You are on page 1of 7

Review

Cakingphenomenain
Caking of free-flowing powders during storage is a deleterious
phenomenon that is ubiquitous in the feed, fertilizer and
pharmaceutical industries, and of economical importance for amorphousfood powders
low-moisture foods. Among other subjects related to caking
of amorphous powders, the following aspects are reviewed
in this article: (1) physical and morphological changes, and Jos~M. Aguilera,Jos~M. dd Valle
quantitative procedures to assesscaking; (2) proposed mech-
anisms of caking phenomena; (3) examples of caking in food
and MarcusKa~l
materials; (4) the relationships between storage-induced cak-
ing and other phenomena and the glass transition of amorph-
ous powders; (5) methods for estimating the evolution of between particles, without a measurable decrease in sys-
caking with time from the physical prol~rties of powder tem porosity. At the onset of caking, small i n t e ~ l ¢
bridges may even disintegrate under mild shaking.
samples and environmental conditions; and (6) measures to
Agglomeration, a later stage, involves an irreversible
minimize the occurrence of caking phenomena. consolidation of bridges but the high porosity of the
particulale system is maintained, resulting in particle
clumps with structural integrity. The mechanisms of
interparticle bonding have been reviewed by Rutlandz
Caking is a deleterious phenemenon by which a low- and SchuberP. Compaction, an even more advanced
moisture, free-flowing powder is first transformed into stage in caking, is associated with a pronounced loss of
lumps, then into an agglomerated solid and ultimately system integrity as a result of thickening of interparticle
into a sticky material, resulting in loss of functionality bridges owing to flow, reduction of intetpanicle spaces,
and lowered quality. The problem is ubiquitous in the and deformation of panicle clumps under prcsstu-¢. In
food, feed, fertilizer, pharmaceutical and related indus- the final stage of caking, i n g l e bridges disappear
tries 1-3. This review deals, in the main, with an import- as a result of sample liquefaction and extensive flow
ant form of caking in foods, namely that of amorphous owing to the high moisture conteut. This stage usually
powders by viscous flow. Caking may also occur as a involves the solubilization of low molecular weight
result of recrystallization, either after fat melting or after fractions and the presence of hygroscopic behavior 6.
solubilization at crystal surfaces; surface wetting fol- Although most publications state only whether caking
lowed by moisture equilibration or cooling; or electro- is observed and under what conditions, quantitative
static attraction between particles4.
A s ~ c t definition of caking is difficult to formulate,
because changes in a particulate system depend on P(t)/Po Do,~/Dp~,kr, Morphology
temperature, moisture and position within the powder,
and involve many different stages, including bridging, 1 0
agglomeration, compaction and fiquefaction (Fig. 1). At
any given stage, lumps may be few or numerous, of dif-
ferent sizes and of varying degrees of hardness.
In practice, a quantitative measure of caking is highly
desirable for following changes in the condition of a Bridgin 8
powder over time. The 'caking index' (a termed coined
by the authors) is defined as the state of the system at
any time relative to an initial state. Two morphological
indicators of the state of the system are: the ratio of in- Agglomeration <1 >0
stant system porosity to initial system porosity, p(t)lpo;
and the ratio of interparticle bridge diameter to particle
diameter, D~dg,IDp=~(see Fig. 1).
Because of the diversity and inconsistency of the Compact on -->0 --)1
terms used to describe caking, some definitions are pro-
posed based on their most common use in the literature.
Bridging, the initial stage in caking, occurs as a result of
surface deformation and sticking at contact points Liquefaction o t ~
JO~ M. Aguilera(correspondingauthor)and le~ M. dd Valle are at the
Departmentof Chemicaland BioprocessEngineering,PontificiaUniversidad
Cat61icade Chile, PO Box 306, Santiago22, Chile (fax: +562-552-4054; Stagesduring ~ typical caking process,indicating the changesin
e-maih jmaguile@ing.puc.cl).Marcus Karel is at the Departmentof Food systemporosity.[p(t)/poland the ratio of interparticlebridge diameterto
Science,RutgersUniversity,New Brunswick,N] 08903,USA. particle diameter [/:~,~/D,~I at each stage.

