Macromol. Symp. 2016, 367, 9–17 DOI: 10.1002/masy.

201500156 |9

Identification of Biodegradable and

Oxo-Biodegradable Plastic Bags Samples
Composition
Cristiane M. Finzi-Quint~ao,*1 K
atia M. Novack,1,2 Ana Claudia Bernardes-Silva1,3

Summary: Plastic films used to make market bags are based on polymers such as
polyethylene, polystyrene and polypropylene. These materials require a long time
to degrade in the environment. Alternative technologies have been developed to
reduce the degradation time and the impact on the environment caused by
the conventional polymer materials, using pro-degrading additives or by the
development of biodegradable polymers. In Brazil, some city’s laws require the use of
biodegradable material in the production of market bags, but the absence of specific
surveillance policies makes their chemical composition unknown. The plastic bags
didn’t show the expected environmental behavior by the manufactures, so it is
important to understand the reasons why they are not biodegradable in Brazilian
landfills. In this paper, 7 samples that were obtained from a trading company and
commercial market of Belo Horizonte were analyzed. The samples were characterized
by biodegradable analysis, XRF, FTIR, SEM and TGA/DTA, which allowed the
identification and evaluation of the thermal behavior of the material in an inert and
oxidizing atmosphere. The results showed that plastic bags were composed by a
mixture of PLA and PBAT, with possible presence of TPS and titanium and calcium
fillers. All samples presented low biodegradability in compostable environment.

Keywords: biodegradable; biopolymers; blends; oxo-biodegradable

Introduction development of different plastic products

The plastic films used to make market bags
were originally produced by petroleum
derivatives such as low density polyethyl-
ene (LDPE), high density polyethylene
(HDPE), polypropylene (PP) and polysty-
rene (PS). The commercial plastic history
started in the 40’s, as polypropylene was
discovered in the previous decade. The
1
Programa de P ~o em Engenharia de
os-GraduaSc a
Materiais (REDEMAT) – Universidade Federal de
Ouro Preto, Rua Tiradentes, Centro, Ouro Preto,
Minas Gerais, Brazil
Fax: þ55 31-35591596; E-mail: finzi@ufsj.edu.br
2
Departamento de Química, Universidade Federal de
Ouro Preto, , Campus Morro do Cruzeiro, s/N, Ouro
Preto, Minas Gerais, Brazil
3
Departamento de Química, Biotecnologia e Engen-
haria de Bioprocessos, Universidade Federal de S~
ao
Jo~ao del-Rei, MG 443, KM 7 Ouro Branco, Minas
Gerais, Brazil
led to the adding of additives to improve
their original characteristics such as durabil-
ity, mechanical and thermal resistance.[1]
The structural stability makes the polymers
materials with several uses, although they
produce urban residues that are difficult
to discard and to treat.[2] These polymers
need long time to effectiveness degradation
on environmental conditions. Due to this
fact, alternative technologies have been
developed to reduce the polymers’ degrada-
tion time and to present renewable fonts.[3]
The biodegradable polymer can be pro-
duced from a renewable font and by a
fermentative process, such as poly(lactic acid)
(PLA), poly(hydroybutirate) (PHB), thermo-
plasticstarch(TPS)ornot,suchasthesynthetic
biopolymers: poly(butylene adipate-co-tere-
phthalate) (PBAT) and poly(ɛ-caprolactone)
(PCL). Biopolymers were used, instead of

