Journalof Food Engineering6 (1987) l-32

Food Particle Technology. Part I: Properties of Particles

and Particulate Food Systems
H. Schubert
Institute for Food Engineering, Federal Research Centre for Nutrition, Engesserstr. 20.
D-7500 Karlsruhe, Federal Republic of Germany
(Received 3 September

1985; revised version received 20 January 1986; accepted 25

February 1986)

ABSTRACT
In Part I the properties and the characterization of individual particles
and particulate systems are reviewed, special emphasis being given to
particle size and shape, particle size distribution, interparticle adhesion,
porosiy, capillary action in porous media, instantand flow properties of
powders. The p~cu~~ar~ties
of particulatefoodstu~s, which become evident
through the use of special techniques for measuring these fundamental
characteristics,are considered in detail.

1.

INTRODUCTION

In the past 20 years, particle technology has changed from a largely

empirical to a structured discipline, involving scientific research in many
parts of the world. Decisive contributions to this development
were
made by Rumpf (1975). Particle technology is that branch of process
engineering concerned with the production, processing, analysis and use
of particles.
The differences between integral and particulate matter occur mainly
when the particles are small, i.e. of the order of micrometres to millimetres. This part of the field is known as fine particle technology or
powder technology. This paper is concerned predominantly with fine
solid particles, the largest sector of particle technology.
Advances in this field have so far received little attention in food technology, although foods are frequently in the form of fine particles during
processing or when used by the consumer. The chemical, pharmaceutical
and other process industries are now using the results of research into
Journal of Food Engineering
Publishers Ltd, England,

0260-8774/87/$03.50

1987. Printed in Great Britain

- 0

Elsevier

Applied

Science

H. Schubert

particle behaviour extensively. The benefits to be obtained also deserve

the attention of food technologists although, in view of the special
characteristics of foods, additional research is necessary if the advances
in particle technology are to be applied successfully to food products.
It is the purpose of this paper to describe some important aspects of
particle technology and to illustrate them by examples from food technology.
2.

PROPERTIES

OF INDIVIDUAL
PARTICLES
PARTICULATE
SYSTEMS

AND OF

The properties of particulate systems differ from those of the integral

form of the solids of which the particles are composed. Many such
properties depend on the particle size. Figure 1 shows qualitatively some
selected individual particle and particle system properties. The figures
indicate only a general tendency as deviations from this general
behaviour may sometimes be observed. Some properties of individual
particles will be considered first (Fig. l(a)). The fracture resistance, a,,
increases with decreasing particle size (as there are then fewer flaws in
each particle and a greater proportion of the particle deformations are
plastic): size reduction therefore requires increasingly more energy if fine
particles are to be produced. This is also one reason for the existence of
a grinding limit, i.e. the particle size below which grinders are not capable
of producing smaller particles. With decreasing size the homogeneity of
the particles also generally increases. This property is used, for instance,
traditionally in cereal grain milling to separate the different components
after comminution.
The terminal settling rate Us,illustrated here by a flour particle in air,
first increases rapidly as a function of increasing particle size ( ug CCx2)
and then more slowly ( I+ a Jx). Small particles settle very slowly. Wheat
flour particles of 1 pm size take more than 6 h to fall a distance of 1 m in
still air. Of special importance is the ratio, S,, surface area per unit
volume of particle, which is inversely proportional to particle size. Small
particles accordingly have a large S, value. If a lump material of 1 cm3 in
volume is subdivided into equal spheres of 1 ,um diameter, the surface
area obtained is more than 3 m2. The surface per unit volume is particularly important in heat and mass transfer, the rates of which for small
particles (x < lo-100 pm) are proportional
to S,. Extremely small
particles can dissolve very rapidly and may be dried within a fraction of a
second, but also may cause violent dust explosions. Because of their
large surface per unit volume, microorganisms are capable of exchanging
metabolites and nutrients solely by diffusion at their external surface.

Food particle technology - Part 1

10-l

10-l

10

lo2

PARTICLE

SIZE

10
PARTICLE

lo2
SIZE

lo3 Pm

loL

IO3 pm

I
loL

Fig. 1 Qualitative dependence of some individual particle and some system properties
on particle size. D is particle deposition in fibrous filters, F is adhesion force, His homogeneity of a particle, S, is surface per unit volume, W is weight of a particle, vg is terminal
settling rate, a, is particle fracture resistance.

The properties of particles do not always increase or decrease regularly with increasing particle size. An example of this is particle deposition, D, in fibrous filters. Particles of x = 1 pm are the most difficult to
collect. The deposition of small particles is promoted by diffusion, that
of larger ones by inertial, gravitational and electrostatic forces (Loffler,
1983).
Most important in particle technology is interparticle adhesion. This
usually increases in proportion to the particle size but the ratio of
particle adhesion, F, to particle weight, W, is of primary importance: this
ratio is inversely proportional
to the square of the particle size. For
particles of 1 ,um, for example, F/W is larger by a factor of lo6 than for
particles of 1 mm diameter. This fact explains why small particles adhere
much more strongly to each other and to surfaces than large particles do.
Adhesion forces are also largely responsible for the cohesive strength
of powders which, at constant porosity, is approximately inversely pro-

H. Schubert

portional to the particle size: thus fine powders show a tendency towards
agglomeration or to form lumps. Hence, the flowability of powders
increases with increasing particle size. A similar behaviour is also
observed in their wettability and dispersibility. These properties are of
importance in instant food powders.
The magnitude of interparticle adhesion forces, as compared to other
competing forces such as gravity, accounts for the difference between
cohesive and non-cohesive powders. In non-cohesive powders, interparticle forces are negligible but in cohesive powders they are significant.
The majority of dry food powders are non-cohesive (and thus freeflowing) only when the particle size exceeds about 100 pm. In wet
powders considerably
stronger adhesion forces appear and the
boundary between the cohesive and non-cohesive
occurs at larger
particle size. Since the adhesion forces may be varied over a wide range,
many powder properties may be influenced as desired.
Interparticle adhesion also influences many bulk properties. Three
examples are shown in Fig. l(b). The porosity (the void fraction of the
total volume) increases with decreasing particle size because the interparticle adhesion allows a looser structure. Very fine particles such as
flow conditioners (anticaking or free-flowing agents, dry lubricants) of a
size below lym can attain porosities of more than 95%. If they are
poured into a container of volume 20 litres, the mass of its contents may
be less than 1 kg although the density of the solid is over 2 kg/litre.
Many other properties such as mixability, colour, water-vapour sorption, flavour, etc, depend upon particle properties. Nowadays many of
these properties can be described quantitatively. Considerable advances
have also been made in the description of fluidized solid flow (Molerus,
1982) in particle transport equipment and in fluidized beds.
3.

