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Critical Reviews in Food Science and Nutrition, 51:432–441 (2011) Copyright C Taylor and Francis Group, LLC ISSN: 1040-8398 print / 1549-7852 online DOI: 10.1080/10408391003646270

print / 1549-7852 online DOI: 10.1080/10408391003646270 Agglomeration of Food Powder and Applications K.

Agglomeration of Food Powder and Applications

K. DHANALAKSHMI, S. GHOSAL and S. BHATTACHARYA

Food Engineering Department, Central Food Technological Research Institute, (Council of Scientific and Industrial Research), Mysore 570020, India

Agglomeration has many applications in food processing and major applications include easy flow table salt, dispersible milk powder and soup mix, instant chocolate mix, beverage powder, compacted cubes for nutritional-intervention program, health bars using expanded/puffed cereals, etc. The main purpose of agglomeration is to improve certain physical properties of food powders such as bulk density, flowability, dispersability, and stability. Agglomerated products are easy to use by the consumers and hence are preferred over the traditional non-agglomerated products that are usually non-flowable in nature. The properties of food agglomerates and the process of agglomeration like employing pressure, extrusion, rewetting, spray- bed drying, steam jet, heat/sintering, and binders have been reviewed. The physical and instant properties of agglomerated food products have also been discussed.

Keywords agglomeration, food powders, binder, functional properties

INTRODUCTION

AGGLOMERATION

Powdery food materials are frequently used for convenience in applications during transportation, handling, processing, and for product formulations. A variety of food powders having a different source are used to serve specific purposes including improving sensory appeal and nutritional status of finished prod- ucts. Powders are characterized in terms of size, shape, and their functionality, while there is a lack of knowledge about their be- havior under varying temperatures and moisture contents. With the increasing quantity of different powders like beverage pow- ders (coffee, tea, cocoa, milk, etc.), table salt, spice powders, cereal and pulses flour, additives, etc., are being produced in food industries, there is a need for detailed information about their handling and processing characteristics, especially for food powders, and because of their complexity. Food powders are occasionally used as such though their main use lies in further processing for developing different products (Table 1). Among the various frequently used processes the food powders undergo, the steps like agglomeration, compaction, instantization and en- capsulation are practiced to get products with specific purposes and for convenience.

Address correspondence to S. Bhattacharya, Food Engineering Department, Central Food Technological Research Institute, Council of Scientific and Indus- trial Research, Mysore 570020, India. Tel.: 0821-2513910, Fax: 0821-2517233. E-mail: suvendu@cftri.res.in

Agglomeration, in general, can be defined as a process dur- ing which primary particles are joined together so that bigger porous secondary particles (conglomerates) are formed (Palzer, 2005). According to this definition, even caking of hygroscopic raw materials during storage can be regarded as a kind of un- desired agglomeration. Agglomeration is basically a physical phenomenon and can be described as the sticking of particulate solids, which is caused by short-range physical or chemical forces among the particles themselves as a result of physi- cal or chemical modifications of the surface of the solid. This phenomenon is triggered by specific processing conditions, or binders and substances which adhere chemically or physically on the solid surfaces to form a bridge between particles (Pietsch,

2003).

The process of agglomeration can be applied to many food and non-food items. The non-food applications include the man- ufacture of ceramic objects formed by granular materials from kaolin, feldspar, silica and silicon carbide, fish and mammal feeds, household products (detergents for fabrics, dish, and hard surface cleaning), microbiological products (enzyme, yeast, and bacterial granules), and a number of pharmaceutical products like feed stock for tabletting, pellets, and encapsulates. The ag- glomeration of food powders is of recent interest in which the control of porosity and density of material is the main interest. These have practical application like dispersability, wettability,

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AGGLOMERATION OF FOOD POWDER AND APPLICATIONS

Table 1 Different functional applications of food powder

433

Function

Details of function

Raw materials

Specific applications

Reference

Used directly

Food additive, taste improver

Salt, spice and sugar powder, milk powder, beverage powder

Spray or drum dried milk powder, baby foods, coffee, tea

Bergquist et al., 1992; Nasirpour et al., 2006; Hogekamp et al., 1996; Colarow, 2006; Sherwood et al., 2008 Snow et al., 1999; Kimura and Teraunchi, 1999; Haefliger et al., 2001; Pietsch, 2005 Teunou and Poncelot, 2002; Jinapong et al., 2008; Kowalska et al., 2005

Requires further processing

Developing granulated and compacted items

Cereal starch/flour, puffed cereals and pulses

Bouillon cubes, compressed bars/cubes, chocolate bars, granulated products and soup mixes Salt-spicy snacks, confectionery, sugar coated products

Coating material

To add taste and flavor like sweet/salty, chocolate, antisticking agents and to improve appearance, and adding nutrients Suitable as a food component only after significant processing

