Minerals Engineering 98 (2016) 122–126 Contents lists available at ScienceDirect Minerals Engineering journal homepage: www.elsevier.com/locate/mineng Acoustic measurement of the bubble Sauter mean diameter d32 W. Kracht ⇑, C. Moraga a b Department of Mining Engineering, Universidad de Chile, Chile Advanced Mining Technology Center, AMTC, Universidad de Chile, Chile a r t i c l e i n f o Article history: Received 7 February 2016 Revised 16 July 2016 Accepted 1 August 2016 Available online 9 August 2016 Keywords: Flotation Bubble Sauter mean diameter Measurement Acoustic technique a b s t r a c t The importance of gas dispersion variables on the flotation process has led to the development of techniques that allow measuring and monitoring them in flotation. In the case of bubble size, the most used methods are based on image analysis and, although these methods are well accepted, they have not been implemented to monitor the flotation process on a regular basis, mainly because they are labor intensive, require the manipulation of a well trained operator, and are difficult to automate. In the current work, an acoustic technique for measuring the bubble Sauter mean diameter, d32, is introduced. The technique is based on the response of bubbles to an acoustic perturbation consisting of a modulated signal with frequencies F1 ± F2, where F1 acts as a carrier set at 1 MHz, and F2 corresponds to the modulating signal that varies from 1 kHz to 10 kHz. A linear empirical relation was found between the average intensity of the acoustic response of the bubbles, Imean, and d32, which allows determining the bubble Sauter mean diameter for a wide range of sizes, from 0.75 to 3 mm, covering the range of interest of flotation. The acoustic method represents an alternative to the image analysis technique as a sensor to monitor the flotation process, however, it still depends on image analysis as an independent method for calibration. Ó 2016 Elsevier Ltd. All rights reserved. 1. Introduction It is well known that flotation performance is affected by the gas dispersion in the flotation cell (Schwarz and Alexander, 2006; Nesset et al., 2006), which is characterised by the variables (Gomez and Finch, 2007): superficial gas velocity, Jg, gas holdup, eg, bubble size distribution, with the bubble Sauter mean diameter, d32, and derived variables such as the bubble surface area flux, Sb ¼ 6J g =d32 , or the specific surface area, Ab ¼ 6eg =d32 . The bubble surface area flux is directly related to the flotation rate constant (Gorain et al., 1997), and can be either estimated (Gorain et al., 1999) or calculated, given that both Jg and d32 are known. Among the available techniques for measuring bubble size (Randall et al., 1989; Grau and Heiskanen, 2002), the most used is the McGill Bubble Size Analyser (MBSA) (Hernandez-Aguilar et al., 2002; Gomez and Finch, 2007), which is a samplingfollowed-by-imaging technique. It consists of a sampling tube that allows bubbles rising towards a sealed viewing chamber, also known as bubble viewer, where pictures are taken. The pictures are then analysed to yield bubble size data. Although the MBSA has been widely used, and some of its issues have been addressed ⇑ Corresponding author at: Department of Mining Engineering, Universidad de Chile, Av. Tupper 2069, Santiago, Chile. E-mail address: [email protected] (W. Kracht). http://dx.doi.org/10.1016/j.mineng.2016.08.001 0892-6875/Ó 2016 Elsevier Ltd. All rights reserved. (Zhang et al., 2009; Kracht et al., 2013), it still has some limitations. In particular, the need for replacing the water inside the bubble viewer between measurements makes it difficult to implement the MBSA as a sensor to monitor the process; therefore, so far it has been used mainly as a diagnostic tool. Acoustic emissions represent an alternative to monitor gasliquid dispersions. There are two kind of methods that can be implemented (Boyd and Varley, 2001): passive measurements, where what is measured is the acoustic signal, sound or ultrasound, generated by the process itself; and active measurements, which rely on the response of the process to a transmitted acoustic wave, usually low powered ultrasound. When a bubble is formed, its surface oscillates (pulsates), which perturbs the surrounding water, and a sound wave propagates through water in all directions (Dawson, 2002). The sound generated by bubbles was first studied by Minnaert (1933), who determined the relationship between bubble sizes and their natural frequency of oscillation. As shown by Leighton and Walton (1987), bubbles behave like lightly damped simple harmonic oscillators that oscillate at the