CHARACTERIZATION

OF PARTICULATE

SYSTEMS

3.1 Characterization of individual particles

3.1.1 Particle size analysis
Particle size is the most important physical particle characteristic. In the
case of simple shapes such as the sphere or cylinder, the size is explicitly
determined by one or several dimensions. In the majority of cases, however, particles are of irregular shape so that a large number of dimensions would be required to describe the size and shape. Since this is not
practicable, essential characteristics must be defined which, depending
on the circumstances, provide adequate description. Because of the
measuring problems involved, particularly in the case of very fine

Food particle technology - Part I

particles, the choice of suitable characteristics defining the particle size is

sometimes tied to particular measuring methods.
To determine the particle size, in principle, any measurable physical
property which correlates with characteristic geometric dimensions or
equivalent dimensions can be used. Equivalent dimensions are dimensions of an imaginary regular particle with the same physical property as
that of the irregularly-shaped
particle being measured. The equivalent
settling rate diameter, for instance, is frequently used; it is the diameter of
a sphere of the same density as the irregularly-shaped particle which in
the same fluid has the same settling rate. In the viscous flow regime, i.e.
for Reynolds number ReSO-25, this equivalent settling rate diameter is
obtained from
x;=

18qv,
g(p, - P)

where Re = (,q, v,x,)/q, r] is coefficient of dynamic viscosity of the fluid,

V~is terminal settling rate of the particle, g is acceleration due to gravity,
pP, ,on are density of the particles and of the fluid, respectively. Equation
(1) applies, for instance, to cereal flour particles in the ranges of X, < 50
pm for sedimentation
in air and x, < 100 pm for sedimentation
in
ethanol.
The attributes usually used to characterize particle size may be classified as follows:

(1) geometrical

characteristics

(such as linear

volumes);
mass;
i:; settling rate in a fluid;
(4) field interferences such as electrical
scattering or diffraction.

dimensions,

field interferences,

areas,

light

Today many devices are available commercially employing one or

other of these attributes from which the particle size or the equivalent
diameter can be determined. However, not all particles of a powder are of
the same size. It .is therefore necessary to measure a great many particles
and produce a particle size distribution. An example is shown in Fig. 2.
The cumulative distribution QAx) as well as the frequency distribution
q,(x) may be measured. Either can be converted into the other, since
q,(x) is the first derivative of Q,(X); x represents the particle size,
frequently an equivalent diameter. Subscript r indicates whether the
distribution is according to number (r= 0), length (r= l), area (r = 2) OI
volume (Y= 3) (see, for example, Leschonski et al., 1974). The cumulative distribution function Q,(X) indicates, for instance, the volume
proportion of particles between x,,,~and x (see Fig. 2).

H. Schubert

0.5

Xmin

X50

Particle
Fig. 2

Cumulative

size

X max

x -

and frequency distribution

of particle size.

This mode of description is advantageous mainly because it allows

several characteristic distribution values to be calculated and converted.
Of special importance in this respect are the various mean values, such
as the weighted mean particle size of the area frequency distribution
%(X)

%lla

x1,2

-w(x

1 dx

(2)

%I,

which is inversely proportional to the surface per unit volume of all

particles of the distribution. A very simple and frequently used mean
particle size is the median value xsOwhich is obtained from the cumulative distribution at Q, = 0.5 or 50% (see Fig. 2).
Before measuring a particle size distribution, a representative sample
must be withdrawn from the powder. To minimize sampling errors a
special sampling technique (Sommer, 1979) is necessary, which includes
sample splitting to provide the necessary quantity for each particle-sizedistribution measurement.
The characterization of individual particles in a collection is possible
only if the particles are separable from each other. Because of the strong
adhesion forces in relation to particle weight, fine particles in particular
require careful dispersion,
otherwise agglomerates
are measured.

Food particle technology - Part I

Depending on the particle measuring method used, the particles are dispersed in gases (Zahradnicek, 1976) or in liquids (Koglin, 1974). Dispersion in gases is satisfactory for particles larger than 2-5 pm; finer
particles have to be dispersed in liquids by means of dispersing agents to
overcome the adhesion forces by repulsion forces. The choice of dispersing liquid is especially important for food powders since the
particles must not swell or otherwise dissolve in or react with the fluid.
After extensive experiment at the authors institute, Hoffmann has established a list of suitable dispersing liquids for all the common food
powders, in which it is still necessary to differentiate between the different particle-size measuring methods. A selection of dispersion liquids is
shown in Table 1.
TABLE 1
Dispersing Liquids Suitable for Use in Particle Size Analysis of Food Powders

Wheat flours
Defatted soya flour
Milk powder
Pea-protein concentrate
Protein concentrate from brewers
spent grain
Microcrystalline cellulose

Wet sieving
refraction or
scattering of
light

Sedimentation

Electrical
impedance
of particles
( Coulter
counter)

1,273
3,8, 10
12,13
2,3, 10, 11

1,1+4,3,5
3,8,11
2,13
2,3, 10, 12

6+7,8+9
8+9,10
8+9,10,14
8+9

12
12,15

2, 12
12,15

10
lo,16

0Dispersant: 1, ethanol, 2, isobutanol; 3, benzene; 4, diethyl phthalate; 5, cyclohexane; 6,

methanol; 7, 5% aqueous lithium chloride; 8, isopropanol; 9, 5% aqueous ammonium
thiocyanate; 10, Isotone (Coulter Electronics); 11, butanol; 12, distilled water + Triton
X lOO@ (Coulter Electronics);
13, octanol; 14, 2% aqueous sodium hydroxide; 15,
acetone; 16, 1% aqueous sodium chloride.

The numerous measuring methods and devices for particle size

analysis will not be discussed here in detail. In recent years, rapid
methods have been developed which usually require expensive equipment. A survey of on-line measurement of particle size distribution in
gases and liquids was published by Leschonski (1978). It should be
noted, however, that not all methods are suitable for foods, even if they
are well proven for other substances such as minerals. For instance, the
densities of foods are in general not very different from those of liquids.

