JFS

E: Food Engineering and Physical Properties

Combined Effects of Proteins and

Polysaccharides on Physical Properties of
Whey Protein Concentratebased Edible Films
K. COUGHLAN, N.B. SHAW, J.F. KERRY, AND J.P. KERRY

Introduction

dible films are generally formed from hydrophilic components

such as proteins or polysaccharides. Films based on proteins
have poor water-vapor barrier properties but are more resistant to
oxygen transfer than are films prepared from polysaccharides
(Kester and Fennema 1986). The properties of edible films formed
from hydrocolloids have been reviewed by a number of authors,
including Kester and Fennema (1986) and, more recently, Cuq and
others (1998). Formation of flexible films from hydrocolloids normally requires 2 essential ingredients: a film-forming polymeric
material that provides the structural matrix and a plasticizer, such
as a low-molecular-weight polyol, which imparts flexibility. In the
absence of sufficient amounts of plasticizer, a brittle inflexible film
is formed and is difficult to peel from the casting surface (McHugh
and others 1993).
Biopolymer films, which contain both protein and polysaccharide ingredients, may advantageously use the distinct functional
characteristics of each film-forming ingredient. Some workers have
indicated that incorporation of polysaccharides into globular protein matrices may extend the functional properties of these ingredients (Zaleska and others 2000; Turgeon and Beaulieu 2001).
Schmitt and others (1999) have shown that protein-polysaccharide
complexes gel more effectively than polysaccharides and proteins
in isolation. These effects may be attributed to the simultaneous
presence of the 2 biopolymers, as well as to the structure of the
complexes. According to Turgeon and Beaulieu (2001), heat treatment of a protein-polysaccharide complex weakens the low-energy
bonds responsible for co-solubilization of the protein and polysaccharide. After breaking of this equilibrium, a competition occurs
between phase separation and protein gelation in the system.

MS 20030228 Submitted 4/28/03, Revised 7/18/03, Accepted 3/31/04. Authors

Coughlan, Shaw, J.F. Kerry, and J.P. Kerry are with the Dept. of Food and
Nutritional Sciences, Univ. College Cork-Natl. Univ. of Ireland, Cork, Ireland. Direct inquiries to author J.P. Kerry (E-mail: joe.kerry@ucc).

2004 Institute of Food Technologists

Further reproduction without permission is prohibited

When protein gelation is favored by the experimental conditions,

a continuous protein network is formed with polysaccharide inclusions, thereby strengthening the complex. Turgeon and Beaulieu
(2001) strengthened the structure of a whey protein gel by incorporating -carrageenan into the gel. From subsequent rheological
investigation, they reported that gelation of the 2 components were
independent, where the protein gel formed 1st and the -carrageenan gel formed during the cooling phase. Zaleska and others
(2000) formed gels from pectin and whey protein isolate, and they
suggested that anionic interactions may occur between the protein
and polysaccharide components if they are electrically compatible.
It may therefore be possible to manipulate combinations of
polysaccharide and protein component edible films to adjust water-vapor resistance or structural strength.
Little information exists in the literature on the film-forming
ability of such combinations of protein and polysaccharide components. Parris and others (1995) formed films from whey proteins
and alginate or pectin and reported that the films formed from protein-polysaccharide blends had lower water-vapor permeability
(WVP) than those formed from protein alone. They also suggested
that future studies should be directed toward improving the physical properties of films through covalent bonding of proteins and
polysaccharides using processing techniques such as spray-drying.
Turgeon and Beaulieu (2001) and Zaleska and others (2000)
formed gels from separate solutions of polysaccharide or protein
powders, often called dry blending, whereby the individual protein and polysaccharide materials are blended together in powder
form. The protein and polysaccharide materials may also be
blended by spray-drying solutions of the combined ingredients
to form a co-dried, biopolymer powder. This process, known as codrying, is a novel process; it is believed that combining the powders in such a way may promote increased interaction between
the protein and polysaccharide constituents. Schmitt and others
(1999) suggested that protein-polysaccharide complexes were
formed with a polyelectrolyte chain bound by several protein
Vol. 69, Nr. 6, 2004JOURNAL OF FOOD SCIENCE E271
Published on Web 7/27/2004

