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Effect of Different Salt Solutions on Coal Flotation in the Absence of Frothers

Article · February 2018

DOI: 10.22059/ijmge.2018.241506.594696

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 1 Effect of Different Salt Solutions on Coal Flotation in the
2 Absence of Frothers
3

4 M. Jahania,1
a
5 School of Mining, Petroleum & Geophysics Engineering, Shahrood University of
6 Technology, Shahrood, Iran.
7

8 Abstract:
9 Flotation is usually performed in the presence of frothers. However, due to the high cost of
10 purchasing frothers, if there is the possibility to remove them from operation, the cost of
11 the operation will be greatly reduced. In this study, coal flotation in KI, Na2SO4, MgCl2,
12 and NaCl salt solutions are investigated in the absence of frothers. When the concentration
13 of Na+, SO42-, Mg2+ and Cl- is relatively high, between 30 and 70 g/L, the presence of fine
14 bubbles is increased, between 0.50 and 1.67 mm in diameter, and this is the favorable
15 conditions of flotation. It was observed that the concentration of Na+ and Mg2+ increased
16 the recovery of coal up to 85%. Solutions with high concentrations of K+ and I- are
17 associated with modest recoveries between 44 and 70%, while the combination of ions Na+
18 and SO42- increases recovery of mineral matter in the concentrate, up to 60%.
19 Keywords: Bubble size, Coal, Flotation, Salt solutions
20 1. Introduction
21 The history of the Semnan province is closely related to mining, with the discovery and
22 exploitation of coal ore since 1969. Currently in the Eastern Alborz Coal Mines Company
23 (EACMCO), between 2000 – 2400 tons of coal is processed daily, which is transferred to
24 different coking plants such as Esfahan Steel Company (ESCO) [1]. However, it has been
25 recognized that coal flotation presents difficulties related to electrochemical phenomena of
26 the mineral pulp and the chemical composition of the process water [1]. These factors
27 compromise the recovery and quality of the coal [1]. At the industrial scale, water demand
28 is satisfied with recycled water as the main source of supply. However, this practice
29 substantially increases the concentration of sulfates, carbonates, chlorides and metal
30 cations [2]. Paulson and Pugh [3] indicated that the recovery of hydrophobic particles in a
31 flotation system depends on the properties of the electrolytes, e.g., valence, ionic strength,
32 among others. Regarding to their contribution to metallurgical efficiency (recovery of
33 coal), these authors classified the electrolytes into three groups: "A" divalent and trivalent
34 salts (Na2SO4, MgSO4, MgCl2), "B" monovalent salts (LiCl, KCl, NaCl) and "C" strong
35 acids and perchlorates (NaClO4, HClO4, LiClO4). Each group (A, B and C) recovery was
36 96.65% (±10.87%), 86.23% (±6.90%) and 28.82% (±3.06%), respectively. However, this
37 classification does not allow to describe the participation of the electrolytes in the
38 interaction mechanism of an air bubble and the surface of a hydrophobic mineral. In this

1- Corresponding author. Tel/Fax: +98 9127277347/+98 2332395509

E-mail address: M.Jahani@shahroodut.ac.ir – M. Jahani.

