Journalof~oodEngineering

25 (lWSl497-507
Copyright 0 1995 Elsevier Science Limited
P&ted in Great Britain. All rights reserved
0260~X774/95/$9.50
0260-8774(94)00029-B

Gas and Water Vapor Barrier Properties of Edible Films

from Protein and Cellulosic Materials
Hyun J. Park* & Manjeet S. Chinnan:
Center
Technology,

for Food Safety & Quality Enhancement, Department of Food Science and
University

(Received

of Georgia,

Agricultural
USA

Experiment

Station,

6 April 1993; revised version received

accepted 10 June 1994)

Griffin, GA 30223,

9 March

1994:

ABSTRACT
Edible films were made from proteins (corn-zein and wheat gluten) and
celluloses (methyl cellulose and hydroxypropyl cellulose), and tested fog
permeability of gases. Oxygen and carbon dioxide permeabilities of edible
films were generally lower than those of plastic films. However, water
vapor permeabilities of edible films were higher than those of plastic films.
The concentration of plasticizer significantly affected the permeability of
gases. The gas permeabilities, O,, CO, and water vapor, of cellulose films
increased as the concentration of plasticizer increased. Addition of lipid
(Myvacet 7-OO) in the hydroxypropyl cellulose (HPC) film decreased
the gas permeability Linear relationships were found between permeability of gases and film thickness in protein films.

INTRODUCTION
Edible films and coatings from biopolymers have been widely used as lipid,
water vapor, gas, flavor barriers for fresh fruits and vegetables, confectioneries,
frozen foods and meat products. Corn-zein and sucrose fatty acid ester coatings
have been applied successfully on fresh fruits and vegetables, such as apples,
bananas and tomatoes, as oxygen and water vapor barriers for extending their
shelf lives (Banks, 1984; Santerre et al., 1989; Park et al., 1994). Casein coating
as a water vapor barrier was used for precut carrot to extend the marketing
period (Avena-Bustillos et al., 1993). Cellulosics containing lipids were very
efficient oil, water vapor and oxygen barriers in confectionery products, ice
cream cones and frozen foods (Kester & Fennema, 1989; Rico-Pena & Torres,
1990; Nelson & Fennema, 1991). Corn-zein coating was a good oxygen barrier
*Present
address:
Mokpo. Korea.

Department

;To whom correspondence

of Food

Engineering,

should be addressed
497

Mokpo

National

University.

H. J. Park, M. S. Chinnan

498

on nut meats and peanuts for preventing oxidation (Cosler, 1958). Corn-zein
coating on paper provided a high barrier to beef fat compared to polyethylene
laminated paper, and had a potential to be used as quick-service sandwich
packaging (Trezza et al., 1992). Edible hydrocolloid coatings showed no detectable oil migration after 47 days at 30C between chocolate and peanut butter
(Brake & Fennema, 1993).
Gas and water vapor barrier properties of an edible film and coatings vary
greatly with composition, and presence of bubbles and pinholes of the films
(Pascat, 1986). Water vapor permeabilities of cellulose films were measured by
Kamper and Fennema ( 1984). Nelson and Fennema ( 199 1) reported a decrease
in water vapor permeabilities of cellulose films with the increase in lipid concentration. Banker et al. ( 1966) also found that the water vapor permeabilities of
cellulose films increased as the film thickness increased. But the effect of coating
thickness of protein films on gas permeabilities is not available. Gontard et al.
(1993) reported that water vapor barrier properties and some mechanical
properties of wheat gluten film were affected by plasticizing agents, but they did
not measure O2 and CO2 permeabilities. Gennadios et al. (1993a) found that the
addition of mineral oil and keratin to film-forming solutions reduced water
vapor permeability in protein-based films. Also, Gennadios et al. (19938)
studied the effect of temperature on edible protein-based films (corn-zein,
wheat gluten and wheat/soy films), but they concentrated only on oxygen
permeability values. Aydt et al. (1991) measured barrier properties of corn
protein film formed from Cozeen TM303 NF (a commercially available formulation) and wheat gluten film; however they did not investigate the effect of film
thickness.
The objectives of this study were to (a) prepare several edible films from food
constituents (corn-zein, wheat gluten, celluloses and lipids), (b) measure
permeabilities of O,, CO, and water vapor of the films, and (c) examine the
thickness effect on the gas permeabilities in protein films.