E: Food Engineering & Physical Properties

ABSTRACT: The water-vapor permeability (WVP) and mechanical properties of edible films formed from dry
blends or co-dried preparations of protein-polysaccharide powders prepared from whey protein concentrate
( WPC)-45 and alginate, pectin, carrageenan, or konjac flour ( WPC-45-to-polysaccharide ratio of 95:5 w/w)
were investigated. Films were prepared from 8% WPC using WPC-45 (45% protein powder), consisting of 17.76
g of WPC-45 in 82.84 g of water per 100 g solution to give 8% protein w/w. Films formed from co-dried powders
had lower WVP and higher tensile strength (TS), elastic modulus (EM) (P < 0.05), and elongation (EL) than
equivalent films formed from the dry blended powders. Films containing alginate had lower WVP and higher TS,
EM, and EL than films containing pectin, carrageenan, or konjac flour. There is potential to alter the physical
properties of hydrophilic films by combining whey protein and polysaccharide components.
Keywords: WPC, alginate, pectin, physical properties, edible films

Properties of WPC/polysaccharide edible films . . .

molecules. These primary complexes may aggregate during spraydrying to form inter-biopolymer complexes with a structure consisting of several interacting polymer chains. To our knowledge,
little exists in the literature on blending ingredients using such codrying techniques.
The objectives of this study were to investigate the effect of both
biopolymer combination and sample preparation technique on the
physical properties of protein-polysaccharidebased edible films.

Water-vapor permeability

Whey protein concentrate, containing 45% protein (WPC-45),

was obtained from Dairygold Ltd. (Mitchelstown, Ireland). Alginate was obtained from Kelco Intl. Ltd. (Surrey, U.K.). Pectin and
carrageenan were obtained from FMC Co. ( Vallenstaek Strand,
Copenhagen, Denmark). Konjac flour (Nutricol) was obtained from
the FMC Corp. (Philadelphia, Pa., U.S.A.). Glycerol was obtained
from Sigma Aldrich Ltd. (Poole, Dorset, U.K.). All chemicals were of
reagent grade.

Circular test cups made of perspex were manufactured to the

specifications outlined by McHugh and others (1993). Distilled
water (4 mL) was placed in each test cup, and a film sample was
mounted across the cup opening. The cups were further sealed
using silicon sealant. The cups were stored in a temperature- and
humidity-controlled room (50% 5% RH, 23 2 C), and a fan set at
an air velocity of 152 m/min was placed over the cups to ensure
uniform movement of air across the WVP test cells. Within 2 h,
steady-state conditions were assumed to have occurred (McHugh
and others 1993). The weight loss of the cups was monitored over a
24-h period with intervals of greater than 2 h between readings. At
least 3 film samples were prepared for each film type, and WVP was
calculated according to the WVP correction method of McHugh and
others (1993). This is a modification of the ASTM E-96 Standard
Method (ASTM 1980) for determining WVP of synthetic packaging,
which has adapted the calculations to consider the more hydrophilic nature of edible films. The WVP correction method was developed to account for the water-vapor partial-pressure gradient in
the stagnant air layer of the test cup (McHugh and others 1993).

Co-dried powder formation

Mechanical tests

After initial screening of WPC at varying protein levels (35%, 45%,

75%) by industrial partners Dairygold Ltd., it was decided to proceed with WPC-45 because it combined optimum gel strength with
cost effectiveness. Co-dried powders were manufactured in Univ.
College Cork in conjunction with Dairygold Ltd. Aqueous solutions of WPC-45 (19% w/w) at 20 C and alginate, carrageenan, pectin, or konjac flour (1% w/w, heated to 60 C for complete miscibility) were fed into a single-stage spray-dryer (NIRO Atomiser-L55432,
Copenhagen, Denmark) with inlet and outlet temperatures set at
200 C and 95 C, respectively. The solutions were dried at a flow
rate of 18 kg/h through an atomizer, 2-mm dia, to form a co-dried
powder containing WPC-45 and the desired polysaccharide at a
protein-to-polysaccharide ratio of 95:5 w/w. Carrageenan required
the addition of salt at 0.5% w/w to lower the viscosity of the solution.

