Minerals Engineering 17 (2004) 847853 This article is also available online at: www.elsevier.

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Assessment of true otation and entrainment in the otation of submicron particles by ne bubbles
P. George, A.V. Nguyen, G.J. Jameson
Received 27 December 2003; accepted 4 February 2004

Special Research Centre for Multiphase Processes, University of Newcastle, University Drive, Callaghan, NSW 2308, Australia

Abstract Entrainment can make an important contribution to recovery in the otation of ne particles. This paper presents an experimental study into the recovery by true otation and by entrainment, of colloidal silica and alumina particles with a size range from 40 to 160 nm in diameter. The otation experiments were carried out in a small laboratory column-type cell with ne bubbles with typical average diameter of about 150 lm. No wash water was used. Cetyltrimethylammonium bromide and Dowfroth 250 were used as the collector and frother, respectively. The particle concentration in the pulp was about 1% by weight. In these experiments the total recovery of particles was low, typically 54% after 50 min. Four techniques, including three previously described in the literature and one newly developed in this study, were used to assess the true otation due to the bubble-particle collection mechanism, and the entrainment. All employed techniques show that the proportion of the colloidal particles recovered by true otation was quite high, varying from about 7986% of the total recovery. The paper also discusses the mechanisms of minimising the entrainment of the colloidal particles in the laminar ow otation regime with ne bubbles. 2004 Published by Elsevier Ltd.
Keywords: Froth otation; Fine particle processing; Flotation kinetics; Flotation bubbles; Flotation froths; Entrainment

1. Introduction The advances currently being made in grinding technology are allowing large, complex low-grade mineral deposits to be exploited economically. The continual reduction in grade is forcing miners to produce ultrane particles in order to liberate mineral particles from the ore, e.g. the McArthur River and Century Zinc precious metal deposits (Potts, 2003). The horizontal Isamill (MIM Process Technologies, Brisbane, Queensland, Australia) is capable of grinding to P80 of )4 lm at the McArthur River mine (Weller and Gao, 2003). To fully exploit these deposits, however, considerable research needs to take place in the area of ultrane particle otation. While the optimum P80 of many ores is substantially less than 10 lm, the optimum particle size for otation still ranges between 10 and 100 lm in diameter (Jameson, 1984).

Corresponding author. Tel.: +61-2-4921-6181; fax: +61-2-49601445. E-mail address: graeme.jameson@newcastle.edu.au (G.J. Jameson). 0892-6875/$ - see front matter 2004 Published by Elsevier Ltd. doi:10.1016/j.mineng.2004.02.002

Techniques such as carrier otation, agglomerate otation, emulsion otation and oil-in-water otation have been suggested as ways of increasing the otation rates of ultranes. All of these methods have their shortfalls and none have been very widely applicable. These processes have been discussed and reviewed elsewhere (Fuerstenau, 1980). It is widely agreed, however, that advances in ultrane otation technology through modications to well-established surface-based methods is better than developing entirely new processes (Sivamohan, 1990). The recovery of ne particles is a function of true otation, entrainment and entrapment. The entrapment of particles occurs in a poly-disperse system with ne particles becoming trapped amongst agglomerates of coarser particles or trapped amongst agglomerates of coarser particles and bubbles. The recovery of ne particles is thus a function of true otation and entrainment only, when no coarse particles are added to the system. The process of true otation occurs when a particle collides with a rising bubble and is attached to its surface. The selected particle is then removed from the cell as part of the froth. On the other hand, particle

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entrainment occurs when particles are dragged from the pulp into the froth in the interstitial liquid. While true otation is a selective process, capture of particles in the interstitial liquid is non-selective. For a system, of mixed species, a high level of particle entrainment will result in a low-grade product. It has been a long held view that the predominant capture mechanism for ultrane particles is entrainment (Fuerstenau, 1980). While this may be true for many systems requiring a high selectivity, no study has been completed to examine particle entrainment of colloidal particles oating alone. The aim of this study is to assess the level of particle entrainment and true otation in a system involving colloidal silica and alumina particles. A novel technique for measuring the entrainment of colloidal particles is also introduced.