Cereal/pulse flour, sugar, salt, maltodextrin, spices, vitamins/minerals, artificial sweeteners, herb/plant extracts Corn flour/starch, rice/wheat/pulse powder, protein concentrates/isolates, modified starches, casein, egg powder Starches, crude gelatin, gums, pectin Yeast media, bacterial culture, enzymes

Intermediate raw material

Soup mix, traditional product like pan cake, dosa/idli, high protein foods like meat analogues

Cunningham, 2007; Takeiti et al., 2008; Pietsch, 2005

Minor ingredient

Increasing consistency and for gelling Microbial culture in dried form

Snacks, jams, jellies, desserts, soups, sauces Formulations containing lactic acid bacteria, yeast powder Cheese flavored extruded snacks, mixed spice flavor Onion/garlic/potato/ tapioca/mango powders, fruit-based beverage powder Bread crumb, rolling/sheeting machines

Zhao and Bertrand, 2007; Caspers et al., 2001 Harkonen et al., 1993

Microbial source

Flavoring

Natural and synthetic flavors

Cheese, spices

Fuchs et al., 2006; Buffo

Fruit and vegetable powders Adds specific fruit and vegetable taste

Dehydrated fruits and vegetables

et al., 2002; Stahl, 2005 Pietsch, 2005; Cremer, et al.,

2008

Aid for drying

Provides a non-sticky surface

Cereal starches/flour

Takeiti et al., 2008 |

sinkability, and solubility. Agglomeration is also referred to as intantizing, because rehydration and reconstitution are impor- tant properties of foods that decide its convenience at domestic as well as industrial sectors. Agglomerates have both coarse and open structures varying from 0.1 to 3 mm. Agglomeration im- proves the dispersability of the formed products that are wetted uniformly when put in either cold or hot water. The present article focuses on different processes of agglom- eration and applications of agglomerated products in food and allied industries. The associated mechanism of formation and structure of the agglomerated products is also discussed.

APPLICATIONS

The major applications of agglomeration in food include easy flow table salt, dispersible milk powder and soup mix, instant chocolate mix and beverage powder, compacted cubes for nutritional intervention programme, health bars using ex- panded/puffed cereals, etc. (Table 1). Compacted cubes may be defined as the cuboids having high density that are made out of powdery food ingredients by the application of pressure.

The most common application of punch-and-die presses in the food industry is for the production of bouillon cubes with di- mensions typically in the range 13–15 mm (Pietsch, 2005). In the context of instantizing, the technique of tumble/growth ag- glomeration is frequently used in the food industries to improve the reconstitutability of a number of products including flour, cocoa powder, instant coffee, dried milk powder, sweeteners, fruit beverage powder, instant soup, and spice. Extrusion is ex- tensively used for shaping the product during the manufacture of a variety of ready-to-eat breakfast cereals (Barbosa-Canovas et al., 2005). A major application of the agglomeration process is in the production of instant products in which primary particles are agglomerated to give a granule-shaped product with improved wettability, dispersability, and dissolution characteristics com- pared to the original primary particles. Food particulates are encapsulated to increase shelf life, masking taste or odor, and improving appearance. Coated agglomerated granules are pro- duced for controlled release of constituents within the particle by providing a coating which dissolves at a given rate in a particular temperature or pH, or to protect unstable ingredients from degradation by heat, moisture, or light (Dewettinck and Huyghebaert, 1998; Teunou and Poncelet, 2002). The materials

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used for coating in food industries are mainly water-soluble biopolymers, lipids, milk proteins or corn proteins, gums such as locust bean gum, carboxymethylcellulose, sodium alginate and kappa-carrageenan, protein concentrates (sodium caseinate, lysozyme), blood plasma concentrate (Dewettinck et al., 1998), gelatin and starch hydrolysates (Dewettinck et al., 1999), and lipids (Eichler, 1996). A process for the production of granular cocoa (Kimura and Teranchi, 1999), agglomerated powdered beverage (Camp and Fischbach, 1990), a gelling aid consisting of particulate sugar (Caspers et al., 2001) and granulation of protein-rich fraction of flour (Berizzi, 2004) have been patented in which agglomera- tion is a critical processing step. Table 1 lists the products and the materials that are used to prepare agglomerated products (Knight, 2001). The patented processes include the production of instant powder (Strommen et al., 2001), infusing flavors into cereal grains and the agglomeration of grains into a unitary food product (Capodieci, 2002), methods for binding agglomerated proteins (Grossman et al., 2007), and agglomerated starch prod- uct which has improved flow properties and disintegrates at sub- stantially the same rate in media of varying pH (Cunningham, 2007). Zhao and Bertrand (2007) have developed a method for producing instantly dispersible pregelatinized starches for dif- ferent food products. The list of products includes fish and dairy products of commercial importance; microbial products and en- zyme granules also find the applications in different food and pharmaceutical industries. As an example, the flow chart for the production of instant agglomerated soymilk powder is pre- sented in Fig. 1 which shows the use of maltodextrin as a binder (Jinapong et al., 2008). Applications of agglomeration also include production of ar- tificial sweeteners (Fotos and Bishay, 2001), a granular flavoring for chewing gum that facilitates for enhanced flavor retention (Hyodo et al., 2003), and a free-flowing granular dried soup mix

