Professional Documents
Culture Documents
To cite this article: B. Adhikari , T. Howes , B. R. Bhandari & V. Truong (2001) STICKINESS IN
FOODS: A REVIEW OF MECHANISMS AND TEST METHODS, International Journal of Food
Properties, 4:1, 1-33, DOI: 10.1081/JFP-100002186
Download by: [Australian Catholic University] Date: 24 August 2017, At: 02:47
INTERNATIONAL JOURNAL OF FOOD PROPERTIES, 4(1), 1–33 (2001)
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
1
Department of Chemical Engineering, The University of Queensland,
St. Lucia, QLD 4072, Australia
2
Food Science and Technology, School of Land and Food Sciences,
The University of Queensland, Gatton, QLD 4345, Australia
ABSTRACT
1. INTRODUCTION
∗
Corresponding author. Fax: +61(7)336-54199; E-mail: tonyh@cheque.uq.edu.au
Copyright
C 2001 by Marcel Dekker, Inc. www.dekker.com
ORDER REPRINTS
2 ADHIKARI ET AL.
Cereal Industries
Stickiness associated with dough can have strongly negative effects on dough
handling and breadmaking quality. Sticky dough causes low dough mixing tol-
erance, reduced dough strength, and reduced bread volume (Martin and Stewart,
1986; Graybosch, et al., 1993). Dough stickiness problem is of particular con-
cern to large mechanized bakeries where it can result in costly disruptions to pro-
duction schedules and in loss of product qualities (Huang and Hoseney, 1999).
Genetically modified, disease-resistant wheat varieties are increasingly cultivated
to produce higher grain yield and improve agronomic performance (Henry et al.,
1989; Dhaliwal et al., 1990). However, flours made from these wheat varieties are
reported to produce doughs with marked stickiness (Martin and Stewart, 1986).
The study of stickiness and its quantification is an important issue in the cereal
industries.
Confectionery Industries
Dairy Industries
Stickiness and the subsequent caking of milk powders has already received
much attention (Papadakis and Bahu, 1992; Chuy and Labuza; 1994; Lloyd et al,
1996; Rennie et al., 1999). Stickiness and collapse of structure are common phenom-
ena in ice cream (White and Cakebread, 1966). Adhesion of milk constituents on the
ORDER REPRINTS
STICKINESS IN FOODS 3
Powder Industries
Adhesion or sticking of food materials in food cans and packages not only
adversely affects consumers’ confidence in the quality of the product but also results
in lower product utility. Sticking of food in packaging causes further damage in
packaging material, and disfigurement of the product surface. In general, the greater
the extent of sticking of food in packages the higher the consumer antipathy to the
product (Kilcast and Roberts, 1998).
Researchers have proposed various mechanisms to explain stickiness in food
depending on the type of food products. These mechanisms also reflect the back-
ground of those who propose them: polymer physics, physical chemistry, rheology,
engineering, and mechanics etc (Lai, 1986). There is no quantitative model that
successfully and generally describes the mechanism of stickiness in food systems.
Mechanisms based on interparticle attraction (Rumpf, 1962; Schubert, 1987; Peleg;
1993) successfully explain the unwanted agglomeration and loss of flowability in
dry powders. Wetting and thermodynamic adsorption based on Young’s force equa-
tion (Young, 1805) and Dupre’s (Dupre, 1869) energy equation explain the sticky
issue based on the surface energies. The mechanisms based on tack and rheology
are used to describe pressure-sensitive adhesives (Hammond, 1989; Satas, 1989;
Kokini et al., 1984) and have found use in the quantification of dough stickiness
(Chen and Hoseney, 1995).
Instrumental methods for quantification of stickiness in food have been
product-specific. Rotational sticky point testers based on Lazer et al. (1956) have
ORDER REPRINTS
4 ADHIKARI ET AL.
been developed and adapted by drying industries (Downton et al., 1982; Wallack
and King, 1988). Measurement of cohesive and adhesive forces based on Jenike’s
shear cell or similar devices has been widely used to characterize the degree of
powder flowability by powder industries (Peleg, 1993; Pasley and Haloulos, 1994;
Teunou et al., 1999). Probe methods that have been in application in pressure-
sensitive adhesives are successfully adapted to measure the stickiness of wheat
dough (Chen and Hoseney, 1995) and candy (Kilcast and Roberts, 1998). Recently,
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
STICKINESS IN FOODS 5
representing a best fit for wide range of materials. However, Peleg (1992) has argued
against the practice of using universal constants in Equation (1). Because C1 and
C2 are product-specific and also vary along with the temperature range and the
chosen reference temperature (Tg in this case) he recommended that the constants
C1 and C2 should be determined for individual material for a given temperature
range considering the reference temperature.
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
2.2. Water
The interaction of water with solids is the prime cause of stickiness and caking
in low-moisture foods. Properties like viscosity, surface tension, and good solvation
all make water a suitable catalyst for stickiness, caking, and collapse of food and
particulate systems. Besides, it is a part of atmosphere and any increase in the
relative humidity of air is associated with the possibility of increased amount of
water being adsorbed to the surface or absorbed in to the bulk (Griffith, 1991).
At room temperature the critical relative humidity, the humidity at which the food
powders exhibit caking, can be as low as 33% in the case of tea and whey powder
(Teunou et al., 1999).
Water is a ubiquitous plasticizer (refers to the process of softening and in-
crease in flexibility of a polymer brought about by the incorporation of a plasti-
cizer, alternatively defined as a process of lowering the glass transition tempera-
ture) for low-moisture foods and biological materials (Slade and Levine, 1991).
