Composites: Part A 38 (2007) 2633 www.elsevier.

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In-line occulation monitoring in a Hatschek machine for brecement manufacture

o, Julio Tijero Carlos Negro *, Angeles Blanco, Ignacio San P
Department of Chemical Engineering, University Complutense of Madrid, Avda. Complutense s/n, 28040 Madrid, Spain Received 20 May 2004; received in revised form 7 July 2005; accepted 25 January 2006

Abstract The aim of this study is to obtain real-time information of occulation processes in the brecement manufacture through a soft sensor. This paper presents three dierent applied trials, carried out in dierent Hatschek machines, representing the main two industrial processes (air curing and autoclaving), in order to monitor the occulant dosage changes, occulant changes and the relationship between nal product properties and occulation. Three dierent anionic poly-acrylamides of low charge with dierent molecular weights were used as occulants. The obtained results demonstrate that focused beam reectance measurement (FBRM) is a valuable in-line sensor as well as a control and predictive process tool to monitor the occulation processes in brecement manufacture. Furthermore, a correlation between the sensor data (counts/s of particles between 50 and 86 lm) and the nal product properties (density) was established, thus minimising the production of brecement outside the intended specications to achieve a better control on the nal product quality. 2006 Elsevier Ltd. All rights reserved.
Keywords: A. Fibres; B. Fibre/matrix bond; FBRM; D. Process monitoring; E. Forming

1. Introduction Asbestoscement is a valuable composite for construction materials because of its excellent cost eectiveness and durability. However, all uses of asbestos are expected to be banned in the future because asbestos may cause adverse health eects. For instance, the use of asbestos as a raw material for industry was forbidden in Europe some years ago and the moratoria for existing installations has nished in January 2005. Cost and reinforcement properties are considered while substituting the asbestos bres. From the many possibilities that have been studied, the most widely used, at industrial scale, are the cellulose bres from unbleached softwood Kraft pulp, either alone or in a mixture with synthetic bres [13]. Asbestos is a naturally occurring brous silicate and the bres size together with its chemical structure allows
*

Corresponding author. Tel.: +34 91 394 42 42; fax: +34 91 394 42 43. E-mail address: cnegro@quim.ucm.es (C. Negro).

cement particles retention. However, the dierent chemical compositions and the hygroscopic character of the cellulose bre pulp make the compatibility of the cellulose bres with the cement much more complex, particularly when low bre content is needed for economical and technological reasons. Therefore, it is necessary to consider the new aspects of manufacturing to improve the bre/matrix bonding and the cement retention. Thus, in the Hatschek process it is necessary to use a suitable occulant to produce the occulation of cement particles on the bres. Therefore, a good optimisation of the occulation process is crucial in the industrial process because of its eect not only on mineral nes retention, but also on dewatering and formation (e.g. elephant skin appearance and delamination) and, as a consequence, on the overall eciency of the machine. So this is a key issue for the industry and there is hardly any published literature available on it. This will specically be useful when mills of the developing countries, with low research capabilities, change to bre cement production.

1359-835X/$ - see front matter 2006 Elsevier Ltd. All rights reserved. doi:10.1016/j.compositesa.2006.01.027

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The objective of this paper is to study the feasibility of using a focused beam reectance measurement (FBRM) as a soft sensor to monitor occulation, in-line in a Hatschek machine, during the manufacture of brecement products and to predict the nal product quality. Flocculation is, in general, a complex process that is difcult to control. It has been monitored in dierent industries by dierent means, without a common approach being agreed. The rst methods were based on the dierent sedimentation rates of particles and agglomerates before and after occulation. However, these methods give very limited information about the occulation process [4]. The most important group of methods relies on the study of the electro-kinetic properties of the suspensions, which are the most common methods used in many industrial processes e.g. the paper industry. Colloidal titration, cationic demand and zeta potential measurements are used at laboratory scale and on-line, in a bypass stream from the process. In many cases, the sample has to be ltered or diluted prior to its analysis. Although these methods are useful, in many cases they are not applicable to this manufacture sector because of the high abrasion character of the brecement suspensions (it will damage the Teon measuring cells), of the colour and the high solid content of the samples [5,6]. Recently the use of a rheometer has also been proposed to monitor the occulation process in some industries, e.g. to follow the occulation of silica-lled rubbers [7] or to study the occulant programme in the paper industry [8]. These are promising technologies that can give important information at the laboratory scale but cannot be applied in-line during brecement manufacture. In principle, the occulation phenomenon is based on the agglomeration of suspended particles and on the increased size of the aggregates. Therefore, the consequences of agglomeration determine the performance of each occulant. The change in oc size gives important information on the interaction between the occulant and the suspended particles which is independent of the occulation mechanism that takes places. Thus a pioneer method based on particle size measurements was proposed by the authors to optimise qualitatively and quantitatively the use of polymers in the paper industry [9,10]. Low-angle laser light scattering or laser diraction has been used as a laboratory technique since 1960s. It is generally used both in the laboratory, when diluted suspensions are being analysed, and on-line, especially for dry-process control [11]. The latest developments have also allowed its use on-line in concentrated slurry suspensions by means of a sampling system that dilutes the sample and passes the suspension across a measuring cell so that the particle size distribution can be measured [12]. Nevertheless, this system cannot be applied to brecement occulation tracking since dilution and ow disturbance, needed for the measurement, can aect the ocs and in this case the results will not be accurate enough.

