ACTA UNIVERSITATIS AGRICULTURAE ET SILVICULTURAE MENDELIANAE BRUNENSIS

Volume 66 37 Number 2, 2018

https://doi.org/10.11118/actaun201866020349

SEM ANALYSIS AND DEGRADATION

BEHAVIOR OF CONVENTIONAL AND
BIO-BASED PLASTICS DURING COMPOSTING

Dana Adamcová¹, Maja Radziemska², Jan Zloch¹, Helena Dvořáčková³,

Jakub Elbl³, Jindřich Kynický³, Martin Brtnický³, Magdalena Daria Vaverková1
¹Department of Applied and Landscape Ecology, Faculty of AgriSciences, Mendel University in Brno, Zemědělská
1, 613 00 Brno, Czech Republic
²Warsaw University of Life Sciences – SGGW, Faculty of Civil and Environmental Engineering, Department of
Environmental Improvement, Nowoursynowska 159, Warsaw, Poland
³Department of Geology and Pedology, Faculty of Forestry and Wood Technology, Mendel University in Brno,
Zemědělská 1, 613 00 Brno, Czech Republic

Abstract

ADAMCOVÁ DANA, RADZIEMSKA MAJA, ZLOCH JAN, DVOŘÁČKOVÁ HELENA, ELBL JAKUB,
KYNICKÝ JINDŘICH, BRTNICKY MARTIN, VAVERKOVÁ MAGDALENA DARIA. 2018. SEM
Analysis and Degradation Behavior of Conventional and Bio-Based Plastics During Composting. A
 cta
Universitatis Agriculturae et Silviculturae Mendelianae Brunensis, 66(2): 349 – 356.

Recently, various materials have begun to be marketed that claim to be biodegradable or compostable.
Terms such as “degradable”, “oxo-biodegradable”, “biological”, “compostable” and “green” are often
used to describe and promote different plastics. Commercial bioplastics and a petrochemical plastic
(claim to be degradable) were used for this study. The research was carried out in real conditions in
the Central Composting Plant in Brno, Czech Republic. SEM analysis of the samples was done in
order to analyze microstructure and morphology of specimens, validating dispersion results. It can be
concluded that samples certified as compostable have degrade in real composting conditions. Samples
(4 – 7) showed significant erosion on surface when subjected to the SEM analysis. Samples labeled (by
their producers) as 100 % degradable (Samples 1 – 3) did not show any visual signs of degradation.

Keywords: bioplastics, biodegradation, real composting environment, SEM analysis

of their biodegradation performance and their

INTRODUCTION environmental impacts have become essential.
Problems associated with an ever-increasing The European Waste Framework Directive
amount of waste from packaging and disposable recommends composting as a method of recycling
products made from conventional durable plastics post-consumer biodegradable waste. At present,
have led to the search for new biodegradable a challenge is to develop composting as a disposal
packaging and disposable products (Sikorska et al., technology and the redirection from landfills to
2015). Biodegradable polymers represent composting facilities. In the Europe packaging
a promising way to reduce the amount of plastic waste and packaging waste management, including a test
disposed in landfills, with composting the preferred scheme and a procedure to assess the compostability,
alternative for their disposal (Adamcová et al., is regulated by the European Norm BSI. 2000, which
2017). Many biodegradable polymers have been defines the criteria for material to be recognized
developed in the last two decades with the desired as “compostable” (Sikorska et al., 2015; BSI., 2000).
performance properties (Castro-Aguirre et al., 2017). Biodegradation of plastics depends on both
Thus, along with the development of these the environment in which they are placed and
novel materials, evaluation and understanding the chemical nature of the polymer. Biodegradation

349
350 D. Adamcová, M. Radziemska, J. Zloch, H. Dvořáčková, J. Elbl, J. Kynický, M. Brtnicky, M. D. Vaverková

