Journal of Food Engineering 84 (2008) 194205 www.elsevier.

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Production of instant soymilk powders by ultraltration, spray drying and uidized bed agglomeration
Nakarin Jinapong, Manop Suphantharika *, Pimon Jamnong
Department of Biotechnology, Faculty of Science, Mahidol University, Rama 6 Road, Bangkok 10400, Thailand Received 1 August 2006; received in revised form 12 April 2007; accepted 30 April 2007 Available online 13 May 2007

Abstract Production of instant soymilk powders was completed in three stages ultraltration, spray drying, and uidized bed agglomeration. Ultraltration increased total solids, protein, and fat contents, but decreased carbohydrate and ash contents of soymilk, leading to an increase in particle size, wettability, and dispersibility of the resultant spray-dried powders. However, all the spray-dried soymilk powders were very small (<25 lm) and very cohesive leading to their poor owability. Agglomeration of the spray-dried powders with maltodextrin as an aqueous binder solution using a uidized bed agglomerator improved the handling and reconstitution properties of the powders. The optimum binder concentration was found to be 10% w/v maltodextrin which resulted in the largest particle size of the agglomerated powder (260 lm) having a good owability and low cohesiveness. The wettability of this agglomerated powder (wetting time = 42 s) was good but its dispersibility (61%) could be improved. 2007 Elsevier Ltd. All rights reserved.
Keywords: Soymilk; Spray drying; Agglomeration; Ultraltration; Fluidized bed

1. Introduction Soymilk is becoming more and more popular as consumers become more health conscious and seek out alternatives to dairy products. Basically, soymilk is a water extract of soybeans, closely resembling dairy milk in appearance and composition. It contains high amounts of protein, iron, unsaturated fatty acids, and niacin, but low amounts of fat, carbohydrates, and calcium as compared with cows milk and human milk (Liu, 1997). Soymilk is also touted as a healthy food because it is cholesterol and lactose free and contains phytochemicals. It is recommended for those who are allergic to milk protein or have lactose intolerance and those who have special health or religious diet requirements (Liu, 1997; Pomeranz, 1991). Ultraltration is a hydraulic pressure-operated membrane technique used as a concentration step in the food industry, including soymilk processing. Its use is an attrac*

Corresponding author. Tel.: +66 2 201 5314; fax: +66 2 354 7160. E-mail address: scmsp@mahidol.ac.th (M. Suphantharika).

tive alternative to conventional evaporation processes as it is a non-thermal treatment, as well as one with mild operating conditions. The applications of ultraltration in soymilk processing are not only concentration, but also removal of anti-nutritional low molecular weight components such as oligosaccharides and phytic acid (Ang, Kwik, Lee, & Theng, 1986; Omosaiye, Cheryan, & Matthews, 1978). The low molecular weight oligosaccharides, ranose and stachyose have been implicated as causative factors in digestive disturbances, such as atulence while phytic acid has been considered to lower the mineral biodegradability by forming insoluble complexes with di- and tri-valent ions at neutral pH (Ang et al., 1986; Omosaiye et al., 1978; Pomeranz, 1991). Spray drying is the most widely used commercial method for drying milks because the very short time of heat contact and the high rate of evaporation give a high quality product with relatively low cost (Liu, 1997). A dry powder product is highly desirable since it not only possesses long shelf-life, but also requires relatively low transportation cost and storage capacity and the product can be distrib-

0260-8774/$ - see front matter 2007 Elsevier Ltd. All rights reserved. doi:10.1016/j.jfoodeng.2007.04.032

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uted over a wide area. Thus, a process for producing a dried soymilk powder that is soluble and without loss of nutritive value is highly desirable. However, relatively little research, especially recent studies have been carried out on dehydration of soymilk. Spray drying has been introduced for production of dehydrated soymilk powders by Wijeratne (1993). A spray-drying system for soymilk has been characterized at various combinations of inlet air temperature, feed rate, and atomizer speed on outlet air and product temperatures, thermal and evaporative eciencies (Perez-Munoz & Flores, 1997a), and particle size of spray-dried soymilk powders (Perez-Munoz & Flores, 1997b). Spray-drying studies were also carried out on the ultraltered soymilk concentrates (Ang et al., 1986). The results revealed that the nitrogen solubility index (NSI) of the spray-dried powder improved with percent water removal during ultraltration and also by the addition of sucrose to the concentrate prior to spray drying. However, the detailed characteristics in terms of physicochemical, physical, morphological, and reconstitution properties of the spray-dried soymilk powders have not yet been evaluated by these previous workers. Agglomeration can be dened as the size enlargement process in which the starting material is ne particles such as dusts or powders join or bind with one another, resulting in an aggregate porous structure much larger in size than the original material, such that the primary particles can still be identied (Ortega-Rivas, 2005; Parikh, Bonck, & Mogavero, 1997; Schuchmann, 1995). The granules are held together with bonds formed by the binder used to agglomerate. Agglomeration is used mainly to improve properties related to handling and reconstitution of powders. In the food industry, agglomeration is used for instant products such as coee, milk, or cocoa that disperse and/or , 2003; dissolve quickly in liquids like water or milk (Caric Schubert, 1993; Schuchmann, 1995). The reconstitution properties such as wettability, sinkability, dispersibility, and solubility are enhanced. These properties depend on the type of agglomeration process and on the operating conditions during agglomeration. Fluidized bed agglomeration is one of the most suitable processes leading to agglomerates with high porosity and good mechanical resistance for handling and packaging (Turchiuli, Eloualia, El Mansouri, & Dumoulin, 2005). This process generally works by spraying binder liquid onto a bed of uidized particles, where upon wetting, the particles will be bound together by liquid bridges. Depending on the type of binder used, the liquid bridge will either solidify with cooling or dry with heating to form a solid bridge (Parikh et al., 1997; Tan, Salman, & Hounslow, 2006). The spray-dried powders obtained from small scale spray dryers often have a small particle size, <50 lm, with poor handling and reconstitution properties (Masters, 1991). These powders require agglomeration in order to improve handling and reconstitution properties (Fuchs et al., 2006; Turchiuli et al., 2005). Wijeratne (1993) suggested that agglomeration will improve the wettability of the spray-dried soymilk