The increase of water content results in a sharp decrease in the glass transition
temperature (Tg ). The Tg of food materials such as sugars, starch, gluten, gelatin,
hemicellulose, and elastin decreases rapidly to about −10◦ C or so when mois-
ture content increases to 30% by mass (Atkins, 1987). Furthermore, the rate of
decrease of Tg attributable to water plasticization is ∼10◦ C per 0.01g of water/g
of material (Slade et al., 1989). Plasticization of amorphous food powders and
the subsequent depression of their glass transition temperature below ambient
temperatures is related to undesired textural behavior such as caking and stick-
iness in food powders including sugar-rich foods (Slade and Levine, 1991), the
mechanism of this effect may be through much lowered viscosity (Downton et al.,
1982; Wallack and King, 1988) or the viscous effects of liquid bridges (Peleg,
1993).
Furthermore, water can exist on particle surfaces as adsorbed mono/multi-
layers or as capillary condensation. This can reduce surface micro-roughness of the
particles thereby allowing them to come closer, which then increases the forces of
attraction between the particles. This may be an important cause of caking of the
particles in the presence of water (Iveson, 1997).
2.3. Temperature
6 ADHIKARI ET AL.
the product temperature is less than the glass transition temperature, phenomena
including stickiness and adhesion will not take place. It is also emphasized that for
amorphous products of any kind the magnitude of T-Tg is a fundamental indicator
of stickiness and adhesion (Slade and Levine, 1991).
2.4. Compression
STICKINESS IN FOODS 7
during storage of spray-dried fermented soy sauce powders (Hamano and Aoyama,
1974).
High molecular weight water compatible ingredients such as carbohydrates
and proteins have a high glass transition temperature because Tg increases with
increasing molecular weight (Fox and Flory; 1950; Roos and Karel, 1991). Hence,
addition of ingredients like low DE maltodextrins is recommended both in drying
(Bhandari et al., 1997b) and storage practices (Nisshin, 1981) to minimize stickiness
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
Protein o
Polysaccharides o
Fats +
Low molecular sugars ++
Organic acids ++
Water/relative humidity +++
Particle size distribution +
Compression/pressure ++
Temperature +++
Viscosity +++
8 ADHIKARI ET AL.
of attraction because of their very high surface to volume ratio. Van der Waals’
forces Fvdw can become significant for particles below 10 micron size where the
interparticle distance becomes sufficiently small (Rumpf, 1962). The most typical
characteristics of food particulate system compared with assemblies or large size
bodies is that minor changes in the surface properties can bring about major changes
in bulk properties. This is because the surface forces become dominant over gravi-
tational forces in small particulates (Schubert, 1987). It is considered that powders
with particle sizes larger than 200 micron are free-flowing while finer powders are
susceptible to cohesion and their flowability is more difficult (Teunou et al., 1999).
The cohesive or adhesive forces are inversely related to the particle size (Buma,
1971; Renne et al., 1999). Furthermore, if particles are of 1 micron size or finer,
these molecular forces can appreciably deform them thereby creating more con-
tact area that results in more intimate contact (Gay and Leibler, 1999). A diagram
showing the strength of agglomerate bond as a function of particle size is given in
Figure 1.
Figure 1. Strength of bridges to hold particles together. The intermolecular and electrostatic forces
will not be active above 10 micron (adapted from Rumpf, 1962).
ORDER REPRINTS
STICKINESS IN FOODS 9
3. MECHANISMS OF STICKINESS
3.1. Interparticle Attraction
The factors rendering the particles adhesive or cohesive may be similar but
higher cohesion is not necessarily associated with higher adhesion or vice versa.
The extent of cohesive or adhesive behavior depends on the nature of the food and
external factors like moisture and heat. According to Rumpf (1962), mechanisms
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
Cohesion between two particles and adhesion between two surfaces without
material bridges is primarily attributable to Fvdw and electrostatic forces. For parti-
cles smaller than 5 micron, these forces become dominant compared with the weight
of the particles and they tend to form agglomerates without the need for solid and
liquid bridges (Walton and Mumford, 1999). The Fvdw can be calculated for two
spheres of diameter d1 (m) and d2 (m) separated from each other by distance x (m), as:
E p d1 d2
Fvdw = (2)
16π(d1 + d2 )x 2
E p , the Van der Waals’ interaction energy, is between 10−19 and 2 × 10−18 J. Van
der Waals’ force (N) is maximum when particles are in intimate contact with each
other. Equation (2) is derived based on ideally smooth and rigid spheres and is also
that applicable in particle-plane interfaces (Schubert, 1987). It should be noted that
the Van der Waals’ attractive force between a sphere and a plane surface is twice
the force between two rigid spheres and also that this force increases if a film of
liquid phase is present between the solid particles (Papadakis and Bahu, 1992).
Electrostatic Forces
10 ADHIKARI ET AL.
of separation between the spheres. Equation (3) is also applicable for sphere-plane
interface (d1 /d2 → 0) (Schubert, 1987).
With electrically conducting particles, electrostatic adhesion arises only when
the particles make contacts attributable to contact potential. The adhesion force,
Fel,c (N ) attributable to contact potential between two rigid spheres is given by:
πεr εU 2 d1 d2
Fel,c = (4)
2(d1 + d2 )x
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
where,Fel,c is force of adhesion (cohesion) between the two spheres and U is contact
potential (N.m.s−1 or volt), which is frequently between 0.1 and 0.7 V. Equation
4 can also be applied when contact between a sphere and a plane (d1 /d2 → 0) is
involved (Schubert, 1987).
b. Liquid Bridges
Wet agglomerates or cakes are held together by forces originating from mobile
liquid between the particles. Based on the extent of occupation of voidage by water,
these bridges can further subdivided into three groups: pendular, funicular, and
capillary.
