PACKAGING TECHNOLOGY AND SCIENCE

Packag. Technol. Sci. 2013; 26(Suppl. 1): 1–10

Published online 5 September 2012 in Wiley Online Library (wileyonlinelibrary.com) DOI: 10.1002/pts.1986

Chinese Packaging Institute -2012 Conference

Fabrication and Characterizations of Zeolite b–filled Polyethylene
Composite Films

By Zhen Huang,* Yu-hua Guo, Tian-ming Zhang, Xiao-hong Zhang and Li-ying Guo

Department of Packaging Engineering, Tianjin University of Commerce, Tianjin 300134, China

A series of low-density polyethylene (LDPE)/linear LDPE (LLDPE)/zeolite H-b composites at different

zeolite contents up to 10 wt% were mixed after melt and blown into film sheets. The resultant films were
characterized by using X-ray diffraction, scanning electron microscope and other physical property
analyzers. X-ray diffraction results reflect that either zeolite or polymer phase has maintained its regularly
ordered microscopic structure without any observable deterioration. The scanning electron microscope
morphological observation shows a good dispersion of zeolite in the PE matrix. Water vapour, oxygen
and nitrogen transmission rates are all found to increase after introducing zeolite H-b. However, tensile
strength, elongation, tear strength and puncture resistance are observed to obviously drop with successive
increment of zeolite content. Composite film clarity becomes poorer than the pristine film as reflected by
the increase of the film haze after adding zeolite H-b. Finally, the composite films were used as packaging
materials for fresh strawberries. The gas composition variations in the packages during 5 days reflect that the
O2 and CO2 contents have varied inside and they are apparently dependent on the zeolite loadings in the
composite films, subsequently affecting respiration rates of fruit. Our experiments suggest that there is a
compromise between zeolite content and film performances like mechanical, optical, barrier and packaging
properties. Copyright © 2012 John Wiley & Sons, Ltd.

Received 3 February 2012; Revised 21 May 2012; Accepted 29 May 2012

KEY WORDS: polyethylene; zeolite H-b; composite films; barrier properties

INTRODUCTION

Fresh fruits and vegetables harvested seasonally must be stored or packaged in suitable environments
to prevent the possible degradation that may render them a lower quality or make them unsuitable for
consumption. Among various preservation methods, physical packaging with polymeric films is usually
preferred as it necessitates the minimal processing of the produce so that it resembles its natural features to
the maximum extent. As a feature of proper sealed packaging films, a fresh fruit or vegetable is capable of
creating modified atmosphere within the package due to the respiratory gases. These gases like oxygen,
carbon dioxide, ethylene and water vapour can permeate through the packaging material at different rates
and thus affect the quality of fresh food packed.
Among various packaging materials, polyethylene is the most extensively used because of its easy
availability, process ability, flexibility and improved optical properties and seal strength. In addition,
no other ingredient is required during processing of polyethylene. Recently, some investigators have
studied the effect of zeolite on the performance of polyethylene packaging material as the zeolite is

* Correspondence to: Z. Huang, Department of Packaging Engineering, Tianjin University of Commerce, Tianjin
300134, China.
E-mail: huangzhen50@yahoo.com

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2 Z. HUANG ET AL.

selectively permeable to different gaseous molecules like oxygen, nitrogen and carbon dioxide.1–8 To
the best of our knowledge, zeolite is widely used to enhance the gas separation properties of the mixed
matrix films.9 It is worth noting that the films, formed by incorporating zeolite particles into a properly
selected polymer, exhibit much better gas separation properties as compared with conventional compo-
sites because of their unique phase morphology and high surface area.9 Furthermore, zeolite can be used
for catalysts for the conversion of agriculture film waste into useful hydrocarbon products.10 The chal-
lenge for these zeolite-filled composites is to improve the film properties to meet the requirements for
the purpose of suitable applications like packaging. Thus, knowledge about the relationship between
properties and zeolite effects is required. In this study, PE/zeolite H-b composites were investigated in
film samples blown with different zeolite contents. Structural, mechanical, optical and barrier properties
of the films were studied and compared; moreover, these films were tested for packaging fresh
strawberries as they are a highly perishable fruit because of their physiological and morphological
properties and their rapid postharvest responses.11,12 In this way, this study was aimed to investigate
the effect of PE/zeolite H-b composites on air-packaged strawberries.