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10 | Macromol. Symp. 2016, 367, 9–17
conventional polymers, based in the addition
of pro-degrading additives, which allow a
photo-oxidation mechanism.[4,5] The oxo-
biodegradable polymers are conventional
polymers with additives based in transition
metals, that break the structure of polymeric
chain in presence of light and oxygen,
allowing the oxidation mechanism.[6] PBAT
presents mechanical properties similar to
the ones that low density polyethylene has
and it is known as Ecoflex, a commercial
biopolymer. Ecovio is a blend of PLA and
PBAT, and both Ecoflex and Ecovio are
produced by BASF.[7] Ecovio presents
characteristics similar to olefins in biode-
gradable material.[8,9] PBAT and TPS have
received more attention as a composite due
to concerns about solid waste disposal, and
also, TPS presents a hydrophilic behavior
that favors the hydrolysis process during
the biodegradation.[10]
According to ASTM- D883-99 standard
degradable plastic material is “a plastic
designed to undergo a significant change in
its chemical structure under specific envi-
ronmental circumstances, resulting in loss of
some properties” and biodegradable plastic
is “a degradable plastic whose degradation
results from the action of naturally occur-
ring microorganisms such as fungi, bacteria
and algae”. The biodegradable behavior
of a material can be quantified by respiro-
metric rates methodology, according to the
NBR14283-1999 standard, which permits
to quantify the biodegradation of CO2
produced in a specific period.[11,12]
Minas Gerais state’s, Brazil, MG 21.412/
2014 law sets standards and restricts the
available market plastic bags in countries
where there is selective collect in compost-
ing plants. In other words, the plastic bags
must be cross out in landfill sites, according
to ASTM-D883-99, about biodegradable
materials.[11] However, despite the legal
requirements about the use of biodegrad-
able bags, there is no guarantee about the
polymeric material used. In first stage of
law (2011) only biodegradable material
should be used to produce plastic bags.
From 2014, bags needed to be biodegrad-
able but their composition was not defined.
ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
Almost all Brazilian plastic waste is
discarded in landfills that don’t have an
ideal environment to degrade it. Actually,
there isn’t a standardization for bags’
composition, and as a consequence, the
biodegradable material that composes bags
doesn’t degrade or biodegrade as expected
when discarded in a compostable environ-
ment. In the other hand, there is a kind of
bag that is 50% composed by high density
polyethylene (HDPE) and 50% composed
by biodegradable material, according to
the producer.
The present work’s goal is to identify the
composition of some commercial plastic
bags composed only by biodegradable
material and to understand why they don’t
degrade or biodegrade as expected. For this
study, some thermal analysis in inert and
oxidant atmosphere were done, to under-
stand the influence of oxygen presence;
some physical and chemical analysis were
also done, to verify the material composi-
tion, while respirometry tests were used
to evaluate the behavior of the samples.
With the results of the characterization of
samples is intended to understand why
the plastic bags don’t show the expected
behavior and, then, propose solutions to
this problem.
Experimental Section
According to manufacturers, the oxo-
degradable bags were composed by HDPE
and pro-degrading additives and they were
completely degraded in 18 months. The
biodegradable bag may be produced by
fermentation or a synthetic process, and
it is completely biodegraded in approxi-
mately 120 days.[13] The identification of
these polymers allows us to know if they