Collector

Solids Recovered (%)

Mass recovered by true flotation No Collector

Water Recovered (%)

Fig. 1. Illustration of the determination of true otation by method of Trahar and Warren (1976).

2. Review of methods and techniques A number of techniques have been developed to evaluate the level of true otation and entrainment. A brief summary of these methods is given below. 2.1. Method of Trahar The rst technique was proposed by Trahar and Warren (1976) and compares the water and solids recovery for two otation experiments. The rst experiment involves a suspension with both a collector and a frother added, while the second involves just a frother. It is assumed that all the particles captured in the froth with no collector added, will be by entrainment only. The dierence between the solids recovered versus water recovered, for the collector and non-collector tests, gives an estimate of the mass recovered by true otation. A schematic representation of this method was given by Subrahmanyam and Forssberg (1988), and is shown in Fig. 1. This rst method assumes that entrainment occurs only when a frother is present. It was argued by Trahar (1981) that ne particles require only a low hydrophobicity, compared to coarser particles, to be captured by the true otation process. Hence, Ross (1991) recommended that Trahars method would be applicable in the otation of coarser particles with a high natural hydrophobicity. Despite this recommendation, it must be pointed out that a bubble in distilled, deionised water has a residual negative zeta potential (Creux, 2000). Assuming the addition of a frothing agent does not alter the surface charge on the bubble, ne particles with a negative surface charge (such as silica) should not attach to the surface of a bubble without the addition of a cationic collecting agent. Thus in the absence of a cationic col-

lector, silica particles will be recovered by entrainment alone. 2.2. Method of Warren A second technique, proposed by Warren (1985), assumes that particle entrainment does not take place in a dry froth. A series of experiments are conducted and the rate of water recovery varied by changing the rate of froth removal and froth depth. A regression line for the relationship between total solids recovery and water recovery is extrapolated to a zero water recovery. The mass of solids recovered at this point is the recovery by true otation alone. This technique may be summarized as Rt F eW t 1 where Rt and W t are the recoveries of the mineral (by true otation and entrainment) and water, respectively, as a function of time, t. F is the recovery due to true otation. The degree of entrainment, e, is equal to the slope of Rt versus W t. A schematic representation of this technique is given in Fig. 2. 2.3. Method of Ross and Van Deventer A third method, attributed to Ross and Van Deventer (1988), assumes the concentration of entrained particles in the froth and concentrate is identical to the concentration of particles in the pulp. Hence, the recovery by entrainment can be estimated by multiplying the mass of water recovered in the froth by the concentration of the pulp, at that time. This method can estimate the rate of otation with a single otation test. Balancing the otation recoveries gives R t F Re t 2 where Rt is the (overall) recovery of the mineral by true otation and entrainment and F is the recovery by true

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Hydrophobic particles

Solids Recovered (%)

Solids Recovered (%)

Slope,e

Mass recovered by true flotation Hydrophilic particles

True flotation recovery,F

Water Recovered (%)

Fig. 2. Determination of true otation by method of Warren (1985). Fig. 3. Determination of true otation by the hydrophobichydrophilic particle method.

otation. The recovery due to entrainment, Re t, is related to the water recovery, W t and the initial concentration, C , of the mineral species in the pulp by Re t W tC bt 3 where b is the slope of the graph of the mineral concentration remaining in the pulp phase versus time, t. Substituting Eq. (3) into Eq. (2) gives F Rt W tC bt 2.4. New method A fourth method is now described, which involves two separate otation tests using dierent colloidal species of equal size. The two species chosen were silica and alumina. The silica, which is naturally negativelycharged, is rendered hydrophobic in the otation suspension by the attachment of a cationic surfactant. In contrast, the alumina particles carry a positive charge, and does not adsorb the cationic collector. Thus in separate otation experiments involving a single species, if the solids are conditioned identically with a cationic collector and a frother, the silica will oat by true otation and entrainment, while alumina will be recovered only by entrainment in the froth. Thus the dierence in recovery between the two experiments gives a measure of the true otation of the hydrophobic species, in this case, the silica. This procedure has a number of advantages over the previously discussed methods, principally related to the eect of the reagents on the bubble size distribution and the froth properties. The technique of Trahar and Warren (1976) requires some tests in the absence of a collector; which has an eect on the bubble size distribution, and hence on liquid entrainment in the froth, and froth drainage and stability. The new procedure is more convenient than the Warren (1985) method which requires many otation tests to be conducted (Fig. 3). 4