Pendular State
According to Newitt and Conway-Jones (1958), the pendular state is the one
in which liquid has occupied only a part of the total voidage between the particles. In
this state the liquid bridges have strength resulting from the pressure drop developed
through curvature of the liquid meniscus and also from the interfacial tension exerted
by the liquid along the wetted perimeter. Hence, liquid bridges result in a combined
pull of the solid particles by these two forces (Rumpf, 1962; Newitt and Conway-
Jones, 1958; Papadakis and Bahu, 1992). Assuming perfect contact between two
rigid spheres, and perfect wetting, the tensile strength, T (Pa) of agglomerate coming
from pendular water is given by (Newitt and Conway-Jones, 1958):
(1 − ϕ) σ
T = 2.8 (5)
ϕ d
where, σ is liquid surface tension (N .m −1 ), ϕ is porosity (dimensionless) of the
agglomerate and d is the particle diameter (m).
ORDER REPRINTS
STICKINESS IN FOODS 11
When the void space between powder particle is completely filled by water
extending to the edge of the pore and forming a concave surface, a negative capillary
pressure is exerted in the entire liquid space boosting the tensile strength of the wet
agglomerate, which is referred to as a capillary state (Papadakis and Bahu, 1992).
The tensile strength of capillary water is given by:
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
(1 − ϕ) σ
T = 8.0 (6)
ϕ d
Comparison of Equations (5) and (6) shows that the tensile strength of the wet
agglomerate or cake is almost three times greater in capillary state than in pendular
one.
The funicular state is the transition between pendular and capillary state. In this
state gas still occupies a small fraction in the water continuum. The tensile strength
provided by the funicular water lies between those provided by the capillary and
pendular water (Fig. 2).
These liquid bridges come in existence when viscous binders are introduced
between the particles. The immobile liquid bridge creates a strong binding force
between the particles through the viscous binder, which is far stronger than the
mobile liquid bridges. Immobile liquid bridging can be observed in spray-drying.
The thermoplastic materials (sugars) at or above glass transition form immobile
liquid bridges ultimately leading to unwanted lumping. This type of liquid bridge
retains a capacity to transform itself into solid bridges in subsequent drying. The
mechanism of this type of bridge formation is viscous flow driven by surface energy
(Downton et al., 1982; Wallack and King, 1988). Wallack and King (1988), through
the independent measurement of sticky behavior and viscosity of sucrose/fructose
Figure 2. Schematic diagram of liquid bridges. a) Pendular state, b) funicular state, and c) capillary
state. P, particle, LB, liquid bridge; A, air (adapted from Peleg, 1977).
ORDER REPRINTS
12 ADHIKARI ET AL.
mixture and instant coffee, found that Frenkel’s (1945) equation relates the rate of
bridge size increase and agglomerate strength to the material properties.
a 2 3 σ t
= (7)
d 2 dµ
Where, a is interparticle bridge diameter (m), d is particle diameter (m), t is time(s),
µ is viscosity (Pa.s) and σ is surface tension (N .m −1 ) of the liquid. It can be seen
from Equation(7) that increase in particle diameter and the viscosity substantially
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
c. Solid Bridges
STICKINESS IN FOODS 13
Complete wetting of the surface will occur when the surface energy of the adherend
is greater than that of the adhesive (Saunders et al., 1992). This is attributable to
the fact that low-energy materials absorb strongly to high-energy surfaces to lower
the surface energy of the system.
The mechanism of thermodynamic adsorption is based on Young’s force equa-
tion (Fowkes, 1964) and Dupre’s energy equation (Michalski et al., 1997). Young’s
equation relates solid and liquid surface tensions γs (N .m −1 ) and γl (N .m −1 ), solid-
liquid interfacial tension γsl (N .m −1 ) and the liquid contact angle θ at the solid/
liquid/ air triple line. Similarly, Dupre’s equation relates adhesive and adherend
surface tensions to the work of adhesion, Wa (J.m−2 ) (Equation 9).
γs = γl cos θ + γsl (8)
Ws = γs + γl − γsl (9)
The adsorption theory based on thermodynamic principles was developed from
the work of number of authors including Girifalco and Good (1957), Fowkes
(1964) and van Oss et al. (1990). From their work it appears that adhesion is
attributable to electrodynamic intermolecular forces acting at the liquid-liquid,
liquid-solid, and solid-solid interfaces and that interfacial attraction between the
adhesive and adherend can be expressed in terms of reversible work of adhesion
that corresponds to material surface tensions. Zisman’s (1963) solid critical sur-
face tension for wetting and van Oss et al.’s (1990) concept of acid base interac-
tions in adhesion process have made substantial contributions to broadening this
theory.
Previously, an objection in the use of this theory was that the work of adhesion,
when measured experimentally was found to be substantially higher compared with
the same calculated theoretically (Michalski et al., 1997). But it was found that
the difference was attributable to viscoelastic dissipation occurring at the site of
adhesive fracture (Shanahan and Carre, 1995). Spreading of liquid on a viscoelastic
solid causes dissipation through the formation of a wetting ridge on the solid at the
triple line. The work of adhesion is now recognized as a function of the reversible
work of adhesion and the irreversible deformation of the substrate (Shanahan and
Carre, 1995; Michalski et al., 1997).