powder. At present, however, there is no report on the agglomeration of the spray-dried soymilk powders for producing instant soymilk products. The objective of this study was to investigate the feasibility of production of instant soymilk powders. The production was completed in three stages ultraltration, spray drying, and uidized bed agglomeration. Inuences of soymilk concentration and binder concentration on spray drying and agglomeration, respectively, were evaluated. Powders were characterized before and after agglomeration in terms of physicochemical, physical, morphological, and reconstitution properties. 2. Materials and methods 2.1. Materials Soymilk (5.2% w/w total solids content) was provided by Green Spot (Thailand) Ltd., Pathum Thani, Thailand. Soymilk was produced as a water extract of ground, soaked soybeans heated at 7080 C for 1015 min and then cooled to room temperature. Maltodextrin (D-Perse 3) of dextrose equivalent (DE) value 14 was supplied by Siam Modied Starch Co., Pathum Thani, Thailand. 2.2. Ultraltration Soymilk (30 l) was concentrated on a Nitto Ultraltration Tubular Module (NTU-2020-P18A, Nitto Electric Industrial Co., Ltd., Osaka, Japan), which used 18 tubes (O.D. = 16 mm, I.D. = 11.5 mm, length = 2619 mm) of tubular membranes, giving an eective membrane surface area of 1.6 m2. A hydrophilic polyolen membrane of 20,000 nominal molecular weight cut-o was used in all experiments. A series of experiments were carried out at temperature of not greater than 40 C and the soymilks were concentrated to dierent solids contents, i.e. 7.0%, 9.9%, 13.0%, 15.6%, and 20.7% w/w. During each run the concentrate was allowed to recirculate back to the feed tank. 2.3. Spray drying Soymilk and concentrated soymilks were fed into a spray dryer (Mobile Minor Spray Dryer, Niro A/S, Soeborg, Denmark) by a peristaltic pump, and atomized to small droplets by a centrifugal vaned atomizer wheel with a rotational speed of 23,000 rpm (4 bar air pressure) in a co-current air ow system. The inlet air temperature was set at 180 1 C and the outlet air temperature was kept at 80 1 C by varying the feed rate in the range of 33 51 ml/min. Finally, the powder was then collected from a cyclone and a sample was taken for further analysis. 2.4. Fluidized bed agglomeration Agglomeration of the spray-dried soymilk powders was performed in a top-sprayed uidized bed granulator and

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dryer (Strea-1, Fluid Bed Laboratory, Aeromatic-Fielder AG, Bubendorf, Switzerland) with 2 l vessel capacity. In this study, aqueous solutions of maltrodextrin DE 14 of various concentrations, i.e. 0%, 5%, 10%, 15%, and 20% w/v, were used as a binder. The spray-dried powder weighing 200 g was placed in the product container, and uidized by means of an upward owing air stream. The temperature of the inlet uidizing air entering the bed was set at 50 C. The binder solution (200 ml) was fed by a peristaltic pump at a ow rate of 1112 ml/min to a two-uid spray nozzle where the binder was sprayed onto the uidized bed of soymilk powder. The air pressure on the nozzle was 1.5 bar. During agglomeration, it was necessary to regularly increase the uidizing air ow to maintain a good uidization of the enlarged agglomerates. When the binder solution was consumed, the product was dried for 15 min at a temperature of 50 C. 2.5. Methods of measurement 2.5.1. Viscosity measurement Viscosity of soymilk and concentrated soymilks was determined by a Programmable Viscometer (Brookeld DV-II+, Brookeld Engineering Laboratories, Inc., Middleboro, MA) with a small sample adapter. The samples (8 ml) were measured by using a spindle No. 18 at an operating shear rate of 105.6 s1 and a temperature of 25 C. 2.5.2. Proximate analysis Proximate analyses for moisture, ash, and protein contents of the spray-dried soymilk and agglomerated soymilk powders were carried out using AOAC methods (AOAC, 2000). Fat content was determined by the modied Mojonnier method (AOAC, 2000). Total carbohydrates content was determined by subtracting the ash, protein, and fat percentages from 100%. All tests were carried out in triplicate and the mean calculated. 2.5.3. Particle size measurement For the spray-dried soymilk powders, the particle size distribution, and volume-weighted mean diameter were measured by the dry method in a laser diraction particle size analyzer (Mastersizer 2000; Malvern Instruments Ltd., Worcestshire, UK) tted with a Scirocco 2000 dry powder feeder unit. The volume-weighted mean diameter (d4,3) was calculated as follows: P 4 ni d 1 d 4;3 P i3 ni d i where ni is the number of particles of diameter di. The particle size distribution of the powder was measured as the span which is dened as span d 90 d 10 d 50 2

For the agglomerated soymilk powders, due to their much larger particle sizes, sieve analysis using a vibratory sieve shaker (Retsch GmbH and Co., Haan, Germany) with a series of seven sieves was used to determine their particle size distributions. The aperture sizes of sieves were 75, 90, 125, 150, 180, 250, and 300 lm. The agglomerated soymilk powder (50 g) was put on the sieves series and shaken at 60 Hz for 30 min. The size distribution was described by log-normal distribution relationship. From the log-probability plots, mass-weighted geometric mean diameter as well as geometric standard deviation dened by the slope of the log-normal curve were determined. 2.5.4. Morphological study The appearance, size, and shape of the powder samples were investigated by placing the powders on aluminum stubs using a double-sided adhesive tape. The samples were then coated with gold and were examined with a scanning electron microscope (SEM S-2500, Hitachi Science Systems, Ibaraki, Japan) operating at 15 kV accelerating voltage. 2.5.5. Bulk and tapped densities Powder was gently loaded into a 100 ml tared graduated cylinder to the 100 ml mark and weighed. The volume read directly from the cylinder was then used to calculate the bulk density (qbulk) according to the relationship: mass/volume. For the tapped density (qtapped), the cylinder was tapped 1250 times, using a VanKel Tapped Density Tester (ASTM Version, Varian, Inc., Cary, NC) with a displacement amplitude of 3 0.3 mm. The volume of the sample was then read and used in the calculation. The results were calculated from three replicate measurements. 2.5.6. Particle density Particle density (qparticle) of the powder sample was analyzed according to A/S Niro Atomizer (1978c) with some modications. The powder sample (1 g) was transferred into a 10 ml measuring cylinder with a glass stopper. Then 5 ml of petroleum ether was added and the measuring cylinder was shaken until all the powder particles were suspended. Finally, all the powder particles on the wall of the cylinder were rinsed down with a further 1 ml of petroleum ether (6 ml in total) and the total volume of petroleum ether with suspended powder was read. The particle density was calculated as follows:
qparticle weight of powder g total volume of petroleum ether with suspended powder ml 6 3

2.5.7. Porosity Porosity (e) of the powder samples was calculated using the relationship between the tapped (qtapped) and particle (qparticle) densities of the powder as shown below: e qparticle qtapped 100 qparticle 4

where d90, d10, and d50 are the equivalent volume diameters at 90%, 10%, and 50% cumulative volume, respectively.