present a biodegradable behavior, accord-
ing to the law. The identification study of
the samples’ composition was performed by
thermal analysis in inert and oxidant atmo-
sphere, solubility tests, Scanning Electron
Microscopy (SEM) and X-Ray Fluorescence
(XRF). The Thermogravimetric Analysis
(TGA) and the Difference Temperature
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Macromol. Symp. 2016, 367, 9–17
Analysis (DTA) show changes in physical
and chemical properties as a function of
temperature. The Fourier Transform Infra-
red Spectroscopy (FTIR) allows the identi-
fication of the functional groups of the
samples, which were confirmed by solubility
tests. The XRF analysis shows the presence
of metals in the samples and the SEM
provides information about the samples’
morphology.
TGA was realized in a TA Instruments,
SDT 2960 Simultaneous DTA-TGA model,
at 20  C/min, in inert (N2) and oxidant
(synthetic air) atmospheres. FTIR analysis
occurred in FT-IR System Spectrum GX/
Perkin Elmer. The SEM was made in a Jeol
1200 with EDS (Energy Dispersive X-Ray
Detector (EDX)) and the XRF, on an X-Ray
Fluorescence spectrophotometer EDX 720/
800HS Shimadzu. The analysis of biode-
gradability was performed according to
NBR14283-1999, which specifies the proce-
dures for the use of Bartha Respirometer.
Solubility tests were developed in presence
of chloroform, xylene, toluene, hexane and
water in room temperature and under
heating of 100  C.
Seven commercial plastic bags were
selected to this study (Table1). Six samples
were provided by a trade representative
and they have the guarantee of biopolymer
origin; and one was collected in a market
with a registration of conventional polymer
with additives.
Results
Biopolymer samples were soluble in chlo-
roform at room temperature, but B100L
Table 1.
Discrimination of the samples used in the analysis.
Name Type Origin
BW10
BG10
BG6
BW6.1 Biopolymer Trade representative
BW6.2
B100L
OXI Oxo-degradable Supermarket
ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
| 11
presented an insoluble residue. All samples
were soluble in xylene at 80  C, but B100L
presented the same insoluble residue.
According to fabricant, OXI bag is formed
by HDPE chains and it was soluble in
xylene under heating. That occurs because
xylene breaks the molecular interactions
of the nonpolar structure of HDPE.
FTIR spectra (Figures 1 and 2) shows that
all samples present a strong absorption band
closer to 1700 cm1 (stretching vibration of
C-O groups) that indicates carbonyl pres-
ence (C¼O),[14] which represents the esters
of biopolymers and the start of the oxidation
for OXI sample. The OXI sample shows
an absorption band referent to HDPE in
2919 cm1 (CH2 asymmetric stretch bonds),
1452 cm1 (crystalline phase of CH2 bend),
874 cm1 (amorphous phase of CH2 rock)
and 720 cm1 (crystalline phase of CH2
rock).[15]
Biodegradable samples present an ab-
sorption band at  2960 c, representing the
asymmetric stretching vibration of CH2 and
an absorption band at  1711 cm1, repre-
senting the stretching vibration of C-O
bonds; BG6, BW6.1 and BW6.20 present
an absorption band at 1268 cm1, repre-
senting a symmetric stretching vibration of
C-O bonds for alcohols; an absorption band
at 1100 cm1, representing the bending
vibration at the surface of the adjacent
hydrogen atoms on the phenyl ring bonds
and an absorption band at  726 cm1,
representing the bending vibration absorp-
tion of CH-plane of the benzene ring
bonds.[16] Data from literature indicates
that PCL/PLA spectral information shows
absorption bands at 2920 cm1 and
2852 cm1, representing the stretching
Function Color Fill
White 10 kg
Green
Green 6 kg
Market bag White
White 6 kg
Garbage bag Brown 100 L
Market bag White 6 kg
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12 | Macromol. Symp. 2016, 367, 9–17