The energy required to separate two objects that are not permanently bound
together is a measure of tack (Russel and Kim, 1999). Tackiness is the word often
ORDER REPRINTS
14 ADHIKARI ET AL.
process, which in turn causes deformation and friction in the contact film. If a good
contact is to be established between two surfaces, some softness of the material
is essential. Hence, a material is tacky when it possesses a right balance between
softness and ability to dissipate energy (Crevoisier et al., 1999). Wettability on
the other hand, is related to the interfacial energy of a material. Green (1942) had
expressed tack (N) as:
π R4µ
Tack = +Cf (10)
D2t
where, D is the sample thickness (m), R is the radius of the contact area (m), t is the
time of rupture (s), µ is viscosity (Pa.s), f is yield stress (Pa), and C is proportionality
constant (m 2 ) depending on D and R. The second term in Equation (10) will be
zero for any nonyield stress materials.
Foods are pressure-sensitive and may behave in a similar manner to pressure-
sensitive adhesives. First, the greater the force used to apply the probes (Section
4.4 deals more with probes) to the surface of the food, the greater the tackiness will
be (Hoseney and Smewing, 1999). Second, the force required to remove the probe
(tackiness) is proportional to the rate at which it is withdrawn (Chen and Hoseney,
1995). Boyd and Sherman (1975) observed that subjective stickiness is analogous
to the high crosshead speeds of Instron testing machine. Stickiness of sugar syrups
was investigated by Brennan and Mohamed (1984) who found that viscosity and
surface tension were directly proportional to the stickiness.
Not only is the bonding between adhesive and adherend essential for sticki-
ness, but the mechanism of failure of this bond is also equally significant (Fig. 3).
The clean failure of adhesive and the adherend surface is termed adhesive failure
while the failure within the adhesive with residue on the adherend surface is known
as cohesive failure (Kilcast and Roberts, 1998). The adhesive industries have been
able to successfully manipulate the failure mechanism so that only adhesive failure
takes place. Cohesive failure may be dominant mode of failure where stickiness of
the food is concerned.
Research on pressure-sensitive adhesives has shown that the mode of failure
depends on the rate of separation and the temperature. Higher rate of separation
of the surfaces favors the adhesive failure while the slow rate the cohesive one
(Kambe and Kamagata, 1969). It was also found that transition from adhesive to
cohesive failure takes place when one moves toward the phase transition (Satas,
1989). Cereal scientists have noted similar effect of rate and temperature in failure
mechanism. They further found that increase in moisture favors cohesive failure
(Dhaliwal et al., 1990).
ORDER REPRINTS
STICKINESS IN FOODS 15
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
Figure 3. Schematic presentation of failure mechanism between adhesive and adherend surfaces
(adapted from Kilcast and Roberts, 1998).
Recently glass transition temperature (Tg ), the temperature at which the switch
between rubbery and glassy phases takes place, is being recognized as a fundamental
parameter to explain and control stickiness (Roos and Karel, 1991; Bhandari and
Howes, 1999) for amorphous and semicrystalline foods particularly in the case of
low molecular weight carbohydrates.
The glass transition temperature is a fundamental property of a amorphous
material. When a glassy material is subjected to moisture and heat and subsequently
approaches the phase transition, the viscosity of the system decreases dramatically
from 1012−14 Pa.s to 106−8 Pa.s. The lowered viscosity is unable to support the
glassy microstructure giving way to structural collapse of freeze-dried products and
stickiness of spray-dried ones (Wallack and King, 1988; Tsourouflis et al., 1976;
Flink, 1983). If the glass transition temperature of a powder is lower than the storage
temperature, the phenomena of stickiness, caking, and unwanted agglomeration
becomes unavoidable.
The literature values of sticky point temperature and glass transition temper-
ature for low-moisture content sucrose: fructose (7:1) mixture has been shown in
Figure 4. It can be seen that the semilogarithmic plots of sticky point temperature
and glass transition temperature with moisture content run almost parallel to each
other; the sticky point temperature is almost 4–11◦ C higher than the glass transition
temperature (Tg end). Hence, glass transition temperature can be used as a reliable
indicator of stickiness.
It has been shown that it is possible to switch on or off stickiness (Crevoisier
et al., 1999). It is generally noticed that surface properties of a polymer change
abruptly when it changes from structured smectic phase to disordered isotropic
phase. This change in the surface properties is brought about by the bulk properties
(e.g., viscosity) through the change of phase which can be manipulated for tuning
of stickiness at will (Crevoisier et al., 1999). These authors also found that for a
copolymer obtained by copolymerization of an acrylate monomer bearing a long
ORDER REPRINTS
16 ADHIKARI ET AL.
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
Figure 4. Plots (semi-logarithmic) of sticky point temperature (Tst ) and glass transition temperature
(Tg ) with moisture content for low moisture sucrose/fructose (7:1); data taken from Downton et al.
(1982) and Roos and Karel (1991b). Solid line (——) indicates variation of sticky point temperature
with moisture content (dry basis), Dotted line (----) indicates variation of glass transition temperature
with moisture content (db).
perfluoro alkyl side chain (C2 H4 -C8 F17 ) and a methacrylate monomer bearing a
long alkyl chain (C17 H35 ) the tack energy was zero at the smectic phase, while
it was 50 J/m2 at the switch temperature (37◦ C) and decreased with increasing
temperature. The surface wetting increased from 10% at smectic phase to nearly
100% in the isotropic phase. It is not difficult to see that thermodynamic and bulk
properties of a substance undergo a sharp change at or around glass transition tem-
perature. The sharp drop in viscosity because of the glass transition is responsible
for rendering the product tacky or sticky. Hence, the glass transition concept can
be successfully used as an approach for characterizing stickiness.
4. TEST METHODS
A brief review of various test methods that have been adapted for charac-
terization of food stickiness is presented in this section. A subjective comparison
of these methods in terms of the degree of automation, extent of application, and
ability of the same to quantify stickiness is presented in Table 2.