Film samples were preconditioned and tested under conditions

of controlled temperature and humidity (50% 5% RH, 23 2 C).
The films were cut into strips 25.4 mm wide and 130 mm long using
a scalpel. The ends of the strips were mounted between cardboard
grips (26 /times/ 70 mm) using double-sided adhesive tape, and
the final film area exposed was 100 /times/ 25.4 mm. An Instron
Universal testing instrument (Instron Model 4301, Instron Corp.
Canton, Mass., U.S.A.) was used to measure the tensile properties
of the films according to the static weighing, constant rate-of-grip
separation standard testing method D882 (ASTM 1985). The Instron was set to tensile mode and the mounted film samples were
clamped into the screw-action grip and jaw faces of the tensile rig.
Initial grip separation was set at 100 mm and crosshead speed at
100 mm/min. At least 16 strips of each film type were analyzed, and
percent elongation at break (% EL), tensile strength at break (TS),
and elastic modulus (EM) were calculated as outlined in ASTM
D882 (ASTM 1985).

Materials and Methods

Reagents

E: Food Engineering & Physical Properties

Film formation
Films were prepared from 8% protein w/w solutions of WPC-45
and dry-blended or co-dried WPC-45/polysaccharide powders (8%
w/w protein). These solutions were stirred continuously at room
temperature for 2 h. It is well documented that the optimal temperature-time profile for whey protein denaturation is 80 C to 90 C
for approximately 0.5 h (McHugh and others 1993; Mate and Krochta 1996; Shaw 2001). The solutions in the current study were heated
in a water bath to 85 C and held at this temperature for 0.5 h. Glycerol was added as a plasticizer (10% w/w) to the cooled heat-denatured solutions at a glycerol-to-protein ratio of 0.35 w/w (Shaw
2001). A control film was prepared from an 8% solution of WPC-45.
For each film, 30 0.5 g of film-forming solution was poured onto
level, circular, teflon-coated perspex plates machined at the physics department workshop in Univ. College Cork. They were dried for
approximately 24 h to constant weight at controlled conditions of
50% 5% RH and 23 2 C. Many researchers have described film
casting and peeling similar to the methods used in the current
study (McHugh and others 1993; Mate and Krochta 1996; Shaw
2001). Films were peeled immediately before testing. To obtain
sufficient samples for WVP and mechanical testing, at least 12 films
were cast from the film-forming solution of each film type. Film
thickness was measured using a 0- to 25-mm micrometer screw
gauge (Mitutoyo Corp., Kawasaki, Kanagawa, Japan), and overall
thickness was expressed as an average of 10 readings taken randomly on each film. All films were cast in triplicate.
E272

JOURNAL OF FOOD SCIENCEVol. 69, Nr. 6, 2004

Statistical analysis
At least 10 films were cast from each of the film-forming solutions of each of the blends being evaluated. Data was analyzed
using SPSS 10.0 for Windows (SPSS, Chicago, Ill., U.S.A.) software
package. A 2-way statistical analysis of variance, least significant
difference multiple comparison tests and regression analyses were
performed. All experiments were conducted 3 times.

Results and Discussion

Film formation
All films prepared were peelable from the casting surface. Average values for film thickness were generally in the range of 0.080 to
0.100 mm and were not significantly different (P > 0.05).

Water-vapor permeability
Overall trends indicated that films formed from co-dried powders had lower WVP than the control film (Figure 1). The films
formed from dry blended powders had higher WVP values (P < 0.05)
than the control film (WPC-45). Overall, the WVP values for films
formed from co-dried preparations were lower than equivalent films
formed from dry blended powders (P < 0.05). Regardless of blending, it was shown that alginate-containing films had lower WVP
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Properties of WPC/polysaccharide edible films . . .

Mechanical properties
Trends indicated that (Figure 2) that films formed from co-dried
preparations were more extensible than the control film (WPC-45)
or equivalent films formed from dry blends of the protein and
polysaccharide materials. Film extensibility was greatest in films
prepared from co-dried WPC-45/alginate powders (indicated by
trends). Films formed from co-dried preparations (Figure 3) had

Figure 1Water-vapor permeability (WVP, g mm/d/m2/kPa)

of control film () (WPC-45), and co-dried () and dry
blended () edible films prepared from WPC-45 and alginate, pectin, carrageenan, or konjac flour. a,b,crefers to test
of significance where means bearing different superscripts
are significantly different (P < 0.05).