Ultrasonic attenuation has been applied in wet mineral processes since the 1970s. Recently it has been combined with gamma-ray transmission and sound velocity measurement for more accurate solid content compensation but the major limitation is its high sensitivity to entrained air bubbles [13,14]. Various optical image analysis methods based on particle counting have been proposed and applied to specic situations, but the wide size distributions present in some suspensions, such as brecement, limits their use because the size number distribution will be heavily weighted towards ne particles. On the other hand, the need for transparency in the medium is another disadvantage of these techniques [15]. Another option is the use of spectral turbidity measurements, which can be done in situ, but these are quasi-realtime measurements [16]. They require a fairly simple optical technology but a complex computational software. This is because the recovery of particle size distribution information from turbidity is a dicult mathematical problem which usually requires the assumption of a certain shape of the particles and the calculation of the refractive index of them. This technique can be useful in crystallization experiments [17]. Focused beam reectance measurement (FBRM) probes that allow in situ measurement of chord length distribution over a wide range of solid concentrations have been available since 1990. Since then a number of studies have been performed in order to monitor particle systems in dierent areas as diverse as oceanography, pharmaceutics, mineral processing, euent treatments, etc. [1825]. Sengupta et al. used FBRM to study the occulation of kaolin by a cationic polyacrylamide in a stirred beaker [26,27]. They studied the eects of mixing speed, time, multiple occulant addition, pH and solid concentrations. Fawell et al. compared classical settling and turbidity measurements with FBRM data for the occulation of ne hematite in stirred beakers [28]. With increasing occulant dosage, the hindered settling rate and FBRM mean chord length showed similar trends and the total counts below 9.3 lm correlated with residual turbidity. Recently, calcite slurries and a lime fraction from a sand-processing operation were studied in order to assess their occulation performance under dierent operating conditions [29]. Finally, the inuence of occulant solution age on occulation performance by FBRM has also been studied [30]. The authors have developed a methodology to study oc stability and resistance to shear forces, re-occulation tendency and reversibility of the ocs. Furthermore, optimal dosage of any polymer and the associated occulation mechanism and occulation kinetics can be determined [31]. This methodology has already been applied in previous studies for the brecement suspensions at laboratory scale. The results allow the selection of the best occulant and the optimal dosage for each particular brecement suspension [15]. Based on those data it was decided to carry out industrial trials to monitor and optimise the occulation process