1
39 respect, Li and Somasundaran [4] evaluated the hydrophobicity of a bituminous coal in
40 NaCl solutions (0.2, 0.3 and 0.5 mol/L). The most relevant observations indicated that at
41 pH = 3 the force of attraction between the bubbles and particles are significant, at pH = 7
42 the charge of the particles (negative) is updated and thus the force is repulsive. This
43 behavior is intensified to pH = 10, the interpretation of the results suggests the participation
44 of electrostatic forces at acidic pH. While at neutral and basic pH, the results suggest that
45 the flotation of coal particles is related to chemical mechanisms (e.g. hydrophobicity).
46 Ozdemir et al. and Kurniawan et al. [5,6] reported that the behavior of coal ore in saline
47 water does not depend on surface chemistry, as previously proposed [7]. In contrast, it has
48 been observed that the bubble contact is instantaneous in the presence of pure water and is
49 independent of the particle size, while the bubble-particle contact in saline water requires
50 longer times. This evidence suggests that coal ore is more floatable in pure water. In
51 contrast, experimental studies reveal that saline water enhances the recovery of coal and
52 thus the recovery of ash. Wang and Peng [8] interpreted the behavior of mineral matter
53 (e.g., quartz, calcite, pyrite, etc.) in coal flotation, entrapment and ash trapping in the
54 collection area to the froth. This effect enhances in the presence of saline water and
55 decreases in the presence of deionized water. In addition, it was found that the entrapment
56 predominates and enhances with the increase in the degree of aggregation of coal particles,
57 a phenomena that depends on the hydrophobicity of the system [9].
58 The available in the literature experimental models and data have shown that solution
59 electrolytes significantly influence bubble coalescence [10,11]. The operating conditions
60 that have been reported indicate that Na+ and Cl- ions control coalescence, equivalent to
61 the effect of an industrial application frother such as methyl isobutyl carbinol (MIBC) [12].
62 Fundamental studies indicate that electrolytes increase surface tension at the water-air
63 interface, whereas MIBC has an inverse effect. This observation suggests that the
64 coalescence of bubbles does not only depend on the surface tension. Craig et al. [13]
65 suggested that the combination of ions in solution is transcendental to control the effect of
66 coalescence. The authors classified the ions as: anions α (Cl-, Br-, OH-, NO3-), anions β
67 (ClO3-, ClO4-, CH3COO-), cations α (Na+, K+, Li+, Cs+, NH4+) and cations β (H+, (CH3)4N+,
68 (CH3)3NH+, (CH3)2 NH+2, CH3NH+3). Experimental observations indicated that
69 electrolytes that do not inhibit coalescence are characterized by the combination αβ or βα
70 (E.g., Mg (ClO4)2, HCl) while the combination αα or ββ controls coalescence (e.g., NaCl,
71 HCH3COO) [13,14].
72 In the above context, the particular objective of the present work is analyzing the effect of
73 solutions of KI, Na2SO4, MgCl2 and NaCl on the recovery of coal by froth flotation in the
74 absence of frothers. The aim of this study is to correlate the recovery of coal with the
75 presence of specific anions and cations and their effect on the distribution of bubble sizes
76 in the collection area and on the distribution of particle sizes that are recovered in the
77 concentrate.
78
79 2. Material and Methods
80
81 2.1. Material and reagents
82 The sample of coal ore used in the present study was obtained from the Shahrood sub-basin
83 (Eastern Alborz Coal Mines Company). Table 1 demonstrates the proximate analysis of
84 the coal sample. The coal sample can be classified as bituminous under volatility, according

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 85 to the content of volatile matter (> 20%). The petrographic characterization allowed to
86 determine the maceral composition of the coal by means of the average random reflectance
87 measured with an MSP-COAL spectrometer. The results indicated high content of vitrinite
88 and mineral matter, the results are shown in Table 2.
89 Saltwater was prepared in the laboratory using water from Damghan groundwater aquifer
90 (Located in Semnan province). The chemical composition of the water is shown in Table
91 3. Four salt solutions were prepared using inorganic salts with analytical grade (> 99%);
92 KI, Na2SO4, MgCl2 and NaCl. The concentrations of the electrolytes used in the
93 experiments were 0.05, 0.25 and 0.50 mol/L, respectively. Industrial grade gasoil was used
94 as a collector. Also, deionized water (conductivity of 0.050 µS/cm) was used to evaluate
95 the recovery of coal in the absence of ions.
96
97 Table 1- Proximate analysis of the sample of coal mineral.
Humidity Ash Sulfur Calorific power Volatile Matter FSI Fixed Coal
6.32% 37.95% 1.05% 2847 kcal/kg 20.4% 6½ 42%
98
99 Table 2- Maceral analysis of the sample of coal mineral.