H. Schubert

In the majority of cases experience

methods to be suitable for foods:

has shown the following measuring

(a) analysis of photographic

images including scanning electron
micrographs;
(b) dry (x 2 40 pm) and wet (x 2 5 pm) sieving;
(c) electrical impedance of particles; for example, Coulter Counter
TA II (0.6 pm I x I 800 pm), Elzone Counter (0.25 pm I x I 1020
pm);
(d) evaluation of laser diffraction patterns; for example, Malvern
( 1 ,uml x I 1800 pm), Cilas ( 1 pm< x I 192 pm), Leeds and
Northrup (0.1 ,umlxl20
pm or 2 ~m1x<lOOO pm).
Because of the time taken in sample preparation, method (a) is timeconsuming despite automatic image evaluation. Method (b) is also timeconsuming but indispensable
for many purposes including quality
control. Methods (c) and (d) are rapid methods using automatic measuring equipment suitable for on-line measurements. Whereas with method
(c) the particles can be measured only in an electrically-conducting
liquid, it is possible with method (d) to measure particle-size distribution
in liquids and gases. Particularly because of their rapidity, diffraction
counters working according to method (d), using the Fraunhofer diffraction pattern of particles, have been increasingly used in recent years
(Polke and Bieger, 1979). Figure 3 shows a comparison of methods (c)
and (d) for pea flour. The particle size x is the equivalent volume diameter (method (c)) or the equivalent diameter of a sphere showing the
same characteristics of Fraunhofer diffraction (method (d)). The differences between the measurements on particles dispersed in air and in
liquid demonstrate that the fines were not completely dispersed in air.
Particle size analysis has been developed to a comprehensive discipline requiring special knowledge and experience taught in special
courses (Leschonski, 1982) which deal in detail with measurement of
other properties such as surface per unit volume and particle shape. The
measurement of particle shape (Scarlett, 1979), for which new methods
have been developed (Weichert and Huller, 1979) has gained increasing
importance for food particle technology (Davis and Hawkins, 1979).
3.1.2 Particle adhesion
Particle adhesion in a gaseous environment is an important property in
characterizing individual particles but, apart from a few exceptions, it
has not been possible so far to calculate the adhesion forces between
real particles with sufficient accuracy. Models were therefore developed
to enable adhesion forces to be estimated: in the majority of cases, these
models are based on the assumption of ideally smooth, rigid spheres.

Food particle technology - Part I

Fig. 3

Cumulative

10

20
Particle

particle size distributions

size x

50
-

100

200
IJm

of particle-size milled pea flour.

Even if surface roughness and deformation of the contact areas inevitable in real particles are responsible for deviations between model calculations and measured values, the calculations still provide useful
information as to how the different variables influence adhesion.
Adhesion mechanisms with and without material bridges can be
distinguished.
The most important
adhesion forces between food
particles are shown in Fig. 4. Solid bridges may be formed by sintering,
by chemical bonds and/or by crystallization. The crystallization of amor-

with

material

bridges

chemical
5

slnter

bondi-

,vithout matenal

bndges

van der

Waals

bldge

9
bonding

by

crystolllsed

soiute

liquid bridge

electrostatic
(conductor

VISCOUS bondmg

Fig. 4

Adhesion

mechanisms

between solid particles and a solid plate in a gaseous

environment.

10

H. Schubert

phous constituents frequently causes an undesirable stickiness to occur

in food powders. These processes have been studied in detail for sucrose
and lactose (Niediek, 1982) and also measured as a function of temperature and water content (Downton et al., 1982). Crystallization of solutes
at contact points between particles during drying frequently leads to
strong particle adhesion.
Liquid bridges represent the dominating adhesion mechanism in
nearly all those cases where sufficient moisture is present, but liquid
bridges may also arise from capillary condensation
in moist atmospheres. Adhesion forces due to liquid bridges can be calculated. The
results of such calculations are available for many particle geometries as
diagrams using dimensionless numbers (Schubert, 1982). Figure 5 shows
a simple example of adhesion forces between two equal spheres. The
distance, a, between the surfaces of the spheres as shown in the figure
arises in real particles from surface roughness, the significance of which
for adhesion forces will be explained below.
Adhesion without material bridges is primarily due to van der Waals
and electrostatic forces. Van der Waals forces (F&,, ) are always present;
they may be calculated for two spheres of diameters X, and x2 separated
from each other by distance a between the two surfaces from
3.0

2.5

F
=

2.0

1.5

1.0

0.5

r\

lcrl, \;?.1oyo-ypo-3

\\,

I\
0.05

\ %

Y42

-y

010

0.15

I _-I
0.20

Fig. 5 Adhesion force F of a liquid bridge between two equal spheres - related to the
surface tension y of the liquid and the sphere diameter x - as a function of the distance
ratio a/x for complete wetting (contact angle 6 = 0). Parameter is the volume V, of the
liquid bridge related to the volume V, of the sphere.

Food particle technology - Part I

E,x, %

vdW 16;rt(x, +x2) a*

11

(3)

The vander Waalsinteractionenergy

E, is between 10-i and 2 X lo- IxJ.
Van der Waals force is a maximum for particles in contact with each
other; the contact distance is assumed to be a= a,, = O-4 nm (Krupp,
1967). It should be noted that eqn (3) applies only to ideally smooth rigid
spheres, and to a sphere at a plane surface (where x,/x2 -, 0).
Electrostatic adhesion forces occur in cases where particles have
opposing charges. These charges may be already present as excess
charges or arise only when the particles come into contact due to differences in the values of the electron work function (contact potential).
Electrically non-conducting
particles frequently have excess charge up
to a maximum per surface of around s,,, = 100 e/pm* (elementary
charge e = 1.6 x lo- I9 As). For ideal electrical insulators the adhesion
forces F,,,i can be calculated from Coulombs law,
2
JG~l~2~1~2
Fei,i=

E,E(xI+x2+2a)

(4)

Equation (4) applies to spheres of diameters x1 and x2 where si, s2 are

electric charge per unit surface area of the corresponding spheres, E*, t
are relative and absolute dielectric constants of the surrounding medium.
a is distance of separation between the spheres. Equation (4) also applies
to the sphere-plate system when x,/x2 -+0.
With electrically conducting particles, electrostatic adhesion arises
only after the particles have made contact and is due to the contact
potential which is frequently between U= 0.1 and 0.7 V. The adhesion
force due to a contact potential between two spheres or between sphere
and plate (x1/x2 -, 0) can be stated by:

Fe,,,=

m,&tiX1X2
2(x1

+ ~2)

(5)

A comparison between the adhesion forces represented by eqns

(3)-(5) is shown in Fig. 6. As mentioned before, however, for particle
adhesion the ratio F/W between adhesion force and particle weight is
more important than the absolute value of the adhesion force. In Fig. 6,
therefore, the ratio F/W for two equal spheres is plotted against sphere
diameter. The distance between the two surfaces in contact is assumed to
be a, = O-4 nm, the particle solid density pS = 1.5 g cme3. As Table 2
shows, this is a reasonable mean density value for many food particles,
but since F/W= ps , a conversion of the values shown in Fig. 6 for other
solid densities is very simple.

