.93 0.90
13 0.51 900 7 0.297 0.85 0.88 0.86 0.86
14 0.51 900 4 0.054 2.69 2.89 3.13 3.36
15 0.34 900 7 0.054 2.52 2.82 2.82 3.36
16 0.51 800 7 0.540 0.86 0.82 0.83 1.02
17 0.34 900 7 0.540 0.78 0.78 0.75 0.83
18 0.51 800 10 0.297 0.85 0.91 0.95 0.90
19 0.51 900 4 0.540 0.81 0.81 0.82 0.84
20 0.51 900 10 0.054 2.95 2.37 2.64 2.27
21 0.51 900 7 0.297 0.83 0.88 0.86 0.86
22 0.51 1000 10 0.297 0.78 0.79 0.88 0.80
23 0.68 800 7 0.297 1.06 0.86 0.95 0.92
24 0.34 900 10 0.297 0.80 0.80 0.88 0.80
25 0.51 1000 7 0.540 0.78 0.82 0.91 0.81
26 0.34 900 4 0.297 0.82 0.78 0.83 0.77
27 0.51 800 4 0.297 0.87 0.96 0.99 0.81

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M.P. Arancibia-Bravo et al. Minerals Engineering 132 (2019) 142–148

Fig. 6. Image analysis processing.

Table 3
Identification of influential factors on bubbles size by each solution.
Term SSW NaCl KCl MgSO4

Constant ✓ ✓ ✓ ✓
XA ✓ X X ✓
XI X X X X
XF X X ✓ ✓
XS ✓ ✓ ✓ ✓
XA2 X X X X
XI2 X X X X
XF2 X X X X
XS2 ✓ ✓ ✓ ✓
XA*XI X X X X
XA*XF X X X X
XA*XS ✓ X X ✓
XI*XF X X X X
XI*XS X X X X
XF*XS X X ✓ ✓

R-Sq 98.86% 95.67% 99.39% 97.95%

R-Sq(pred) 98.30% 94.03% 98.82% 93.89%
R-Sq(adj) 98.66% 95.31% 99.28% 97.33%

Fig. 7. Response surface for the bubbles size of the SSW solution (air flow, XA ;
impeller speed, XI ; frother dosages, XF ; salt concentrations, XS ).
Da3
D32 =
Da2
The image size was 100 × 64 mm with a standardized resolution for
all experiments of 60 pixels/mm and a rate of one frame per second
controlled through the Nikon Software Camera Control Pro 2. At least
3.000 bubbles were measured per test to ensure robustness in the re-
sults (Quinn et al., 2014).
The analysis of the images was made sequentially starting with the
binarization of the image to continue with the transformation of the
distance and filling of spaces to reach the segmentation of watersheds
(3) as per the stages detailed in Fig. 6 following the methodologies sug-
gested by Hernandez-Aguilar et al. (2004) and Lichti and Bart (2018).
3. Results and discussion
The results of all the experiments are shown in Table 2. The bubble
size varied between 3.36 and 0.73 mm. The central points in the design