Trends in Food Science& Technology May 1v~5 [Vol. 6]


methods have been utilized in some cases to character- flow and deformation. Ts is often determined by differ-
ize caking phenomena; these methods are adaptations emial scanning calorimetry (DSC) as a shift in the
of techniques commonly employed to assess powder specific heat curve during a temperature scan 1°.
flowability7.s, angle of repose7,s, interparticle cohesion7,s,Food glasses are usually formed from the liquid state
size distribution3.9 and particle morphology3. Some of by rapid dehydration and/or cooling". For example,
these methods are described in Fig. 2. food powders produced by spray drying are likely to
Early physical events related to caking are not always include components in an amorphous state. Starch, amyl-
undesirable. For instance, in the agglomeration of pow- ose, amylopectin, starch hydrolyzates and some non-
ders, particles are purposely forced to interact and form starch polysaccharides, low molecular weight sugars,
granules with improved shape, appearance and handling food proteins and their hydrolyzates are known to form
prope~es, including better flow characteristics, im- glasses~°. For a homologous series of amorphous poly-
proved packing density, dust-free operation and faster mers, T~ decreases as the average molecular weight of
dissolution in liquidss. the polymer decreases or the concentration of plasticizer
increases'°q2. Water, being the universal plasticizer
Current theories of caking of amorphous powders of biomaterials, decreases the Ts of amorphous foods
and its relationship to the gbLsSystate below the T8 for the food in the anhydrous state (T~)
Amorphous food materials exist below the glass at a rate of ~10°C/0.01 g watcr/g material (Ref. 13).
transition temperature (Tg) in a non-equilibrated, 'stable' Liquid bridging, believed to occur as a result of solidi-
glassy state, because of the high viscosity, which fication of a saturated solution formed by vapor con-
assures that the material supports its own weight I°. Rel- densation, was the main mechanism claimed to be
evant to caking, a dramatic reduction in viscosity R (or responsible for caking two decades ago ~,4,'4.It is import-
mechanical modulus) of an amorphous solid occurs at ant to note that for moisture condensation to occur, the
the so-called glass-rubber transition, and Tg is the most temperature of the sample must be lowered below the
representative parameter of this transition. As the prod- dew point of the air.
uct temperature exceeds Ts, amorphous materials enter More recently, and with the introduetinn of the Tg
the rubbery state and the decreasing viscosity induces concept, most cases of food caking have been attributed
to viscous flow induced by a de-
creased viscosity of the material in
the rubbery state 's-iT. As explained
Method Description earlier, amorphous foods may enter
the rubbery state either at constant
moisture owing to an increase in the
Flowability Discharge mass flow rate from a ambient temperature or, most com-
bin or funnel monly, as a result of moisture
adsorption, which reduces the Ts of
the material. The net result is that the
viscosity fv/) of amorphous powders
Angle of Angle formed between the side of a may decrease from ~s = 10n-10'3 Pa.s
repose heap of powder and a horizontal plane; at Tz to an approximate value of
<.40° for free-flowing powders ~ = 106-108 Pa.s (Refs 15, 16). In fact,
the viscosity of a lyophilized fish
hydrolyzat¢ powder dried to 33% rela-
Cohesion Extrapolated shear stress for a 0 tive humidity (RH) was estimated to
normal stress, determined using a be 10~ times smaller after equili-
Jenike Flow Factor Tester or annular bration to RH = 52%, for a change in
cells; negligible for free-flowing powders moisture (w) from 0.075 to 0.150g
water/g material (Ref. 17).
Caking index Weight fraction of sample retained by
Some examples of caldng
a mesh with an opening size equal _ ~ ~ Several examples have been re-
to a specified multiple of the
ported in the literature relating the
maximum particle size of the powder
caking of sugar products to glass
transitions. Freeze-dried lemon juice
Microscopical Ratio of system porosity to initial concentrate was found to be ex-
I aRributas system porosity, or ratio of interparUcle