H. Schubert

12

F= theor. ddhesion f&ce~~~,

W=weight of one sphere
_ <X

1
Sphere

\
\\,

(9 = 1.5 g/cm31
I

10

lo2 Pm

diameter

lo3

Fig. 6 Calculated adhesion force F between two equal spheres (as a fraction of the
weight W of one sphere) for various interparticle adhesion mechanisms vs. sphere
diameter.

TABLE 2
Densities and Bulk Densities of Some Food Powders
Food

Wheat flour
Rye flour
Corn flour
Corn starch
Potato starch
Rice, polished
Cocoa powder (10% or 22% fat content)
Sucrose
Instant dried whole milk
Instant dried skimmed milk

Solid derlsityp,
g cm --;

1.45-1.40
I.45
I.54
1.62
1.65
1.37- 1.39
1.45 or 1.42
1.60
1.3(-1.45)
1.2(-1.4)

Bulk density p,,

g cm --.<

0.55-0.65 (0.4-0.75)
0.45-0.7
0.5-0.7
0.55
0.65
0.7-0.8
0.35-0.4 or 0.4-0.55
0+x5- 1.05
0.45-0.55
0.25-0.55

Figure 6 shows on a log scale that all adhesion forces related to the
particle weight are inversely proportional to the square of the particle
diameter (F/WCCX-*), except for the electrostatic adhesion of insulators
). Particle
adhesion decreases in the order: liquid bridge
lFel,il
WCC
x-1

Food particle technology - Part I

13

forces: van der Waals forces: electrostatic forces. The strong adhesion
between small particles is remarkable. The interparticle force between
spheres of 10 pm diameter, for instance, is in the case of a liquid bridge
2.6 x lo5 greater than the particle weight.
The dependence
of adhesion. forces upon the distance between
particles is important. Large volume liquid bridges - as Fig. 5 shows are little influenced by the distance between particles, whereas small
volume bridges formed by capillary condensation,
for instance, are
strongly affected. As eqns (3)-( 5) show, van der Waals forces decrease
rapidly with separation distance ( FvdW~ a-), whereas the decrease in
electrostatic forces with separation distance is less in the case of electrical conductors (F,,i 0~a - *) and negligible (sphere/sphere) or even zero
(sphere/plate) in the case of electrical insulators. Attraction from greater
distances is consequently due only to the electrostatic forces between
charged particles. If the particles are already in contact, the adhesion is
primarily due to solid bridges, liquid bridges and van der Waals forces.
The effect of distance on adhesion forces is of great significance in the
case of real particles in which surface roughness, which is usually
present, increases the separation distance. In the case of van der Waals
forces and very small liquid bridges, adhesion is determined almost
entirely by the size and shape of the roughness peaks. In such cases
adhesion forces between real particles are frequently smaller by more
than an order of magnitude than the values calculated for perfectly
smooth model solids.
This effect can be illustrated by using the model of a very small sphere
which has been placed between two equally large spheres, as shown in
Fig. 7. Such finely divided solids are added to food powders, for
instance, as flow conditioners to reduce interparticle adhesion and hence
improve flowability (Hollenbach and Peleg, 1983). However, the interstitial sphere may also be regarded as a model for a roughness peak.
Figure 7 shows the ratio of adhesion force F between two spheres of
diameter x2 = 10 ,um and the weight W of one of these spheres (p, = l-5 g
cm-) vs. the diameter x, of the interstitial sphere. According to eqn (3),
the van der Waals force between the two spheres of diameter xx is

Here a, is the distance between the interstitial sphere and the large
sphere in contact, again assumed to be 0.4 nm. For a given x2, the
adhesion force FvdWpasses a minimum at
x: = $x,a$

- 2U

(7)

14

3
Fig. 7

lo5

3
0.1
3 1o-2
Diameter x1 of the interstitiat

pm
sphere

adhesion force F between two equal spheres (as a fraction of the

weight W of one sphere) VS.diameter x, of an interstitiai sphere.

Calculated

For the sphere diameter xz = 10 pm as selected in Fig. 7 the minimum

adhesion force appears at X: = O-01 1 pm. A compa~son with Fig. 6
reveals that this van der Waals force is smaller by a factor of cu. 300 than
the adhesion force between a pair of perfectly smooth spheres. In case of
electrostatic attraction between electrical conductors (not shown in Fig.
7), the adhesion force takes a similar course to that of the van der Waals
force.
The adhesion of the electrical insulator, on the other hand, is independent of x1 and thus also of roughness. Large liquid bridges are also
little influenced by roughness. This is illustrated in Fig. 7, for example,
where the course of the related liquid bridge force is shown for a ratio of
liquid bridge volume Vi, to sphere volume IS,of I,,/ r/, = 0.0 1; this corresponds to a bridge angle of /!I= 20-27, depending on the size of xl_ Very
small liquid bridges resulting from capillary condensation from the moist
atmosphere behave quite differently. Figure 7 shows two examples for
relative air hu~dities of 50 and 80%, which correspond to water activi-