145
M.P. Arancibia-Bravo et al.
Table 4
Mathematical representation obtained for D32 per each solution evaluated.
Solution
SSW
NaCl
KCl
MgSO4
of experiments were measured with three replicas, observing that the
experimental deviations in the bubbles diameter are under ± 0.02 mm.
The largest bubble size was observed in the MgSO4 solution, with the
smallest in the NaCl solution. Small bubbles were not necessarily con-
ditioned to low air flows, but to combinations of factors and mostly to
the salt concentration of the solution.
First, Eq. (1) was used to model the bubble size including all input
factors and their interaction. The regression coefficients were obtained
using the software Minitab 18. Eq. (4) is the model for the SSW solution.
The coefficient of determination, R squared, was 99.43% and the R-
squared Adjusted was 98.76%. This means that 99.43% of the variance
in the bubble size can be explained by the model of Eq. (1). The re-
gression coefficients for the other saline solution studied are shown in
Table A1 in the supplementary material.
D32MSS Fullmodel = 0.837 + 0.110XA 0.045XI + 0.031XF
+ 0.07XA2 + 0.000XI2 + 0.026XF2 + 0.939XS2
+ 0.047XA XF 7 0.13XAXS 0.003XI XF
0.063XF X S
Fig. 7 shows the response surface when two input factors vary be-
tween their upper and lower values, while the other input factors have
central values. From Fig. 7, it is clear that the solution concentration
exerts an important effect.
The analysis of variance, ANOVA test, was used to identify which
terms in Eq. (1) were significant in the prediction of the bubble size.
Table 3 shows the significant terms for each solution studied, where the
significant terms are the ones with p-value smaller than 0.05 (identified
with the symbols ✓, the no significant terms were identified with the
symbol X. Salt concentrations including XS and XS2 were the only input
factor that affected the bubble size in all saline solutions. The air flow
was significant in the bubble size of SSW and MgSO4 solutions. The
frother dosages affected the bubble sizes of the KCl and MgSO4 solu-
tions. The only important interactions were air flow—salt concentration
(for SSW and MgSO4 solutions) and frother dosages—salt concentration
(for KCl and MgSO4). The simpler model was the bubble size of NaCl
solutions (see columns in Table 3), whereas the more complex model
was the bubble size of the MgSO4 solutions. The coefficients of de-
termination (R squared, R-squared adjusted) are also shown in Table 3.
These values were acceptable considering that only the significant input
factors were considered. For example, the value of R-squared for the
SSW solution was 98.96%, which could be compared with the values of
99.43% when all input factors were considered.
Second-degree polynomial models including only significant terms
are given in Table 4. More details on these models are presented in
Tables A2–A5 in the supplementary material.
The results showed the importance of evaluating several factors si-
multaneously. For example, it is known that airflow affects the size of
bubbles (Sovechles et al., 2016), but the effect of some electrolytes,
such as the electrolytes studied here, can eliminate this bubble si-
ze–airflow relationship because the coalescence is reduced at least in
the conditions considered in this work. In the case of SSW and MgSO4,
Minerals Engineering 132 (2019) 142–148
Models obtained per each solution
D32 = 0.888 + 0.110XA − 0.993XS − 0.130XAXS + 0.919XS2
D32 = 0.884 − 0.897XS + 0.816XS2
D32 = 0.888 − 0.042XF − 1.052XS + 0.133XFXS + 1.002XS2
D32 = 0.840 − 0.027XA − 0.088XF − 1.039XS + 0.175XAXS + 0.273XFXS + 1.064XS2
the airflow affected the size of the bubbles, but this effect was not seen
in the case of NaCl and KCl. It is necessary to indicate that similar re-
sults have been obtained with other water qualities (Gordiychuk et al.,
2016) (Rafiei et al., 2011) (Vinnett et al., 2012).
The concentration of the salt affected the size of the bubbles in all
the saline solutions studied. This effect was significant including first
and second order effects as well as interactions with other input factors.
This can be explained by the positioning of the ions in the air-water
interfacial region which inhibits the coalescence of bubbles (Collins,
2004; Parsons et al., 2010; Quinn et al., 2014).
Some salts have been proven to inhibit bubble coalescence above a
certain concentration called the transition concentration, which is the
concentration corresponding to 50% bubble coalescence. This transi-
tion concentration is sharp and occurs over a narrow concentration
range (usually < 0.1 M) (Christenson et al., 2008). The transition con-
0.993XS centration for 50% coalescence for MgSO4, NaCl, and KCl were 0.032,
+ 0.003XAXI 0.175, and 0.23, respectively (Lessard and Zieminski, 1971)). There-
0.05XI X S fore, it was expected that in the 0.054 M experiments, the NaCl, SSW,
and KCl solutions showed coalescence, but the MgSO4 solution should
(4)
not show coalescence. However, the results showed coalescence in the
MgSO4 solution at 0.054 M independent of the injected air flow, with
bubble sizes of 2.68 mm for air flows of 0.68 cm/s and 3.36 mm for air
flows of 0.34 cm/s for the same conditions of agitation and foaming
dose, since the coalescence in the presence of this type of solutions does
not depend on the agitation or aeration (Machon et al., 1997) (Tsang
et al., 2004) (Nguyen et al., 2012) Although the ionic strength of MgSO4
quadruples to NaCl and KCl, it does not directly affect the size of
bubbles. However, the differences in ionic strength in combination with
other factors such as aeration and foaming dose do generate differences.
This can be observed in Fig. 8, which shows a photograph of the bub-
bles at an air flow of 0.51 cm/s, impeller speed of 900 rpm, frother
dosage of 4, 7, and 4 ppm for the solution concentrations of 0.054 M,
0.297 M, and 0.540 M, respectively. The coalescence of bubbles in
MgSO4 can be explained by the saturation of the frother at the air-water
interface which produces an increased bubble size through the addition
of the frother in some electrolyte solutions (Chu et al., 2016; Sovechles
et al., 2016). Based on the ANOVA test, the frother dosage influenced
the bubble size for the KCl and MgSO4 solutions, which was in agree-
ment with the previous discussion. Kurniawan et al. (2011) observed
that the transition concentration could be associated with the effect of
the frother in electrolyte solutions.
4. Conclusions
The RSM was used to study the effect of air flow, impeller speed,
frother dosages, and salt concentrations on the bubble size in saline
solutions. Under the conditions studied, it was found that the salt
concentration was the only input factor that affected the bubble size in
all saline solutions (NaCl, SSW, KCl, and MgSO4). The air flow was
significant in the bubble size of the SSW and MgSO4 solutions. The
frother dosages affected the bubble sizes of the KCl and MgSO4 solu-
tions. The only important interactions were air flow–salt concentration
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M.P. Arancibia-Bravo et al. Minerals Engineering 132 (2019) 142–148

Fig. 8. Photograph of bubbles at the flow of 0.51 cm/s, impeller speed of 900 rpm, frother dosage of 4, 7, and 4 ppm for solution concentration of 0.054 M, 0.297 M,
and 0.540 M respectively.

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M.P. Arancibia-Bravo et al.
(for SSW and MgSO4 solutions) and frother dosages–salt concentration
(for KCl and MgSO4). Good agreement between the experimental values
and second-degree polynomial models was observed. These models
only considered the significant terms based on the ANOVA tests. Bubble
coalescence was detected in the MgSO4 solutions even at concentrations
smaller than the transition concentration, which can be explained by
the saturation of the frother at the air–water interface.
Acknowledgments
Authors thank the financial support from INNOVA CORFO Projects
Csiro Chile 10CEII-9007.
Appendix A. Supplementary material
Regression coefficients and p-values are included in the supple-
mentary material. Supplementary data to this article can be found on-
line at https://doi.org/10.1016/j.mineng.2018.12.001.
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