3. Experimental Batch-wise otation tests were carried out in a 1 l column-type cell of internal diameter 70 mm and of height variable in the range 305405 mm. Bubbles are produced by introducing gas through a ne frit sparger in the bottom of the column. Nitrogen gas was sparged through 68 mm pyrex glass sintered disc of porosity three (Corning Ltd, Artington, Surrey, UK), to produce an average bubble diameter, determined photographically, of 150 lm. The volumetric gas ow rate was 80 cm3 /min. The height of the froth phase was 285 mm and was maintained by a constant feed of otation solution from a large diameter feed tank. A 10 ml sample was taken from the pulp every ve minutes to determine the concentration change with time. The froth was collected, dried and weighed. A mass balance was performed around the cell and the overall recovery determined. The total recovery was calculated by dividing the cumulative mass of particles recovered in the froth by the initial mass of particles in the otation cell. Tests were done using each of the four procedures described above, in triplicate, with a total of twenty ve otation tests being performed. The particles used in the otation tests were silica and alumina. The silica suspension was composed of 1.5% Snowtex ZL and 0.5% Snowtex 20 L (Nyacol Chemical America Corporation, Houston, Texas, USA). The particle size distribution of this suspension, determined using transmission electron microscopy, was found to range from 40 to 160 nm. The transmission electron micrographs were taken using a JEM-1200EX11 transmission electron microscope (Jeol USA, Peabody, Massachusetts, USA). The alumina suspension was composed of 0.6% AKP-50 particles (Sumitomo Chemicals, Tokyo, Japan). The AKP-50 particles have a mean particle diameter of 150 nm, determined using an Accoustosizer IIs (Colloidal Dynamics, Warwick, Rhode Island, USA).

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Prior to conditioning, the alumina and silica particles were dispersed at 100 W power for 5 min using a Sonicator 3000 (Misonix incorporated, Farmingdale, New York, USA). Since the rate of otation is a function of particle size, the zeta potentials of the particles were checked to ensure that the charge they carried was sufcient to ensure a stable suspension. For a quiescent colloidal pulp a zeta-potential at the mineral interface greater than 25 mV absolute is generally indicative of dispersion (Ross and Long, 1969). The zeta potential was assessed using a ZetaPlus apparatus (Brookhaven Instrument Corporation, Holtsville, New York, USA). The zeta potential was )35 mV for the silica particles and +34 mV for the alumina particles. The pH was measured as 9.25 and 6.31 for the silica and alumina suspensions, respectively. A settling test was performed over a 24 h period, for each suspension, and no sign of settling occurred. Hence, the suspensions were assumed to be fully dispersed. The frother used in the experiments was Dowfroth 250 (Dow Chemical Corporation, Ludington, Michigan, USA) at a concentration of 30 ppm. The collector used during the experimental tests was cetyltrimethyl ammonium bromide (CTAB) (Ajax Chemicals, Sydney, Australia) at a concentration of 5 105 M. In these experiments the total recovery of particles was low, typically 54% after 50 min. 4. Results and discussion 4.1. Results obtained by the technique of Trahar The solids recovered versus water recovered, for a system with and without collector, obtained for silica particles with the method of Trahar and Warren (1976) is shown in Fig. 4. The collector CTAB, was added to render the surface of the silica hydrophobic, to enable the particles to be captured by true otation. It is assumed that particle entrainment is the only method for
50