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in real time in a Hatschek machine during brecement production using a FBRM probe as a soft sensor. 2. Experimental 2.1. Description of the dierent applications The objective of this work was to prove the suitability of using a FBRM probe for in-line occulation monitoring in a Hatschek machine. In order to reach the objective three dierent trials were performed: 1. Monitoring the eect of occulant dosage changes. 2. Monitoring the eect of occulant change. 3. Correlating sensor data with nal product properties. In order to obtain results that could be applied to a wide range of industrial installations, the trials were performed in three dierent Hatschek machines using two dierent technologies (air cured and autoclave curing), with dierent mineral raw material compositions and using unbleached softwood pulp alone and in a mixture with poly-vinylalcohol (PVA) as reinforcing bres. 2.2. FBRM probe description and location An FBRM M500P probe supplied by Lasentec was used to perform the trials. The focused beam reectance measurement oers the possibility of in situ particles characterization in a wide concentration range. The FBRM instrument operates by scanning a highly focused laser beam, at a xed speed, across the particles in suspension and measuring the time duration of the reected light from these particles. The temporal duration of the reection from each particle or oc multiplied by the velocity of the scanning laser, which is known, results in a characteristic measurement of the particle size known as the chord length. Thousands of chord length measurements are collected per second, producing a histogram in which the number of the observed counts is sorted in several chord length bins over the range from 0.2 to 2000 lm. Total counts, counts in specic size regions (population), mean chord length, and other statistical parameters can be easily calculated from the data. The evolution of these various statistics under varying process conditions allows us to follow the evolution of the occulation process. The right selection of the probe location with respect to the full ow sheet of the process and the orientation inside the pipe is essential to obtain accurate data. It was decided to install the unit in a process pipe after occulant addition but before it is being fed to the vat machine. Fig. 1 shows the FBRM probe location. The best location in the process is the inlet of the vat, where the primary thin brecement layer is formed on the Hatschek machine, because this is the place where the occulant has just been added and, therefore, the eects will be seen quickly. Moreover, since the critical step for the retention of solids is this

Fig. 1. Location of the FBRM probe.

primary sheet formation, the selected probe location could allow the correlation to be made between oc size and nal product properties. A set of preliminary tests was performed to check the adequacy of the probe location and its sensitivity to process changes. A cleaning sequence was dened in order to avoid window probe plugging. It comprised cleaning with pressurized water if any machine stopped for longer than 10 min, as well as at the beginning of each working shift (every 8 h). This cleaning programme ensured that all the considered data properly reect the chord length distribution of the suspension. Under these conditions the sensor was working throughout several weeks without any problem. A control sheet of the machine shutdowns and of the process variation was used to check any process problem that could aect the FBRM measurements. 3. Results and discussion 3.1. First trial: FBRM monitoring the eect of occulant dosage changes This trial was carried out in a Hatschek machine with four vats working at 6065 m/min using a mixture of highly rened Pinus radiata unbleached Kraft pulp, polyvinylalcohol (PVA) bres and silica fume on a matrix of ASTM Type II cement as raw material. As occulant an anionic polyacrylamide (A-PAM1) of high molecular weight (7.5 106 g/mol) and low anionic charge (1.6 meq/g) was used. Fig. 2 shows the evolution of the median of the chord length distribution over an hour of industrial production. Several occulant ow changes were made to see their eects on the chord length distribution, as it can be seen in the right axis. The evaluation of noise in stable periods

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Median chord length evolution on changing commonly used flocculant flow

1000 900

Median chord length (m)

33 32 31 30 29 28 27 26 25 24 16:00 16:10 16:20 16:30 16:40

Median chord length Median +/- STDev Flocculant flow

Flocculant flow (L/h)

800 700 600 500 400 300 200 100 0 16:50 17:00

Time (h:min)
Fig. 2. FBRM data tracking: the eect of occulant dosage changes.

gives a standard deviation of 0.30 lm, which is shown by the upper and lower limits in the gure. Thus, all changes over those limits can be considered signicant. A decrease in the median chord length, from 31 lm to 30 lm, is seen when occulant is reduced from 750 to 420 L/h. Stopping the occulant dosing was also tried and its eect on the suspension is clearly seen in the gure, where the median chord length decreases to 25 lm. This value corresponds to the median chord length of the raw suspension, without any agglomeration, because of the stability of the measured values during this period. After several minutes the occulant was introduced again rst at a slightly higher dosage than initial (900 L/h), in order to go back to the normal situation, and then at the same dosage (700 L/h). As it can be observed, the sensor started to detect higher values with

900 L/h and then there is a decrease up to similar values to the initial ones. In Fig. 3, the chord length distributions in the three main experimental points are presented, showing a small change in the rst occulant reduction (from 700 to 420 L/h, see D(700420) values in Fig. 3), and a signicant change if occulant is stopped (D(4200) values are the differences between 420 L/h and 0 L/h of occulant addition). Based on the standard deviation of each statistic (STDev), obtained with noise evaluation in stable periods, it was observed that in all cases there are signicant changes and, therefore it is concluded that the three curves are signicantly dierent. A few minutes after reducing the occulant dosage to 420 L/h delamination of the sheets started to occur and it

Fig. 3. Chord length distribution for dierent occulant dosages.