L%
tremely hygroscopic, to exhibit a
bridge diameter to particle diameter, high tendency to caking at ambient
determined using microscopical techniques conditions of 25°C and 60% RH,
and to cake even at low water ac-
r~.z tivities's. The solids in dehydrated
Quantitativemethodsutilizedto characterizecakins phenomena. fruit juices comprise mostly fructose

150 Trendsin FoodScience& TechnologyMay 1995 IVol. 6]


(T a = 5°C) i', glucose (T~ = 31°C) n and sucrose
(T~ = 62°C) ", and the T~ of fructose~glucose/sucrose
blends equilibrated to 30% RH (w = 0.05g water/g
material), similar in composition to dehydrated fruit
juices, can be estimated to be below typical room tem- 5O
perature valueslL This also explains why it is rec-
ommended that the wails of spray dryers used to de-
hydrate these types of products are cooled to reduce
stickiness problemsz°~'
The T~ of amorphous lactose is IOI°C (Ref. 11) and
has a Ts that is below room temperature at --O.05g
water/g material (Ref. 19), which is usually the maxi-
mum moisture content of dried milk products showing
adequate chemical stability. As expected, the stability
against caking of several dairy-based mfam formula
powders increased with increasing amounts of high
molecular weight carbohydrates (mahodextrins), which -20 t *
raised the Tg oftbe sampleszu~.
In addition to amorphous sugars, low molecular
weight inorganic salt¢ and protein hydrolyzate¢ 24 are
-3°o ; ; ; ~ ~ g ; ~ ;t~.
known to exhibit hygroscopicity and to cause caking i Moisture content (g/1 O0 g dry ma~er)
problems during storage. A fraction mainly containing Iqg.3
nitrogenous compounds (presumably amino acids) was
Effectof sample moisture content(vOon glasstransition temperature(Tt), sticky
held responsible for the hygroscopicity and caking of
spray-dried fermented soy sauce powders :4. point temperature(Ts)and collapse temperature(To)of dehydratedfruit juices
An important related phenomenon is aggregation of and an amorphousfruit juice model system.(% midpoint Ts determined using
proteins in the dried state. There are examples in the differential scanningcalorimetry'9; (,D),Tsdetermined using thermal mechanical
literature of aggregation reactions (e.g. thiol-disulfide analysis(V.T. Huang, unpublished);(o), T~of an amorphoussucroseand fructose
interchanges, other covalent bonds mediated by lysine (7:1) model system'S;(=), Tsof spray-driedorangeiuice with added glucose2°;
residues, and conformational changes) resulting from and T( of slow- (A) and fast-frozen(&) lyophilized orange juice~. The curve
water sorption during processing, storage and delivery. representsthe predicted Tgof amorphoussucroseusing Ihe Gordon-Taylor
The aggregation of biomoleculcs in the 'dry" state has
equation28and equation parametersestimatedby Ronsand Karelu.
importan~ implications in the modern biotechnology
industry, as it may be responsible for a pronounced
decrease in biological activity2s~6. temperature range over which the glass transition occurs.
The T,. and -~Tvalues measured for several dairy-based
Caking and related phenomena infant formula powders by using the techniques of
Collapse, stickiness and caking appear to be related Lazar el al. :7 and Tsouroflis et al. ~, respectively, were
phenomena. When a solid matrix (usually freeze dried) dependent on the scanning rate (i.e. the heating rate),
reaches its "collapse" temperature (To), an initial occur- and T~ was found to be higher than Tc which, in turn,
rence of interpartiele bridging (or surface caking 22) is was 30-50°C higher than Ts at a constant scanning
manifested as a loss of structure and decrease in sample rate ~. These differences were attributed to variations in
volume23. At the 'sticky point' temperature (T~)` a sharp sample size and viscous flow time constants between the
increase in the force required to stir a powder is methods.
observed 27, which is indicative o f a more advanced stage
o f caking 2z. Figure 3 presents the effect o f sample moist- Cakingkinetics
ure content on Ts, Tc and T~ of dehydrated orange juice An obvious goal for food technologists is to be able to
and an amorphous fruit juice model system, as assessed predict the degree of caking of a food powder during
by several authors using different instruments, together storage. When a dry powder is packed, it picks up water
with the predicted T8 of mixtures of water and sucrose, from the moist air in the headspace (or through the
the main component in anhydrous fruit juices. Although package material or seal) to a degree that depends on
some data seanecing is evident, Tg values for mixtures the sorption characteristics of the food (if a pseudo-
of water and the main non-aqueous component of a equilibrium can be assumed). The caking rate of the
sample appear to predict the phenomena of collapse and powder will depend on its instantaneous moisture con-
stickness as a function of temperature reasonably well. tent (through its effect on Tg) and the ambient tempera-
Some caution should be exercised in the measurement ture.
and interpretation of glass transition temperatures, Modeling the kinetics of caking is a difficult task be-
which vary not only because of instrumental differences cause many factors are known to affect it, both internal
and variations in the physical events that constitute the [such as particle size (Dp)` charge, hygroscopic behav-
definition of T~, T= and T,, but also because of the broad ior, and the physical state of particles] and external