Food particle technology - Part I

15

ties a, = 0.5 and 0.8. The related adhesion force decreases rapidly with
increasing diameter x1 of the interstitial sphere until finally the liquid
bridge becomes unstable (Schubert, 1982) and breaks (dotted line in Fig.
7). Thereafter the related adhesion force increases with increasing
diameter x1 proportionally to x1 and practically independently of a,; in
this case liquid bridges have formed between the sphere of diameter
x2 = 10 ,um and the small sphere (x1).
The liquid bridge forces caused by capillary condensation hence may
decrease by a factor of more than 1000 (cf. Fig. 7) as compared to
perfectly smooth particles without the interstitial sphere. This illustrates
the effect of flow conditioners on powders which are stored in moist
atmospheres (see also Schlitz and Schubert, 1980).
Since the size and shape of actual roughnesses, in contrast to the
model considerations in Fig. 7, are largely unknown, it is necessary to
measure the adhesion forces between real particles if quantitative information is required. Such measurements generally yield adhesion force
distributions over a wide range even with equal-size particles. This is due
to roughnesses of different size which are irregularly spread over the surfaces. Hence, depending on the random contact, the geometry of the
contact area changes in the micro-range. Adhesion force distributions
often range over more than one order of magnitude even for monosize
particles (Schlitz, 1979).
In addition to the above influences there are many other factors to be
taken into account such as adhesion force enhancement due to inelastic
deformation
of the contact areas of the adherents. Interactions of
particles in liquids where repulsive and attractive forces frequently compete with each other also belong to the field of interparticle adhesion.
Review papers provide a survey of the entire field (Schubert, 198 1 a, c). A
research project at present attracting much attention is the adhesion of
microorganisms
to solid surfaces (Ellwood, 1979; Notermans and
Kampelmacher,
1983). Much of classical particle adhesion knowledge
may be used in this field. The same applies to particle adhesion involved
in surface fouling in food processing (Hallstrom et al., 1981).
3.2 Characterization

of powders

3.2.1 Porosity bulk density

Porosity E has been defined as the ratio of void volume V, to total volume
I, of the powder:

H. Schubert

16

In eqn (S), V>is the solid volume. If the particles themselves are porous
(particle porosity EJ then
Fl

-(I -Ep)(l -&J

(9)

where the bulk porosity E,, is the ratio of void volume between particles
to the total volume. The bulk density of a powder is also frequently used:
Ph=(I-&p)(l-&b)Pu=(l-&)P,

(IO)

where p, is the solid density. Table 2 lists the bulk densities of some food
powders. In the case of bulk material made up of closely sized, nonporous particles, if adhesion forces may be neglected, i.e. if the particles
are sufficiently large, the porosity is about E = 0.4. If interparticle
adhesion is significant, porosity increases. Especially in wet powders, or
upon exceeding the relative humidity (RH) at which capillary condensation may take place (frequently at RH > 0.6-0.7) porosity increases, or
the bulk density decreases as compared to the dry condition. Scoville
and Peleg (1981) and Moreyra and Peleg (198 1) studied and quantified
these effects in model substances and various food powders.
Bulk density is of importance because consumers expect that the mass
indicated on the package corresponds to a volume filling the package
almost completely. This frequently presents difficulties in food processing. In many cases producers wish to offer powders combining a large
volume with a small mass. As may be recognized from eqn (lo), this can
be accomplished by producing porous particles. In practice, porous
particles may be produced as hollow spheres or by instantizing fine
particles to larger agglomerates of the desired porosity sp. The following
example demonstrates the wide range of variability in bulk density. A
beverage powder (sugar-cocoa mix) which is sold direct to consumers is
usually expected to show a bulk density of p,=O.30-0.35
g cmm3. A
powder of the same composition intended for use in vending machines,
however, is required to have a bulk density of pb = 0.5-0.6 g cmm3 (Kniel,
1980).
3.2.2 Capillar?, action in powders, pore size distribution
Many food powders are obtained from the wet phase and have to be
dried, frequently after mechanical dewatering. Prior to consumption, or
in the course of further processing, most of the powders have to be
rewetted. Both dewatering and reconstitution - mostly with water are governed by capillary behaviour. It is therefore necessary to characterize powders with regard to their capillary properties. For this reason
capillary pressure curves (Schubert, 1982) have been established which
indicate the capillary pressure p, in a porous medium as a function of the
liquid saturation S; S is the ratio of liquid volume to void volume of the

porous solid system. The capillary pressure curve indicates a distribution

comparable to the particle size distribution. The measuring methods are
explained in detail elsewhere (Schubert, 1982).
Figure 8 shows a typical capillary pressure curve. Starting from the
porous system filled with liquid (S= 1) the capillary drainage curve D,
applies until finally at S= S, only isolated liquid remains. If liquid is
admitted to the pores in the state S = S,, the capillary imbibition curve I
applies until finally at S = 0.8 1 the capillary pressure p, = 0 prevails. Subsequent dewatering leads to curve D. The capillary pressure curve
accordingly shows a hysteresis which may be explained by the existence
of narrow pore necks followed by larger cavities, and by the contact
angle hysteresis (receding contact angle (r, < advancing contact angle 6,,
see drawing in Fig. 8). A frequently used characteristic capillary pressure
is the entry suction p, which is obtained approximately, for complete
wetting (6, = 0), from
PC=:

w -- 4 Y

(11)

&X1,2

-0 i,

0.2

Ok
Liquid

0.6
saturation

0.8

Fig. 8 Capillary pressure of a bulk material (glass spheres, weighted mean diameter
.*11.2
= 79 ym, porosity E = 0.38) vs. degree of liquid saturation (p,(S) = capillary pressure
curve).

18

H. Schubert

(y = surface tension of the liquid; X,,z see eqn (2)). The constant was
found to be b = 6-8 (Schubert, 1972). According to eqn (1 l), the capillary pressure increases with decreasing particle size.
Although the capillary pressure curve holds a key position for the
understanding of the capillary action in porous systems, and is necessary
also for the quantitative description of wetting and dewatering processes,
it is not sufficient to describe capillary processes completely. In wetting
of powders, a dynamic capillary pressure may play an important role in
addition (Schubert, 1978~). This wetting behaviour is of importance for
instant powders: it is discussed below in section 3.2.3.
The capillary pressure so far has been assumed to be a suction pressure, i.e. liquid is sucked into the pores by capillary action. This is indeed
always correct for sufficiently small contact angles, i.e. powders having
good wettability. Mercury, however, which forms a contact angle of
6 = 140 with most solids, behaves differently. In this case mercury must
be pressed into the pores to overcome the capillary pressure. This effect
is used in the so-called mercury porosimetry to determine the pore size
distribution. Since, because of the lower capillary pressure, large pores
are filled first, followed by finer pores which are subsequently filled
under increasing applied pressure, it is possible to deduce from the capillary pressure curve the pore size distribution. To evaluate the measured
results, pore models are required: usually, a cylindrical model is preferred. The excess pressure which is identical with the capillary pressure
p,, and the pore diameter dare correlated by the equation
4Y
p<.= / cos b