frequency determined by Minnaert. Bubbles oscillate at their natural frequency when they form or coalesce (Strasberg, 1956; Manasseh et al., 2001; Manasseh et al., 2008; Ajbar et al., 2009; Kracht and Finch, 2009; Kracht and Rebolledo, 2013), and also when they are excited by an external source such as ultrasound (Leighton, 1994). It has been established that, when W. Kracht, C. Moraga / Minerals Engineering 98 (2016) 122–126 123 exposed to two signals of high (ultrasound) and low frequency, F1 and F2, the bubbles couple both fields and return, as a result, a signal with frequencies F1 ± F2 (Leighton et al., 1996; Buckey et al., 2005). The dual-frequency approach is used in the current work to measure bubble Sauter mean diameter, d32, in the range of bubble sizes of flotation systems. 2. Experimental 2.1. Sampling process The technique consists of sampling bubbles from the flotation cell, exposing them to an acoustic perturbation, and analysing their response. A schematic of the sampling procedure is shown in Fig. 1. Bubbles are sampled from the cell with a 1/2 in sampling tube connected to an acoustic chamber made of transparent acrylic, and equipped with two transducers (Reson TC3027) to perform the measurements. The transparent acoustic chamber allows for bubble images to be taken, which are later analysed to yield bubble size as an independent method of measuring d32. In order to allow for continuous sampling, and to keep the acoustic chamber full of water, the chamber is connected to a peristaltic pump that sucks water and bubbles, returning the sample to the flotation cell. The measurement can be automated in such a way that no operator is needed. The dimensions of the acoustic chamber are: 35 cm height, 24 cm width, and 20 cm depth. The actual acoustic chamber can be seen in Fig. 2. Fig. 2. Acoustic chamber showing transducers. 2.2. Acoustic technique As the bubbles pass through the acoustic chamber, they are exposed to a modulated signal produced with two function generators, each of them generating a sinusoidal signal, but of different frequencies: a carrier signal, which corresponds to an ultrasound frequency, F1, and a modulating signal, of lower frequency, F2 (Fig. 3). The two signals are mixed to obtain a modulated signal with frequencies F1 ± F2 that is transmitted to the water and bubbles inside the acoustic chamber by one of the transducers that acts as a transmitter. In order to transmit only the frequencies F1 ± F2, it is necessary to suppress the carrier signal during the modulation. This is done by using a modulator (Motorola MC1496) with carrier suppression as the one shown in Fig. 4. The bubbles respond to the transmitted signal inside the acoustic chamber, and their response is received by the second transducer, which acts as a receiver. Both transducers, transmitter and receiver, are located perpendicular to each other on the center of their respective chamber walls. The received signal passes through a band-pass filter that passes ultrasound frequencies, filtering out the audible range, before being demodulated by mixing it with F1, and sent to a (National Instrument) data acquisition unit Fig. 3. Schematic of acoustic measurement method. Fig. 4. Modulator with carrier suppression. (DAQ), and finally to a computer, where it is analysed. The carrier, F1, is set at 1 MHz, whereas the modulating signal, F2, varies for each measurement from 1 kHz to 10 kHz with a step of 50 Hz. 3. Results and discussion 3.1. Liquid-air system Fig. 1. Experimental setup. A series of tests were performed in a two-phase system (liquidair) to determine the relation between the signal received and the size of the bubbles being sampled (Fig. 5). The conditions of bubble generation were defined in order to have values of d32 covering at least the range between 1 and 1.5 mm, which is a typical range in 124 W. Kracht, C. Moraga / Minerals Engineering 98 (2016) 122–126 Imean ¼ m d32 þ n 60 Sound intensity, dB 55 50 45 2 R = 0.94 40 35 30 25 20 0 0.5 1 1.5 2 2.5 Bubble mean diameter d32, mm Fig. 5. Sound intensity vs d32 in a two-phase system. where Imean corresponds to the average received signal intensity, in decibels (dB), m and n are the parameters of the curve, and d32 is the bubble Sauter mean diameter, in millimetres (mm). The values for m and n for the 2-phase system are 16.29 dB/mm and 60.0 dB respectively, with a coefficient of determination R2 equal to 0.94. Fig. 6 shows two bubble size distributions, determined by image analysis, corresponding to the extreme values of d32 presented in Fig. 5. One of them is a uni-modal, narrow distribution, whereas the other is wider and bi-modal, which suggest that the technique allows determining the bubble Sauter mean diameter from distributions of different shape. 