EXPERIMENTAL

Materials
Commercial grade of low-density polyethylene (LDPE) (LD-163; Melt flow index (MFI), 5 g/10 min;
density, 0.941 g/cm3) from SINOPEC Yanshan Chemical Corporation, Beijing, China, and linear LDPE
(LLDPE) (FV-149M; MFI, 2 g/10 min; density, 0.931 g/cm3) from SKCorporation, Korea, were used
at a mass ratio of 4:1 as the base polymer. Zeolite H-b, with a Si/Al ratio of 38 and a particle size of
approximately 1 mm, was purchased from the Catalyst Plant of Nankai University, Tianjin, China.
Compounding and film blowing
LDPE, LLDPE and zeolite H-b were melt-mixed to obtain pelletized composite using a twin-screw
co-rotating extruder (LTE-26-52; Labtech Engineering Co. Ltd, Thailand) with a temperature profile
of 155  C to 185  C during the compounding process. The obtained composite was then blown into
75-mm-thick film samples using a double-layer co-extrusion film blowing machine (SFM-200,
L/D = 25 and D = 25 mm; Beijing Plastics Industry Co., Ltd, Beijing, China). Film blowing was
performed at a temperature profile of 170  C to 190  C. To study the effects of zeolite content, a few
PE/zeolite composite films with different zeolite contents were prepared while the mass ratio of LDPE
to LLDPE was kept at 4:1 for all composites. The compositions of these PE/zeolite H-b composite films
are summarized in Table 1.
Characterization methods
The PE/zeolite H-b composite films obtained were examined by a few characterization methods given
as follows.
Morphology and structure analysis. Powder X-ray diffraction (XRD) analysis,13 performed on a
Shimadzu XRD-6000 spectrometer using Cu Ka radiation (1.5406 Å) with the samples scanned from
5 to 50 in steps of 0.02 , was carried out to investigate the composite microstructure and to confirm
the presence of zeolite structure and whether zeolite affects the structure of the polymer matrix.

Table 1. Contents of PE/zeolite H-b composites prepared.

Compositions (wt%)
Samples LDPE LLDPE H-b
S0 80.0 20.0 0.0
S1 78.0 19.5 2.5
S2 76.0 19.0 5.0
S3 74.0 18.5 7.5
S4 72.0 18.0 10.0