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was necessary to increase the occulant dosage again. This trial shows the high sensitivity of the FBRM sensor to detect any occulant dosage change in the brecement manufacture process. 3.2. Second trial: Monitoring eects due to occulant change This trial was carried out in a dierent production line with a similar Hatschek machine and the same raw material composition as in the rst trial. As new occulant an A-PAM2 with higher molecular weight (17 106 g/mol) and similar anionic charge as that of the former was used. Fig. 4 shows how a change of the occulant commonly used in the process to a new occulant aected the chord length distribution. As it can be seen, directly after the oc-

culant change an unstable time period was observed due to adjustment of machine parameters that were necessary with the new occulant and after that a high increase of the median chord length was observed. The increase is signicant, from 31 lm to 35 lm for the rst dosage. Even at the lowest dosage of the occulant 2 the median chord length was higher (32.5 lm) than with the reference occulant (30.8 lm). The increase in oc size is due to the higher molecular weight of the new occulant. When the suspension behaviour is studied in greater detail it is also possible to monitor the counts per second evolution for dierent chord size ranges. As an example, Fig. 5 shows the evolution of particles for three dierent particle size ranges 150 lm, 5086 lm and higher than 86 lm. It can be observed that the number of particles

Median chord length evolution when flocculant is changed from flocculant 1 to flocculant 2
36 800

Flocculant 1
35

Flocculant 2

750 700

Median chord length (m)

34 650 33 32 31 30 400 29 28 12:00 Median chord length Flocculant Flow 12:20 12:40 13:00 13:20 13:40 350 300 600 550 500 450

Flocculant flow (L/h)

Time (h:min)
Fig. 4. Evolution of median chord length during occulant change.

Fig. 5. Evolution of counts/s at dierent chord range sizes during occulant change.

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smaller than 50 lm decreases when occulant is changed because the higher level of aggregation, while in the other size intervals the counts increase. The occulant changes have also induced an increase and a decrease of counts depending on the chord size range studied. The increase in occulation reported by FBRM was also noticed in the production line since retention of llers grew signicantly during this period and machine productivity was improved. No quality problems were found in the nal product from this trial. After the trial the mill used the new occulant for several weeks without any production problems. In order to validate these results in other industrial cases, trials were performed with another occulant change in another Hatschek machine using the same reinforcing bre but in a dierent amount and with dierent mineral raw materials. The new occulant had a much higher molecular weight and it was used to increase the dewatering rate of mineral sludge. Fig. 6 shows the occulation evolution during this trial. As it can be seen, a very high increase of the median chord length was produced when the occulant was changed (4053 lm), even at the same dosage level. This change was reected in machine productivity as an increase in drainage rate that allowed a considerable increase in machine speed, even when applying less vacuum, and therefore, an increase in machine productivity. Retention of llers was increased too, which was expected because of the higher oc size.

3.3. Third trial: Correlating the sensor data with product properties Finally, after the occulation process had been monitored by FBRM, the next step in the research was to focus on establishing the correlation between the sensor data and the nal product properties. If this can be achieved in the future, the sensor could be used as a predictive control tool. Therefore, to probe the relationship between the sensor data and the nal product properties, it was decided to install the probe during three dierent full weeks of machine operation in order to process sensor data to nd correlations between the obtained FBRM values and the nal product properties. These trials were carried out in a Hatschek machine with four vats working at a speed of 6065 m/min using a mixture of rened Pinus radiata unbleached Kraft pulp and standard ground silica on a matrix of ASTM Type II cement as raw material. As occulant an anionic polyacrylamide (A-PAM) of high molecular weight (7.5 106 g/mol) and low anionic charge (0.6 meq/g) was used. The steps followed to establish these correlations were:  To nd machine stable periods in which sensor data were processed and product properties were measured.  To select statistics to correlate with a given parameter.  To select an averaging method and data discrimination to have good correlations.

Median chord length evolution when flocculant is changed from flocculant 1 to flocculant 3
55 53 51 49 47 45 43 41 39 37 35 16:48

Median chord length Flocculant flow (L/h)

Flocculant 1

Flocculant 3

900 800 700 600 500 400 300 200 100 0

19:08

Median chord length (m)

Flocculant FLow (L/h)

17:08

17:28

17:48

18:08

18:28

18:48

Time (h:min)

Fig. 6. Evolution of median chord length during occulant programme change.