Soybean

Soaked, heated to 70-80 o C for 10-15 min, ground with water and extracted

Soymilk

Concentrated at 40 o C using ultrafiltration unit

Concentrated soymilk

Spray dried

Spray dried soymilk

Maltodextrin

Agglomeration in a top spray fluidized bed granulator

Instant agglomerated soymilk powder

Figure 1 Flowchart for the production of instant soymilk powders.

with relatively narrow particle size distribution to aid dispersion (Haefliger et al., 2001). Besides the mentioned agglomerated and granulated products, there exists ample scope to develop many more such convenience products. Table 2 gives the list of the various applications of agglomeration processes in food and allied industries.

AGGLOMERATION PROCESSES

The process of agglomeration may be conducted in several ways in conjunction with other unit operations such as spraying, steaming, and drying. The selection of a specific agglomeration process depends on several factors including physical and chem- ical properties, average particle sizes of initial raw material(s) and product, thermal sensitivity, and on the requirement of spe- cial properties like instant solubility, easy flowability, etc. The technologies applied vary widely in their process conditions and adhesion principles to bind the primary particles together. The commonly used agglomeration processes can be divided into three groups (Schuchmann, 1995; Pietsch, 2002; Hogekamp et al., 1996) like (a) pressure agglomeration (e.g., tableting), (b) growth agglomeration (e.g., granulation, pelleting) such as wet agglomeration and dry agglomeration and (c) agglomeration by drying (e.g., spray drying). Depending on whether or not a binder liquid is involved in the process, it can be subdivided into “wet” and “dry” agglomera- tion methods. Each method exploits certain binding mechanisms (Ennis et al., 1991) for granulation. For wet growth agglomera- tion processes, the term “granulation” is often used. The subse- quent sections describe the different processes of agglomeration that is frequently used in agri-food processing industries.

Pressure Agglomeration

Compaction is a process whereby small particles are bound together to form larger cohesive masses in which the original particles can still be identified (Snow et al., 1999). Examples of dry granulation methods are roll compaction and uniaxial die compaction. Dry granulation is of particular interest in industry as the final product requires no liquid binder and drying process, and therefore costs less to operate as it requires simpler equip- ment (Augsburger and Vuppala, 1997). It has special advantage for handling of moisture sensitive material. In pressure agglomeration, compressive force acts on a con- fined mass of particulate solids, which are then shaped and densified. Pressure agglomeration is normally carried out in two stages; the first stage comprises a forced rearrangement of particles due to applied pressure, and the second step consists of a steep pressure rise during which brittle particles break and malleable particles deform plastically. The success of compression or compaction agglomeration process depends on the effective utilization and transmission of the applied external force, and on the ability of the material

AGGLOMERATION OF FOOD POWDER AND APPLICATIONS

Table 2 Application of agglomeration processes in food and allied industries

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Technology

Method

Equipment

Application

Reference

Agitation Methods

Tumbling agglomeration

Rotary drums, pans, bowl and plate granulators Horizontal pan, pin mixer Powder blenders like conical, vertical shaft, ribbon mixers, agglomerators, flow jet mixing systems Compacting/tabletting presses Compacting rolls Piston/screw extrusion systems Vertical jet agglomeration Fluidised bed dryers Spray dryers

Fruit and vegetable powders Cereal powder/starch Beverage powder, cereal powder/starch

Pietsch, 2005; Cremer et al., 2008 Cunningham, 2007 | Kowalska and Lenart

Mixer agglomeration

Powder clustering

 

2005

Pressure methods

Piston/rotary type

Bouillon cubes,

Snow et al., 1999; Pietsch, 2005 Snow et al., 1999 Pietsch, 2005

compaction

nutritional bars

Roll pressing

Health bars

Extrusion

Cereal powder/starch

Thermal methods

Steam jet agglomeration Fluidised bed Spray drying

Cereal powder/starch Milk powder, baby food Milk powder, coffee granules, ice cream mixes, flavors, lipids, caroteniods Milk powder, baby food, cereal flour Cereal powder/starch

Hogekamp et al., 1996 Buffo et al., 2002 Vega et al., 2005; Gharsallaoui et al.,

2007

Spray and dispersion methods

 
 