Figure 2Percentage elongation (% EL) of control film ()

(WPC-45), and co-dried () and dry blended () edible films
prepared from WPC-45 and alginate, pectin, carrageenan,
or konjac flour. a,b,crefer to test of significance where means
bearing different superscripts are significantly different
(P < 0.05).
URLs and E-mail addresses are active links at www.ift.org

greater tensile strength than equivalent films formed from dry

blends (P < 0.05). Tensile strength was greatest in the films prepared from co-dried WPC-45/alginate and WPC-45/pectin powders
(P < 0.05). The elastic modulus values (Figure 4) obtained for films
containing co-dried blends were greater than those obtained for
the equivalent films formed from dry blends (P < 0.05). Overall,
elastic modulus was affected more by the sample preparation
method than the polysaccharide included in the protein-polysaccharide complexes.

Discussion
It is generally regarded that protein-polysaccharide complexes

Figure 3Tensile strength (TS, MPa) of control film ()

(WPC-45), and co-dried () and dry blended () edible films
prepared from WPC-45 and alginate, pectin, carrageenan,
or konjac flour. a,b,c,d,erefer to test of significance where
means bearing different superscripts are significantly different (P < 0.05).

Figure 4Elastic modulus (EM, MPa) of control film ()

(WPC-45), and co-dried () and dry blended () edible films
prepared from WPC-45 and alginate, pectin, carrageenan,
or konjac flour. a,brefer to test of significance where means
bearing different superscripts are significantly different
(P < 0.05).
Vol. 69, Nr. 6, 2004JOURNAL OF FOOD SCIENCE

E273

E: Food Engineering & Physical Properties

values than films containing other polysaccharides (indicated by

trends), and WVP of the films could be arranged in the following
increasing order: WPC-45/alginate < WPC-45/pectin < WPC-45/
carrageenan < WPC-45/konjac flour.

Properties of WPC/polysaccharide edible films . . .

E: Food Engineering & Physical Properties

exhibit more effective functional properties (for example, gelation

and aggregation) than proteins or polysaccharides alone (Schmitt
and others 1999; Zaleska and others 2000). This may explain why
films containing co-dried powders had slightly lower WVP than
films formed from WPC-45 exclusively (Figure 1). Parris and others
(1995) formed films from combinations of whey protein and alginate or pectin and, similar to the current study, reported lower WVP
values than films formed from proteins in isolation. As suggested
by Zaleska and others (2000), the effects reported in both studies
may be attributed to an electrical incompatibility between the protein and polysaccharide components. Such incompatibility may
lead to the formation of 2 separate protein and polysaccharide gels,
which may in turn lead to a decrease in intermolecular interaction
between the components. Furthermore, the lower WVP values reported for films containing co-dried powders, rather than equivalent dry blended-based films, may be attributed to an increase in
electrical compatibility between the protein and polysaccharides
arising from the spray-drying process, which may have promoted
more intermolecular interactions in the co-dried powders, leading
to more effective moisture barrier properties. Bangs and Reineccius (1988) and Trubiano and Lacourse (1988) reported that encapsulating properties of protein-containing powders increased with
the addition of polysaccharide material during spray-drying. The
polysaccharide material led to changes in the surface active properties of the powder, which subsequently led to improvements in
the functional properties of the powders.
Overall, it was shown that alginate-containing films generally
had lower WVP values than films containing other polysaccharides
and that the WVP of films could approximately be arranged in the
following increasing order: WPC-45/alginate < WPC-45/pectin <
WPC-45/carrageenan < WPC-45/konjac flour. The differences in
WVP reported between films formed from blends of WPC and
polysaccharides may be attributed to differences in gel formation
and interactions between WPC and each of the polysaccharide components. As suggested by Ustunol and others (1992) and Zasypkin
and others (1997), the complex gel network, which is set up between protein and alginate, may be because of hydrogen bonding
and electrostatic interactions between oppositely charged polyelectrolytes. Zaleska and others (2000) formed gels from blends of pectin and WPI and indicated that attractive forces between the protein and anionic polysaccharide were responsible for the formation
of the structural matrix. Parris and others (1995) formed edible
films from combinations of whey protein and, in agreement with
the current study, alginate or pectin and reported lower WVP in
films containing alginate than for films containing pectin. They
attributed this effect to an increase in intermolecular hydrogen
bonding between polymer molecules in the alginate-containing
films when compared with the pectin-containing films. As a result,
spacing between the macromolecules may be decreased, leading
to a reduction in WVP (Parris and others 1995).
Many workers have shown that protein-carrageenan complexes
form 2 distinct gel phases, which occur at different time-temperature intervals ( Turgeon and Beaulieu 2001; Euston and others
2002) and may explain why the WVP values of films incorporating
carrageenan were higher than those reported for films containing
alginate or pectin. Drohan and others (1997) suggested that the
gelation of carrageenan occurs in 2 stages: helix formation followed
by aggregation. When heated in solution, carrageenan undergoes
a structural transition somewhat analogous to protein denaturation, adopting a helical form in solution that is disrupted to a random coil during heating. On cooling, the random coils reassociate
into double helices. Consequently, the gelation of carrageenan is
usually achieved by lowering the temperature, whereas denaturE274