MATERIALS

AND METHODS

Materials
The following materials were used to prepare the edible film solution: corn-zein
(INC Biomedical, Inc., Cleveland, OH); wheat gluten (ADM Arkardy, Inc.,
Olathe, KS); methyl cellulose (25cp), hydroxypropyl cellulose (mw, 370 000),
polyethylene glycol (mw, 400), glycerin, citric acid and ammonium hydroxide
(Aldrich Chemical Company, Inc., Milwaukee, WI); ethanol, 95% (Fisher Scientific, Pittsburgh, PA); Myvacet 7-00 TM (Eastman Chemical Product, Inc.,
Kingsport, TN). In the Myvacet numbering system, the first number refers to the
degree of acetylation (e.g. 7 indicates approximately 70% acetylation) and the
second number (e.g. 00) refers to the iodine number, which is a measure of
unsaturation in the monoglyceride fatty acid.
Preparation of the edible film
The edible film solutions (Table 1) were prepared by dissolving corn-zein in an
ethanol solvent, and wheat gluten, methyl cellulose (MC) and hydroxypropyl

TABLE

325
1 g citric
acid

High level (H)

95% Ethanol (ml)

Water (ml)

in protein films, polyethylene

360
240
60 ml
NH,OH( 6N)

7SgWG
24

54gCZ
11

Wheat gluten
(WC;,

Protein film
Methyl
(3X]

200
100
-

YgHPC
1

Hydroxopropyl
(HPCI

Cellulose film

glycol was used as a plasticizer

200
100

YgMC
1

of Edible Film Solutions

Low level (L)

Corn-zein
cm

oGlycerin (density 1.26 g/ml) was used as a plasticizer

cellulose lipid films.

Solvent
Other

Base
ingredient
Plasticizer
U(ml)

Components

Compcktion

in cellulose and

20

100
Y g Myvacet
(7-00TM)

YgHPC
3

HPC/Lipid

Cellulose/lipid
film

2.
2
*
g
6

3
a
5

H. J. Park, M. S. Chinnan

500

cellulose (HPC) in an ethanol-water mixture (Aydt et al., 1991; Kamper &

Fennema, 1984). In the case of wheat gluten, ammonium hydroxide was added
to produce one or more of various water-soluble inorganic bases which aided in
dispersing the wheat gluten in the solvent. There were two levels of plasticizing
agent in cellulose films (MC and HPC), low level and high level. MC was
dissolved in ethanol first, and HPC was dissolved in water first, because of their
solubilities. A homogenizer (Brinkmann, Inc., Westbury, NY) was used to mix
the edible film solution. For degassing, the edible film solution was heated to
85C until it started boiling. The solution was then poured onto a glass plate and
dried. The film thus formed was carefully detached from the glass plate and kept
in a desiccator until permeability measurements were made.
Thickness of the film
A micrometer was used to measure the film thickness
0.0025 mm. Ten measurements were made on each film.

to an accuracy

of

Gas permeability
The permeation process can be described mathematically by Ficks first law.
The flux (J), which is proportional
to the concentration
gradient, can be
expressed in one direction as follows
J= - D.(dC/dX)
where J is the flux, the net amount of solute that
unit time (g/m2*s or ml/m2.s), D is the diffusivity
of the diffusing substance (g/m or ml/m3) and X
(Crank, 1975).
With the two assumptions that ( 1) the diffusion
diffusivity is constant, the flux (J) is given by

(I)
diffuses through unit area per
(m2/s), C is the concentration
is the thickness of the film (m)
is in a steady state, and (2) the

J= D.( C, - C,)/X= Q/(A. t)

(2)

where Q is the amount of gas diffusing through the film (g or ml), A is area of
the film (m2) and t is the time (s).
Application of Henrys law allows expression of the driving force in terms of
partial pressure differential of gas. Rearrangement of terms yields the following
equation in terms of permeability
Q/(A.t)=

D+(p,-p,)/X=

P.Ap/X

(3)

where S is the Henrys law solubility coefficient (mole/atm), p is partial pressure

difference of the gas across the film (Pa) and P is the permeability ((ml or g).m/
m2*s.Pa).
Then, the permeabilities of O,, CO, and water vapor can be calculated from
the following equation
P= Q*X/(A- t. Ap)

(4)

Oxygen permeability
An OX-Tran 100 0, transmission tester (Macon Modern Control, Inc.,
Minneapolis, MN) was utilized to measure the O2 permeability. Samples were

Properties of edible films

501

exposed to 0% relative humidity (RH) and tested at 30C (Aydt et al., 199 1;
Park et al., 1994).
Carbon dioxide permeability

This was measured using a modified permeability cell designed by Gilbert and
Pegaz (1969). The films were tested at 0% RH and 21C. The permeability
measurement using gas chromatography
is based on the measurement of the
amount of gas diffusing through the film being tested.
Water vapor permeability

A small cup filled with desiccant and covered with the film to be tested was held
at 85% RH and 21C and the weight change of the cup was recorded periodically. No forced air movement was provided and the procedures described by
Kamper and Fennema (1984) and Aydt et al. ( 1991) were employed. The Ap,
partial pressure difference of water vapor, was obtained from the vapor pressure
of pure water.