Trends in Food Science & Technology May 1995 [Vol. 6] 151


[temperature and relative humidity of the enviroament, T8 + 100°C may be related to sn.nple temperature using
applied mechanical stress and the presence of moisture the Williams-Landel-Ferry (WLF) modeP°'3°-~2:
barriers, among others]3.
As an illustration, the data necessary for estimating _ C,~T
caking of a fish protein hydrolyzate prepared by spray Iog(~//7/g) - C.--~-T (2)
drying (with a D v of 74-125 p,m) will be presented29.
First, caking was induced by exposing small Petal dishes where constants Ci and C2 correspond to average values
eontaiimng a thin layer of dried powder to different rela- estimated by adjusting experimental viscosity data for
tivc humidifies, by placing them in desiccators together various polymers. However, as individual values of C1
with saturated salt solutions under controlled tempera- and C2 for these polymers were in the ranges 13.7-34
rare conditions. This method might be improved by (avenge= 17.44) and 24-84°C (average=51.6°C), re-
using a permeable film to control the rate of vapor trans- spectively, Peleg32 proposed that C, and C2 are treated
mission to the sample. A caking index was estimated at as adjustable parameters to model kinetic processes of
progressive times by mildly sifting the samples through foods above the glass transition region.
a screen with openings of a larger size than the particles As caking is attributed to viscous flow, and sample
(115 mesh or 1251xm). However, any method for viscosity may be modeled by WLF kinetics, the relax-
assessing caking such as those presented in Fig. 2 could ation time for caking may also be related to the differ-
have been used. ence between the environmental temperature (7") and Tg
The curves shown in Fig. 4 were determined by fitting (AT= T - Tg) by a WLF-type relationship31. The value of
experimental data to a first-order kinetic model, with a I- for caking of the amorphous fish hydrolyzate powder
delay factor to account for the time required for the onset was estimated to be ~'~=7.57 X 109 h, con-oborating that
of the caking phenomenon (i.e. the time required for caking is not observed when a powder is in the glassy
moisture diffusion into the outer layers of the particles): state.
The key state variables required to estimate the rate
and extent of caking (equilibrium RH and T;) arc
1- ~(~t~)= exp( - / - t d ) (1)
IUu ~" depicted in Fig. 5 for fish hydrolyzate powder samples.
The moisture sorptiou isotherm was determined by a
where 0(t) represents the caking index (%, w/w of gravimetric procedure and Tg values at equilibrium
sample comprising particles large enough that they are moisture contents by DSC. Changes in moisture content
retained by a given mesh screen), t is the time (in (w, expressed as gwater/g dry matter) of the powder
hours), re=5.60 ± 0.19 h is the delay time, and ~'is the may be followed by the sorption isotherm (Fig. 5a),
relaxation time for caking (in hours). modeled using Henderson's equation33:
The viscosity and other mechanical relaxation or rate
parameters of amorphous food materials between T~ and w= [-0.196 In (1 - RH/100)] °'990 (3)