CaCO3 and TiO2 and are used as a fill. They

Figure 1.
FTIR for plastic bags samples.
Figure 2.
FTIR of samples: (a) OXI, (b) BW10, (c) BG10, (d), B100L,
(e) BG6, (f) BW6.1, (g) BW6.2.
vibration of CH2 bonds; 1756 cm1, repre-
senting C¼O bonds, 727 cm1 representing
CH bonds and bands between 1280 cm1
and 1000 cm1, representing C-O bonds.
The SEM/EDX and XRF results (Table 2)
showed a higher presence of calcium and
titanium in the samples. According to
literature,[15,17] these metals are present as
increase the polymer mechanical resistance
and may act as a pro-degrading material.[18]
In biodegradable samples, BW10 presents
higher proportion of calcium (Ca) than
titanium (Ti), instead of others that present
approximately 80% of Ti. For the OXI
sample, the presence of TiO2 (63% of
metals) associated with the additives con-
firms the presence of a carbonyl group,
observed for this sample in FTIR analysis.
The XRF results showed the presence of
sulfur (S), zinc (Zn) and manganese (Mn),
which may be associated with the pro-
degrading additive.
The thermal analysis curves (TGA)
indicated a great thermal stability of oxo-
degradable sample in inert and in oxidizer
atmosphere. This behavior is expected due
to the presence of HDPE,[14] The OXI
sample lost 88% of its mass at degradation
temperature (Td), approximately 490  C, in an
inert atmosphere (Figure 3a). However,
in an oxidant atmosphere, the thermal degra-
dation occured in two stages (Figure 4a).
First stage starts at initial temperature (Ti) of
315  C with 53% of mass lost, and the second
presents Ti at 400  C completing 87% of
mass lost.
OXI sample is stable in inert atmo-
sphere (Figure 3a), but presents an expres-
sive influence in degradation when the
analysis is made in synthetic air atmosphere
(Figure 4a), which leads to the assumption
that the OXI samples degrade better in an
aerobic environment. The expressive sta-
bility of the OXI sample under heating and
in an inert atmosphere indicates that other
components are necessary to accelerate
the deterioration time. In air atmosphere,