3.2. Validation of the technique mechanical flotation cells. The bubbles were generated in a 5 L laboratory mechanical cell (Labtech-ESSA), with a square crosssectional area of 397 cm2. The cell allowed controlling both impeller speed, and gas flow rate. The superficial gas velocity, Jg, was varied between 0.3 and 0.5 cm/s, and the impeller speed between 300 and 600 rpm, which considering the impeller dimensions (D = 10.7 cm), corresponds to a peripheral velocity between 1.7 and 3.4 m/s respectively. The frother used in all the tests was MIBC, at a concentration of 30 ppm (well above the critical coalescence concentration, CCC). At each condition, the response of the bubbles was recorded and analysed. The bubbles were also photographed in order to size them by image analysis and determine their bubble Sauter mean diameter, d32 (two of them are presented in Fig. 6). The results of the measurements are presented in Fig. 5. It can be seen that there is a linear relation between the mean intensity of the received signal, i.e., the response of the bubbles to the acoustic stimulus, and the values of d32. The relation between both variables can be written as: 25 d32 = 1.84 mm Number frequency, % ð1Þ In order to validate the technique, a series of 25 tests were run in a 2-phase system. To obtain a wide range of bubble sizes in the flotation cell, the agitation was varied between 300 and 600 rpm, the Jg between 0.3 and 0.7 cm/s, and the frother (MIBC) concentration was varied between 5 and 30 ppm. From the 25 tests, 5 were run with NaCl instead of MIBC, with a concentration between 0.1 and 0.3 M. The values of d32 for each condition were determined using both the acoustic technique and image analysis, and are presented in Fig. 7. In the case of the acoustic technique, the bubble Sauter mean diameter was determined using the linear relation (Eq. (1)), with the parameters m and n presented above. The data shown in Fig. 7 correspond to a new set of results, independent from those presented in Fig. 5, which were used to determine the coefficients of Eq. (1). The results validate the acoustic technique. The bubble Sauter mean diameters determined with the acoustic technique correlate well with those determined using image analysis, with a coefficient of determination R2 equal to 0.99. Originally, the condition of 0 ppm of frother had been included, but it was found that the acoustic technique underestimates the d32 for values higher than 3 mm. The acoustic technique is therefore valid for values of d32 between 0.75 and 3 mm. 20 3.3. Reproducibility 15 In order to test the reproducibility of the technique, a series of measurements were performed, in triplicate, in a 2-phase system, at different conditions of bubble generation in the flotation cell: the frother (MIBC) concentration was varied from 5 to 30 ppm, whereas the agitation and superficial gas velocity, Jg, were kept 10 5 0 0.5 1 1.5 2 2.5 3 diameter, mm 25 Number frequency, % d32 = 0.99 mm 20 15 10 5 0 0 0.5 1 1.5 2 2.5 3 diameter, mm Fig. 6. Bubble size distributions generated at 300 rpm (up), and 600 rpm (down); Jg 0.5 cm/s. d32 measured using acoustic technique, mm 0 3 2.5 2 1.5 2 R = 0.99 1 0.5 0 0 0.5 1 1.5 2 2.5 d32 measured using image analysis, mm Fig. 7. Comparison between methods. 3 125 W. Kracht, C. Moraga / Minerals Engineering 98 (2016) 122–126 60 55 Sound intensity, dB constant at 400 rpm and 0.5 cm/s, respectively, which allowed generating bubble Sauter mean diameters, d32, ranging from 0.84 to 2.63 mm. The results, and the relative standard deviation (RSD) are presented in Table 1. The three runs follow the same trend, which corresponds to a typical curve of bubble size against frother concentration (Cho and Laskowski, 2002). The results show a good reproducibility for a wide range of mean bubble sizes, and, since the shape of the bubble size distribution changes when increasing the frother concentration (Finch et al., 2008), it can also be said that with the technique it is possible to estimate d32 from different distributions, as it was suggested from Fig. 6. 50 2 R = 0.97 45 40 35 30 25 20 0 0.5 1 1.5 2 2.5 Bubble mean diameter d32, mm Fig. 8. Sound intensity vs d32 in a three-phase system. 