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2.5.8. Flowability and cohesiveness Flowability and cohesiveness of the powder were evaluated in terms of Carr index (CI) (Carr, 1965) and Hausner ratio (HR) (Hausner, 1967), respectively. Both CI and HR were calculated from the bulk (qbulk) and tapped (qtapped) densities of the powder as shown below: qtapped qbulk 100 qtapped qtapped HR qbulk CI 5 6

transferred to a weighed and dried aluminum pan and dried for 4 h in a hot air oven at 105 1 C. The dispersibility of the powder was calculated as follows: % dispersibility 10 a % TS b a 100 100 7

where a = amount of powder (g) being used, b = moisture content in the powder, and % TS = dry matter in percentage in the reconstituted soymilk after it has been passed through the sieve. 2.6. Statistical analysis All measurements were made in triplicate for each sample. Results are expressed as mean standard deviations. A one-way analysis of variance (ANOVA) and Tukeys test (p 6 0.05) were used to establish the signicance of dierences among the mean values of the physicochemical, physical, and reconstitution properties of the spray-dried and agglomerated soymilk powders. The data were analyzed using SPSS version 12.0 Windows program (SPSS Inc., Chicago, IL). 3. Results and discussion 3.1. Ultraltration of soymilk Multiple-eect evaporators are commonly used in the food industry to concentrate dilute solutions prior to spray drying because it is generally less expensive to remove water by evaporation rather than using a spray dryer. However, evaporation might cause thermal degradation of food components and loss of volatiles like avors. Ultraltration could overcome these disadvantages. The main advantages of membrane concentration over evaporation are that (1) the food is not heated, (2) there is a negligible loss of quality, (3) there is less loss of volatiles, and (4) it uses energy more eciently because there is no phase change (Ramaswamy & Marcotte, 2006). In this study, a few batches (40 l each) of soymilk were concentrated using a double-eect climbing-lm evaporator (QVF Process System Ltd., Staord, UK) (data not shown). The maximum solids content of the resultant soymilk concentrates was about 20%. Above this level of concentration the viscosity rapidly increased and the concentrates tended to form curd. This concentration is comparable to that obtained by ultraltration (see Section 3.3). However, ultraltration was preferable not only for concentration, but also removal of anti-nutritional low molecular weight components of soymilk (Ang et al., 1986; Omosaiye et al., 1978) which cannot be achieved by evaporation. 3.2. Spray drying of soymilk Relationships between feed rate of ultraltered soymilks during spray drying, viscosity and their concentrations are

Classication of the owability and cohesiveness of the powder based on the CI and HR values are presented in Tables 1 and 2, respectively. 2.5.9. Wettability Wettability of the powder sample was determined according to A/S Niro Atomizer (1978a) with some modications. An amount of distilled water (100 ml) at 25 1 C was poured into a 250 ml beaker. A glass funnel held on a ring stand was set over the beaker with the height between the bottom of the funnel and the water surface of 10 cm. A test tube was placed inside the funnel to block the lower opening of the funnel. The powder sample (0.1 g) was placed around the test tube and then the tube was lifted while the stop watch was started at the same time. Finally, the time was recorded for the powder to become completely wetted (visually assessed as when all the powder particles penetrated the surface of the water). 2.5.10. Dispersibility Dispersibility measurement was performed according to the procedure described in A/S Niro Atomizer (1978b) with some modications. Distilled water (10 ml), at 25 1 C, was poured into a 50 ml beaker. The powder (1 g) was added into the beaker. The stop watch was started and the sample was stirred vigorously with a spoon for 15 s making 25 complete movements back and forth across the whole diameter of the beaker. The reconstituted soymilk was poured through a sieve (212 lm). The sieved soymilk (1 ml) was
Table 1 Classication of powder owability based on Carr index (CI) CI (%) <15 1520 2035 3545 >45 Flowability Very good Good Fair Bad Very bad

Table 2 Classication of powder cohesiveness based on Hausner ratio (HR) HR <1.2 1.21.4 >1.4 Cohesiveness Low Intermediate High

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shown in Fig. 1. As would be expected, in order to control the outlet air temperature of 80 1 C, the feed rate was increased with increasing the total solids content of soymilks. Soymilk viscosity also increased from 2.2 to 22.4 mPa s with increasing concentrations from 5.2% to 20.7%. Correlation between the mean particle size of the spraydried soymilk powders and total solids content of the feed solutions is shown in Fig. 2. The mean particle sizes of soymilk powders sharply increased from 14.54 to 23.59 lm with increasing the solids contents from 5.2% to 13.0% and then increased slightly thereafter. According to Masters (1991), for rotary atomizers, the mean liquid droplet size varied directly with feed rate and viscosity of the feed liquid at constant atomizer speed. The dierence between the mean sizes of wet spray and dried particles showed different trends when feed-solids concentration was changed at constant inlet temperatures. For products characterized by their lm-forming properties, there was little dierence between the mean sizes at high feed concentration. At low concentrations, however, the dierence was signicant. Therefore, the lower the solids content of soymilk, which resulted in the lower feed rate and viscosity (Fig. 1), the

Fig. 3. Particle size distributions of spray-dried soymilk powders produced from soymilk (control) and ultraltered soymilk concentrates of dierent concentrations.