Spray onto dispersed powder Agglomeration in liquid media

Fluidized/sprouted beds

Thomas et al., 2004; Nasirpour et al., 2006 Buffo et al., 2002

Ribbon mixers

to form and maintain inter-particle bonds during pressure com- paction (or consolidation). This aspect is controlled in turn by the geometry of the confined space, the nature of the applied loads, and the physical properties of the particulate material and of the confining walls (Snow et al., 1999). The different advantages of compaction agglomeration include an increase in product density and requirement of a small amount of liq- uid binder. Compaction agglomeration is carried out by using the equipment like the piston and moulding presses, tabletting presses, and roll presses. Tablet presses require highly flowable feed material to uniformly fill the press chambers prior to com- paction. Uniformity of particle size, particle shape, roughness of surface, cohesiveness due to the chemical nature of the com- pound, and moisture content contribute to the flow and filling of the tablet presses (Snow et al., 1999). High-pressure agglomeration is characterized by a large de- gree of densification resulting in low-product porosity. Typi- cally, the products from high-pressure agglomeration feature high strength immediately after discharge from the equipment. Low and medium pressure agglomeration yield relatively uni- form agglomerates of elongated spaghetti-like or cylindrical shape, whereas high-pressure agglomeration produces pillow or almond-like shapes (Barbosa Canovas et al., 2005). Mukherjee and Bhattacharya (2006) and Ghosal et al., (2010) reported the inter-relationship between rheology of powder and texture of compacted mass using model food powder system in presence of binders. One of the most common binding mechanisms in these pro- cesses is caused by the short-range molecular attraction forces, that is, electrostatic and van der Waals forces, rather than solid bridging forces. Because these forces are reduced in liquids by

a factor of around 10, the particles bonded by them can disperse easily in liquid, exhibiting expected instant properties (Pietsch,

1999).

Extrusion Agglomeration

In pressure agglomeration, applying external forces to partic- ulate solids in more or less closed dies forms new and enlarged entities. Pressure or press agglomeration using an extruder is possible for commercial applications of size enlargement by ag- glomeration. In the extrusion agglomeration process, a powder mixture is blended with binder liquid, additives, or dispersants and then extruded at low pressure followed by drying, cooling, and crumbling to get the final instant product (Pietsch, 1999). Many food products such as snack bars and confectioneries are processed and/or finished by pressure agglomeration, mainly extrusion (Pietsch, 2005). Extrusion has also been used to en- capsulate flavors, vitamin C, and colors (Dziezak, 1988). The major advantage of extrusion is its outstanding protection of flavors against oxidation (Barbosa-Canovas et al., 2005) while being a commercially-viable continuous-processing technique.

Tumbling of Powders (Rewetting Agglomeration)

The tumbling agglomeration involves both disintegration of weaker bonds and re-agglomeration by abrasion transfer and co- alescence of larger units. Coalescence occurs at contact points and additional growth of the agglomerate may proceed by fur- ther coalescence, or by layering, or both. The particles to be

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agglomerated are larger; however, the particle-to-particle adhe- sion needs to be increased by the addition of binders, such as water or other more viscous liquids, depending on the properties of the particles being agglomerated and the required strength of the agglomerate structure (Barbosa-Canovas et al., 2005). In food industries, most units use static and vibrating flu- idized beds to mix the powder, promote inter-particle collisions and dry the granules (Coucoulas, 1992). Granules are formed by shear processing in planetary mixers, ribbon blenders, Z-blade units, and high-speed intensive mixers. For example, granulated enzyme products can be manufactured by mixing enzyme solu- tion with a suitable filler to form dough, which is then pressed into fine granules. The granules are then sprayed with a suit- able binder and further dried in a fluidized bed dryer (Harkonen et al., 1993). Sometimes, a large amount of fine products are reprocessed, causing economical burden to this technology.

Straight through Agglomeration

A liquid concentrate is used in this process. When powders

are produced by spray drying, the agglomeration process can be accomplished in a fluidized bed connected directly to the spray dryer, where the operating conditions can be controlled so that the partially dried particles formed in the upper part of the dryer are still sticky. Fine particles, either from recycle or the drying chamber, are fed into an external fluidized bed to undergo cluster formation. Sometimes, steam or atomized water can be injected into the fluidized bed to assist in the agglomeration process. Final drying and cooling are also accomplished in the bed, and the agglomerated product is removed for storage or packaging. This procedure is more adequate for coffee and baby foods (Masters and Stoltze, 1973), skim and whole milk, non- caking whey, milk replacer, and ice cream mix. In instant whole milk production, the straightthrough process is followed by the addition of lecithin that improves wettability and dispersability.