particle capture when no collector is added. The dierence in overall solids recovery for otation froths, with and without collector, for a xed water recovery, gives a measure of the true otation taking place. Fig. 4 indicates that the overall water recovery decreased as the froth height increased. As the drainage of liquid from the foam increased, so did the proportion of particles captured by true otation. The total fraction of particles recovered by true otation was determined to be 76% 3% for a 20 mm froth height and 83% 3% for a froth height of 120 mm. One benet of Trahars method over that of Warren (1985), is that only two otation tests are required to estimate the level of true otation taking place. It must be noted however that the froth character changed substantially when the CTAB collector was added. For the system with no collecting agent, no particles were captured by true otation and hence the concentration of particles remaining in the interstitial liquid increased. An increase in particle concentration causes a linear increase in the eective uid viscosity (Einstein, 1906). Hence the rate of drainage from the froth decreased signicantly. This low rate of drainage ensured the froth remained wet with small bubble sizes and mobile interfaces, accordingly. 4.2. Results obtained by the technique of Warren The rates of true otation and entrainment were assessed using the technique of Warren (1985). A plot of the recovery of silica particles versus overall water recovery, obtained with CTAB collector, is given in Fig. 5. The overall water recovery was changed for each test by altering the froth depth from between 20 and 120 mm in height. The procedure of Warren assumes that entrainment occurs when particles are transported in the interstitial liquid. When the line of best t is extrapolated to zero water recovery, for a 60 mm froth height, the intercept suggests that over 79% 2% of the solids are recovered
45

Solidids Recovered (%)

40 30 20 10 0 0 5

Solids Recovery (%)

20

20mm FH 40mm FH 100mm FH NoCollector

30mm FH 60mm FH 120mm FH

35

25

10

15

Water Recovered (%)

15

Fig. 4. Recoveries of silica particles versus water recovery obtained with and without collector by the technique of Trahar and Warren (1976). The numbers in the legend shows the froth heights (FH) and the data obtained with CTAB. During the experiment in the absence of the collector the froth height was maintained at 60 mm.

Water Recovery (%)

Fig. 5. Recovery of silica particles versus water recovery obtained after 20 min of otation, using the technique of Warren (1985).

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by true otation. The overall recovery for the 120 mm froth height is 26% 2%, indicating that around 75% 9% of all recovered particles are captured by true otation. When the test is performed for a froth height of 20 mm, over 32% 6% of all particles are recovered, revealing around 66% 1% are captured by true otation. The reduction in recovery as the froth depth increases is presumably due to coalescence of the bubbles, as the froth drains while rising up the column. This labor-intensive method requires many otation tests to be carried out to obtain an accurate estimate of the true otation and entrainment rates. Tests must be conducted with a wide range of froth heights, to obtain a range of water recoveries. As the froth height is increased the character of the froth changes. The upper layers of the froth in the column tend to be drier than those at the bottom. For a three-phase system, the bubble size increases signicantly as coalescence takes place in the froth. This coalescence improves froth grade by dislodging entrapped particles and detaching weakly held true otation particles. Hence the problem of the Warren (1985) technique is that it does not distinguish between particles captured by true otation in the pulp and improvements made in the froth. 4.3. Results obtained by the technique of Ross and Van Deventer A otation test was performed for a froth height of 60 mm and a mass balance was completed around the cell. The technique of Ross and Van Deventer (1988) was used to estimate the rate of entrainment and true otation. The otation test was performed over 28 min and the results for recovery are shown in Fig. 6. In this technique, it is assumed that the concentration of entrained particles in the interstitial liquid is the same as the concentration of particles in the pulp. Flotation tests were performed with froth heights ranging from 20 to 120 mm. The level of true otation was determined using Eq. (4). The true otation was found, using the
60 50 Overall Flotation True Flotation Entrainment