Table 2.
XRF for % of metals for each sample.
% BW10 BG10 BG6 BW6.1 BW6.2 B100L OXI
Calcium (Ca) 67.1 12.8 19.4 2.0 18.2 28.1 34.6
Titanium (Ti) 32.2 86.1 80.1 94.1 80.4 25.3 63.7
Copper (Cu) 0.12 0.51 0.14 0.18 0.17 0.15 0.04
Iron (Fe) 0.21 0.33 0.24 0.49 1.18 44.7 –
Sulfur (S) – – – 2.7 – – 0.5
Potassium (K) – – – – – – 0.6
Zinc (Zn) – – – – – – 0.4

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Macromol. Symp. 2016, 367, 9–17
Figure 3.
TGA curves of samples in inert (N2) atmosphere.
(a) OXI, (b) BW10, (c) BG10, (d), B100L, (e) BG6, (f) BW6.1,
(g) BW6.2.
the sample lost mass in different stages of
heating, which confirms that the presence
of oxygen and another component such as
pro-degrading additive is necessary in its
base polymer. In this case, XRF showed
that OXI presents a higher concentration
of titanium (Ti) than calcium (Ca) (approxi-
mately 63% for Ti and 35% for Ca), and
1.5% of other possible specific metals that
may compose the additives.
For biodegradable samples, the degrada-
tion peaks in an inert atmosphere (Figure 4b–
e) are between 330  C and 440  C, and
indicate possible blends composed by bio-
polymers such as TPS, PLA, PCL, PBAT
and PHB. According to literature, TPS[10]
presents two defined stages of degradation,
the first between to 50  C and 150  C, followed
Figure 4.
TGA curves of samples in oxidant (air) atmosphere.
(a) OXI, (b) BW10, (c) BG10, (d), B100L, (e) BG6, (f) BW6.1,
(g) BW6.2.
ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
| 13
by a second stage in which Td is approximately
330  C.[19] According to literature, pure
ECOVIO is a mixture of PLA and PBAT
(Figure 5), that presents Ti of approximately
337,75  C and a degradation temperature of
approximately 360  C for PLA and 388,37  C
for PBAT.[20] Also according to literature, Ti
of PBAT is approximately 364  C, while PLA
presents Td of approximately 325  C.[9]
TGA curves in inert atmosphere for
samples BW10 (Figure 3d) and BL100
(Figure 3e) and in oxidative atmospheres
(Figure 4d and e) show a similar stage of
loss of mass (approximately 3%), related
to the presence of coordination water in
chain, which is confirmed by DTG, that
shows temperatures of approximately
142  C for inert atmosphere (Figure 6).
Temperatures of approximately 50  C and
330  C are related to the degradation of
TPS, while it appears in B100L for both
atmospheres and only in inert atmosphere
Figure 5.
Thermal analyses for Ecovio.
Figure 6.
DTG of samples in inert (N2) atmosphere.
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14 | Macromol. Symp. 2016, 367, 9–17
for BW10 (Figures 6 and 7). For the other
bio samples, DTG showed Td of approxi-
mately 145  C (Figure 7), which may be
related to the melting transition of PBAT/
PLA with the presence of Td for PLA and
PBAT at both atmospheres.
PHB was discarded because the results
of thermal analysis did not show a Td close
to the one expected in literature. Besides,
this material is originated by an expensive
fermentation process and it is designated to
products with a higher added value.[21] PCL
was also discarded because, according to
literature, it should show a Ti of approxi-
mately 223  C and this value is not present
in the thermal analysis conducted.
DTG in an oxidative atmosphere showed
the presence of calcium carbonate (CaCO3)
by characteristically decomposition stages
and a Td of approximately 583  C (Figure 8),
confirming the presence observed on XRF
(Table 2). According to literature, CaCO3
Figure 7.
DTG curves of samples in oxidant (air) atmosphere.
Figure 8.
TG/DTG curves for BW10 sample in N2 an air
atmosphere.
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starts its degradation at 550  C and ends it
at 800 C,[22] so the DTG (Figure 7) in an
oxidant atmosphere show peaks between
483  C and 590  C.[23]
FTIR and TG analysis assumed that
biodegradable samples were composed by
a mixture of PLA and PBAT. Considering
that TG and DTG curves in oxidized and
inert atmospheres allows the study of the
influence of the environment in the degra-
dation process, for BW10 (Figure 6), the
thermal curves showed that an oxidant
environment did not present a great
influence in the degradation process, which
means that the similar process may occur in
an aerobic or an anaerobic environment.
The XRF analysis (Table 2) showed a
higher presence of calcium and titanium in
BW10 and the inverse for the other bio
samples. It is known that calcium is used
like a fill and that titanium may also be used
as a fill or as a degradant agent.[4]
The proportion of calcium and titanium
showed that the higher concentration of
calcium is not important for the degrada-
tion thermal analysis, but when the con-
centration of titanium is higher than
calcium the degradation presents better
results in oxidative atmosphere. SEM/EDS
showed a granular surface for samples
BW10 (10 kg of load) (Figure 9a) and
BG10 (Figure 9b) and for other samples
(6 kg of load) the surface is smoothed
(Figure 9c–g). EDS information was obtained
for samples of BW10 (Figure 9a), BG10
(Figure 9b) and OXI (Figure 9g), but it was
not possible to do it for other samples because
the films burned during analysis.
BW10 is a plastic bag composed by a
mixture of TPS, PLA and PBAT, added
with CaCO3 in a higher concentration than
TiO2, which promotes similar degradation
in both atmospheres. The bio samples
(BG10, BG6, BG6.1, BG6.2 and B100L)
composed by a mixture of PLA and PBAT
showed a higher concentration of TiO2
than carbonate and presented a preference
for an oxidative atmosphere, having a
similar behavior to the oxo-degradable
sample. The composition of plastic bags
was not informed by manufactures and this
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Macromol. Symp. 2016, 367, 9–17
Figure 9.
SEM/EDS of samples (a) BW10, (b) BG10, (c) Bw6, (d) Bg6.1, (e) Bg6.2, (f) B100L, (g) OXI.