Spray-bed Dryer Agglomeration

A fluidized bed is integrated into a spray dryer chamber, com-

bining spray drying with fluidized-bed agglomeration. Particles formed in the spray drying-zone enter the integrated fluidized bed at the bottom of the dryer with high moisture content, and become agglomerated in the bed where they are vigorously ag- itated by high fluidization velocity (Quek et al., 2007; Gong et al., 2008). An external fluidized bed is connected to the inte- grated fluidizer for final product drying and cooling. This type of dryer is most suitable for small to medium sized plants and can produce agglomerated powder with excellent properties. As an example, the flow chart for the production of granular encap- sulated flavor powder has been cited in Fig. 2 where maltodex- trin/gum acacia/modified starch have been used as a carrier of flavor. The raw materials are subjected to agglomeration using a fluidized bed granulator (Buffo et al., 2002).

Atomizer Wheel

This method is used when powder cannot withstand a forceful agglomeration process or where small-sized agglomerates are desired. The layout closely resembles the agglomerating tube method. The only difference is that a rotary atomizer replaces the agglomerating tube. The powder falls around the rotating atomizing wheel and is sprayed with water or binder solution. This system is used for certain baby foods, beverage whiteners, and cocoa/sugar mixtures (Masters and Stoltze, 1973; Jinapong et al., 2008).

Steam Jet Agglomeration

Steam jet agglomeration is a continuous process, which has been used in the food industries for several years to produce agglomerates with favorable instant properties from fine pow- ders. Free falling particles are wetted by turbulent free jets of steam. The colliding wetted particles form agglomerates pro- vided that their relative kinetic energy can be dissipated by the viscous liquid layers on the particles surfaces (Schuchmann et al., 1993). The material to be agglomerated should preferably be water-soluble; insoluble or water-repellent substances can be processed if mixed with a sufficient amount of water-soluble material such as sucrose or a monosaccharide. Furthermore, the wettability of hydrophobic substances can be improved by adding a surface-active agent, for example, in the case of co- coa powder, lecithin. A typical application is instant beverages intended for reconstitution with water or milk. The steam jet- agglomeration process combines a low number of particles per

Carriers (maltodextrin/gum acacia/modified starch)

Dissolved in water at 82 o C for 45 min

Dispersion containing carrier substances

Allowed to stand overnight at room temperature

Hydrated carrier + flavour

Emulsification for 5min using a high speed mixer

Carrier-flavour emulsion (1:4)

Spray drying

Spray dried encapsulated flavour powder

Agglomeration using fluidized bed

Agglomerated encapsulated flavour powder

Figure 2 Flowchart for flavor encapsulation.

AGGLOMERATION OF FOOD POWDER AND APPLICATIONS

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unit volume with short average residence time and narrow res- idence time distribution (Schuchmann et al., 1993) to produce products with uniform size and properties. If the feed contains dry agglomerates, for example, fines bound together by van der Waals forces, these agglomerates also take up water, further stabilizing these agglomerates. After an average residence time ranging from 1 to 2 s, the particles leave the agglomeration zone and enter the drying zone. Drying of the agglomerates causes crystallization of soluble substances in the liquid bridges joining the primary particles, finally turning the liquid bridges into solid ones. On the other hand, depending on the drying rate and temperature, these bridges may consist of an amorphous structure. In any case, the agglomerates formed by collision in the wetting zone as well as any agglomerates having entered with the feed are stabilized.

Binders

Binders are adhesives that provide the cohesiveness essential for the bonding of solid particles during the process of ag- glomeration. In wet granulation process, binders promote size enlargement and thereby improve flowability of the blend dur- ing the manufacturing process. During wet massing, the binder may be dissolved in the granulating solvent, which is then added to the powder, or mixed dry with the powder and the granulat- ing solvent (generally water) (Barbosa-Canovas et al., 2005). Binders are classified as natural polymers, synthetic polymers, or sugars. Some commonly used binders in wet granulation are starch, gelatin, acacia gum, sodium alginate, alginic acid, methylcellulose, Na-carboxymethylcellulose, glucose, sucrose, and sorbitol. In the food system, binders are used in aqueous solution of lactose or dextrose, gelatine, or a food gum. In prod- uct, the nature of the binder is a major factor that determines the granule strength, attrition resistance, and granule dustiness. It affects the dispersion and dissolution properties, ingredient re- lease rate, and the chemical stability of the ingredients (Knight,

2001).

The factors influencing the binder efficiency are concen- tration, viscosity, mechanical properties of the binder, inter- particulate interactions between the binder and the substrate, and binder distribution. Binders differ in their bonding effi- ciency. For example, gelatin or acacia provide high hardness and slow disintegration to the agglomerate. Methylcellulose pro- duces granulations that compress easily. Glucose or sucrose can be applied as syrups in concentrations above 50% in wet gran- ulation processes exhibiting good bonding properties, although sucrose produces hard and brittle bridges (Barbosa-Canovas et al, 2005). In the agglomeration process, the binder provides capillary and viscous forces that give the wet granules mechan- ical strength and particularly with high shear mixer granulation. The viscosity of the binder is a very important variable affecting the rate of size enlargement, morphology of the granule, and the size distribution obtained (Mills et al., 2000; Keningley et al., 1997). A multidimensional model enables the study of critical parameters in binder granulation such as the reaction rate (so-

lidification of binder) and the size of the added binder droplets, which demonstrates its promising potential (Braumann et al.,

2007).