STICKINESS IN FOODS 17
Table 2. Comparison of Various Test Methods Currently Used to Assess Food Stickiness
Degree of
Test Method Test Products Quantification Automation Usage
o, base point (not much use); +, wide usage; ++, wider usage; +++, widest usage.
Figure 5. Schematic diagram of a) split type rotational shear cell and b) Jenike shear cell used for
measuring cohesive and adhesive force of particulates (adapted from Peschl (1989) and Jenike (1962),
respectively).
ORDER REPRINTS
18 ADHIKARI ET AL.
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
Figure 6. Yield loci of noncohesive a) and cohesive b) powders. OC represents the cohesive force
and OT represents the tensile strength (adapted from Peleg, 1993; Peschl, 1989).
Figure 7. Schematic diagram of Mohr Circles. σ1 andσ2 : major and minor consolidating stresses, f c :
unconfined yield strength, OC and OT: cohesive force and tensile strength of the powder, respectively
(adapted from Peschl, 1989).
ORDER REPRINTS
STICKINESS IN FOODS 19
yield strength (Pa) (normal stress where the Mohr semicircle drawn through the
origin intercepts the normal stress axis). The extent of cohesiveness or adhesiveness
of a powder is determined based on this index.
This method is successfully adapted by industries for characterizing the flow
behavior of powders through chutes and hoppers. It has also been widely used to
characterize the caking properties of the dry particulates. However, it is confined
to dry particulate systems. It is not possible to use the shear cells for semi-solid
foods. Furthermore, it is very hard to adapt it to high temperature and high humidity
systems.
A sticky point tester was developed by Lazar et al. (1956) to assess the effects
of temperature on the powder and subsequently modified and used by Downton et
al. (1982) and Wallack and King (1988). The sticky point tester used by Wallack
and King (1988) consists of a test tube in which a powder with known moisture
content is placed. This test tube can be rendered airtight using a rotating mercury
seal. The tube is then immersed in a controlled temperature bath and the bath tem-
perature is raised slowly. The powder within the test tube is intermittently stirred
either by hand or through a machine-driven impeller that is imbedded in the sam-
ple. When temperature is slowly raised, a temperature is reached at which the
force experienced to drive the impeller is maximum; this is called sticky point
temperature. The sticky point temperature is a function of moisture content. This
test is repeated for other moisture contents and corresponding sticky points are
determined. Finally, the sticky point temperatures are plotted as a function of mois-
ture content. The drying industry uses this sticky point versus moisture content
curve to identify a safe drying regime. Schematic diagram of this sticky point
tester is provided in Figure 8. Recently additional improvements to this tester by
introducing double and curved blades have been reported (Pasley and Haloulos,
1994).
Although the information based on this test is very important for determination
of safe drying regime, it fails to provide information regarding the stickiness status
(flowability status) of a powder below the sticky point temperature (Peleg, 1993).
Its use is confined to empirically determine the safe drying regime, especially in
spray-drying operations.
ORDER REPRINTS
20 ADHIKARI ET AL.
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
Figure 8. Schematic diagram of sticky point testing apparatus (adapted from Wallack and King,
1988).
STICKINESS IN FOODS 21
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
Figure 9. Schematic diagram of optical probe used for sticky point determination free-flowing
particulates (Adapted from Lockemann, 1999). 1, illuminator-receiver; 2, light pipe; 3, fiber-optic
sensor; 4, test-tube; 5, oil or water bath (oil or water); 6, rotating drive; 7, temperature probe; and 8,
tube mount.
The signal recording system gives a sharp rise in reflectance, which is indication
of the sticky point. Schematic diagram of this instrument is provided in Figure 9.
This instrument is novel and may prove very useful for online monitoring of
stickiness in powders as a function of moisture and temperature. So far, it has only
been used to determine the sticky point temperature of solid β-carotene. It needs to
be tested with particulates that tend to be transparent on softening and melting. Like
other sticky point temperature methods it can not be used to quantify the stickiness
of a powder system below the sticky point temperature.
The tack test involves the contact of a probe with adhesive material and mea-
suring the tensile strength of the bond. One of the earliest tackmeters was used to
study the tackiness of different inks applied on top of the other. A probe is brought
in contact with the ink surface and subsequently pulled back and the force needed
to separate the probe from the ink surface and the time taken for failure to occur is
recorded (Green, 1941). Schematic diagram of Green’s type tack meter is presented
in Figure 10.
Research on pressure-sensitive adhesives has made intensive use of flat-faced
probes. During the separation of probe from adhesives force and time of separation
are recorded and area under the curve is determined (tack) (Kilcast and Roberts,
1998). The tack values of doughs have been found to increase with both the contact
force and contact time. The increase in contact force, rate of withdrawal and contact
time all seem to have positive correlation with tack energy (Saunders et al., 1992).
The increase in temperature casts profound influence both in tack and the failure
mechanisms.
ORDER REPRINTS
22 ADHIKARI ET AL.
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
Figure 10. Schematic diagram of tack meter used for measurement of ink tackiness (Adapted from
Green, 1941). a) 1, constant temperature bath; 2, sample holder; 3, tack probe; 4, support; 5, probe
holder lever; 6, position knob; 7, load lever; 8, loads; and 9, stand. b) tack probe in action.
Special tackmeters (such as: TA.XT2, Stable Micro Systems, England) have
been developed (Chen and Hoseney, 1995) and widely being used to measure wheat
dough stickiness and can work in a lower load range. However, the use of tackmeters
has been confined to semi-solid foods and paste systems.