Fig. 1. Eect of total solids content of soymilk (control) and ultraltered soymilk concentrates on viscosity and feed rate during spray drying of soymilks.

smaller liquid droplets formed during atomization resulting in much smaller dried particles than those obtained at high solids content. For a two-uid nozzle atomizer, Keogh, Murray, and O Kennedy (2003) found that the particle size of the spray-dried powders increased linearly with the viscosity of the ultraltered whole milk concentrates. The particle size distributions for various spray-dried powders produced from dierent soymilk concentrations are shown in Fig. 3. All the powders showed smooth unimodal size distribution curves of which their peaks shifted to larger particles as the soymilk concentration increased. This result implies that the solids content of soymilk aected mainly on the mean particle sizes and to a much lesser extent on the size distributions of the spray-dried powders. The scanning electron micrographs of spray-dried soymilk powders show an increase in particle size with increasing total solids content of soymilks (Fig. 4) which is consistent with those determined by the particle size analyzer (Table 4). The particles produced from the low solids soymilks are more wrinkled than those produced from the high solids ones. These dierences in the microstructure could be due to the higher amount of water was removed from the low solids liquid droplets during dehydration resulting in higher shrinkage of the droplets, which tended to form wrinkles. 3.3. Proximate analyses of spray-dried soymilk powders Table 3 shows the composition of the dierent spraydried soymilk samples. It can be seen that the powders obtained from the ultraltered concentrates exhibited a signicant (p 6 0.05) increase in protein and fat contents, but decrease in carbohydrate and ash contents as compared with that obtained from the non-ultraltered soymilk. This was due to the removal of low molecular weight oligosaccharides and inorganic salts by ultraltration as described by Ang et al. (1986) and Omosaiye et al. (1978). Most of the soy proteins have molecular weights ranging from 200,000 to 600,000 (Ang et al., 1986; Pomeranz, 1991). The use of 20,000 molecular weight cut-o membranes

Fig. 2. Eect of total solids content of soymilk (control) and ultraltered soymilk concentrates on the mean particle size of spray-dried soymilk powders.

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Fig. 4. Scanning electron micrographs of spray-dried soymilk powders produced from soymilk (control) and ultraltered soymilk concentrates of dierent concentrations: (a) 5.24% (control), (b) 9.85%, (c) 12.98%, and (d) 20.69% w/w total solids contents at 1000 magnication.

Table 3 Proximate analyses (% w/w, dry basis) of spray-dried soymilk powders produced from soymilk (control) and ultraltered soymilk concentrates of dierent concentrations Soymilk concentrationA 5.24 0.03f,B 7.04 0.01e 9.85 0.01d 12.98 0.13c 15.57 0.01b 20.69 0.27a Protein 48.79 1.04b 52.34 0.45a 51.51 1.09a 50.98 0.29a 51.61 0.29a 50.31 1.03ab Fat 28.77 0.36d 30.43 0.19c 33.99 0.33a 32.12 0.14b 31.33 0.20b 33.54 0.39a Ash 4.97 0.01a 4.39 0.05ab 3.43 0.01cd 3.80 0.54bc 3.14 0.07d 3.48 0.09cd Carbohydrate 17.47 1.40a 12.84 0.30bc 11.06 1.42c 13.12 0.94bc 13.91 0.16b 12.67 0.80bc

Assays were performed in triplicate. Mean SD values in the same column with dierent superscripts are signicantly dierent (p 6 0.05). A Soymilk concentration is expressed in terms of % w/w (wet basis) total solids content. B Control soymilk as received without ultraltration.

should retain these proteins. Fat globules are also larger than the pore size of the membrane and are thus expected to be retained by the membrane. Ash content was not reduced as much even though salts should freely permeate through the membrane. This is probably due to solutesolute interaction between the salts and a rejected species such as protein as suggested by Ang et al. (1986) and Omosaiye et al. (1978). In comparison among the soymilk powders obtained from the ultraltered soymilks of dierent concentrations, the powders exhibited practically no dierence in their compositions. This means that the removal of the low molecular weight components occurred mainly at the beginning of the ultraltration experiments. The explanation could be due to the presence of high molecular weight solute or colloid and insoluble matter which resulted in solute accumulation at the membrane surface during ultral-

tration and produced a layer of nite, and frequently large, hydraulic ow resistance and thereby decreased the overall hydraulic permeability of the membrane as the solution was being concentrated. In this study, it was found that concentration to more than approximately 20% total solids was impractical due to rapid increases in viscosity and pressures. 3.4. Physical, handling, and reconstitution properties of spray-dried soymilk powders Physical, handling, and reconstitution properties of the dierent spray-dried soymilk samples are presented in Tables 46, respectively. All physical properties of the soymilk powders seemed to be unaected by the total solids content of soymilks from which the powders were produced except for the mean particle sizes which increased

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Table 4 Physical properties of spray-dried soymilk powders produced from soymilk (control) and ultraltered soymilk concentrates of dierent concentrations Soymilk concentrationA 5.24 0.03 7.04 0.01e 9.85 0.01d 12.98 0.13c 15.57 0.01b 20.69 0.27a
f,B

Moisture (%) 4.45 0.11 3.81 0.16c 3.29 0.17c 5.57 0.15a 4.38 0.23b 3.50 0.29c
b

Particle size (lm) 14.54 0.16 14.92 0.14e 19.00 0.09d 23.59 0.07c 22.78 0.22b 24.08 0.04a
f

Span 1.34 0.05 1.26 0.00bc 1.48 0.04a 1.21 0.02c 1.25 0.04bc 1.07 0.05d
b

qbulk (g/cm3) 0.21 0.00 0.22 0.01a 0.21 0.00a 0.21 0.01a 0.21 0.01a 0.22 0.00a
a

qtapped (g/cm3) 0.35 0.00 0.32 0.01bcd 0.31 0.00d 0.31 0.01cd 0.33 0.01ab 0.33 0.01ab
a

qparticle (g/cm3) 1.25 0.00 1.25 0.00ab 1.04 0.06c 1.11 0.00bc 1.31 0.10a 1.31 0.10a
ab

Porosity (%) 72.00 0.00ab 74.13 0.46a 70.02 1.77b 71.77 0.52ab 74.71 2.08a 74.47 1.71a

Assays were performed in triplicate. Mean SD values in the same column with dierent superscripts are signicantly dierent (p 6 0.05). A Soymilk concentration is expressed in terms of % w/w (wet basis) total solids content. B Control soymilk as received without ultraltration.