Group macerals
Vitrinite Liptinite Inertinite Mineral matter
75.67% 13.13% 0.77% 10.43%
100
101 Table 3- Chemical composition of cations and anions of Damghan ground water aquifer (mg/L).

pH Conductivity (mS/cm) Cations Anions

Na+ K+ Ca2+ Mg2+ Cl- (SO4)2-
6.6 1.59 100 1 165 30 284 252
102
103
104 2.2. Coal flotation
105 Flotation experiments were performed with a sample of saline water previously prepared.
106 The suspension was prepared with addition of 200 g of coal in a 2.5 L cell equipped with
107 a Denver mechanical stirring system and the operation was performed in batch mode (at
108 25 °C). Fig. 1 shows the general configuration of the experimental equipment. The water-
109 solids suspension was achieved by setting the impeller speed at 900 rpm (estimated time
110 10 minutes). Then the collector was added with the dosage of 1000 g/t of gasoil for a time
111 interval of 10 minutes. The pH of the suspension was maintained between 6 and 7 (i.e.,
112 natural pH). Once the conditioning time was reached, the stirring speed was increased to
113 1200 rpm, the air flow in the mechanical cell was enabled and the floatable material was
114 removed for 2 minutes. Simultaneously samples of gas dispersion (i.e., bubble size and air
115 velocity) were collected. The concentrate and tailing samples were filtered and dried at 90
116 °C in an oven. The ash analysis was performed with the combustion of a 1 g concentrate
117 sample in a muffle furnace at 750 ° C for 2 h (ASTM D-3174-04). Eq. (1) was used to
118 calculate the fuel recovery.
119
𝑀𝑐 (100−𝐴𝑐 )
120 𝑅= × 100% (1)
𝑀𝑓 (100−𝐴𝑓 )

3
121
122 where, Mc and Mf correspond to the weight of the sample in the feed and concentrate
123 streams, respectively, Ac and Af are the ash content in the concentrate and feed sample.
124

125
126 Figure 1. Schematic diagram of the flotation system. (1) rpm indicator, (2) 2.5 L acrylic
127 cell, (3) impeller speed setting, (4) start switch, (5) air valve, (6) photographic system (7)
128 sampling tube.
129
130 2.3. Measurement of bubble size and air velocity
131 The bubble size measurements were made based on the sampling technique developed by
132 Hernandez-Aguilar [15]. The image analysis was performed according to the protocol
133 described by Bailey et al. [16]. The device consists of a visualization camera box with 17
134 cm length, 17 cm width and 17 cm depth. The camera box was manufactured in acrylic of
135 4 mm of thickness, with a capacity of 4.9 L (the front of the camera box is graded with
136 divisions of 0.5 cm3). The reservoir allows the connection of a pipe (of PVC, CÉDULA
137 40) of adaptable length and 1.27 cm of diameter. In the upper part, the visualization camera
138 has a lid of 16 cm of diameter that allows to clean the interior properly. The bubbles were
139 filmed with a high resolution photographic system equipped with an EF 100 mm f/2.8
140 Macro USM lens. A 400 W light source was placed behind the viewing camera to improve
141 the visibility of the bubbles. The analysis of the images was done offline. To represent the
142 distributions (composed of 2500 objects) of bubble sizes the average Sauter is reported
143 according to Eq. (2).
144
∑𝑛 (𝑑 )3
𝑖
145 𝑑32 = ∑𝑖=1
𝑛 (𝑑 )2 (2)
𝑖=1 𝑖
146
147 where, di is the equivalent diameter, obtained from the image analysis.