RESULTS AND DISCUSSION

Oxygen permeability

Oxygen permeabilities of edible film are shown in Table 2 and compared with
plastic films. Oxygen permeabilities of most edible films were lower than the
common plastic films. The 0, permeabilities of protein films were lower than
those of polyethylene (low density), polyethylene and polyvinyl chloride, and
were close to that of polyester film. The OZ permeabilities of protein films, cornzein and wheat gluten were also lower than those of cellulose films, MC(L) and
HPC(L). The addition of lipid (Myvacet 7-OOT) in HPC film decreased the 0,
permeability only slightly.
Oxygen permeability of corn-zein film prepared in our laboratory were lower
than the CozeenTM film, and higher than the corn-zein film prepared by
Gennadios et al. (1993b) as shown in Table 2. CozeenTM film is a commercial
corn-zein based film and primarily developed for coating nuts, acting as a gas
barrier to extend marketing life. The glycerin/protein (w/w) ratio of corn-zein
films made by Gennadios et al. (1993b), and that in this study, were 0.20 and
0.26, respectively. A lower ratio of glycerin in the film by Gennadios et al.
( 1993 b) probably resulted in lower oxygen permeability. The oxygen permeability of wheat gluten film prepared in this laboratory ranged from 0.11 to O-28
fl*m/m2*s*Pa and were slightly higher than those of other wheat gluten films.
The glycerin/protein (w/w) ratio of wheat gluten films prepared in this study was
slightly higher than others, which most likely caused higher oxygen permeability.
Park et al. (1992) reported that oxygen permeability increased as glycerin/
protein ratio increased in wheat gluten film.
Carbon dioxide permeability

The CO, permeabilities of protein films, corn-zein and wheat gluten were lower
than those of plastic films, polyethylene (low density), polyethylene and polyvinyl chloride, except for polyester film which exhibits a greater barrier to CO,

H. J. Park, M. S. Chinnan

502

TABLE 2

Oxygen and Carbon Dioxide Permeabilities

Film

Edible films
Corn-zein
Wheat gluten
MC(L)
HPC (L)
HPC/Lipids

Thickness
(mm)

of Edible Films

Permeability
02

CO:

0.12-0.31
0.23-0.42
0.04-0.07
0.05
015

0.36 f 0.16
0.20 k 0.09
2.17 kO.45
3.57 f 0.03
3.4450.06

2.67 k 1.09
2.13 f 1.43
69.00 f 19.33
143.99 f 3.76
81,75k4.58

0.09
0.14
0.08
0.15

0.89
0.09
0.16
0.08

Permeability
ratio

cCozloJ
7.5
9.5
31.6
40.6
23.7

Edible films from the literature

Cozeen
Wheat gluten
Corn-zein
Wheat gluten

5.25
0.03
-

5.9
0.3
-

Other films

Polyethylene, low density

Polyethylene
Polyvinyl chloride
Polyester

22.50
8.30
0.09-17.99
0.13-0.30

121.40
26.10
1.35-26.98
0.67-1.12

5.4
3.1
-

Unit of permeability is in fl.m/m*.s.Pa; f is an abbreviation for femto ( 10-s).

Composition of edible films is described in Table 1; L in MC (L) and HPC (L) refer to
low level of plasticizer. MC - methyl cellulose, HPC - hydroxypropylcellulose.
Aydt et al. ( 1991); oxygen permeability data for 37.8C and 0% RH; carbon dioxide
permeability data for 22.8C and 0% RH.
Gennadios et al. (1993); data for 25C and 0% RH.
Modern Plastic Encyclopedia (1987).

permeation
(Table 2). CO, permeabilities of cellulose films, MC(L) and HPC( L)
were higher than those of plastic films. The addition of lipid (Myvacet 7-OOTM)
in HPC film decreased with CO, permeability by 43.2%. COJO, permeability
ratios were also calculated for various films (Table 2). This ratio has an implication in designing films/coatings suitable for fruits and vegetables. Higher ratios
will allow less accumulation of CO, and vice versa. The permeability ratios of
edible films were higher than those of plastic films, and protein films had lower
values than those of cellulose films. Carbon dioxide permeability of CozeenTM
film was higher than the corn-zein films prepared in this study (Table 2). Like
corn-zein film, COJO, permeability ratio of CozeenTM film was lower than
those of cellulose films. Carbon dioxide permeability of wheat gluten film
prepared by Aydt et al. (1991) was much lower than that of wheat gluten film
prepared in this study. In addition CO,/O, permeability ratio of their film (Aydt
et al., 1991) was less than one. In general, CO2 is more permeable than 0, due
to greater solubility in films, thus resulting in a CO,/O, permeability ratio
greater than one (Pascat, 1986).