Table 5 Flow characteristics (Carr index, CI, and Hausner ratio, HR) of spraydried soymilk powders produced from soymilk (control) and ultraltered soymilk concentrates of dierent concentrations Soymilk concentrationA 5.24 0.03 7.04 0.01e 9.85 0.01d 12.98 0.13c 15.57 0.01b 20.69 0.27a
f,B

CI (%) 40 0 33 2c 32 0c 32 1c 37 2ab 34 2bc

a

HR 1.67 0.00a 1.49 0.05c 1.48 0.00c 1.47 0.02c 1.60 0.05ab 1.52 0.06bc

Assays were performed in triplicate. Mean SD values in the same column with dierent superscripts are signicantly dierent (p 6 0.05). A Soymilk concentration is expressed in terms of % w/w (wet basis) total solids content. B Control soymilk as received without ultraltration.

Table 6 Reconstitution properties (wettability and dispersibility) of spray-dried soymilk powders produced from soymilk (control) and ultraltered soymilk concentrates of dierent concentrations Soymilk concentrationA 5.24 0.03 7.04 0.01e 9.85 0.01d 12.98 0.13c 15.57 0.01b 20.69 0.27a
f,B

Wetting time (s) 308.0 68.5 57.4 15.3c 121.0 12.9b 91.6 17.1bc 112.6 22.8bc 75.4 10.8bc
a

Dispersibility (%) 62.3 4.7c 94.0 5.3a 83.6 3.1b 92.0 2.8ab 86.9 2.5ab 92.1 1.9ab

Assays were performed in triplicate. Mean SD values in the same column with dierent superscripts are signicantly dierent (p 6 0.05). A Soymilk concentration is expressed in terms of % w/w (wet basis) total solids content. B Control soymilk as received without ultraltration.

with increasing the total solids contents (Table 4). The small variations of both the mean particle sizes and particle size distributions (spans = 1.11.5) could be responsible for very small changes in the physical properties of the soymilk powders. According to Masters (1991), the mean particle sizes that ranged from 20 to 40 lm were classied as very ne particles. In terms of handling properties, the spray-dried soymilk powders had similar ow characteristics and were considered as very cohesive powders by their Hausner ratio (HR) given in Table 5 as classied in Table 2. This is in accordance with their high Carr index (CI) (Table 5) which

indicated that their owability was very poor (Table 1). The rationale behind this poor owability at small particle sizes is due to the large surface area per unit mass of powder. There is more contact surface area between powder particles available for cohesive forces, in particular, and frictional forces to resist ow (Fitzpatrick, 2005; Fitzpatrick, Iqbal, Delaney, Twomey, & Keogh, 2004). Moreover, the spray-dried soymilks obtained in this study contained approximately 30% fat (Table 3). This high fat content also caused the powder to have very poor owability (Fitzpatrick et al., 2004; Perez-Munoz & Flores, 1997b). For the small variation of the particle sizes observed in this study, one could not notice a major change in owability, however, there should be a noticeable change in owability if the powder size is dierent by an order of magnitude, for example, 100 vs 10 lm (Fitzpatrick, 2005). This is true when a comparison was made between the owability of the spray-dried powders and the agglomerated powders which will be discussed later. The wettability and dispersibility of the spray-dried powders produced from the ultraltered soymilk concentrates were signicantly (p 6 0.05) higher than those of the powder obtained from non-ultraltered soymilk but this eect seemed to be independent of the total solids content of soymilk (Table 6). It can be concluded that the ultraltration improved the reconstitution properties of the obtained soymilk powders. This could be attributed to the partial removal of sugar such as sucrose by the ultraltration (Omosaiye et al., 1978). The high sugar content made the powder absorbed moisture rapidly which caused a signicant reduction in its glass transition temperature. The crystallization of sugar could be initiated and solid crystal bridge formation between the particles might occur, which could cause caking (Bhandari, Datta, & Howes, 1997; Fitzpatrick, 2005; Shittu & Lawal, 2007). This might contribute to reduced wettability and dispersibility as the particles absorb moisture. In this study, it was found that the powder obtained from non-ultraltered soymilk formed lumps on the surface of water during the wettability and dispersibility assays while the other powders showed much less tendency to form lumps. In general, it is known that water wets very ne powders poorly because of its high surface tension (Schubert, 1993). A bed of powder remains on the surface of water, with a viscous layer stopping cap-

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illary ow in the interparticle porosity (Vu, Galet, Fages, & Oulahna, 2003). 3.5. Proximate analyses of agglomerated soymilk powders The proximate analyses of the dierent agglomerated soymilk samples are presented in Table 7. As would be expected, the total carbohydrates content of the agglomerated powders increased, whereas protein, fat, and ash contents decreased with increasing the binder concentrations. However, it is known that composition of dehydrated soymilk without additives should contain about 4050% protein, 2126% fat, and 2030% carbohydrate (Wijeratne, 1993). Therefore, the compositions of the agglomerated soymilk powders obtained in this study have not been adversely aected by the addition of the binder in the concentration range tested. 3.6. Physical and morphological characteristics of agglomerated soymilk powders Physical properties of the agglomerated soymilk powders as a function of binder concentrations are presented in Table 8. The spray-dried soymilk (control) from which the agglomerates were produced was also included for comparative purposes. The moisture contents of the agglomerated powders are acceptable for this product (Wijeratne, 1993). In general, the mean particle sizes of the soymilk agglomerates were more than an order of magnitude larger than that of the control. The size distributions were generally found to be in good agreement with the lognormal distribution (R2 = 0.9500.972). The mean particle

size increased with increasing binder concentrations up to 10% and then decreased with further increments. The agglomeration of soymilk powder also occurred by using pure water, i.e. 0% binder concentration, indicating that a part of the soymilk powder dissolved during agglomeration which eventually acted as a binder. The particle size distributions of agglomerated soymilk powders obtained with dierent binder concentrations are presented in Fig. 5. The agglomerated powders obtained with 0% and 20% binder exhibited high percentage of the ne particles retained on the pan. In contrast, those obtained with 5%, 10%, and 15% binder had high percentage of the coarse particles (>300 lm) with negligible amounts of the nes. This result indicates that the binder

Fig. 5. Particle size distributions of agglomerated soymilk powders produced from spray-dried soymilk (control) powder and aqueous solution of maltodextrin of dierent concentrations as a binder.