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The cross-sectional morphology14 of the composite film was examined with a scanning electron
microscope (SEM; JEOL JSM-6700F). Before the SEM examinations, the sample strips were chilled
in liquid nitrogen for at least 30 s and then folded with forceps to make a sharply broken cross
section of the films. The resultant film was vertically adhered to an aluminium stub with a tape to
render the film cross-sectional surface parallel to the stub surface and gold coated under vacuum
using a sputter coater.
Mechanical properties. The tensile strength (TS)15 of the composite films was determined on a
universal testing machine at a rate of 200 mm/min. The defect-free strip sample was cut in a dumbbell
shape with a size 15  100 mm, and 20 strips were prepared for each film with 10 for transverse
direction (TD) tests and the remaining for machine direction (MD) tests.
Tear strength16 was determined using a universal testing machine at a rate of 200 mm/min, similar to
the case of TS measurements. The samples were prepared with 10 strips for TD tests and the other 10
for MD tests for each film.
The puncture strength17 of plastic films was evaluated using a pendulum impact tester. The sample
was exposed, at right angle to its surface, to a semispherical punch of 12.7 mm in diameter at a
controlled impact rate. The strength in joules is taken to be the maximum energy consumed at the moment
of film failure and is essentially a measure of the capacity of the film to absorb energy.
Optical properties. The haze and the transparency18 of the composite films were quantitatively
measured on a WGT-S tester (Labthink Technology Co., Ltd, Jinan, China) for more than 10 samples
of each film. Haze and transparency are two important parameters for transparent or translucent films.
The former refers to the percentage of the total transmitted light that, in passing through the sample, is
scattered and/or refracted from the incident beam by more than 2.5 , whereas the latter is the percentage
of incident light that, in passing through the sample, is deflected by less than 0.1 from the axis of the
incident light. It should be noted here that transparency is also called clarity because it is directly related
to whether it is visible or not for the contents packed inside the film bags.
Barrier properties. Oxygen transmission rate (OTR) and nitrogen transmission rate (NTR)19 were
tested using a manometric gas permeability tester (L100-5000; PBI Dansensor, Denmark). The test
samples used were of circular shape with a diameter of 10 cm and stored before testing in desiccators.
The test was performed at constant temperature and constant relative humidity (RH) of 23  C and 50%
in this work. Water vapour transmission rate (WVTR)20 was determined using a water vapour
permeability tester (L80-5000; PBI Dansensor). The film separated the permeation cell into lower and
upper chambers where the lower chamber was saturated with water vapour whereas the upper one was
dried via a silica filter under air purge flow to a defined level of RH of 9.8%. The experiment was carried
out in the room with a constant temperature of 23  C and a constant RH of 50%.
Strawberries packaging. Strawberry fruit was obtained from a commercial fruit grower at Shandong
province, China. Fruit was harvested at commercial maturity judged on the basis of fruit skin colour as
it is considered as the best indicator of the harvest maturity in fruits. Therefore, fruit having a sharp-red
skin colour was harvested and transported to the Packaging Engineering Laboratory of Tianjin Univer-
sity of Commerce, China. The fruit was sorted for uniformity in size, maturity and freedom from
defects before packed in PE/zeolite H-b composite films. The films were cut into control sheets with
a size of 25  25 cm for making plastic bags. For each film variant, 10 replicate packs, each containing
five fruits, were tested. The randomly selected fruit was placed in a plastic tray, then loaded into film
bags and sealed through appropriate thermal treatment. The packed fruit was then transferred onto a
home-made plastic mesh for avoiding any fruit injury and stored at ambient conditions (25  C–28  C
and 60%–70% RH) to simulate marketing conditions. Figure 1 shows fresh strawberries packaged
in PE/zeolite H-b composite films blown in present study. The percentage concentrations of O2 and
CO2 in the fruit bags were measured through a self-sealing rubber septum using a gas analyzer (Model
Checkmate 9900 O2/CO2; PBI Dansensor). The gas composition was measured daily for 5 days.
Statistical analysis. The experiment was carried out in a completely randomly way, and the results
were subjected to ANOVA using Stastica Software 99 at a significance level of P < 0.05. The standard
deviation was then calculated, and all the data points were obtained in this work as mean values along

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4 Z. HUANG ET AL.

Figure 1. Fresh strawberries packaged in PE/zeolite H-b composite films.

with a deviation within 10%, indicative of the reliability of the method used and the acceptable
reproducibility of experimental results determined.

RESULTS AND DISCUSSION

XRD analysis and SEM observations

Figure 2 shows XRD patterns for PE film and PE/zeolite H-b composite films. As evidenced by the
XRD results, there are two distinct diffraction peaks in 17 –24 and 35 –38 , respectively, for the
S0 sample, which are probably related to crystalline features of LDPE/LLDPE materials used. The
very high peak intensity confirms that the PE obtained is still highly structurally crystalline. Because
PE is the substrate material, thus these two peaks are very clearly preserved in the XRD spectra for
all composite samples. After adding zeolite H-b, a few more peaks at approximately 2θ =7.16, 9.90
and 22.44 are observed, which are characteristic of the zeolite b structure and identical to those
reported in the literature.13 Besides, with an increase in the zeolite content, the intensity of these peaks
becomes more pronounced, as shown in Figure 2. On the other hand, the incorporation of zeolite
particles has not been found to observably affect the crystalline structure of polyethylene matrices.