(12)

where y is surface tension of mercury, and b is contact angle. Pore size

analyses to characterize porous systems are gaining in importance. In
addition to mercury porosimetry (measuring range: 5 nm < d < 200 pm),
and adsorption methods (0.2 nm < d < 2 nm), sorption isotherms in the
range of capillary condensation (3 nm < cl < 0.5 pm) and micrographs
(d > 0.1 pm) may also be used to determine pore size distribution. The
pertinent literature is discussed in a review paper by Orr ( 1980).
3.2.3 Irutunt properties of powders
Fine powders are difficult to wet with water or aqueous liquids (for
instance, milk) and tend to form lumps which hinder dispersion. By
agglomeration of fine powders of about 100 pm into particles of up to
several millimetres in size, wetting is improved and lump formation
avoided. The causes of this behaviour have been elucidated (Schubert,

Food particle

technology

Part I

19

1978b, 1982). Materials with poor wetting properties such as fatty

particles, for example, which form a large contact angle with the liquid,
may also be changed in respect of their surface properties by reducing
the contact angle and thus improving wettability; this is often done by
spraying with lecithin. The commercial treatment of powders to improve
their wetting, dispersing and, in the case of soluble particles, their dissolving characteristics is called instantizing. The different instantizing
processes are described in a great many publications but the main principles of these processes have been compiled by the present author in a
previous paper (Schubert, 1980).
If a powder is spread on the surface of a liquid, the following processes take place:
(a) penetration of liquid into the porous sysem due to capillary action
(the ability of the powder to be penetrated by the liquid is called
wettability);
(b) sinking of the particles below the liquid surface (sinkability);
(c) dispersion of the powder with little stirring (dispersibility);
(d) solution of the particles in the liquid, provided the particles are
soluble (solubility).
The properties wettabihty, sinkability, dispersibility and solubility are
all subsumed under the term instant properties. In the case of particulate solids having good instant properties, the processes (a)-(d) are
expected to be completed satisfactorily in a few seconds if the layer
thickness of the powder spread on the surface of the liquid is about 10
mm.
Many objective measuring methods to determine instant properties
are available; they are discussed in a review paper (Schubert, 198 16). In
many cases, the disadvantages and shortcomings of these methods are so
great that they have not achieved practical importance, and subjective
evaluation methods have therefore been preferred. In view of the known
disadvantages of subjective evaluations, however, satisfactory objective
measuring procedures have been developed for the most important
properties, wettability and dispersibility (Schubert, 1980, 198 1 b). The
wetting test has also proved useful for non-food products; the dispersion
test used previously, however, is, because of the technical expense
involved, suitable only for research purposes. Dispersibility is most reliably determined from the change with time in the particle-size distribution during dispersion; this is possible by using modern on-line
particle-size analysers, but is too expensive for works practice. A relatively simple method for the determination
of dispersibility has been
developed for non-food powders (Polke et al., 1979) and has worked

20

H. Schubert

well. However, the method is not suitable for the majority of food
powders. This underlines the fact that it is not always possible to apply
methods of general particle technology directly to foods.
As far as food powders are concerned it is essential that, following a
short dispersing phase, soluble particles be dissolved as completely as
possible and the remaining particles be suspended in the liquid for a
sufficiently long time, i.e. neither deposit on the bottom of the receptacle
nor accumulate at the surface*. In accordance with a measuring method
(Mel, 1978) standardized by the International Dairy Federation (IDF) to
characterize the instant properties of dried milk, the following dispersibility value (which also includes the wetting properties) may be defined:

pc;d
cmt

(13)

where c,,,~ is mass concentration of the dispersed proportion and c,[ is

total mass concentration of the mass of the sample in the total liquid
mass. All dissolved and suspended particles are regarded as dispersed;
the remaining particles, i.e. those deposited and those floating at the surface, mostly non-wetted, accordingly are not dispersed. They form the
residual material, mass concentration c,,.
A dispersibility value may also be defined as:

Q=h

I.

(14)

If the dispersed total sample is divided according to the IDF test into
residual mass and dispersed mass, the following correlation between D,
and D, is obtained:
D

125QU +a
99D,+ 151

(15)

The constants 125,99 and 15 1 are obtained from the standardized division ratio according to IDE
In the IDF method the concentrations
c,,,~ and c,,,~are determined
gravimetrically or from the sample weight. The time required for the
determination
of dispersibility is thus 4-5 h. A rapid photometric
method has now been developed in which the concentration is related to
the loss in light transmission T according to the Lambert-Beer
law:
In TK c,. This law is valid only at sufficiently low concentrations and
*This requirement is not sufficient for the dispersion of certain other particles such as
colour pigments. The dispersion test described here is hence not suitable for all instant
powders, only for food powders.

Food particle technology - Part I

21

only when the particle-size distributions of the residual and dispersed

material are the same. Either condition can be fulfilled by adequate pretreatment. From eqn (14), for the photometric dispersion measure
In Td
Dfr=In T,

(16)

orfromeqn(15)
D

125% 1 + D,r)
99D,,+ 151

(17)

D, and D, are the same within the limits of measuring accuracy.

The equipment shown in Fig. 9 is used to measure photometrically the
dispersibility. In a modified IDF method, the powder is dispersed,
divided into residual and dispersed fractions which are then separately
homogenized and filled into the corresponding loading funnel (Fig. 9).
Each fraction is pumped in turn continuously through a cuvette where
the light transmission T, and Td are measured. The apparatus works
automatically. The data are evaluated by a mini-computer. Dispersibility,
which may fluctuate between 0 and lOO%, is indicated digitally.
Measurements, including sample preparation, take only a few minutes.

transmission

Fig. 9

Instrument

for measuring

the dispersibility
transmission.

of instant food powders by light

The instrument has been tested on nearly all instantized food powders
and has been found useful. Figure 10 shows the results for various commercial instant dried skimmed and whole milk products. Four samples of
each product were measured and the standard deviations determined
(indicated by bar-lines in the figure). The photometrically-determined

22

H. Schubert

(II

2
.-

o instant dried
skimmed milk

T=

33
iii
gO.8-

instant dried
whole milk

-0
+

C
.E
;

,/
0.6.