Ross and Van Deventer (1988) technique, to account for between 75% 3% and 85% 1% of all particles oated. A mass balance was performed around the otation cell and only 3% of the silica was unaccounted for. The linear behaviour of the recovery curve is due to the low overall recovery of solids, to be expected in the otation of particles of the size used here. Total recovery could have been increased by increasing the otation time, or the gas owrate. The recovery can also be enhanced by using another frother capable of forming ner bubble sizes in the pulp. A preliminary test revealed that reagent-grade ethanol at 0.5% concentration, in conjunction with CTAB, was capable of achieving an overall recovery greater than 85% after 20 min of otation. However, ethanol is unable to form a stable froth when no collector is added. Hence Dowfroth 250 was chosen as the preferred frothing agent as it was able to produce stable froth with and without collector and could be used to examine all four models. 4.4. Results obtained by the new technique This technique involved comparing the otation of hydrophilic alumina particles, against a system of hydrophobised silica particles, conditioned with the same reagents. The addition of the cationic collector, 30 ppm CTAB, rendered the silica hydrophobic while leaving the alumina particles hydrophilic in the slurry. Hence, all particles captured during the otation of alumina with a cationic surfactant were entrained. The otation tests were carried out at a 60 mm froth height. The overall solids recovered versus water recovered, for a system with hydrophobic silica and a system with hydrophilic alumina is given in Fig. 7. This technique indicates that true otation accounts for 82% 3% of all the particles recovered for a 60 mm froth height. This gure compares to 86% 3% using the technique of Ross and Van Deventer (1988), 79% 2% using the technique of Warren (1985) and 82% 3% using the technique of Trahar and Warren (1976). One

70

Solids Recovery (%)

Recovery (%)

60

Silica
50 40 30 20 10 0 0 2 4 6 8 10 12 14

40 30 20 10 0 0

Alumina

10

20

30

40

50

60

Water Recovery (%)

Fig. 7. Recoveries of hydrophobised silica particles by true otation and of hydrophilic alumina particle by entrainment using the hydrophobichydrophilic particle technique.

Flotation Time (minutes)

Fig. 6. Recoveries by true otation and entrainment obtained with the technique of Ross and Van Deventer (1988).

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possible diculty with this technique, however, is that it does not take account of dierent particle morphologies. A particle with angular surfaces has a higher specic surface energy (Fuerstenau, 1980) and is more able to attach to a bubble surface upon collision. The silica and alumina particles were both examined under a transmission electron microscope and the morphology was shown to be markedly dierent. The silica particles, formed by precipitation, had a uniform spherical shape, where as the alumina particles were very angular. The eect of the morphology of the hydrophilic solids on liquid entrainment and drainage in the froth is not known. 4.5. Mechanisms of minimising the entrainment of colloidal particles in the laminar ow otation regime with ne bubbles The recovery of colloidal silica by true otation was found to be very high ranging between 79% and 86%, depending on the technique used to measure this value. This is a very signicant portion considering the froth height was only 60 mm and no wash-water was added to ush the mechanically entrained particles back into the pulp. It is known that the entrained particles can enter the pulp-froth interface by the pulp agitation (mechanical entrainment), and/or by the bubble wake and the bubble swarm (crowding) eects (hydraulic entrainment). Since no mechanical agitation was used in our experiments, the contribution of mechanical entrainment was insignicant. The formation of a wake behind a rising bubble is limited by the hydrodynamic conditions. The wake volume is a function of the velocity, U , of the bubble rise, the bubble radius, Rb , and the liquid viscosity, l, and density, q. The wake volume decreases with decreasing the bubble Reynolds number, Re 2qRb U =l (Batchelor, 1967; Clift et al., 1978). Indeed, Miyahara et al. have reported that bubbles rising with a Reynolds number between 600 and 5000 form a helical vortex wake with a wake-to-bubble volume ratio of 2.5. The bubbles rising with a Reynolds number greater than 5000 form a symmetrical wake with a wake-to-bubble volume diameter of 4.7 (Miyahara et al., 1988). In this work the numerical computation uid dynamics (CFD) program (FLUENT, Fluent Inc., Lebanon, New Hampshire, USA) was used to study the wake formation behind rising bubbles. An example for the liquid streamlines and the wake is shown in Fig. 8. The numerical study shows that no wake can be formed if the bubble Reynolds number is smaller than about 20. The wake volume, Volw , can be correlated with the bubble volume, Volb , and the Reynolds number. The following correlation was empirically obtained from the numerical data: Volw Volb 0:045Re0:649 0:314 20 6 Re 6 400 5 Therefore the reduction in the bubble diameter signicantly reduces the size of the associated wake, by
Fig. 8. CFD simulation of the formation of wakes travelling with a rising bubble with Re 50. The lines show the liquid streamlines passing the bubble.