Figure 2. XRD patterns of PE/zeolite H-b composite films.

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Figure 3 displays cross-sectional SEM images for the PE/zeolite H-b composite films at 10 wt%
zeolite loading, from which the particle distribution and morphologies may be examined. As we can
see from Figure 3, zeolite H-b particles are generally homogeneously distributed throughout the whole
polymer matrix, indicative of the feasibility of the melt mixing and co-extrusion film blowing
processes used. The film thickness can also be approximately observed from Figure 3, and it is
approximately 80 mm and agreeing rather well with the value for film-blowing design. At high magni-
fication, SEM image reflects that zeolite particles used are generally uniform and have a particle size of
approximately 1 mm. It is clearly observed that the zeolite particles are rather well contacted in the PE
phases, indicative of good interfacial compatibility formed between dispersed phase and continuous
phase. In contrast, Yong et al.14 reported that void-rich microstructures were created in polyimide films
after filled with only zeolite particles. Thus, we can deduce that some fine interfacial voids might have
formed around zeolite particles as well.

Mechanical property measurements

Table 2 presents zeolite/zeolite H-b composite films. It can be seen that for PE/zeolite composite films,
the TS in two different direction tests firstly decreases with the zeolite content to 5.0 wt% of zeolite
loading and then slightly increases. As for the MD TS, it is 22.2 MPa without adding zeolite but
reduces to 15.8 MPa after introducing 5.0 wt% of zeolite. For the TD tests, the values are 20.9 and
14.5 MPa, respectively, for the films without zeolite and at 5.0 wt% of zeolite loading. The decrease
in film TS may be mainly due to the decrease in the polymer content of the films. One may note that
the polymer content will drop correspondingly as the loading of zeolite H-b in the polymer matrix be-
come higher, thus reducing the TS of the resultant films with the zeolite content. After adding more
zeolite, the melt mixing and co-extrusion film-blowing method used here may have rendered the inter-
facial interactions between polymer macromolecules and zeolite particles slightly stronger, thereby
recovering TS to an extent and reaching a plateau value. On the other hand, very fine voids around

Figure 3. Cross-sectional SEM images of the S4 film sample: (a) low magnification and (b) high
magnification.

Table 2. Mechanical properties of PE/zeolite H-b composite films.

TS (MPa) Elongation (%) Tear Strength (kN/m)
Puncture
Films MD TD TD MD TD MD strength (J)
S0 22.2  2.3 20.9  2.1 108  10 445  36 98.6  5.4 109.4  8.6 7.85  0.62
S1 16.3  1.8 16.4  1.7 97  9 322  25 99.5  4.3 99.0  9.3 7.16  0.37
S2 15.8  1.2 14.5  0.8 72  12 291  13 90.7  6.1 89.1  7.5 7.24  0.57
S3 15.9  0.9 14.7  1.2 88  7 280  18 89.4  3.2 92.8  4.8 7.53  0.29
S4 17.1  1.5 15.7  1.3 74  8 291  21 82.1  5.1 89.7  6.7 7.47  0.46

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6 Z. HUANG ET AL.

zeolite particles once created could contribute to the loss of film TS. Similar observations have applied
to percent elongation, tear and puncture strengths, as can be seen from Table 2. Although there are cer-
tain decreases in mechanical properties for these composite films, they could still be used as flexible
packaging materials for storing fresh fruit.