As w increases, 7"= values diminish; these changes


30~'C/75% RH were modeled using the Gordon-Taylor equation2~
(Eqn 4) and are represented in a phase diagram
(Fig. 5h):
~ 90 .
71.9-918.0w
~ ~o
Ts 1.0+6.8w (4)

6o,. II / 3Soc/~%RH Finally, a WLF-type relationship~ with adjustable Ci


and C2 coefficients (F,qn 5) was utilized to characterize
the effect of AT on ~"(Fig. 5c):
40 -ll.16AT
g 3o l°g(~r/~rs) 10.7 + AT (5)
~ ~o According to Fig. 5c, as AT increases from O, ~-de-
creases markedly. When AT = 20°C, caking occurs ~10T
times faster than it does in the glassy state, and may be
0 observed within days. When AT is doubled to ~40°C,
0 10 20 30 40 50 60 70 80 the rate of caking is further increased almost 100 times,
Storage time (h) and changes may occur within hours. What is important
to the practitioner is that as long as the T8of 'he sample
Fig.4 is maintained below T (i.e. when w is maintained at or
Caking kinetics of fish hydrolyzate samplesas a function of storageconditionszg. below 0.05 g water/g dry matter; see Figs 5a and 5b), no
Seetext for details. caking will be observed.

152 Trends in Food Science & Technology May 1995 [vol, 61


(a) (c)

°t
0.2
/ A 10":

A m

3T ~I0"
o.t2

~o 0.08 10-
0 -

," . . . . .
- lo- , = , k i | t t i
0 10 20 30 40 50 60 70 0.00 0.04 0.08 0.12 0.16 0.20 0.24 2o 4o 6o 8o too
Equilibrium RH (%) w (g watedg dry matter) &T = r - r, (°cI

FgS
Data requiredto predictthe advanceof cakingin fishproteinhydrolyzatepowdersamples.(a),~ f i o n is~3~%~m:(~),ext~memai data from
Aguilerael'al.tT; (--), modelusingHenderson'sequation~3(/~qn3). (b), Phasediagramplot:(n),experimentaldata fromAguihraet al?7; (--), model
usingthe Gordno-Taylorequation28(Eqn4). (c),Williams-Landel-Fea'y(WLF)plotof relaxationtimesfor caking:(n),exl~meatal data fromAguiletaand
del Valle~; ( - - ) , universal WLF plot for viscosity of polymers (Eqn 2); (--), model using a WLF-lype relationship3owith adjustableC~and Czcooffa:ients
(Eqn 5). Condition ~)indicates the stability of powder samplesagainstcaking; condition ( ~ signalsthe onset of caking phenomena(just perceptible in a
few days);and condition ~ indicates that powder samplescake fast enough to allow the easy identifa-.ationof the defect. Seetext for further details.