1.56 1.54 Density (kg/L) 1.52 1.50 1.48 1.46 1.44 1.42 1.40 22000 22500 23000 y = 4E-05x + 0.5871 2 R =0.6044 23500 24000 Counts/s 50-86 m 24500 25000

Fig. 7. Product density versus counts/s of particles between 5 and 86 lm size range.

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These studies were applied to correlate the density of the brecement sheet produced in the trial and measured 7 days after its production, as explained in EN494:1994 standard. Several sets of statistics as well as dierent averaging methods were used to nd these correlations over dierent periods of stability in the measured data with the FBRM. Good correlations were found with the evolution of the counts per second cubic weighted in the interval from 50 to 86 lm, as it can be seen in Fig. 7. The results show good correlation between sensor data and density of the nal product (R2 = 0.6). These results prove the relation between occulation and nal product properties and that the FBRM probe can be used in-line to control the process. Thus, the quality of the nal product can be better controlled minimising the production of material out of the required specications. However, this is not an easy task as there are many parameters in the brecement manufacture process that aect the nal properties of the product. At this moment further research is under development in order to use advanced mathematical tools, like articial neural networks, to make predictions of brecement properties based on FBRM sensor data. 4. Conclusions Results show that occulation has to be addressed in the manufacture of brecement products to increase retention because of the low anity between cellulose bres and cement. Furthermore, the occulant dosage has to be well optimised to avoid problems in machine productivity and product quality. Traditional measurement techniques used in other industries to control occulation cannot be applied in this case because of the high abrasion, the high solid content and the colour of the brecement suspensions. Furthermore, occulation has to be monitored in-line to avoid the alteration of oc characteristics due to sample manipulation. The feasibility of using a focused beam reectance measurement (FBRM) as a soft sensor to monitor occulation, in-line in a Hatschek machine, during the manufacture of brecement products and to predict the nal product quality has been proved. FBRM provides useful information about the evolution of particle chord size over time, monitoring the occulation process. It was possible to quantify the occulation changes produced by both occulant dosage and type of occulant changes, for dierent furnish formulations. A good correlation between the sensor data and the density of the nal product was obtained. This will allow the mill to predict product quality based on oc properties and to detect out of specication production in real time instead of waiting 7 days to get the product data. Thus, FBRM data can be used to control the occulation process and as an alarm sensor to predict quality problems related to low density values.