Optical properties
For packaging applications, optical properties such as haze and clarity are of considerable importance
in the development of polyethylene films. Figure 4 shows the haze and transparency measurements for
PE/zeolite H-b composite films blown in current work. It can be seen that the pristine PE film has a
transmittance of approximately 85%, and the film transmittance is reduced to 80% after adding zeolite.
In contrast, the film haze increases from 80% to 85% with introduction zeolite H-b. These results
suggest that the addition of inorganic zeolite particles has adversely affected the film optical properties.
It is known to us that the high haze in PE films has arisen from surface irregularities because of the
extrusion roughness of the elastic melt flow effects and the crystallization roughness due to the
presence of crystal aggregates.21 For the film composites, the PE crystalline structure may not have been
affected by the presence of zeolite H-b, but the zeolitic crystal structure is still retained in the films as
reflected by XRD spectra. Then, the combined crystal aggregates of PE and zeolite H-b near the film
surface could subsequently make the composite film surface smoothness worsen. In the meantime, the
presence of rigid zeolite particles can affect the elastic melt flow at the exit of the extrusion die, possibly
rendering the film surface become relatively rougher. As a consequence, the composite films have higher

Figure 4. Optical properties of PE/zeolite H-b composite films: (a) haze and (b) transparency.

Copyright © 2012 John Wiley & Sons, Ltd. Packag. Technol. Sci. 2013; 26(Suppl. 1): 1–10
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haze and poorer transparency than the one without zeolite. However, one may note from Figure 1 that the
clarity properties of the composite films are still satisfactorily acceptable as they allow us to “see” what is
contained within the packages.

Barrier properties
Table 3 displays the WVTR curve of PE/zeolite H-b composite films at different zeolite loadings. Neat
PE film exhibits good resistance to water vapour transfer with a WVTR value of 5.66 g/m2
24 h due to
the hydrophobic nature of polyethylene macromolecules. With the introduction of zeolite H-b into
polymer matrices, the water vapour transmission rate increases considerably, and its value depends
on the zeolite content added. As zeolite H-b loading is 5.0, 7.5, 10.0 wt%, the WVTR increases by
approximately 46%, 55% and 78%, respectively. The significant increase in WVTR for the PE compo-
sites may be mainly attributed to the large pore size of introduced zeolite H-b.13 Besides, the presence
of aluminium element and hydrogen ion in the zeolite H-b might make itself slightly more hydrophilic
than the PE substrate, possibly resulting in some increase in WVTR. In view of packaging fresh fruit
and vegetables, the increase in WVTR may be helpful as water vapour, upon food respiration or retained
water from washing, may transport readily to certain degree out of sealed films to avoid condensing on the
film inner wall. Once water vapour is saturated inside the packaging, it will unavoidably attract the yield
of bacteria and consequently shorten the life span for consumption.
The gas permeation performance of PE/zeolite H-b composite films was individually tested for N2 and
O2. Table 3 shows the permeation results thus obtained for these composite films with different zeolite load-
ings. As seen from Table 3, the PE substrate film (S0) has an O2 transmission rate of 1880 ml/m2
24 h and
N2 transmission rate of 760 ml/m2
24 h, respectively. After adding zeolite, the composite film has higher
OTR and NTR values compared with the film without zeolite. In the case of the S3 film with 7.5 wt%
zeolite H-b, the OTR and NTR values are 2450 and 824 ml/m2
24 h, respectively. In addition, the ratio
of OTR/NTR increases from 2.5 for the S0 film to 3.0 for the S3 film. As discussed earlier, XRD spectra
of the composite films reveal no obvious change in bulky PE crystallinity upon formation of the compo-
sites, which means that the changes in OTR or NTR are probably not due to the result of disruptions in
polymer microstructures. Therefore, the gas permeation results could probably be attributed to the large
pore size of zeolite H-b 13 introduced into the polymer matrix. Note that if some fine interfacial voids were
created around zeolite particles, the gas transmission rate would also have increased. These barrier results
suggest that the incorporation of porous zeolites in the conventional packaging films may produce
modified-atmosphere-packaging effect for fruits and vegetables.