Peel tests have often been used for testing the strength of adhesives. Two
peeling modes (i.e., 90 and 180◦ ) are most often used for this purpose. The 180◦
peeling mode is easier to perform but if the adhesives are sensitive to bend-
ing, structural damage may occur when the adhesive bends through 180◦ . A bend
test through 90◦ requires a relatively complex holding system that maintains
the peeling angle at 90◦ throughout the experiment (Kilcast and Roberts,
1998).
These peeling tests are less applicable to quantify the food adhesion. Rosinski
et al. (1989) used 180◦ peeling test to study the adhesion of meat on packaging
surface using an Instron-testing machine and reported that the degree of adhe-
sion of meat on different can be determined. These peel tests are mainly confined
to adhesive and tape industries and seem unlikely to be embraced by the food
industries.
ORDER REPRINTS
STICKINESS IN FOODS 23
4.6. Weighing
both the viscosity of the foods and the surface engergies of the adherend influenced
the amount of food adhesion (Michalski et al., 1999).
Although this test method is simple, it is difficult to say quantitatively which
force, adhesive or cohesive, is dominant. A monolayer of food sticks on the adherend
surface because of adhesive force and the remaining mass may simply remain there
because of the cohesive force.
The sticky point test described before at first instance appears to be somewhat
empirical in nature. But, in reality, it is based on the softening of powders above
their glass transition temperature when the glassy phase yields to a rubbery one.
From the work of Schubert (1987) it is known that the magnitude of Van der Waals
and electrostatic attraction is not as high as the attraction force that comes from
liquid bridges. According to Rumpf (1962) liquid bridges offer strong bonding that
has a significant practical significance in particulate aggregates having a size of
1 mm or less. Hence, formation of liquid bridges should be prevented if caking and
sticking of powders is to be avoided. In reality, liquid bridging can only occur when
at least some of the particle surface is viscous (or if there is a presence of an external
moisture or a second liquid phase). The surface of particle can become viscous either
because of the adsorption of moisture from the surroundings or plasticization by
the moisture already present. The plasticization of the particle surface accelerates
once the glass transition temperature is exceeded (Peleg, 1993).
Work by Slade et al. (1993) explains that unwanted agglomeration and caking
of food powders in storage can be avoided simply by storing them below their glass
transition temperature provided that adsorption of moisture from the environment
is avoided. The sticky problem in drying can best be explained from the notion
of glass transition. By determining the glass transition temperature of a system, it
is possible to predict a bulk temperature and moisture matrix, which renders the
product sticky. Furthermore, a safe drying regime can be designed by manipulating
the glass transition temperature by simply controlling the drying parameters or
introducing some drying aids.
The instruments that are used to measure the glass transition temperature are
based on three basic measurement techniques viz. calorimetric, molecular mobil-
ity, and mechanical-thermal (Blanshard, 1993). Calorimetric methods make use
of changes in specific heat capacity (C p ). The differential scanning calorimeter
ORDER REPRINTS
24 ADHIKARI ET AL.
entire molecule, but also the mobility of individual groups or region within a food
structure (Blanshard, 1993). Mechanical-thermal methods measure the changes in
loss modulus, elastic modulus, and their ratio as a function of temperature. A sharp
change in these properties is indicative of glass transition temperature (Rahman,
1995).
Although the glass transition temperature is a fundamental property directly
related to food stickiness, techniques to measure the Tg itself require complex
instruments and a high level of professional expertise. Current research on glass
transition temperature shows that it may be possible to quantify stickiness in a
broad range of food products. But, to this date, it has only been used to characterize
low molecular weight carbohydrate systems. There is a real need to develop simple
methods and instruments for measuring glass transition temperature for foods.
The Instron universal tester has been used by some researchers to study the
stickiness of sugar syrups (Brennan and Mohamed, 1984). It involves the contact of
crosshead or crosshead attached to a flat plate (resembling a flat-faced tackmeter)
to a food surface at a low speed. It is then allowed to rest for some time and
finally withdrawn from the food surface at greater speed. The force required for
separating the crosshead from the food sample correlates with stickiness. Juliano
(1985b) used an Instron for characterization of stickiness of cooked rice. Kumar
et al. (1976) studied the stickiness of cooked rice by shaking and tapping a sieve with
a suitable opening and allowing the cooked rice to pass through the sieve opening.
The higher the amount of rice retained on the sieve, the greater the stickiness. A
Tensipresser is used for characterization of stickiness in waxy and nonwaxy rice
having various amylose contents (Okadome et al., 1999). Through its use, it is
reported that the waxy rice (0.2–1.5% amylose by dry basis) is correlated highly
with adhesiveness (stickiness). Furthermore, a salient feature of this device is that it
is able to differentiate the decrease in stickiness of cooked rice with gradual increase
in amylose content and also that surface stickiness of a single kernel of cooked rice
can be measured with ease (Okadome et al., 1999). The working principle of this
device is similar to a texturometer or an Instron universal tester.
Contact angle is the measure of wettability and it can ultimately be linked with
the degree of adhesion on a surface. For good adhesion, the contact angle of the fluid
and the rigid phase must be zero, or nearly so. The contact angle is, thus, a useful
inverse measure of the wettability of a surface, in the sense that smaller contact
ORDER REPRINTS
STICKINESS IN FOODS 25
angles are obtained with highly (or easily) wettable surfaces. Furthermore, lower
the contact angles and higher the wettability more force will be required to separate
these surfaces (Baier, 1970). The tilted plane technique of contact angle measure-
ment was adapted by Lai (1986) to measure the extent of stickiness of the food
products such as salad dressing and tomato sauce on various packaging materials.
STICKINESS
5.1. Spray-Drying Operations
Various methods have been used to overcome the sticky problem in spray-
drying operations; some common ones are given below.