503

Properties of edible films

TABLE 3

Water Vapor Permeabilities of Edible Films

Film

Thickness (mm)

Permeability

Edible films

0.12-0.33
0.38-0.42
0.04-0.07
0.05
0.15

0~116+0~019
0.616 IIIo.013
0.092 -t 0.003
0.110 + 0.004
0.082 f 0.003

Edible films from the literature

Cozeen

0~09

Wheat gluten
Wheat gluten

0.14
0.05

0.407
1.254
0.136

Corn-zein
Wheat gluten
MC(L)
HPC (L)
HPC/Lipid

Other films

Polyethylene,/ low density

Polyvinyl chloride/
Cl&C16 HPMC
Cl&C16 MC/HPMC

0~04
0~02

04~005 5
0~0007 1
0.004
0~003

Unit of permeability is in ng.m/m2.s.Pa; n is an abbreviation for nano (lo-).

%omposition of edible films is described in Table 1. MC - methyl cellulose, HPC hydroxypropyl cellulose, HPMC - hydroxypropylmethyl cellulose.
Aydt et af. (1991); data for 25C and 100% RH gradient.
Gontard et al. ( 1993); data for 25C and 100% RH gradient.
Kester & Fennema (1989); all measurements taken at 25C.
RH gradient (100 to 90-O)%.
RH gradient (97-O)%.

Water vapor permeability

Water vapor permeabilities (WVP) of edible films were much higher than those
of plastic films, as shown in Table 3. WVP of wheat gluten film was 0.603-0.630
ng.m/m.s.Pa,
which was the highest among all the edible films tested. Wheat
gluten film exhibited high permeability to water vapor, probably because wheat
gluten was dispersed by addition of ammonium hydroxide (6N) as part of the
formulation, and also contained a higher concentration of plasticizer (wt. plasticizer/wt. protein = O-4). The addition of lipid (MyvacetT 7-00) in HPC film
decreased the water vapor permeability by 24.7%.
WVP of edible films are compared with other edible films from the literature
in Table 3. WVP of Cozeen TM film was higher than that of corn-zein film
prepared in this laboratory, which could be due to differences in the formulation
of films or the temperature of measurement. WVP of wheat gluten film reported
by Aydt et al. (1991) was higher than that prepared by the authors. Aydt et al.
(1991) measured the properties at 26C, in comparison to 21C in this study,
which could be the reason for the difference in WVP values. WVP of wheat
gluten film of Gontard et al. ( 1993) was lower than that of this study. This difference is probably due to the difference in glycerin/protein
(w/w) ratios; these

H. .I. Park, M. S. Chinnan

504

ratios were 0.3 and O-4 in their and these authors wheat gluten films, respectively.
Effect of plasticizer
The gas permeabilities, 0, and CO,, of cellulose films increased as the concentration of PEG increased (Table 4). Park et al. (1993) also observed similar
trends in the range of plasticizer used in this study; they attributed this effect to
an increase in flexibility of films due to a long carbon chain in polyethylene
glycol (PEG). The water vapor permeabilities of cellulose films, MC and HPC
increased 2.7 and 2.2 times, respectively, as the ratio of PEG/cellulose (ml of
PEG/g of cellulose) increased from O-11 to 0.33. Banker et al. (1966) reported
that the plasticizer could enhance or retard moisture permeation, depending
upon its concentration. The surface of cellulose film which contained a higher
level of plasticizer was smoother than that of the cellulose film which contained
a low level of plasticizer. Also, cellulose films became more flexible as the
concentration
of plasticizer increased. Formation of bubbles and possible
pinholes are influenced by the film preparation technique and the chemical
composition, including the level of plasticizer agent. Extent of bubbles and
pinholes then in turn affect the film permeability characteristics. A conceptual
picture of a section of edible film is shown in Fig. 1. Heiss (1959) reported that
waxed paper showed an especially high increase in water vapor permeation after
being creased, which demonstrated that the loosened fibers act like wicks.
Kamper and Fennema (1984) perforated stearic acid emulsion film, about
O*OOS%of exposed film area, and observed that the water vapor transmission
rate increased by 2.7 times; they indicated that small disruptions in film integrity
will considerably lessen the ability of this film to retard the passage of gases.
Effect of the film thickness
Gas permeabilities of a particular type of film are, theoretically, independent of
the film thickness (Schwartzberg, 1986). However, in this study it was observed