4
148 The surface velocity of air (Jg, cm/s) is represented by Eq. (3) and is derived from the
149 measurement of the volumetric air flow (Qg, cm3/s) divided by the cross-sectional area the
150 cell (At, cm2). The Jg measured with the method of the "inverted probe". That is, by
151 measuring the time it takes for the bubbles to move a known volume of liquid. Since the
152 dimensions of the visualization camera are known, this same device was used as a reference
153 volume to quantify the volumetric flow of air.
𝑄𝑔
154 𝐽𝑔 = (3)
𝐴𝑡
155
156 Finally, the participation of the properties of the gas dispersion is summarized in the bubble
157 surface area flux density (Sb) Eq. (4). This variable integrates the effect of the bubble size
158 (db), represented by the mean Sauter diameter (d32) and the air surface velocity (Jg).
159
6𝐽𝑔
160 𝑆𝑏 = (4)
𝑑𝑏
161
162 3. Results and Discussions
163
164 3.1. Distribution of bubble sizes in water-air system
165 Fig. 2(a) illustrates the behavior of the bubbles in the collecting area in the water system.
166 Increasing the concentration of the electrolytes increases the ionic strength and decreases
167 the average bubble size. The trend of the data suggests that a limit is reached, after which
168 the bubble size remains constant. This behavior is related to a concept called transition
169 concentration [13] equivalent to the critical coalescence concentration developed for
170 frothers [18]. In both cases the concentration is difficult to establish. According to the
171 literature, the transition concentration of sodium chloride (NaCl) is 0.078 mol/L [3,13].
172 The experimental observations of Fig. 2(a) suggest that it is close to 0.25 mol/L.
173 Information related to magnesium chloride and sodium sulfate has not been reported in the
174 literature. The trend of the data indicates that the stability of the bubble sizes with these
175 electrolytes (i.e., MgCl2 and Na2SO4) is reached above 0.05 mol/L. Due to the limited
176 information on potassium iodide, the results obtained by Marrucci and Nicodemo [17] were
177 conveniently integrated. It is observed that the results are equivalent when the
178 concentration is less than 0.25 mol/L, however, the bubble size continues to decrease above
179 0.50 mol/L. These observations do not allow to recognize the transition and stability of the
180 bubble sizes in the presence of KI. The interpretation of the results suggests that the effects
181 that retard the bubble coalescence mechanism increase according to the presence of the
182 electrolytes in the following order: KI <NaCl <MgCl2 <Na2SO4. In the presence of KI the
183 bubbles lose spherical shape and rise at high speeds. As a result, during flotation, these
184 bubbles have a low probability of collecting valuable material (see Fig. 2 (b)). In the
185 presence of Na2SO4 (NaCl and MgCl2) multiple, fine, rigid bubbles are observed as spheres
186 traveling slowly (see Fig. 2(c)). These bubble sizes favor the likelihood of collision,
187 adhesion and the stable transport of valuable material into the concentrate.
188

5
189
190

191
192

193
194 Figure 2. (a) Impact of the type and concentration of salt on the bubble size, the average
195 Sauter diameter is reported. Data from Marrucci and Nicodemo [17] are included to
196 explain the effect of potassium iodide. (b) Experimental observations of the bubbles in

6
197 the presence of KI at 0.50 M. (C) Experimental observations of the bubbles in the
198 presence of Na2SO4 at 0.50 M.
199
200 3.2. Distribution of bubble sizes in water-air-solid systems
201 Fig. 3(a) illustrates the behavior of the bubbles in the collection zone in the presence of
202 coal particles. The effect of the electrolytes on the bubble size is equivalent to the
203 observations in the water-air system (Fig. 2a), when the ionic strength increases the bubble
204 size decreases. However, in the presence of solids the size of the bubbles increases slightly
205 [19].
206 The solution of KI and deionized water relates the presence of large bubbles between 1 and
207 6 mm. The experimental evidence from Fig. 3(b) indicates that bubbles are limited to
208 transport material. In contrast, solutions of NaCl, Na2SO4 and MgCl2 link up bubbles
209 between 0.5 and 3.0 mm. The experimental observations of Fig. 3(c) indicate that the
210 charge of the bubbles is remarkable. The analysis of the data suggests that the presence of
211 electrolytes increases the metallurgical performance in terms of the C/F concentration ratio
212 in the following order: KI <Na2SO4 <NaCl <MgCl2.
213