JOURNAL OF FOOD SCIENCEVol. 69, Nr. 6, 2004

ation of globular proteins such as WPC-45 occurs during heating

(Turgeon and Beaulieu 2001; Euston and others 2002). In the case
of konjac flour, it was suggested by Maekaji (1978) that the crosslinks forming the junction zones within the gel structure were
formed by weak noncovalent bonds. Nishinari and others (1992)
suggested that these cross-links may be formed by hydrogen bonding between konjac mannan deficient in acetyl groups.
Little exists in the literature on the physical properties of films
formed from blends of proteins and polysaccharides; however,
Parris and others (1995) reported that films formed from proteins
and polysaccharides in combination had greater tensile properties
than films formed from proteins or polysaccharides in isolation.
Consistent with the current study, many authors have indicated
that protein-polysaccharide complexes exhibit more effective functional properties than systems containing proteins or polysaccharides in isolation (Parris and others 1995; Schmitt and others 1999;
Zaleska and others 2000; Turgeon and Beaulieu 2001). The higher
elastic modulus values (Figure 4) obtained for films containing codried preparation than equivalent films formed from dry blends
suggests that there were a greater number of intermolecular crosslinks within the matrices of the films formed from co-dried preparations because elastic modulus is regarded as an indication of the
number of intermolecular cross-links within the film matrix (Doolittle 1965).
Overall, it was shown that alginate-containing films generally
had slightly higher tensile strength, elongation, and elastic modulus than films containing other polysaccharides. These results were
consistent with those of Parris and others (1995), who reported that
whey protein/alginate biopolymer films were stronger and more
extensible than equivalent films formed from whey protein and
pectin dry blends. This effect may be attributed to differences in gel
formation and in the nature of their protein-pectin interactions, as
suggested by Zaleska and others (2000). To our knowledge, it has
been reported that the strongest effect on the physical properties
of mixed gel systems is the difference in electrical charge of the
different components (Zaleska and others 2000). Within the confines of this study, it was difficult to determine exactly how the different protein-polysaccharide mixtures affected WVP. The results
reported provide an indication only of the differences between the
different protein-polysaccharide systems, but they cannot explain
fully why these differences exist. A more detailed study of the powders on a molecular level may be required to provide these answers. This study only served to highlight the potential film-forming ability of protein-polysaccharide blends formed from the novel
co-drying technique.

Conclusions

here is potential to improve the physical properties of hydrophilic films by incorporating a hydrocolloid component into the
film system. Protein-polysaccharide films formed from co-dried
blends were more effective moisture barriers and had higher tensile
properties than films formed from protein in isolation. There are advantages to combining proteins and polysaccharides by the process
known as co-drying, such as lower WVP and higher tensile properties
than equivalent films formed from the dry blended powders. Future
work in this area should focus on improving the physical properties
of co-dried whey protein-polysaccharide edible films.

Acknowledgments
This research was co-funded by the European Regional Development Fund and Enterprise Ireland Strategic Research Grants
Scheme. We also acknowledge the assistance of Dairygold Ltd. and
Kerry Algae.
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Properties of WPC/polysaccharide edible films . . .

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