TABLE 4
Effect of Plasticizer on the Permeabilities
Film

Thickness (mm)

Permeability

02
MC(L)
MC (HI

HPC (L)
HPC (H)

of Edible Films

co,

Water vapor

0.04-0.07

2.17 rf:0.45

69.00 + 19.33

0.092 f 0.003

0.1 l-0.15
0.05
0.10

11.68 k 0.06
3.57 k 0.03
10.53 kO.69

670.46 k 0.62
143.99 k 3.76
648.86 k 34.03

0.245 + 0.018
0~110Ik0~004
0.247 k 0.006

Composition of edible films is described in Table 1; L and H refer to low and high level
of plasticizer, respectively.
Oxygen and carbon dioxide permeabilities
are in fl.m/m*.s.Pa;
water vapor
permeability is in ng.m/m*.s.Pa.

Properties of edible films

505

that the 0, and CO, permeabilities of protein films, corn-zein and wheat gluten,
increased as the thickness of the film decreased, and the permeabilities of water
vapor of films increased as the thickness of the film increased. Banker et ul.
( 1966) also reported that the water vapor permeability constants of hydrophilic
films increased linearly with film thickness over the range of thickness studied.
Various reasons for thickness effects on edible films have been reported in the
literature. The reasons vary from a change in structure due to thickness as well
as swelling of hydrophobic films again altering the structure. McHugh et al.
(1993) have addressed some of these effects from their own work and those
reported in literature.
Linear relationships were fitted between permeabilities of gases and film
thickness for protein films. The plots of permeability of protein films against
film thickness were linear, as shown in Fig. 2. These relationships may be
expressed by the following equation
P= ax+ h

i:5)

matrix
bubble
pinhole

Fig. 1.

Pathways of gases through the film.

Thickness

(mm)

Fig. 2. Thickness effect of the gas permeability of protein films. CZ-O,, CZ-CO, and
CZ-H,O are the O,, CO, and H,O permeability of corn-zein film, respectively. W-02,
W-CO, and W-H,0 are the O,, CO, and H,O permeability of wheat gluten film,
respectively.

H. J. Park, M. S. Chinnan

506

where P is the permeability (l.m/m2*s.Pa for 0, and CO,; g.m/m2.s.Pa for

water vapor), x is the thickness (m) and a and b are constants. The a values of
O,, CO, and water vapor are - 1.7, - 12.0 and 18 for corn-zein film and - 0.9,
- 19.7 and 5.5 for wheat film, respectively; the b values of O,, CO, and water
vapor are O-7, 4.9 and 0.7 for corn-zein film, and 0.5, 8.2 and 4-O for wheat
gluten film, respectively.

SUMMARY

AND CONCLUSIONS

The 0, and CO, permeabilities of protein films were lower than those of plastic
films, polyethylene (low density), polyethylene and polyvinyl chloride. The 0,
permeabilities of cellulose films were lower than those of polyethylene (low
density) and polyethylene and were higher than those of polyvinyl chloride and
polyester, whereas the CO, permeabilities of cellulose films were usually higher
than those of plastic films. The CO,/O, permeability ratios of edible films were
higher than those of plastic films. The water vapor permeabilities (WVP) of
edible films were much higher than those of plastic films and the WVP of wheat
gluten film was highest among all edible films tested. The CO, and O2 permeabilities of cellulose films increased as the concentration of polyethylene glycol
increased. The permeabilities of 0, and CO, of protein films, corn-zein and
wheat, increased as the thickness of the film decreased, and the water vapor
permeabilities of the films increased as the thickness of the film increased.
Comparison of permeability data of corn-zein films in the literature revealed
that increasing the glycerin/protein ratio increases the oxygen, carbon dioxide
and water vapor permeabilities. The authors hope that the information generated here will be useful in predicting the migration of gases and water vapor
when using these films/coatings on different food materials, which in turn could
aid in assessing quality changes of food products coated with the edible films
studied.

ACKNOWLEDGEMENT
The authors wish to acknowledge Dr Robert
comments about film formation properties.

D. Phillips for his valuable

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SO7

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