• Introduction of cold air: Cold air is introduced at the bottom of a drying
chamber (Lazar et al., 1956). A limited amount of air can only be intro-
duced because the cooling process increases the relative humidity of the
air, which is capable of reviving the sticky problem again (Bhandari et al.,
1997a).
• Control of wall temperature: Application of this technique to orange
juices, black currants, and raspberries (Bhandari, et al., 1993) are re-
ported to minimize the wall deposition. High wall temperature (>sticky
point) not only causes stickiness and wall deposition of thermoplastic
powders but also discoloration, self-heating and burning of deposited
powder. However, low wall temperature (<sticky point) leads to heat loss
and underdried products.
• Scraped surface drying chamber: It has been used by Karatas and Esin
(1990) for tomato paste to continuously remove the wall depositions that
improved the yield and quality.
• Low temperature drying (Birs dryer): Air of 30◦ C and 3% relative hu-
midity is used in association with a very large spray-drying tower. This
is a humidity-driven rather than temperature-driven process. Today this
dryer is no longer in use (Hayashi, 1989).
• Drying aids: Addition of high molecular weight additives, in the feed,
before drying has long been practiced. The additives raise the glass tran-
sition temperature of the drying particle and also reduce hygroscopicity
and thermoplasticity of the resultant mixture. Maltodextrin has been used
widely for many juices such as orange (Gupta, 1978), black currants, and
raspberry (Bhandari et al., 1993), honey, and pineapple (Bhandari et al.,
1997b). The use of additives is the most common way of spray-drying
sugar-rich foods.
• Control of Drying Parameters: Based on the knowledge of glass transition
temperature and drying kinetics (drying rate, particle temperature, and
skin formation etc.), it is possible to define a safe drying regime at which a
successful drying operation can be accomplished. Fundamental studies to
ORDER REPRINTS
26 ADHIKARI ET AL.
finely divided. These particulates undergo a phase change when they reach
Tg . Moisture acts as a plasticizer effectively depressing the glass transi-
tion temperature. The combined effect of temperature and moisture of a
food powder and its surrounding is responsible for stickiness and caking.
Hence, storage of the food powders below their Tg is recommended to
avoid stickiness and caking during storage and transportation (Roos and
Karel, 1991; Peleg, 1993). The temperature during storage and transporta-
tion frequently jumps above the Tg and makes the foods quite vulnerable
to stickiness and unwanted agglomeration. Regarding food powders with
high-fat content, it is desirable to store them below the melting point of
the fat to prevent fat induced caking.
r Addition of flow conditioners: Flow conditioners and anticaking agents are
chemically (or practically) inert, finely divided particulates that are added
to host particles to improve their flowability or tendency to cake. These
conditioners are effective when added up to 2%. The main food grade
conditioners are silicon dioxide, silicates, phosphates, salts of stearic
acid, starches, and modified carbohydrates (Peleg et al., 1973; Peleg and
Hollenbach, 1984). Flow conditioners inhibit the caking of food powders
and improve the flowability of host powders through various mechanisms
including physical separation, interruption of liquid bridges, lubrication,
competitive adsorption of water (increased availability of sites for wa-
ter sorption through coating action) and cancellation of molecular and
electrostatic charges (Peleg and Mannheim, 1977; Peleg and Holenbach,
1984; Lai et al., 1999). They are effective, partly, because of their low
particle size (<5 µm). Except the chemicals mentioned above various
substances like oils in raisins (Kostaropoulos et al., 1997) and low DE
maltodextrin in sugars (Nisshin, 1981) etc are also recommended as anti-
caking or antisticking agents. Commonly used flow conditioners in food
systems are listed in Table 3.
STICKINESS IN FOODS 27
Table 3. Commonly Used Flow Conditioners and Anticaking Agents in Food System
Silicondioxide (silica) Egg powder, flavors, salts, spices, Peleg and Hollenbach (1984),
dried soups and bases, cocoa, Lai et al. (1999), Onwulata
milk substitute, coffee whitener, et al. (1996)
sucrose, cheese, dates, citric acid,
lactose, modified corn starch
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
28 ADHIKARI ET AL.
6. CONCLUSIONS
ize the problem of food stickiness. Because all the mechanisms and test methods
have been limited in one or two products, glass transition temperature-based mech-
anism and test methods seem to be generally applicable where the stickiness and
caking of low molecular weight carbohydrate system are involved.
REFERENCES
Angell, C.A.; Stell, R.C.; Sichina, W. Viscosity-Temperature Function for Sorbital from
Combined Viscosity and Differential Scanning Calorimetry Studies. J. Physical Chem.
1982, 86, 1540–1542.
Allen, K.W. Current Theories of Adhesion and Their Relevance to Adhesive Technology.
J. Physics IV 1993, 3, 1511–1516.
Atkins, A.G. The Basic Principles of Mechanical Failure in Biological Systems. In Food
Structure and Behavior; Blanshard, J.M.V., Lillford, P.J., Eds.; 1987; 149–176.
Baier, R.E. Surface Properties Influencing Biological Adhesion. In Adhesion in Biological
Systems; Manly, R.S. Ed., Academic Press: New York, 1970; 15–45.
Bhandari, B.R.; Senoussi, A.; Dumoulin, E.D.; Lebert, A. Spray Drying of Concentrated
Fruit Juices. Drying Technol. 1993, 11 (5), 1081–1092.
Bhandari, B.R.; Datta, N.; Howes, T. Problems Associated with Spray Drying of Sugar-Rich
Foods. Drying Technol. 1997a, 15 (2), 671–684.
Bhandari, B.R.; Datta, N.; Crooks, R.; Howes, T.; Rigby, S. A Semi-Empirical Approach to
Optimize the Quantity of Drying Aids Required to Spray Dry Sugar-Rich Foods. Drying
Technol. 1997b, 15 (10), 2509–2525.