214
215

216

7
217
218 Figure 3. (a) Distribution of bubble sizes in the presence of solids; the 0.5 M
219 concentration of the solutions of KI, NaCl, Na2SO4 and MgCl2. (b) In the presence of KI,
220 the bubbles carry light loads of material. (C) In the presence of MgCl2, the bubbles carry
221 significant material loads.
222
223 3.3. Recovery of coal
224 Fig. 4 indicates that the recovery of coal increases as a function of the molar concentration
225 of the electrolytes, except for the Na2SO4 that has an inverse effect. The theory indicates
226 that the hydrophobicity of coal increases substantially in the presence of pure water [5].
227 Most of the experimental results reported in the literature illustrate the opposite [8,20]. The
228 results of the present work indicate that the recovery of coal with deionized water is 40%,
229 significantly lower in comparison with the solutions of KI, NaCl and MgCl2. Thus, it is
230 possible to associate that NaCl and MgCl2 solutions promote recoveries between 53 and
231 89% while KI solution promotes lower recoveries, between 44 and 69%.
232

233

8
234 Figure 4. Recovery of fuel according to the type and concentration of salt; the effect of deionized
235 water is also included.
236
237 The theory of Paulson and Pugh [3] recognizes that the electrostatic force undergoing an
238 air bubble and a coal particle is repulsive. Both interfaces are negative at natural pH [4].
239 However, the particular presence of the Na+ and Mg2+ cations significantly influences the
240 electro-kinetic behavior of the bubbles and particles (the magnitude of the zeta potential of
241 the bubble and the particle is reduced). The adsorption of these cations on the surface of
242 the coal acts in such a way that the electrostatic repulsion force decreases and allows the
243 hydrophobic forces to control the bubble-particle interaction [21]. This theory explains the
244 recoveries that are achieved in the presence of NaCl and MgCl2. However, this hypothesis
245 does not justify the recovery of hydrophilic minerals that intensifies in the presence of
246 Na2SO4, as shown in Fig. 5. The analysis of the data suggests that the ash content increases
247 in the concentrate as a function of the ionic strength. Mineral matter includes quartz,
248 kaolinite, pyrite, vermiculite and calcite. The results are illustrated in Fig. 6.
249

250
251 Figure 5. Ash recovery depending on the type and concentration of salt; the effect of deionized
252 water is also included.
253

9
254
255 Figure 6. XRD results of ashes.
256
257 3.4. Recovery of mineral matter
258 In the recovery of mineral matter the participation of the mechanical drag is significant.
259 The mechanical drag is related to the formation of a monolayer of water that covers the
260 bubble and moves along with it. This allows the formation of an interstitial liquid network
261 or water flow that forms between the air bubbles and ascends to the froth zone. As the
262 water flow in the froth zone increases, the entrainment of hydrophilic particles intensifies.
263 That is, the water flow in the froth zone is inversely proportional to the bubble size in the
264 collection zone [22]. The analysis of Fig. 7 suggests that high ionic strength increases the
265 total surface area of the bubble [23] which is represented in terms of the concept of Sb [24].
266 It was observed that potassium iodide is related to low levels of Sb, between 32 and 36 s-1,
267 while sodium sulfate reaches the highest levels, compared to the rest of the electrolytes,
268 between 48 and 90 s-1. When Sb increases, the probability of collecting hydrophobic
269 particles increases. However, to the same extent, it is possible to increase the recovery of
270 water and therefore the recovery of minerals through the mechanical drag [25]. This means
271 that the presence of sodium sulfate has arguments for enhancing the recovery of mineral
272 matter by means of the bubble surface flux density (Sb). Fig. 8 indicates that the presence
273 of total iron in the concentrate increases in the presence of Na2SO4 and decreases in the
274 presence of deionized water. The analysis of the data suggests to integrate the concept of
275 Sb as an appropriate element in the understanding of the recovery of mineral matter.
276 However, the behavior of MgCl2 does not coincide with this hypothesis. In contrast, under
277 equivalent magnitudes of Sb, the presence of MgCl2 favors the recovery of coal particles.
278 Fundamental studies indicate that inorganic species dissolved in water interact with the
279 dispersion of particles, bubbles, and small droplets of collector (gasoil) in a flotation system
280 [9]. The presence of electrolytes in the mineral pulp motivates the neutralization of the
281 surface charges of the coal particles and eliminates electrostatic repulsions. This allows the
282 particle/particle collision to be intensified by the effect of the hydrophobic forces
283 prevailing in the system. The particles form an aggregate because they remain adhered after
284 colliding, under these conditions entrapment of mineral matter takes place. The ash is
285 occluded in the aggregate of coal particles. However, Wang and Peng [8] indicate that the