In the fish hydrolyzate example, caking started to be observed extensively. Similar .microstmctural obser-
apparent as samples reached average moisture contents vations were made for spray-dried powders of whole
of 0.04-0.08 g water/g dry matter, corresponding to a milk supplemented with lactoses .
delay factor of - 6 h. This reveals nothing about the Microstructoral changes in lyophilized samples of fish
actual moisture content on the surface of the particles. myofibrillar protein hydrolyzate were also observed
Hence, factors that should be controlled when establish- using SEM ~. Samples equilibrated for three weeks to
ing actual caking kinetics include water vapor transmis- _<44% RH retained their original highly porous structure
sion rate and uniform exposure of particles to the vapor with fine walls. At 56% RH, pore walls were observed
phase. to thicken, whereas at 67% RH they had fused into thick
and continuous masses, reducing considerably the po-
Microslmctural aspects of caking rosity of the system. The sample equilibrated to 75%
Morphological changes in a powder undergoing cak- RH presented evidence of crystaUine-Ilke structures.
ing can be best visualized using microscopical tech- Image processing by digitization can be used to cor-
niques~*. Thus, it is surprising that microscopical analy- rect defects in the original microstractural image (e.g.
sis has not been used to any great extent to characterize non-informational noise), enhance or suppress data,
caking, but it is likely that quantitative information select important features, extract numerical data (e.g.
related to caking phenomena and the determination of particle area or characteristic size) and perform statisti-
a caking index (see Fig. 1) will be easily derived by cal analysis. Figure 6 depicts three images from the
microscopy and the aid of computational image analysis SEM micrograph of milk powder in an agglomerated
in the future. state that can be used to characterize stages in caking
Amorphous components in spray-dried powders are in and caking kine:ics by the analysis of geometrical
the met~table amorphous state and exposure to high features.
relative humidity results in an irreversible transition to
the crystalline state. Amorphous lactose crystallizes and Prevention of caking
releases water during equilibration at 42-52% RI-I (at As should be evident at this point, the strict control of
25°C). Scanning electron microscopy (SEM) was used moisture content and storage at low temperatures, when
to follow caking of skim milk powder stored at 20°C possible, are key factors in. miinimi;zing the effects of
during equilibration at 43-94% RH (Ref. 35). After two caking of powders. However, in many instances, anti-
weeks, changes had occurred only for powder equilib- caking agents are added to hygroscopic food powders to
rated at >54% RH, whereas at ~74% RH lactose crys- improve their flowabifity and/or to inhibit caking; they
tallization as well as bridging between particles were achieve this by one of several mechanisms.

Trends in Food Science & Technology May 1995 lVol. 61 153


• By acting as surface physical barriers between
particles b f ' : (1) interfering with liquid bridging
mechanisms (e.g. silicon dioxide); (2) decreasing inter-
particle friction, by smoothing the surfaces or acting
as 'minirollers' (e.g. the slearates); (3) reducing or
~euLtalizing supe~cial molecular at~active forces,
particularly electrostatic forces; or (4) inhibiting crys-
tal growth and/or altering its lattice pattern. These
types of anticaking agents, like those in the previous
category, do not need to cover the powder surface
completely in order to exert their positive action.
!. • By i n ~ i n g the Tg of the amorphous phase. This
mechanism has already been shown for dairy-based
infant formula powders with added high molecular
weight carbohydrates22. In protein hydrolyzates, we
have observed that a lower degree of hydrolysis (i.e. a
higher average molecular weight) diminishes caking.
Some fipids have been shown to exert an antiplasti-
cization effect in a fipid-compatible polymer plasti-
cized by water, increasing Ts (Ref. 13).
• By forming a moisture-protective barrier (e.g. lipids)
on the surface of otherwise hygroscopic particles,
without entering the amorphous phase of the powder.

Conclusions
Caking of amorphous powders is a continuous and
complex, time-dependent phenomenon in food powders
and related biomaterials. Surface flow and stickiness,
needed for interparticle bridging and adhesion, occur
when the Ts of the amorphous powder is below the
ambient temperature, 7". As resistance to flow is in-
versely proportional to AT= T - T v caking rates can be
modeled as a function of AT using a WLF-type relation-
ship. Moisture is a critical parameter in caking of ~ -
ous foods through its 'del~essing' effect on Ts, and it is
usually conh-olled by the use of proper packaging and/or
anficaking agents. The modification of Ts as a mechan-
ism for reducing the caking rate needs to be studied.
Microstracture and image analysis may become import-
ant tools in the characterization and quantification of the
caking phenomenon.