Table 7 Proximate analyses (% w/w, dry basis) of agglomerated soymilk powders produced from spray-dried soymilk (control) powder with dierent binder concentrations Binder concentration (%) ControlA 0 5 10 15 20 Protein 48.79 1.04ab 49.77 0.18a 48.02 0.80b 45.78 0.35c 43.21 0.22d 41.91 0.24d Fat 28.77 0.36a 27.91 0.29a 26.17 0.35b 25.08 0.48c 23.51 0.29d 21.85 0.36e Ash 4.97 0.01a 4.62 0.05b 4.39 0.01c 4.28 0.06d 4.10 0.04e 4.29 0.05cd Carbohydrate 17.47 1.40e 17.70 0.16e 21.42 1.02d 24.86 0.83c 29.17 0.13b 31.95 0.11a

Assays were performed in triplicate. Mean SD values in the same column with dierent superscripts are signicantly dierent (p 6 0.05). A Control is a spray-dried soymilk powder without agglomeration.

Table 8 Physical properties of agglomerated soymilk powders produced from spray-dried soymilk (control) powder with dierent binder concentrations Binder concentration (%) Control 0 5 10 15 20
A

Moisture (%) 4.45 0.11 3.70 0.23c 4.48 0.31ab 4.63 0.46ab 4.28 0.05bc 5.02 0.19a
ab

Particle size (lm) 14.54 0.16 131.20 2.25 243.61 1.49 259.57 1.47 222.76 1.51 116.95 2.64

qbulk (g/cm3) 0.21 0.00 0.31 0.00b 0.27 0.01d 0.31 0.00b 0.32 0.01a 0.29 0.00c
e

qtapped (g/cm3) 0.35 0.00 0.46 0.00b 0.35 0.00e 0.38 0.00d 0.45 0.01c 0.47 0.00a
e

qparticle (g/cm3) 1.25 0.00 1.11 0.00b 1.11 0.00b 1.04 0.06b 1.07 0.06b 1.11 0.00b
a

Porosity (%) 72.00 0.00a 58.56 0.00c 68.47 0.00a 63.26 2.18b 58.27 2.87c 57.66 0.00c

Assays were performed in triplicate. Mean SD values in the same column with dierent superscripts are signicantly dierent (p 6 0.05). A Control is a spray-dried soymilk powder without agglomeration.

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concentrations aected both the mean particle sizes (Table 8) and size distributions (Fig. 5) of the resultant agglomerated powders which in turn inuenced their physical and reconstitution properties. The variation of the particle sizes with binder concentrations could be interpreted that at lower binder concentrations, the particles were coated with only a small proportion of binder which bonded powder particles together, while at higher binder concentrations, the binder started to spread over the particles in several layers and the cohesion of binder molecules to each other was such that powder particles were not bonded to each other by a binder ek, Pis ek, Trojak, & Src ic , 2000; Rohera & bridge (Planins }s, Src di, ic , & Pintye-Ho Zahir, 1993; Tu ske, Regdon, Ero 2005). Therefore, when the amount of binder added to the powder was increased, the friability of the agglomerates became higher. Also, at the equilibrium agglomeration state, the weight of the agglomerate exceeded the strength of the interparticle bond. The gravitational force due to the weight of agglomerates along with forces of shearing among the particles and between particles and uidizing chamber, induced by the uidizing air, caused the agglomerates to break apart, consequently, reduced the particle size (Mort, 2005; Rohera & Zahir, 1993; Tan et al., 2006). Turchiuli, Eloualia, et al. (2005) also found that agglomerates of zein particles obtained with the 14.3% maltodextrin DE 12 solution were larger and more irregular than those obtained with the 28.6% solution. This was due to the agglomerates obtained with the higher binder concentration were more friable, while they being subjected to attrition during the process preventing their growth and leading to regular shaped particles. The eect of viscosity of the binder solutions could be negligible in this study due to the very low viscosity of the solutions in the concentration range used. For 20% binder concentration, the viscosity of the solution was 3.1 mPa s at a shear rate of 132 s1 and 25 C. The bulk and tapped densities of the agglomerated powders were signicantly higher, whereas their intergranular porosities were lower than those of the spray-dried powder (Table 8). This can be interpreted mainly as the eect of size enlargement. As particle size increased, the cohesivity of powder was expected to decrease. A more free-owing powder should have a higher bulk density, as the interparticle forces between particles become weaker, therefore powder should pack in a denser condition (Abdullah & Geldart, 1999). When the above physical properties were compared among the agglomerates obtained with dierent binder concentrations, the inuences of both the mean particle sizes (Table 8) and particle size distributions (Fig. 5) should be accounted for their dierences. The agglomerates containing the ne particles, i.e. those obtained with 0% and 20% binder, showed signicantly higher tapped densities but lower porosities than those without the nes, i.e. those obtained with 5% and 10% binder. This can be attributed to the occupation of the ne particles in the voids between the large particles as pointed out by Abdullah

and Geldart (1999). The agglomerate obtained with 15% binder had high amounts of the small particles (<90 lm) so that its tapped density and porosity were similar to those containing the ne particles. The bulk densities of all agglomerates, however, were not much dierent, indicating that their structural strength was similar under the inuence of gravity. The particle density of the agglomerated powders was signicantly (p 6 0.05) lower than that of the spray-dried powder, indicating a more porous structure of the agglomerates. The particle density seemed to be constant for all the agglomerates produced with the dierent binder concentrations. This means they had similar intragranular porosity. The agglomerated powders obtained in this study had a loose, porous structure and an irregular shape (Fig. 6). The thicker maltodextrin layers were found on the surface of agglomerates obtained with the higher binder concentrations particularly with the 20% concentration (Fig. 6e). The particle sizes estimated from the visual inspection of the micrographs are consistent with those determined by the sieve analysis. 3.7. Handling and reconstitution properties of agglomerated soymilk powders The Carr index (CI) and Hausner ratio (HR) of the spray-dried (control) and agglomerated soymilk powders obtained with dierent binder concentrations are presented in Table 9. Size enlargement by agglomeration seemed to improve ow characteristics of the powders. The agglomerates obtained with 10% binder concentration exhibited a good owability and low cohesiveness as classied by the CI and HR values given in Tables 1 and 2, respectively. In contrast, the smaller particle sizes and the presence of the ne particles obtained with the higher or lower binder concentrations gave poorer ow characteristics as evidenced by their higher CI and HR values as compared with those of the agglomerate obtained with 10% binder. Clearly, the mean particle size and particle size distribution had a major inuence on powder owability. The coarser powder in the absence of the ne particles owed better, as expected. These observations are in agreement with the ndings of other studies (Fuchs et al., 2006; NDri-Stempfer et al., 2003; Turchiuli, Eloualia, et al., 2005; Turchiuli et al., 2005; Vu et al., 2003). The eects of binder concentration on particle size, wettability, and dispersibility of the agglomerated soymilk powders are shown in Fig. 7. It can be seen that the wettability markedly increased from the wetting time of 218 s to a satisfactory mean value of 42 s with an increase in binder concentrations from 0% to 10% and then decreased sharply to 197 s at 20% binder concentration. This is opposite to the variation in particle sizes with binder concentrations. The dispersibility increased from 41.5% to 60.8% with increasing binder concentrations from 0% to 10% and then decreased to 52.8% at 20% binder concentration. It is known that size enlargement by