10
286 recovery of mineral matter is associated with the entrapment of particles smaller than 38
287 μm when the concentration of Na+ and SO42- ions is greater than 20 g/L. This observation
288 coincides with the results of Fig. 9, the effect of Na2SO4 concentrates particles smaller than
289 36 μm. However, the impact of MgCl2 is equivalent, this observation indicates that the
290 recovery of coal and mineral matter (ash, gangue) does not depend only on the presence of
291 fine particles [8]. Thus, Fig. 9 suggests that the particle size distribution increases
292 proportionally with the bubble size. That is, bubble sizes between 0.80 and 0.90 mm carry
293 particles smaller than 36 μm, while bubbles between 3.0 and 3.3 mm carry particles smaller
294 than 100 μm.
295

296
297 Figure 7. Surface flow of the bubble as a function of the bubble size represented by the Sauter
298 diameter.
299

11
300
301 Figure 8. Behavior of the total Fe concentration in the ashes when the concentration of Na2SO4
302 increases.
303

304
305 Figure 9. Distribution of particle sizes in the concentrate of 0.50 M.
306
307 4. Conclusions
308 Based on the results obtained in the present work, it was observed that the presence of Na+,
309 Mg2+, SO42- and Cl- ions dissolved in the water favors the formation of fine bubbles. The
310 effect is similar to that of an industrial frother. In contrast, the ions of K+ and I- favor the
311 presence of large bubbles. Thus, it is recognized that the concentration of transition is lower

12
312 in solutions containing ions of different charge (e.g., Mg2+, Cl-), compared to solutions with
313 monovalent ions (e.g., K+, I-). The analysis of the data allowed to find a correlation between
314 the size of the bubble and the ionic strength. These observations are important for froth
315 flotation, because it makes it possible to tentatively strengthen the control of air bubbles.
316 The results also suggest that increasing the concentration of Na+, Mg2+ and Cl- ions, the
317 recovery of coal ore increases, while the recovery decreases with the presence of K+ and I-
318 ions. However, in particular, it was identified that the presence of Na+ and SO42- ions is
319 associated with high recoveries of mineral matter, which are undoubtedly due to the nature
320 of the anion. The use of water with high concentrations of metals and anions represents an
321 important reason for considering the effect of bubble size on the flotation of coal particles.
322
323 Acknowledgment
324 The author thanks the mineral processing laboratory of the School of Mining Engineering,
325 University College of Engineering, University of Tehran for the service provided during the
326 characterization of the mineral samples, especially the Engineer Ali Ghorbani. Likewise, the
327 author is grateful for the support received from School of Mining, Petroleum & Geophysics
328 Engineering, Shahrood University of Technology.
329
330 Nomenclature
331 Ac Ash content in the concentrate stream (%)
332 Af Ash content in the feed stream (%)
333 At Cross-sectional area of the flotation cell (cm2)
334 C/F Metallurgical efficiency (%)
335 db Bubble diameter (mm)
336 di Equivalent diameter (mm)
337 d32 Sauter diameter (mm)
338 Jg Surface air velocity (cm/s)
339 Mc Mass of the concentrate (g)
340 Mf Mass of feed (g)
341 R Fuel recovery (%)
342 Sb Surface bubble flow (s-1)
343 Qg Volumetric flow of air (cm3/s)
344
345 References
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347 http://www.eacmco.ir/default.aspx.
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351 solutions of inorganic electrolytes,” Langmuir, 12, 4808-4813, 1996.
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