fig.6 Admow~
Image processing of a scanning electron micrograph (SEM) The authors appreciate the comments of Dr Micha
of agglomerated spray-dried milk. (a), original SEM image; Peleg, who reviewed the manuscript. The present
(b), digitized gray-scale image with contour of particles; work was partially funded by the National Fund of
Science and Technology of Chile, projects FONDECYT
(c), image with selected objects for measurement and data analysis.
193-0620 and 194-0648. This is a contribution of
Scale bars = 200pro. the CYTED-RIPFADI Ibero American Network on
Physical Properties of Foods.
• By competing with the host powder for available
moistureI. Several of these agents are of a porous References
1 Pele~M. andHollenbach, A.M.(1984)FoodTechnol. 38(3),93-102
nature and exert their protective action in foods by
2 Ru~land,D.W.(1991)Fert. Res.30,99-114
preferentially adsorbing large amounts of water vapor 3 Provent,B.,Chulia, D. andCary, J.(1993)Eur.l. Pharm. Biopharm.
onto specific surface sites with high binding energy. 39, 202-207
Because further increases in moisture cause large 4 Pele~M.(1983)inPhysicalPrupettiesofFoods(Pelc~,M. and
increases in the equilibrium RH, the optimum per- Rasley, E., eds), pp. 293-323, AVI
formance of these agents is observed with short S Schubert,H. (1981) Int. Chem. Eng.21,363--377
exposures to moist atmospheres. 6 Dziedzic, S.L and Kearsley,M.W. (1984) in GlucoseSyrups:Science

1.54 Trends in Food Science & Technology May 1995 [Vol. 6]


and Technology (Dziedzic,S.Z.and Kearsley,M.W., edsi, 22 Chuy,L. and labuza,T.P.(1994)J. Fo~J..¢ci.59, 43-46
pp. 137-168,Elsevier 23 Tsourotlis,S.,Flink,J.M.andKaeeI,M.I1976)l..T¢/.Fo0dA~. 27,5(R-519
7 Pel~M(1q77).l. FoodProcess. Prescrv.1,303-328 24 Hamano,M. andAoyama,Y. (1974)Nippon Nogei Kaga~ ~ishi
R Pe!~.M.(1993)inTheGlassyStateofFoods(81anshard, l.M.V, and 4g, 6i9-625
Lillford, PJ.,eds),pp. 435-451, NottinghamUniversityPress 25 Liu.W.R.,Langer,R.and Klibanov,A.M.(1991)Biotechnol. Bioeng.
9 Lowrison,G.C.(1989)Fertilizer Technology, EllisHo~ood 37,177-184
10 Slade,L. and Levine,H. (1991)CRCCrit. Rev.FoodSci. Nutr. 30,115-360 26 Townsend,M.W.and DeLuca,P.P.~1991|/.Rtanll.5ci.80, 63-66
11 Roos,Y. and KareI, M. (1991) Faod Technol. 45(12), 66, 68-71,107 27 lazar, M.L, Brown,A.H.,Smith,G.S.,Won8, F.F.and Lind~ia, F.E.
12 Buera,M. del P., Levi,G. and KamI,M. (1992) Bk:~chnoI.Ptog,8,144-148 (1956)Food Technol. 18,129-137
13 Slade,L., Levine,H. and Finley,J.H.(1989)in Protein Ouali~, and the 28 Gordon, M. and Taylor,I.S.(19521L.4pp/.~ . 2, 493-500
Effects of Processing (Dixon-Phillips,R. and Finley,I.W.,eds), 29 Aguilera,J.M.and del Valle,J.M.in ISOPOWPract/cum//.'Food
pp. 9-124, MarcelDekker Preservation by MoistureConlro/(Bafbosa-C.dnovas,G. and
14 Peleg,M. and Mannheim, C.H. (1977) l. Food Process. Pmserv. 1, 3-11 Welti,I-, edsi(in press)Technomic
15 Downton,G.E.,Flores-Luna,I.L.and King,I.C.(1982)Ind. Eng. Chem. 30 Williams,M.L.,Landel,R.F.and Ferw,J.D. (19551LAm.Chem..Toc.
Fundam. 21,447--451 77, 3701-3707
16 Wallack,D.A.and King,J.C.(1988)BiorechnoL Prog.4, 31-35 31 Karel,M. andSaguy,I. (19911in Water ~e!a!ions in Foods(tevine,H.
17 Aguilem,J.M., Levi. G. and lC~reI,M. (1993) RioCechnnl Pr~joa 6=;1-65~t ~ndSlade.L.,eckl ~ 157-174, PlenumPress
18 Kopelman,I.J.,Meydav,S.andWeinberg,S.(1977)~ Food TechnoL 32 Peleg,M. 11992)CRCCdt.Rev.FoodSci. Tec/mo/.32, 59-66
12,109-116 33 Henderson,S.M.(1952)Agr/c.Eng.33, 29-33
19 Roos,Y. and Karel, M. (1991) J. Food Sci. 56, 38-43 34 Aguilera,I.M.and Stanley,D.W.(1990)M i c ~ r a ! Aspects of
~0 8rennan,J.G., Herrera,J. and lowiff, R. (1971)l. Feod Technol.6, 295-387 Food Processingand Engineering,Elsevier
21 King,J.C.(1986)in Engineeringand F c ~ - Vol. 2: Processingand 35 /ai, H-M.and Schmldt,S.(1990)J.FoodSci.55, 994-999
Applicarions (McKenna,B.M.,ed.),pp. 559-574,Elsevier 36 Aguilar,C.A.and Ziegler,G.R.(1994)J. Dairy SoL 77,1198-1204