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Fig. 6. Scanning electron micrographs of agglomerated soymilk powders produced from spray-dried soymilk (control) powder and aqueous solution of maltodextrin of dierent concentrations as a binder: (a) 0%, (b) 5%, (c) 10%, (d) 15%, and (e) 20% w/v at 500 magnication.

agglomeration not only increases the rate of water penetration into the space between the agglomerates, but also the capillary-driven ow of water into the ne pores within the agglomerates and consequently shortens the , 2003; Hla & Hogekamp, 1999; wetting time (Caric Knight, 2001; Schubert, 1993). Hla and Hogekamp
Table 9 Flow characteristics (Carr index, CI, and Hausner ratio, HR) of agglomerated soymilk powders produced from spray-dried soymilk (control) powder with dierent binder concentrations Binder concentration (%) Control 0 5 10 15 20
A

(1999) pointed out that agglomerates with higher content of the ne particles showed longer wetting time which conrmed our results in case of the agglomerates obtained with 0% and 20% binder concentrations.

CI (%) 40 0 33 0b 22 2d 18 0e 28 1c 38 0a
a

HR 1.67 0.00a 1.48 0.00c 1.28 0.03e 1.23 0.00f 1.38 0.02d 1.62 0.00b Fig. 7. Eect of binder concentration on the mean particle size, wettability, and dispersibility of agglomerated soymilk powders.

Assays were performed in triplicate. Mean SD values in the same column with dierent superscripts are signicantly dierent (p 6 0.05). A Control is a spray-dried soymilk powder without agglomeration.

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From the point of view of dispersibility, the particle adhesion within the agglomerates should be strong enough to avoid abrasion during packaging and transportation, but should largely dissolve in an aqueous environment, preferably with minimum mechanical energy. In the reconstituted dispersion, the particles should neither oat to the surface nor sediment to the bottom of the container within a certain time period (Schubert, 1993). The dispersibility of the agglomerates obtained with the 10% binder was the highest among the other samples probably due to their highest particle size, owability, and wettability (Vu et al., 2003). Surprisingly, the powder agglomerated with water only (0% binder) had a lower dispersibility than the original spraydried powder (41.5% vs 62.3%). This could be due to the particle adhesion within the agglomerates being too strong to separate easily on contact with water. However, the dispersibility of all the agglomerated powders (<61%) was much lower than that of the spray-dried powders obtained with the ultraltered soymilk concentrates (8494%; Table 6). This could be improved probably by modifying agglomeration conditions and/or by using other binder materials such as maltodextrins with dierent DE values. In general, the best particle size for rapid dispersion during reconstitu , 2003; Schubert, 1993). From tion is 150200 lm (Caric these results, therefore, it can be concluded that the optimum binder concentration is 10% w/v maltodextrin. However, no test was carried out on the agglomeration of the spray-dried powders produced from ultraltered soymilk concentrates, as there were only limited amounts of the powders available, and at the time this experiment was performed most of the samples were used up for the chemical and physical tests of the primary powders. Nevertheless, it is interesting to further investigate if the dispersibility of the agglomerates could be improved like the spraydried powders. 4. Conclusions It was possible to produce instant soymilk powders in a three-stages process consisting of ultraltration, spray drying, and uidized bed agglomeration. Ultraltration concentrated soymilk up to 20% solids content, leading to an increase in viscosity, a small change in the proximate composition, and consequently an increase in particle size of the resultant spray-dried powders. However, handling and reconstitution properties of the powders, i.e. owability and wettability, were very poor probably due to their very small size (<25 lm). Fluidized bed agglomeration of these spray-dried powders was carried out by varying the binder (maltodextrin) concentrations from 0% to 20% w/ v. The optimum concentration was found to be 10% which gave the agglomerated powder of the highest particle size (260 lm) and in turn the best handling and reconstitution properties. Despite the powder wettability being increased to an acceptable value (42 s), its dispersibility (61%) was not suciently improved. This is an aspect requiring further improvement.