Agglomeration by Heat/Sintering

Sintering is a process in which the particles in a powder mass can be bonded in solid state at elevated temperatures below the melting or softening temperature of the materials. The driving force for sintering is diminution of the surface area of the as- sembly of original particles. The accessible internal surface of the particles or surface of the pores between the particles fea- tures a specific surface energy. This specific energy is due to the fact that surface atoms have no neighbors. The reduction of the

free surface leads to the reduction in surface energy. Therefore, sintering occurs with a reduction in the total surface energy and accordingly, the total free energy of the powder decrease with sintering (Pietsch, 2002). The viscosity of material can be de- creased by increasing temperature or moisture level to enable the material to build viscous bridges between the particles by viscous flow and the process is called sintering (Palzer, 2005).

A simple method for the production of chocolate beverage gran-

ules has been reported by Omobuwajo et al. (2000) wherein al- kalized cocoa powder (91–94%), malt extract (2–3%), skimmed milk powder (3–5%), and vitamins and minerals (0.5–0.8%) are

mixed with granular sugar to obtain the chocolate drink powder blend; later, it is heated over a metal plate with constant agitation

to produce instant chocolate beverage granules.

At a certain elevated temperature, atoms and molecules be- gin to migrate across the interface where particles touch each other in solid state. Depending on the temperature, time, and the intensity of contact, the diffusion of matter forms bridge-like structures between the surfaces, which solidify upon cooling. This may result in a densification of the compact, which is due

to an elimination of pores and associated shrinkage.

It is desirable to understand the nature of the bonds between particles in agglomerates that are formed during the process of agglomeration. The bonding mechanism involved is inter- molecular forces (Van der Waals force and hydrogen bond), electrostatic force, liquid bonds, solid bridges, and mechanical interlocking. The intermolecular attractive force between par- ticles is inversely proportional to the seventh power of their separation distance. As the roughness of surface increases the effective separation distance, Van der Waals forces are of low importance in granulating systems; electrostatic force is also of the same order of magnitude as the Van der Waals forces. Absorbed liquid binder layers on the particle surface have the effect of smoothing out surface roughness and thus particle sep-

aration distances tend to decrease leading to an increase in Van der Waals forces. The mobile liquid bonds have an important role during the granulation process. An increase in the quantity of liquid thus changes the nature of the bonds and influences the overall granule strength. Particles containing liquid bonds

at

the contact point between individual particles are stated to be

in

the pendular state; an increase in the liquid content gives rise

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to the funicular state, and finally to the capillary state in which the inter-particle space is saturated with liquid. Though theory on the binding of particles by liquid is avail- able, the same is not true on solid bridges between particles. The strength of such bridges depends on the amount of mate- rial present and its structure. A finer crystal structure results in stronger bonds and there exists some correlation between bond strength and higher drying temperatures. Granule strength is a function of the structure and physical properties of the binder used. In agglomeration processes, granules grow by the successive addition of primary particles to an agglomerate that is already formed; this happens when two particles or two granules are brought into contact with sufficient liquid binder. In tumbling beds of powder, two agglomerates colliding are kneaded to- gether by the tumbling action of the mixer to form near spherical- shaped granules. Subsequent growth occurs by a crushing and layering mechanism in which the smallest and weakest granules are crushed by larger ones and the material becomes redis- tributed around the surface of the large granule in a uniform layer (Smith, 2003).

CHARACTERIZATION OF AGGLOMERATED PRODUCTS

The knowledge and characterization of raw materials and products are essential to select appropriate method and ma- chine, optimize processes, functionality, product formulation, and reduce the cost of the product. The bulk properties of food powders are a function of physical and chemical properties of the material, the geometry, size, and surface characteristics of the individual particles, as well as the whole system. Parameters that determine the properties of agglomerates include those related to primary particles and agglomerates. Thus, the measurement of powder property is important because these properties in- trinsically affect powder behavior during storage, handling, and processing.

Physical Properties

Bulk Density and Porosity

The density of the sample is conventionally referred to as mass per unit volume. It is considered quite relevant for deter- mining other particle properties such as bulk powder structure and particle size requiring a careful definition. Density of a powder system decides the container volume, requirement of packaging materials, and selection of machinery for processing. Depending on how the total volume is measured, different def- initions of particle density can be given; these are true particle density, the apparent particle density, or the effective (or aero- dynamic) particle density. Most food particles have densities considerably lower of about 1000–1500 kgm 3 .