Packaging applications
Figure 5 shows O2/CO2 concentration evolution in the packages for stored strawberries during 5 days
for the PE/zeolite H-b composite films. As can be seen, the respiratory rates of strawberry fruit
increases with the progression of storage irrespective of the films with or without zeolite loadings.
The CO2 content in the packages are 2.0–2.4 times higher at 112 h than that at 20 h, but for the O2
content it is 4.4 and 2.1 times higher for the S0 and S4 films, respectively. Thus, the respiration rates
were modified during ambient storage to some extent, depending on the zeolite loadings. Figure 5
shows that at higher zeolite H-b loadings in the composites, higher O2 and lower CO2 content could
be obtained. This may be explained as follows. During strawberry fruit respiration, O2 in the packages

Table 3. Permeation results of PE/zeolite H-b composite films.

WVTR NTR OTR
Films (g/m ∙24 h)
2
(ml/m ∙24 h)
2
(ml/m2∙24 h)
S0 4.66  0.14 760  9 1880  48
S1 4.57  0.28 789  18 2145  69
S2 6.79  0.49 815  21 2333  24
S3 7.23  0.37 824  27 2450  112
S4 8.30  0.63 845  16 2605  85

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8 Z. HUANG ET AL.

Figure 5. O2/CO2 concentration changes in the packages for strawberries during storage for 5 days:
(a) O2 and (b) CO2.

was consumed whereas CO2 was generated. Hence, CO2 will permeate out and O2 will permeate into
the packages based on concentration gradient. However, as discussed earlier, the gas permeation
properties of the composite films are different from each other because the one with higher zeolite
content bears higher gas transmittance rate. As a result, more O2 or CO2 molecules can pass through
the S4 film with highest zeolite loading, leading to lowest CO2 content and highest O2 content inside
the packages. Subsequently, the variations of gas concentrations in the packages could influence the
respiration rates of strawberry fruit affecting fruit quality. Our experiments show that the S4 film with
highest zeolite content had led to the best storing performance but at the cost of the film clarity to
certain extent for packaging fresh strawberry fruit. Therefore, there should be a compromise between
zeolite content and film performances like mechanical, optical, barrier and packaging properties and
further work along this line will be carried out soon.

CONCLUSIONS

In this article, we have fabricated numerous PE/zeolite H-b composite films by using a double-layer
co-extrusion film blowing machine after having compounded LDPE/ LLDPE/zeolite H-b at different

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zeolite contents through a twin-screw co-rotating extruder. The following conclusions can be drawn
from the present study.
1. After incorporating zeolite H-b particles, the polyethylene composite films exhibit considerable
decrease in mechanical properties like TS, elongation, tear strength and puncture resistance,
whereas the regularly ordered microscopic structure of either zeolite or polymer phase retains
rather well as reflected by XRD spectra.
2. The addition of zeolite H-b into the PE film has shown a good dispersion of zeolite particles in the
PE matrix as reflected by SEM images, whereas the film haze, possibly arising from surface crystal
aggregations and the effect of rigid zeolite particles on the elastic melt flow, is seen to increase with
zeolite loadings, subsequently making the film surface smoothness worsen and the clarity poorer.
3. The PE/zeolite H-b composite films exhibit obvious increase in water vapour, O2 and N2 transmis-
sion rates after introducing zeolites, possibly due to the large pore size of zeolite H-b.
4. The packaging application results for fresh strawberries show that the O2/CO2 composition had
varied over time in the composite film packages and higher zeolite H-b loadings had resulted in
higher O2 content and lower CO2. These variations of gas compositions inside could modify sub-
sequent respiration rates of strawberry fruit and possibly extend shelf-life of air-packaged straw-
berry fruit.
5. There are certain improvements in the barrier properties after adding zeolites, but the film clarity
and mechanical properties are sacrificed. Thus, a compromise between the zeolite content and the
film properties should be taken into account, and more investigations are required to further
achieve the integrated performance for these zeolite-filled composite films.

ACKNOWLEDGEMENTS

The authors thank Tianjin University of Commerce for partially supporting this research.

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