Acknowledgements This study was supported in part by the Thesis Scholarships for Masters degree students, Faculty of Graduate Studies, Mahidol University in the academic year 2004 and by the Higher Education Development Project, Subproject: Graduate Study and Research in Agricultural Biotechnology, Ministry of Education. The authors would like to thank Green Spot (Thailand) Ltd. (Pathum Thani, Thailand) for providing the soymilk samples used in these experiments. References
Abdullah, E. C., & Geldart, D. (1999). The use of bulk density measurements as owability indicators. Powder Technology, 102, 151165. Ang, H. G., Kwik, W. L., Lee, C. K., & Theng, C. Y. (1986). Ultraltration studies of foods: Part 1 The removal of undesirable components in soymilk and the eects on the quality of the spray-dried powder. Food Chemistry, 20, 183199. AOAC (2000). Ocial methods of analysis (17th ed.). Gaithersburg, MD, USA: Association of Ocial Analytical Chemists. A/S Niro Atomizer, Copenhagen, Denmark (1978a). Determination of wettability. In I. H. Srensen, J. Krag, J. Pisecky, & V. Westergaard (Eds.), Analytical methods for dry milk products (4th ed., pp. 2627). Copenhagen: De Forenede Trykkerier A/S. A/S Niro Atomizer, Copenhagen, Denmark (1978b). Determination of dispersibility. In I. H. Srensen, J. Krag, J. Pisecky, & V. Westergaard (Eds.), Analytical methods for dry milk products (4th ed., pp. 3233). Copenhagen: De Forenede Trykkerier A/S. A/S Niro Atomizer, Copenhagen, Denmark (1978c). Determination of particle density, content of occluded air and interstitial air. In I. H. Srensen, J. Krag, J. Pisecky, & V. Westergaard (Eds.), Analytical methods for dry milk products (4th ed., pp. 5253). Copenhagen: De Forenede Trykkerier A/S. Bhandari, B. R., Datta, N., & Howes, T. (1997). Problems associated with spray drying of sugar-rich foods. Drying Technology, 15, 671684. , M. (2003). Milk powders: Types and manufacture and physical and Caric functional properties of milk powders. In H. Roginski, J. W. Fuquay, & P. F. Fox (Eds.), Encyclopedia of dairy sciences (pp. 18691880). New York: Academic Press. Carr, R. L. (1965). Evaluating ow properties of solids. Chemical Engineering, 72, 163168. Fitzpatrick, J. J. (2005). Food powder owability. In C. Onwulata (Ed.), Encapsulated and powdered foods (pp. 247260). Boca Raton, FL: CRC Press. Fitzpatrick, J. J., Iqbal, T., Delaney, C., Twomey, T., & Keogh, M. K. (2004). Eect of powder properties and storage conditions on the owability of milk powders with dierent fat contents. Journal of Food Engineering, 64, 435444. Fuchs, M., Turchiuli, C., Bohin, M., Cuvelier, M. E., Ordonnaud, C., Peyrat-Maillard, M. N., et al. (2006). Encapsulation of oil in powder using spray drying and uidised bed agglomeration. Journal of Food Engineering, 75, 2735. Hausner, H. H. (1967). Friction conditions in a mass of metal powder. International Journal of Powder Metallurgy, 3, 713. Hla, P. K., & Hogekamp, S. (1999). Wetting behaviour of instantized cocoa beverage powders. International Journal of Food Science and Technology, 34, 335342. Keogh, M. K., Murray, C. A., & O Kennedy, B. T. (2003). Eects of ultraltration of whole milk on some properties of spray-dried milk powders. International Dairy Journal, 13, 9951002. Knight, P. C. (2001). Structuring agglomerated products for improved performance. Powder Technology, 119, 1425.

N. Jinapong et al. / Journal of Food Engineering 84 (2008) 194205 Liu, K. S. (1997). Soybeans: Chemistry, technology, and utilization. New York: Chapman & Hall. Masters, K. (1991). Spray drying handbook (5th ed.). Essex, UK: Longman Scientic & Technical. Mort, P. R. (2005). Scale-up of binder agglomeration processes. Powder Technology, 150, 86103. NDri-Stempfer, B., Oulahna, D., Eterradossi, O., Benhassaine, A., & Dodds, J. A. (2003). Binder granulation and compaction of coloured powders. Powder Technology, 130, 247252. Omosaiye, O., Cheryan, M., & Matthews, M. E. (1978). Removal of oligosaccharides from soybean water extracts by ultraltration. Journal of Food Science, 43, 354360. Ortega-Rivas, E. (2005). Handling and processing of food powders and particulates. In C. Onwulata (Ed.), Encapsulated and powdered foods (pp. 75144). Boca Raton, FL: CRC Press. Parikh, D. M., Bonck, J. A., & Mogavero, M. (1997). Batch uid bed granulation. In D. M. Parikh (Ed.), Handbook of pharmaceutical granulation technology (pp. 227302). New York: Marcel Dekker, Inc.. Perez-Munoz, F., & Flores, R. A. (1997a). Characterization of a spray drying system for soymilk. Drying Technology, 15, 10231043. Perez-Munoz, F., & Flores, R. A. (1997b). Particle size of spray-dried soymilk. Applied Engineering in Agriculture, 13, 647652. ek, O., Pis ek, R., Trojak, A., & Src ic , S. (2000). The utilization of Planins surface free-energy parameters for the selection of a suitable binder in uidized bed granulation. International Journal of Pharmaceutics, 207, 7788. Pomeranz, Y. (1991). Functional properties of food components (2nd ed.). California: Academic Press, Inc.. Ramaswamy, H., & Marcotte, M. (2006). Food processing: Principles and applications (pp. 317377). Boca Raton, FL: CRC Press.

205

Rohera, B. D., & Zahir, A. (1993). Granulations in a uidized-bed: Eect of binders and their concentrations on granule growth and modeling the relationship between granule size and binder concentration. Drug Development and Industrial Pharmacy, 19, 773792. Schubert, H. (1993). Instantization of powdered food products. International Chemical Engineering, 33, 2845. Schuchmann, H. (1995). Production of instant foods by jet agglomeration. Food Control, 6, 95100. Shittu, T. A., & Lawal, M. O. (2007). Factors aecting instant properties of powdered cocoa beverages. Food Chemistry, 100, 9198. SPSS for Windows (2003). Users manual, version 12.0. Chicago, IL: SPSS Inc. Tan, H. S., Salman, A. D., & Hounslow, M. J. (2006). Kinetics of uidised bed melt granulation I: The eect of process variables. Chemical Engineering Science, 61, 15851601. Turchiuli, C., Eloualia, Z., El Mansouri, N., & Dumoulin, E. (2005). Fluidised bed agglomeration: Agglomerates shape and end-use properties. Powder Technology, 157, 168175. Turchiuli, C., Fuchs, M., Bohin, M., Cuvelier, M. E., Ordonnaud, C., Peyrat-Maillard, M. N., et al. (2005). Oil encapsulation by spray drying and uidised bed agglomeration. Innovative Food Science and Engineering Technologies, 6, 2935. }s, I., Src di, K. (2005). The role ic , S., & Pintye-Ho Tu ske, Z., Regdon, G., Ero of the surface free energy in the selection of a suitable excipient in the course of a wet-granulation method. Powder Technology, 155, 139144. Vu, T. O., Galet, L., Fages, J., & Oulahna, D. (2003). Improving the dispersion kinetics of a cocoa powder by size enlargement. Powder Technology, 130, 400406. Wijeratne, D. B. T. (1993). Spray drying of soymilk. Ph.D. Thesis, University of Illinois at Urbana-Champaign.