The density is of primary importance in applications involv- ing bulk flow of air around the particles like in fluidization, of liquid as sedimentation, or flow-through packed beds. The mea- surement of bulk density is of fundamental use by the industry to adjust storage, processing, packaging, and distribution con- ditions. Bulk density is the mass of the particles that occupies

a unit volume of a bed, whereas porosity is defined as the vol-

ume of the voids within the bed divided by the total volume of the bed. There are several types of bulk density based on the method of volume determination. The bulk density ( ρ b) of pow- ders is the mass of the particles that occupies the unit volume of a bed. It is determined by particle density, which in turn is determined by solid density, particle internal porosity, and also by special arrangement of the particles in the container. Bulk density includes the volume of the solid and liquid materials,

and all pores. Compact or compacted density is determined af- ter compressing the powder’s bulk mass by mechanical pressure and impact(s). Tap or tapped density results after a volume of powder has been tapped or vibrated under specific conditions. Loose bulk density is measured after a powder is freely poured into a container. Aerated bulk density is used for testing under fluidized conditions or during pneumatic conveying. The vol- ume fraction of air over the total bed volume is called porosity (Barbosa and Juliano, 2005).

Flowability

Powder flow is defined as the relative movement of a bulk

of particles among the neighboring particles or along the con- tainer wall surface (Peleg, 1978). The forces involved in powder flow are gravity, friction, cohesion (inter-particle attraction), and adhesion (particle-wall attraction). Particle surface properties, particle shape, size distribution, and the geometry of the system are factors that affect the flowability. It is, therefore, quite dif- ficult to have general theory applicable to the flow of all food powders in all possible conditions that might be developed in practice (Peleg, 1978). The practical objective of powder flowability determination

is to provide both qualitative and quantitative knowledge of pow-

der behavior which can be used in the designing of equipment. In order to flow, the powder must fail and its strength must be less than the load put on it. The basic properties describing the failure condition are: (i) the angle of wall friction (ii) the effective angle of internal friction (iii) the failure function (iv) the cohesion and (v) the ultimate tensile strength (Barbosa-Canovas et al., 2005). The cohesion is a function of inter-particle attraction and is due to the effect of internal forces within the bulk, which tend to prevent planar sliding of one internal surface of particles upon another. The ultimate tensile strength of a compact powder is the most fundamental strength mechanism, representing the mini- mum force required to cause separation of the bulk structure without major complication on particle distribution within the plane of failure. There are many empirical tests used to assess flowability, including measurement of angles of repose (Teu- nou et al., 1995), Johanson indicizer (Johanson, 1992), Hausner

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ratio, and Carr indices, flow-through opening and compression testing (Peleg, 1978), Jenike shear cell (Jenike, 1964), and by the upward and downward movement of a rotating blade employ- ing a texture measuring system (Mukherjee and Bhattacharya,

2006).

Structural Features

Particle Size and Shape

Particle size is one of the most important physical character- istics of particles. In the case of simple shapes such as the sphere or cylinder, the size is explicitly determined by one or several dimensions. However, particles are of irregular shape so that a large number of dimensions would be required to describe the size and shape. The term size of a powder or a particulate mate- rial is relative. To determine the particle size, in principle, any measurable physical property which correlates with characteris- tic geometric dimensions or equivalent dimensions can be used (Schubert, 1987). The bulk density, compressibility, and flowa- bility of food powders are highly dependent on particle size and its distribution. The common convention considers that for a particulate material to be considered a powder, its approximate median size (50% of the material is smaller than median size and 50% larger) should be less than 1 mm. It is also a com- mon practice to talk about “fine” and “coarse” powders; several attempts have been made to standardize particle nomenclature in certain fields. A significant number of food powders may be considered to be in the fine range. Methods for measuring particle size are sieving, microscope counting techniques, sed- imentation, and stream scanning. The median particle sizes in common food commodities have been indicated by Barbosa- Canovas et al. (2005). Particle shape influences factors such as flowability of pow- der, packing, interaction with fluids, and coating of powders such as pigments (Barbosa-Canovas et al., 2005). Generally the particle shapes are defined as acicular (needle shape), an- gular (roughly polyhedral shape), crystalline (freely developed geometric shape in a fluid medium), dentritic (branched crys- talline shape), fibrous (regular or irregular thread-like), flaky (plate-like), granular (approximately equidimensional irregular shape), irregular (lacking any symmetry), modular (rounded ir- regular shape), and spherical (global shape), etc.