reducing the Reynolds number and terminal velocity. The reduction in the size of the wake in-turn reduces the number of ne particles captured behind the bubble which are later transferred hydraulically to the froth. For ne bubbles with a mean diameter of 150 lm, produced in this study by sparging nitrogen gas through a ne glass frit, the rise velocity determined by the available predictions (Nguyen, 1998) is about 16 mm/s, and the bubble Reynolds number is about 3. Clearly, for such small Reynolds numbers the entrainment due to the bubble wake mechanism is insignicant and can be neglected in our experiments. However, when bubbles of the size generated in mechanical cells are used, typically 13 mm in diameter, entrainment of solids in the wakes of the bubbles could be very signicant. The small degree of entrainment in the otation tests can be due to the bubble swarm crowding eect, which is a function of the bubble concentration. In otation cells, bubbles rise through the pulp, slow down as they approach the pulp-froth interface and then crowd together at the interface. The liquid cannot be rapidly squeezed out between the rising swarm of bubbles, due to the restricted paths for drainage through the bubble swarm. As each layer crosses the interface, another layer of bubbles will form and push more liquid upwards in a continuous process and entrain particles into the froth phase. Further work needs to be conducted relating entrainment rates to the bubble size and gas holdup in order to verify this mechanism. 5. Conclusion Batch otation tests were conducted in a small laboratory column-type cell using ne bubbles to assess the rate of true otation and entrainment using four dierent techniques. The four techniques employed were those of Trahar and Warren (1976), Warren (1985), Ross and Van Deventer (1988), and the new hydrophilichydrophobic particle technique introduced here. Tests were conducted in triplicate with a total of twenty ve ota-

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tion tests being performed. The average bubbles size of sparged nitrogen was 150 lm. A 1% suspension of silica particles ranging in diameter from 40 to 150 nm was used as the oatable species, while alumina particles with a d50 of 150 nm were used as the hydrophilic species. A mass balance was performed around the cell for each test and the level of true otation and entrainment determined. The level of true otation and entrainment was found to vary linearly with froth height. The true otation was found to account for 76% 3% of all silica particles recovered for a froth height of 20 mm, and over 83% 3% for a froth height of 120 mm, using the technique of Trahar and Warren (1976). This indicates that the proportion of particles captured by entrainment is relatively small, despite the absence of any wash-water. The four techniques were compared and were found to reveal highly consistent results. For a constant 60 mm froth height, the level of true otation was found to be 82% 3% for the method of Trahar and Warren (1976), 79% 2% for the method of Warren (1985), 86% 3% for the method of Ross and Van Deventer (1988), and 82% 3% for the method of hydrophilichydrophobic particles. Each of these techniques has their drawbacks including changing froth structure for the methods of Warren (1985), Trahar and Warren (1976) and the hydrophilichydrophobic particle technique. The changing particle morphology and surface chemistry for the hydrophilichydrophobic technique aects the measured rate of entrainment, along with changing particle concentrations in the interstitial liquid for the Ross and Van Deventer (1988) method. The high eciency of true otation obtained with colloidal silica is due to the ne bubble size, 150 um, used in the experiments. As the bubble collides with the froth it rapidly decelerates causing the particles entrained in its wake to wash over its surface and entrain hydraulically into the froth. A smaller bubble size has a smaller associated wake and hence fewer particles are entrained into the froth. Acknowledgements The authors gratefully acknowledge the nancial support of the Australian Research Council.

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