3.4. Three-phase system In order to test the technique in a more realistic condition, a series of measurements were performed in a 3-phase system (waterair-particles), with quartz as the solid phase, at a P80 of 200 um, and a solid weight content of 30%. The conditions of bubble generation were the same as were previously used in the 2-phase system, i.e., impeller speeds varying between 300 and 600 rpm, Jg between 0.3 and 0.5 cm/s, and a frother (MIBC) concentration of 30 ppm. As it can be seen in Fig. 8, the relation between the average signal intensity and the bubble Sauter mean diameter, d32, is linear as in the case of the 2-phase system. The values for m and n in this case are 16.24 dB/mm and 65.9 dB, with a coefficient of determination R2 equal to 0.97. The coefficients for both conditions, 2-phase and 3-phase, are summarised in Table 2. Note that the linear relation is maintained but the value of n changes. The slope of the curve, on the other hand, does not change significantly. As noted in Table 2, the intensity of the signal with a 30% solids is 5.9 dB higher than in the case of the water-air system. This result suggests that the particles inside the chamber affect the behaviour of the acoustic signal. The surface of the particles may be acting as a signal reflector, which could explain the difference. This implies that the relation between d32 and the mean intensity of the received signal, Imean, is influenced by the presence of solids, and, therefore, the calibration of the acoustic technique would be specific for the particular conditions of the system to be evaluated. With the technique presented in this work it is possible to determine the bubble Sauter mean diameter, d32, for a wide range of sizes, from 0.75 to 3 mm, covering the range of most interest of flotation. The configuration presented here considers the use of a pump to take the samples (see Fig. 1), therefore, it is easy to set up in such a way that it can operate continuously. Since the relationship between signal intensity and d32 is not derived from fundamentals, but from an empirical model, the technique requires calibration against an accepted method such as the MBSA. Therefore, although the acoustic method represents an alternative to the MBSA as a sensor to monitor the flotation process, it does not completely replace the image analysis technique because it still depends on it for calibration. Table 1 Reproducibility. MIBC (ppm) 5 10 15 20 25 30 d32 (mm) RSD (%) Run 1 Run 2 Run 3 2.61 1.41 0.98 0.85 0.84 0.87 2.51 1.29 0.88 0.91 0.92 0.94 2.63 1.40 0.90 0.84 0.93 0.94 2.3 5.1 5.4 4.6 5.6 4.4 Table 2 Coefficients for the intensity – d32 curves. System m n 2-phase 3-phase 16.29 16.24 60.0 65.9 4. Conclusions An acoustic technique for measuring the bubble Sauter mean diameter, d32, is introduced. The technique consists of exposing the bubbles to an acoustic perturbation, and analysing their response. The perturbation corresponds to a modulated signal with frequencies F1 ± F2, where F1 acts as a carrier set at 1 MHz, and F2 corresponds to the modulating signal, which varies for each measurement from 1 kHz to 10 kHz with a step of 50 Hz. The configuration considers the use of a peristaltic pump to sample liquid and bubbles from the flotation cell, which can be automated to operate continuously and in such a way that no operator is needed. An empirical relation was found between the average intensity of the acoustic response of the bubbles, Imean, and d32. The relation is linear and can be written as Imean ¼ m d32 þ n, with coefficients m and n that are determined with the aid of an independent method such as the MBSA. The acoustic technique allows determining d32 in the range between 0.75 and 3 mm, covering the range of most interest of flotation, and represents an alternative to the image analysis as a sensor to monitor the flotation process; nevertheless, it does not completely replace image analysis, which is still needed for calibration. Acknowledgements The authors would like to acknowledge the Chilean Economic Development Agency (CORFO), project number 11IDL2-10687, and the Chilean National Commission for Scientific and Technological Research (CONICYT), Basal Financing Program FB0809, for funding this research. This work made use of the free software package GNU Octave, and the authors are grateful for the support of the Octave development community. References Ajbar, A., Al-Masry, W., Ali, E., 2009. Prediction of flow regimes transitions in bubble columns using passive acoustic measurements. Chem. Eng. Process.: Process Intens. 48, 101–110. Boyd, J.W.R., Varley, J., 2001. The uses of passive measurement of acoustic emissions from chemical engineering processes. Chem. Eng. Sci. 56, 1749–1767. Buckey, J.C., Knaus, D.A., Alvarenga, D.L., Kenton, M.A., Magari, P.J., 2005. Dualfrequency ultrasound for detecting and sizing bubbles. Acta Astronaut. 56, 1041–1047. 126 W. Kracht, C. 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