Acknowledgements The authors want to express their gratitude to Uralita S.A. for sponsoring this project. We are grateful for technical discussions with Jose Ma Tejera. The funding from the European Union and from the Spanish Department of Science and Technology to the FEDER project Optimisation of occulation, retention and drainage processes is also acknowledged. References
[1] Daniel JI et al. State-of-art-report on bre reinforced concrete. Reported by ACI Committee 544. Report ACI 544.1R-96, 1996. [2] Bentur A, Mindess S. Fibre reinforced cementious composite. UK: Elsevier Applied Science Publishers; 1998, p. 111. [3] Coutts RSP, Michell AJ. Wood pulp bercement composites. J Appl Polym Sci 1983;37:82944. [4] Fuente E. Mechanism and kinetic of occulation process in the paper manufacture. Madrid, Spain: Complutense University, PhD Thesis, 2003. [5] Blanco A, Negro C, Tijero J. Developments of occulation in papermaking. Leatherhead, UK: PIRA International; 2002, p. 38 58. [6] Hubbe M. Selecting and interpreting colloidal charge measurements. In: Proceedings of scientic and technical advances in wet-end chemistry PIRA international conference. Barcelona, Spain, June, 2000. p. 123. [7] Lin CJ, Hergenrother WL, Alexanian E, Bohm GCA. On the ller occulation in silica-lled rubbers part I. Quantifying and tracking the ller occulation and polymer-ller interactions in the unvulcanized rubber compounds. Rubber Chem Technol 2002;75(5):86590. [8] Anker LS. Practical experiences in additive screening using a torquebased occulation analyser. Tappi J 2002;1(6):38. [9] Blanco A, Negro C, Tijero J, Hooimeijer A. Inuence of salt on the interaction of polymers with the dierent pulp fractions. In: Proceedings TAPPI papermakers conference, San Francisco, April 2427, 1994. p. 556. [10] Blanco A, Negro C, Hooimeijer H, Tijero J. Polymer optimization in papermills by means of a particle size analyser: an alternative to zeta potential measurements. Appita J 1996;49(2):1136. [11] Ma Z, Merkus HG, Smet JGAE, Heels C, Scarlett B. New developments in particle characterization by laser diraction: size and shape. Powder Technol 2000;111:6678. [12] Crawley GM. Particle sizing online. Powder Metall 2001;44(4):304. [13] Coghill PJ, Millen MJ, Sowerby BD. On-line measurement of particle size in mineral slurries. Miner Eng 2002;15:8390. [14] Hibberd DJ, Robinson BH, Robins MM. Ultrasonic characterisation of colloidal dispersions: detection of occulation and adsorbed layers. Colloids Surf B 1999;12:35971. o I. Methodology to optimise occulation in the manufacture of [15] SanP brecement without asbestos. Madrid, Spain: Complutense University PhD Thesis, 2003. [16] Crawley G, Counil M, Benedetto DD. Size analysis of ne particle suspensions by spectral turbidimetry: potential and limits. Powder Technol 1997;91:197208. [17] Herri JM, Gruy F, Pic JS, Cournil M, Cingotti B, Sinquin A. Interest of in situ turbidimetry for the characterization of methane hydrate crystallization: application to the study of kinetic inhibitors. Chem Eng Sci 1999;54:184958. [18] Barrett P. Selecting in-process particle-size abalysers. Chem Eng Prog 2003;99(8):2632. [19] Abbas A, Nobs D, Romagnoli JA. Investigation of on-line optical particle characterization in reaction, and cooling crystallization systems. Current state of the art. Meas Sci Technol 2002;13(3): 34956.

C. Negro et al. / Composites: Part A 38 (2007) 2633 [20] Jeers P, Raposo S, Lima-Costa ME, Connolly P, Glennon B, Kieran PM. Focused beam reectance measurement (FBRM) monitoring of particle size and morphology in suspension cultures of Morinda citrifolia and centaurea calcitrapa. Biotechnol Lett 2003;25(23):20238. [21] Pearson AP, Glennon B, Kieran PM. Comparison of morphological characteristics of Streptomycess natalensis by image analysis and focused beam reectance measurement. Biotechnol Prog 2003;19(4): 13427. [22] Choi YC, Morgenroth E. Monitoring biolm detachment under dynamic changes in shear stress using laser-based particle size analysis and mass fractionation. Water Sci Technol 2003;47(5):6976. [23] Hukkanen EJ, Braatz RD. Measurement of particle size distribution in suspension polymerization using in situ laser backscattering. Sens Actuators B Chem 2003;96:4519. [24] Kukkanen EJ, Braatz RD. Measurement of particle size distribution in suspension polymerisation using in situ backscattering. Sens Actuators B Chem 2003;96(1-2):4519. [25] OSullivan B, Barret P, Hsiao G, Garr A, Glennon B. In situ monitoring of polymorphic transitions. Org Process Res Dev 2003; 7(6):97782.

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[26] Sengupta DK, Kan J, Taweel AM, Hamza HA. Dependence of separation properties on occulation dynamics of kaolinite occulation. Int J Miner Process 1997;49:7385. [27] Besra L, Sengupta DK, Roy SK, Ay P. Flocculation and dewatering of kaolin suspensions in the presence of polyacrylamide and surfactants. Int J Miner Process 2002;66:20332. [28] Fawell P, Richmond W, Jones L, Collisson M. Focused beam reectance measurement in the study of mineral suspensions. Chem Aust 1997;64(2):46. [29] Swift JD, Simic K, Jonhston RRM, Fawell PD, Fartow JB. A study of the polymer occulation reaction in a linear pipe with a focused beam reectance measurement probe. Int J Miner Process 2004;73(24): 10318. [30] Owen AT, Fawell PD, Swift JD, Farrow JB. The impact of polyacrylamide occulant solution age on occulation performance. Int J Min Process 2002;67(14):12344. [31] Blanco A, Fuente E, Negro C, Tijero J. Flocculation monitoring: focused beam reectance measurement as a measurement tool. Can J Chem Eng 2002;80(4):73440.