I
CL 0.2V
0.L
0.2
Gravimetrically
Fig. 10

WJ

I
0.6
determined

I
0.8
dispersibility

1
D,

Comparison
between the photometrically
and gravimetrically
dispersibility of instant dried skimmed and whole milk.

determined

dispersibility, D,, is the same, within the measuring accuracy limits, as

the gravimetrically-measured
IDF value D,. None of the commercial
instant dried whole milk products tested had satisfactory instant properties. According to IDF, D, should be L 85% for instant dried whole milk
and h 90% for instant dried skimmed milk. The rapid method which,
because of its ease in handling, is also suitable for routine measurements,
enables instant properties to be determined with sufficient accuracy; the
measurements
may also be used for product and process control
(Schubert, 1985).
3.2.3 Flow properties ofpowders
To ensure that powders are easily discharged or metered from containers, or fluidized and transported by pneumatic conveyors in the
course of a process without difficulties, they must be sufficiently flowable and even tricklable. Numerous empirical studies have been made
on the flowability of powders. However, none of these enables the flowability characteristics to be described independently of the particular
application. This is because of the complicated flow behaviour of particulate solids which differs basically from the flow behaviour of liquids
and fluidized solids. The pressure in a powder stored in a bin, for

23

Food particle technology - Part I

example, does not increase linearly with height, but tends towards a
maximum value. Only fluidized beds show some similarity to liquids.
Jenike ( 1970) established the fundamentals of powder mechanics,
allowing the flowability of particulate solids to be characterized and bins
and hoppers to be designed reliably. Only a brief explanation will be
given here; for details see the original work by Jenike (1970), the survey
papers by Schwedes (1970) and, with regard to food powders, by Peleg
(1977). To obtain the first reliable data as a basis for statements of
general applicability, Jenike developed a shear cell which is shown diagrammatically in Fig. 1 l(a). After consolidation to a certain porosity E,
or bulk density ,ob, the powder is subjected to different normal loads N
and caused to shear by the force S in the horizontal direction. If N is
plotted vs. S, or the normal stress o = N/A,vs.
the shear stress r = S/A,
an experimental yield locus as shown in Fig. 12 is obtained indicating the
yield point of the powder at a particular porosity E. If the yield point of
the same powder is required at a lower porosity, the experiment is
repeated at a higher consolidation degree. In this case the experimental
yield locus would be above that shown in Fig. 12. There is an individual
termination E to every yield locus; at this point steady-state flow is
reached, i.e. no changes in stress or volume take place.

a) Jetike shear cell

cover
ring
powder
base

b1Annular

shear cell

-loading

ring

powder
shear tr *ough

I-

C-R, -j
Ra
&

Fig. 11

Devices

for measuring

the shear resistance of powders.

Annular shear cell.

(a) Jenike shear cell. (b)

H. Schubert

24

tension
Fig. 12

Experimental

compression

Normal

stress

u ---

yield curve and effective yield locus of a cohesive powder.

The stress condition of each point on the yield locus may be decribed
by Mohr stress circles, Two Mohr stress semi-circles which are characterized by special properties are shown in Fig. 12. The larger semi-circle
characterizes the stress conditions during steady-state flow since it is
passing through point E. This stress circle intersects the axis at the two
principal stresses o1 and 02, O, being the major, or the consolidation
stress, and ~7~the minor principal stress. The smaller semi-circle shown
in Fig. 12 is characterized by the fact that the minor principal stress
becomes zero; the major principal stress, f,, is called the unconfined
yield strength by Jenike. Since the minor principal stress is zero, fc represents the compressive strength of the powder at the particular porosity.
Jenike showed that a powder flows more easily out of a bin the greater
the consolidation stress, o,, relative to the unconfined yield strength f,.
The ratio flC= a,/fc is called the flow function ff,; it characterizes the
flowability of powders, an important property in designing bins and
hoppers. According to Jenike, powders may be classified according to
their flowability, as shown in Table 3.
It should be noted that whilst the flow function 8: is a useful guide to
the flowability of powders, it does not completely describe the flowing
behaviour of particulate solids. A complete description is possible only
by means of the yield loci measured at various porosities.
By using the Jenike shear cell, however, only a certain region of the
yield locus curve can be determined experimentally. This region is indicated in Fig. 12 by a bold line, the remaining curve by a dashed line. The

Food particle technology - Part I

Flowability

fs,<2
2<ff,<4
4<fs,<lO
10 <ffc

TABLE 3
of Powders, Classified According
Flow Function #c = a,/fc

25

to the Jenike

Very cohesive, non-flowing

Cohesive

Cohesive
powders

Easy-flowing
Free-flowing

Non-cohesive
powders

point of intersection with the vertical axis corresponds to the cohesion

C. For non-cohesive powders C= 0. Since C depends not only on the
powder properties, but also very much on the consolidation conditions,
C is less suitable as an index of flowability than the flow function &,
Another property used to describe powders is the tensile strength 0,
which lies in the yield locus at the point of intersection with the horizontal axis. a, can be measured by using special equipment (Schubert,
1975). Since it is sometimes difficult to measure the yield locus in the
region in which the Mohr circle is plotted to determine f,, a, may be used
to interpolate the yield locus and hence to improve the measuring accuracy of f, (Eckhoff et al., 1978). This is of particular importance when
slightly cohesive powders are to be investigated, such as instant food
powders for vending machines.
Figure 12 also shows the tangent to the major stress circle from the
origin. This straight line, as experiments have shown, touches (approximately) the major Mohr circles of all other yield loci of a given particulate solid under different consolidation
conditions, i.e. at different
porosities. This straight line which is called the effectve yield locus
characterizes all steady-state flows of a material. The ratio of the two
principal stresses 0, and B, and the effective angle of friction tir are
correlated by the equation
o1

1 + sin &

a,=l-sin~r

(18)

which is interpreted by Jenike as a general law describing the steadystate flow of powders.
Many food powders tend to consolidate with time under the action of
static pressure. Interparticle adhesion increases with time, and flowability decreases correspondingly.
This effect is of importance for the
discharge of material from bins after intervals of time during which the
material may consolidate. The increase in adhesion force with time is