Review
Rapid water determination
Water is present in practically all foodstuffs. The water con-
tent is of great significance in determining the physical charac-
teristics, technological processes, microbiological stability,
in foodstuffs
shelf life and sensory properties of foods, as well as having
legal and economic ramifications. Determination of the water
content is one of the most frequent analyses performed on
H-D. Isengard
foodstuffs. To avoid the manufacture of products with an
undesired, unadvantageous or non-permitted water content water, in a product; the difference in mass after drying
and keep the amount of out-of-specification products to a should not, strictly speaking, be referred to as 'water
minimum, water determination methods should not only content' but rather 'mass loss on drying'. Experimental
determinations of mass loss on drying vary according to
yield correct results but also deliver them very quickly, poss-
the conditions employed and do not provide information
ibly even continuously and within the requirements of quality- about an absolute property of the product, but rather
management systems. about its behaviour under certain drying conditions,
which should, consequently, be mentioned as parameters.
This mass loss is sometimes called "moisture', but this
term is problematic too, as it is commonly used to mean
To avoid misunderstanding, it must be clearly stated at water, possibly including other liquids. However, some
the outset that the water content of a product is not necess- of the mass loss may result from in~n~ie gaseous and
arily equivalent to the original mass minus the mass after volatile solid compounds; on the other hand, liquids with
a drying process. Cases where this is true are extremely very high boiling points may escape such detection.
rare, because methods based on measuring the mass of a A further complication is posed by the existence of
product before and after a drying process cannot distin- "free" water molecules and different forms of "bound
guish between water and other volatile substances, water' that are hound more or less strongly to other food
which may even include those produced by and during components, often evading determination.
the process itself. The term 'water content' should be
reserved to refer to all of the water, and nothing but the Primary and secondary methods
Primary methods arc those methods that directly
H-D. Isenganlis at UniversitatHohenheim,Institutfor Lebensmitteltechnologie, measure the true water content. From a scientific point
Garbenslr.25, D-70599Stullgart,Germany(fax:+4%711-397-3935). of view, only primary methods should serve as reference

Trends in FoodScience& Technology May 1995 [Vol. 6] ©1995,ElsevierScienceLtd0924-2244/95/S09.50 155

You might also like