Bhandari, B.R.; Howes, T. Implication of Glass Transition for the Drying and Stability of
Foods. J. Food Eng. 1999, 40 (1–2), 71–79.
Blanshard, J.M.V. The Glass Transition, its Nature and Significance in Food Processing.
In Glassy State in Foods; Blanshard, J.M.V., Lillford, P.J., Eds.; Nottingham University
Press: England, 1993; 18–48.
Boyd, J.V.; Sherman, P. The Mechanics of Stickiness Evaluation in Foods. A Comparison
of Oral and Instrumental Methods of Evaluation in Selected Foods. Biorheology 1975,
12, 317–322.
Brennan. J.G.; Herrera, J.; Jowitt, R. A Study of Some of the Factors Affecting the Spray
Drying of Concentrated Orange Juice, on a Laboratory Scale. Food Technol. 1971, 6,
295–307.
Brennan, J.G.; Mohamed, A.M.A. Relating Sensory Stickiness and Physical Properties of
Foods. In Engineering and Food; MacKenna, B.M., Ed.; 1984; Vol. 1, 489–498.
Buma, T.J. Free Fat in Spray Dried Whole Milk 5. Cohesion: Determination, Influence of
Particle Size, Moisture Content and Free Fat Content. Netherlands milk Dairy J. 1971,
25, 107–122.
ORDER REPRINTS
STICKINESS IN FOODS 29
Burton, H. Deposits From Whole Milk in Heat Treatment Plant-A Review and Discussion.
J. Dairy Res. 1968, 35, 317–330.
Chen, J.J.; Lu, S.; Lii, C.Y. Effect of Milling on the Physico-Chemical Characteristics of
Waxy Rice in Taiwan. Cereal Chem. 1999, 76 (5), 796–799.
Chen, W.Z.; Hoseney, R.C. Development of an Objective Method for Dough Stickiness.
Lebensm.-Wiss.-u.-Technol. 1995, 28 (5), 467–473.
Chuy, L.E.; Labuza, T.P. Caking and Stickiness of Dairy-Based Food Powders as Related
to Glass Transition. J. Food Sci. 1994, 59 (1), 43–46.
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
30 ADHIKARI ET AL.
STICKINESS IN FOODS 31
Martin, D.J.; Stewart, B.J. Dough Mixing Properties of a Wheat-Rye Derived Cultivar.
Euphytica 1986, 35, 225–232.
Matthews, D.B. Electrochemical Studies on the Adsorption of Amino Acids in Relation to
Compatibility of Prosthetic Materials and Human Body. J. Biomed. Material Res. 1969,
3, 475–496.
Michalski, M.C.; Desobry, S.; Hardy, J. Food Material Adhesion: A Review. Crit. Rev.
Food Sci. Nutr. 1997, 37 (7), 591–619.
Michalski, M.C.; Desobry, S.; Babak, V.; Hardy, J. Adhesion of Food Emulsions to
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
32 ADHIKARI ET AL.
Roos, Y.; Karel, M. Plasticizing Efffect of Water on Thermal Behavior and Crystallization
of Amorphous Food Model. J. Food Sci. 1991b, 56 (1), 38–43.
Roos, Y.; Karel, M. Effects of Glass Transitions on Dynamic Phenomena in Sugar
Containing Food Systems. In Glassy States in Foods; Blanshard, J.M.V.; Lillford, P.J.,
Eds.; Nottingham University Press: England, 1993; 207–222.
Rosinski, M.J.; Barmore, C.R.; Dick, R.L.; Action, J.C. Film Sealant and Vacuum Effects
on two Measures of Adhesion at the Sealant-Meat Interface in a Cook-in Packaging
System for Processed Meat. J. Food Sci. 1989, 54 (4), 863–866.
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
STICKINESS IN FOODS 33
Van Oss, C.J.; Good, R.J.; Busscher, H.J. Estimation of the Polar Surface Tension
Parameters of Glycerol and Formamide, for use in Contact Angle Measurements on
Polar Solids. J. Dispersion Sci. Technol. 1990, 11 (1), 75–81.
Wallack, D.A.; King, C.J. Sticking and Agglomeration of Hygroscopic, Amorphous
Carbohydrate and Food Powders. Biotechnol. Prog. 1988, 4 (1), 31–35.
Walton, D.E.; Mumford, C.J. Spray Dried Products-Characterization of Particle Morphol-
ogy. Chem. Eng. Res. Des. 1999, 77 (A1), 21–38.
White, G.W.; Cakebread, S.H. The Glassy State in Certain Sugar-Containing Food
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
Interested in copying and sharing this article? In most cases, U.S. Copyright
Law requires that you get permission from the article’s rightsholder before
using copyrighted content.
All information and materials found in this article, including but not limited
to text, trademarks, patents, logos, graphics and images (the "Materials"), are
the copyrighted works and other forms of intellectual property of Marcel
Dekker, Inc., or its licensors. All rights not expressly granted are reserved.
Downloaded by [Australian Catholic University] at 02:47 24 August 2017
The Materials are for your personal use only and cannot be reformatted,
reposted, resold or distributed by electronic means or otherwise without
permission from Marcel Dekker, Inc. Marcel Dekker, Inc. grants you the
limited right to display the Materials only on your personal computer or
personal wireless device, and to copy and download single copies of such
Materials provided that any copyright, trademark or other notice appearing
on such Materials is also retained by, displayed, copied or downloaded as
part of the Materials and is not removed or obscured, and provided you do
not edit, modify, alter or enhance the Materials. Please refer to our Website
User Agreement for more details.
Order now!