H. Schubert

26

primarily due to inelastic deformations at the contact points between the

particles and to the formation of solid bridges caused by crystallization
processes, for example. The influence of consolidation with time on the
flow behaviour of powders can be measured by using the Jenike shear
cell, provided that the particulate material is exposed to a normal load
for different periods of time before shearing. Yield loci are obtained
which are shifted towards higher shear stresses than without timedependent consolidation. The flow function fs,, and hence also the flowability, decrease correspondingly.
It is necessary, in all studies of the
influence of time on the flow behaviour of particulate material, that the
external conditions during exposure to normal load are kept constant.
This applies particularly to the relative humidity, RH. Many food
powders tend to consolidate with time only at RH > 0.5-0.6. The temperature during the compression may also be of importance, particularly
in cases where interparticle adhesion is promoted by sintering or crystallization processes.
Jenikes theory and the corresponding
measurements
are applied
primarily to the design of bins and hoppers (ter Borg, 198 1). Mass flow
bins in which the entire bulk material is in motion during the discharge
process (compare Fig. 13(a)) are to be preferred. In plug flow bins, the
base angles of which are less steep and smooth, the powder flows
through an outlet with some powder remaining stationary at the sides
(Fig. 13(b)). For foo d s of limited shelf life plug flow bins should be
avoided since the dead regions retain material for an indeterminate
length of time. By using the Jenike procedure, the critical cone angle BC,
which is a function of the effective friction angle 4, and the friction angle
&, between bulk material and wall, may be taken from diagrams giving

ldk
al

Fig. 13

MASS

FLOW

bl PLUG

FLOW

Mass flow and plug flow from bins.

Food particle technology - Part I

27

When the cone angle 8 5 8,, mass flow occurs. For the particulate
solid flow out of the bin, the outlet must have a minimum diameter
d, otherwise the material forms a stable arch. According to Jenikes
stability criterion, a stable arch is possible only for 0; <f,; a; is the major
principal stress acting at the abutment of an arch and which may be
calculated from the equation (see Jenike, 1970)

(20)
The flow factor fl, as a function of 8, 9, and #w, may be taken from
the diagrams of Jenike ( 1970). The condition ai =f, supplies the
critical stress a,, which acts at the abutment of an arch (see Fig. 14) from
which, by means of equation

(21)
the critical minimum diameter d, of the outlet can be determined. In eqn
(2 1), pb is bulk density, g is acceleration due to gravity; H( 0) is a function
of the geometry of the hopper given by published diagrams (Jenike,
1970). If d > d,, the formation of a stable arch which would prevent the
material from being discharged is avoided. Details of Jenikes theory are
beyond the scope of this paper; the reader is referred to Jenikes original
publication (1970) or to an excellent review paper presented by Arnold
et al. (1979).

In practice it is often difficult to determine the f, curve experimentally

in the presence of low stresses. To determine the point of intersection
with the straight line ai = a,/fl, an extrapolation of the f, curve is neces-

Fig. 14

Graphical

construction

to determine
the critical
explanation
see text).

diameter

of a bin outlet

(for

28

H. Schubert

sary. Molerus (1982) suggested a method of avoiding these difficulties.

Starting from interparticle adhesion he established a relation for the
group of yield loci which in the relevant range may be represented as
straight lines. Peleg (1971) has demonstrated
in experiments that the
yield loci of the majority of food powders may be approximated as
straight lines. The linearized yield loci allow the conclusion that the function SC=f( a,) can also be represented as straight line. Molerus formulated the equation for such straight lines as a function of the bulk
properties,
which can be experimentally
determined
in shear tests
(Molerus, 1982). The practical importance of this method will be discussed in Part II.
The accuracy of results obtained in this way would be increased
further if, for the determination of a,,, reliable shear force measurements could be made at very low normal stress; the Jenike shear cell is
not suitable for such experiments, however (Eckhoff et al., 1978). Shear
force measurements at very low normal stresses are, however, possible
by using an annular shear cell as shown diagrammatically in Fig. 1 l(b).
The powder is contained in a shear trough which rotates at angular
speed w. The torsional moment h4 is measured at the non-rotating loading ring which transmits the normal load N. From M, shear force and
hence shear stress can be derived by means of the equation
3M
=2n(R;-

R;)

(22)

which has been confirmed theoretically and experimentally (Gebhard,

198 1). The radii R, and Ri are explained in Fig. 11 (b). To transfer the
shear stress to the powder, the loading ring is roughened at its surface in
contact with the powder. One advantage of the annular shear cell over
the Jenike device is the shorter time required for a complete measurement, but the greatest is the continuous shear displacement possible with
constant sheared area. In the case of the Jenike device, despite an initial
offset (see Fig. 1 l(a)), the practical shear displacement is so small that
some cohesive food powders such as dried onion with more than 6%
moisture, some soup mixes and citric acid cannot be measured (Peleg,
1977), since neither shear failure nor steady-state flow are reached. The
annular shear cell (Walker, 19671, as further developed by Miinz ( 1976)
and modified by Ehlermann of the authors institute to meet the requirements of foods, is therefore preferred. For this purpose the measuring
accuracy particularly in the range of extremely low normal stresses has
been improved. This device is connected to a computer and thus suitable
for automatic operation.

Food particle technology - Part I

29

However, the annular shear cell is a complicated and expensive

device. For preliminary studies and comparative measurements, simpler
methods and equipment may be preferable which were proposed
especially by Peleg et al. for studies of the influence of moisture (Scoville
and Peleg, 198 1; Moreyra and Peleg, 1981) and of flow conditioners
(Hollenbach et al., 1982; Hollenbach and Peleg, 1983) on the flowability
of different food powders. The compression behaviour of powders in the
low pressure range, for instance, may be used to evaluate cohesion. For
food powders, the equation (see also Peleg, 1977)
at, = ~,,o + b 1% ~1~0

(23)

is well proven, where pb and pbo are the bulk density at pressure p, and
the reference pressure p,, (p, = ambient pressure), respectively; b is a
constant called compressibility. There is a clear correlation between b
and the cohesiveness. Powders showing a high compressibility have poor
flowing properties. The change in loose bulk density may also serve as a
measure of the effectiveness of anticaking agents, for example (Hollenbath et al., 1982). This is explainable physically from the influence of
interparticle adhesion on porosity or bulk density as mentioned above. If
quantitative information
regarding flowability is required, however,
shear tests are necessary.

ACKNOWLEDGEMENT
Many of the results reported in this paper were obtained within the
framework of research projects which were kindly supported by the
Deutsche Forschungsgemeinschaft,
Bonn.

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30

H. Schubert

Eckhoff, R. K., Leverson, P. G. and Schubert, H. (1978). The combination of

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Food particle technology - Part I

31

Notermans, S. and Kampelmacher, E. H. (1983). Haften von Bakterien bei der

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