Solid and Liquid Bridges

In general, interaction between particles is regulated by the relationship between the strength of the attractive (or repul- sive) forces and gravitational forces. For all particles in the amorphous rubbery state (or above glass transition tempera- ture), forces causing primary particles to stick together are inter- particle attraction forces (Van der Waals or molecular forces and electrostatics forces), liquid bridges, and solid bridges (Hartley et al., 1985; Seville et al., 2000). Inter-particle forces are in- versely related to the particle size (Rennie et al., 1999; Adhikari

et al., 2001). Van der Waals and electrostatic attraction are not as high as the inter-particle connecting force coming from liq- uid bridges (Schubert, 1987). Van der Waals forces arise from electron motion among dipoles and act over very short distances within the material structure, becoming prevalent when the par- ticle size is less than 1 µm (Hartley et al., 1985). Electrostatic forces are longer ranging forces that arise through surface dif- ferences on particles and are present when the material does not dissipate electrostatic charges. Solid bridge is formed as a result of sintering, solid diffusion, condensation, or chemical reaction and arises from the material deposited between the agglomerated particles. Solid bridges can also be built up by chemical reaction, crystallization of dissolved substances, hardening of binders, and solidification of melted components (Loncin and Merson, 1979). Liquid bridges are re- lated to chemical interactions between particle components and result from the presence of bulk liquid (generally unbound wa- ter or melted lipids) between the individual particles. In liquid bridges, the force of particle adhesion arises either from sur- face tension of the liquid/air system (as in the case of a liquid droplet) or from capillary pressure. Composition of the liquid in the bridge varies in different food materials. The “bridging potential” or “stickiness” is related to factors such as powder moisture, fat or low-molecular-weight sugar content, and the shape of the particles (Barbosa-Canovas et al., 2005).

Instant Properties

The instantaneous properties of agglomerates are the most desirable properties of agglomeration processes and they can be measured by the following four dissolution properties when ag- glomerates are spread on the surface of liquid (Schubert, 1987). These are wettability (liquid penetration into a porous agglom- erate system due to capillary action), sinkability (the sinking of agglomerates below the liquid surface), dispersibility (the dispersion of agglomerates with little stirring), and solubility (dissolving of soluble agglomerates in the liquid). The ability of the bulk powder to imbibe a liquid under the influence of capillary forces is called wettability (Freudig et al., 1999) and it is the ability of the powder particles to overcome the surface tension between themselves and the liquid (Fang et al., 2008). In technical processes, the wetting of the particles is often the rate-controlling step and depends largely on particle size. The importance of wettability lies in the development and quality control of several food powders like milk powder, instant tea and coffee, and instant mixes for which claims have been made that they have instant properties like solubility. The con- ditions favoring good wettability are large particles with large pores in between, high porosity as long as a critical porosity is not exceeded, and small contact angle (Freudig et al., 1999). The presence of free fat in the surface reduces wettability. The selec- tive use of surface-active agents, such as lecithin, can sometimes improve wettability in dried products containing fat. Sinkability is defined as the falling of powder particles be- low the surface of an aqueous phase or liquid (Thomas et al.,

440

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2004). It depends mainly on the particle size and density, since larger and denser particles usually sink faster than the finer and lighter ones. A higher particle density combined with a lower quantity of air content enclosed within powder particle results in a faster sinking rate (Caric and Milanovich, 2002). Swelling can strongly inhibit sinking (Freudig et al., 1999). Dispersability describes the ease with which the powder may be distributed as single particles over the surface and throughout the bulk of the reconstituting water. In dispersability measuring test, it is essential to assume that following a short period of dispersing, soluble particles are completely dissolved and sus- pended particles are regarded as residual material. There are several techniques for measuring the dispersibility, including the measurement of dispersion kinetics using an optical fiber sensor to collect the light backscattered by the particles in sus- pension (Galet et al., 2004; Vu et al., 2003). Solubility refers to the rate and extent to which the com- ponents of the powder particles dissolve in water. Solubility depends mainly on the chemical composition of the powder and its physical state. It is also the final step of powder dissolution and is possibly the key determinant of the overall reconstitu- tion quality. It is used to represent the complete phenomenon of milk powder recombination, comprising soluble components such as lactose, undenatured whey protein, and salts, as well as dispersible components like casein (Thomas et al., 2004). Solu- bility is also used to quantify the rate of dissolution to describe the various combinations of milk powder reconstitution proper- ties. Generally, the dissolution rate is flavored by the presence of small hydrophilic molecules on the surface (Lillford and Fryer,

1998).

CONCLUSIONS

Properties of food powder and their conversion to agglomer- ated products are important areas that directly affect the selec- tion of process equipment, storage ability, and product formu- lation. The area of understanding the behavior of food powder is still at an infant stage though there is considerable progress in other areas like ceramic, mining/metallurgy, and pharmaceu- tical technology. Scope exists to study the properties of food powder with an emphasis on application in developing different food formulations. The specific areas that require attention are characterization and understanding of food powders along with functional behavior. It is also desirable that raw materials from different sources are also considered for research investigations that would improve our existing knowledge on food powders.

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