information is important to understand
their biodegradation behavior in Brazilian
landfills.
TGA evaluates the degradability behav-
ior under heated and controlled atmos-
pheres. The biodegradability analysis
verified the capacity of the samples to
release CO2 during the biodegradation
process. This test was realized for the
samples of BW10, BG10 and OXI in a
compostable environment and at a con-
trolled temperature. Considering the fact
that the biodegradable samples were com-
posed by PBAT/PLA/TPS, for BW10.
BG10, HPDE and OXI, a complete
biodegradation for the first samples and a
partial degradation for OXI sample were
expected. Several studies showed that
PBAT and PLA or their blend presented
a good biodegradation behavior in tests
under soil during 120 days, but also showed
that the biodegradation did not occur up to
80%.[16,24]
According to NBR14.283–1999, after 9
weeks in Bartha Respirometer (Figure 10),
in a dry compostable environment and at a
ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
| 15
controlled temperature, the biodegradable
material lost between 60 and 90% of its
mass. BW10 lost 23% of its mass and
produced a higher amount of CO2 (Figure 9)
than BG10, which lost 12% of its mass, while
OXI sample lost approximately 3% of its
mass. According to ASTM D5209-91, tests
of Sturm Respirometry (Figure 11), after
120 days in a wet compostable environment,
at a controlled temperature and in presence
of oxygen, the biomaterial should lose mass
to be biodegradable. In this case, sample
OXI lost 38% of its mass, BW10 lost 4%
of its mass and BG10 lost 3% of its mass.
BW10 is a degradable and biodegrad-
able material and the presence of TPS and
calcium carbonate can favor the absorption
of water by accelerating the biodegradation
process. However, the absence of TPS and
the smaller concentration of Ca in BG10
reduced the biodegradation capacity of this
biopolymer. OXI samples with no presence
of oxygen, at controlled temperature
but without UV light didn’t have a degrad-
able and biodegradable behavior in a com-
postable environment. However, in the
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16 | Macromol. Symp. 2016, 367, 9–17
Figure 10.
Curve of quantify of CO2 mass produced due to biodegradation process in Bartha Respirometer. (a) BW10,
(b) BG10, (c) OXI.
presence of oxygen and in a wet environ-
ment, the OXI sample presents better
degradability than the others samples.
The samples used in this study were
composed only by biodegradable polymers,
according to the representant, and did not
degraded as expected. Actually, the samples
failed in the biodegradation test, according
to ASTM- D883-99, NBR14283-1999 and
ASTM D5209-9. The higher concentration
of calcium and the presence of TPS indicated
that both components improve the degrada-
tion/biodegradation process and the pres-
ence of titanium retards it. TiO2 is an
additive with several functions and in
general it is used in polymers to conferee
Figure 11.
Curve of quantification of CO2 mass produced due to the biodegradation process in Sturm Respirometer.
(a) BW10, (b) BG10, (c) OXI.
ß 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
color, resistance and a pro-degrading action,
however, this last function depends on the
presence of oxygen.
Biopolymers are present as a solution
for substituting conventional polymers,
because they present a better and a faster
degradation when discarded in the ideal
conditions. In Brazil, there are no compost-
able plants to meet the biodegradable
disposal; most of the residuals are for-
warded to landfills with no degradable
waste. The lack of standardization of the
composition of plastics bangs, associated
with specific landfill features indicate the
importance of studies for a best composi-
tion of biopolymers and additives to
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Macromol. Symp. 2016, 367, 9–17
improve the biodegradation of plastic bags.
In countries that assume a pattern compo-
sition for the biodegradable materials and
the use of disposal plants, materials such as
PBAT, PLA and TPS and their mixture or
the polyolefin with pro degrading additives
present an expected behavior of biode-
grading. However, in countries with a lack
of compostable plants, it is important to
know the composition and the behavior of
the biodegradation of these materials to
make it possible to propose useful alterna-
tive technologies for their reality.
Conclusion
The Brazilian biopolymer samples may have
blends with PLA, PBAT and two of them
with TPS, with unknown mass percentage.
The samples presented calcium and titanium
as CaCO3 and TiO2, and the oxo-degradable
sample presented pro degrades additives
based in zinc, sulfur, titanium, besides
HDPE. Oxo degradable samples are oxygen
dependent, according to the fabricant, for
degradable and biodegradable process.
BW10 had presented a better thermal
degradation and biodegradation behavior
than other samples, which can be associated
with the presence of TPS and the higher
concentration of calcium. The biodegrad-
able samples without TPS and higher
concentration of titanium had presented
influence of oxygen in the degradation
process and had half of the biodegradation
capacity. Despite using biodegradable mate-
rials known in literature, the composition
of bags did not allow the biodegradation
in Brazilian landfill because they need a
compostable environment to promote the
biodegradation process. Landfills have an
acid environment with no oxygen or light to
allow the biodegradation process for the
material studied. Knowing the used material
and its thermal and biodegradation behavior
is important to develop efficient technolo-
gies for a country reality.
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| 17
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