is an enzymatic reaction; hence it is very specific to processing biological wastes. The composting plant
the chemical structures and bonds of the polymer is used for the conversion of biologically degradable
(Vaverková et al., 2014). waste (bio-waste) from the city of Brno and its
There are different mechanisms of polymer surroundings (Vaverková et al., 2014). The compost
biodegradation. The biodegradation of polymers (three-month-old mature compost, which was
consists of three important steps: (1) provided by a full-scale aerobic composting) was
Biodeterioration, which is the modification of the following physicochemical properties: moisture
mechanical, chemical, and physical properties of 30 ÷ 65 (%), combustibles min. 20 (%), total nitrogen
the polymer due to the growth of microorganisms min. 0.6 (% DM), pH 6.0 ÷ 8.5, undecomposable
on or inside the surface of the polymers. (2) ingredients max. 2.0 (%), C : N max. 30, cadmium
Biofragmentation, which is the conversion of 2.0 (mg/kg), lead 100 (mg/kg), mercury 1.0 (mg/kg),
polymers to oligomers and monomers by the action arsenic 20 (mg/kg), chromium 100 (mg/kg),
of microorganisms and (3) Assimilation where molybdenum 20 (mg/kg), nickel 50 (mg/kg), copper
microorganisms are supplied by necessary carbon, 150 (mg/kg), zinc 600 (mg/kg).
energy and nutrient sources from the fragmentation The investigated materials were single-use
of polymers and convert carbon of plastic to CO2, plastic bags available in various networks of
water and biomass (Emadian et al., 2017). shops on the European market, advertised as
Recently, various materials have begun to 100 % – degradable (Sample 1 – 3) or certified as
be marketed that claim to be biodegradable compostable (Sample 4 – 7). The thickness of each
or compostable. Terms such as “degradable”, sample was 0.2 mm. The material composition of
“oxo‑biodegradable”, “biological”, “compostable” the samples is presented in Tab. I.
and “green” are often used to describe and The samples were made of high density
promote different plastics. These materials include polyethylene (HDPE) with the Totally Degradable
conventional plastics amended with additives meant Plastic Additives (TDPA) (Sample 2) and made of
to enhance biodegradability as well as bio‑based polyethylene (PE) with an addition of pro-oxidants
plastics and natural fiber composites (Gómez and (d2w) (Sample 1 and 3). The eighth, control sample
Miche, 2013). was cellulose paper (CP) (with dimensions 0.3 mm
Our previous study was conducted to investigate thickness) (Sample 8). CP was to check the potential
whether the plastics marked “biodegradable”, of biological decomposition in the tested
100 % – degradable or certified as compostable are environment (positive control). Samples (1 – 8) were
really biodegradable in real composting conditions. placed into frames. The frames were designed and
Original research was carried out in 2011 and 2012. made by the authors themselves of wooden slats
The major goal of this study was to verify information as follows: width = 280 mm, length = 340 mm and
obtained by repeated research and repeatedly height = 50 mm. A 1 × 1 mm polyethylene mesh was
examine the texture of the original samples and fixed onto the frames. The frames were designed
samples that underwent composting process. so that they would facilitate the placement and
The rate of biodegradation has been analyzed by identification of the samples in the compost pile.
investigating the morphological properties using The frames with the samples were properly marked
scanning electron microscopy (SEM). and photographed to document future visual
comparison (Vaverková et al., 2014). All 8 samples
were inserted into one clamp within the compost
MATERIALS AND METHODS
pile (Fig. 1). The samples were installed at a height
Commercial bioplastics and a petrochemical of 1m from the upper side of the compost pile and
plastic (claim to be degradable) were used for this at 1.5 m from the lower side of the pile. In these
study. The research of biodegradability was carried conditions, the experimental period was estimated
out in real conditions in the Central Composting to be 12 weeks. The samples were checked visually
Plant in Brno, Czech Republic. The company operates at regular intervals of about 14 days. After the end
a regionally important (South Moravia) facility of the experiment, the samples were lifted from

I: Material composition of the samples.

Sample Type Description
1 N/A BIO-D Plast
2 HDPE + TDPA 100 % degradabel
3 N/A 100 % degradabel
4 Starch Compostable 7P0147
5 Starch and Plycaprolactone OK Kompost AIB VINCOTTE
6 N/A Compostable 7P0202
7 Natural material Compostable 7P0073
8 Cellulose (blank) –
 Sem Analysis and Degradation Behavior of Conventional and Bio-Based Plastics During Composting 351

the compost pile and all samples were subsequently The evaluation of the samples by means of
photographed and assessed (Vaverková et al., 2014). Electron Microscopy
In addition, all original samples as well as samples
obtained after the end of the experiment were SEM analysis technique allows examining
submitted for SEM. of changes in the morphology of materials at
the micro scale. In order to perceive monitoring
and the changes in the structure of the samples,
RESULTS images from the SEM were used. All samples
were subsequently submitted for SEM. Surface
Visual assessment of the samples morphology by scanning electron microscopy was
Upon the end of the experiment in composting determined on a FEG Quanta 200 (ESEM, USA)
plant the samples were taken to laboratories of in Analytical Centre of Warsaw University of Life
the Department of Applied and Landscape Ecology Sciences – SGGW.
at Mendel University in Brno where they were The experiment involved images of both
subjected to detailed evaluation. In all samples, the original samples and samples that underwent
a visual comparison was made of their initial and composting process. Each sample was depicted at
final states. Samples 1, 2 and 3 did not show any 50 ×, 100 × and 500 × magnification. The illustrations
significant visual changes or signs of decomposition, are presented in Figs. 2 – 8. Via SEM images analysis,
the test material remained completely intact. No is was possible to verify the considerable quality of
breakthrough in disintegration was observed after the samples.
12 weeks of composting. The surface was smooth, The figures from SEM (Figs. 2 – 4) illustrate that
and there were no pinholes observed on the surface the structure of surface of the original samples
after the test. However, Sample 3 exhibited some (defined as A) compared to the composted samples
changes in pigmentation. (defined as B) show the smallest difference in case of
The biodegradation of the certified compostable Sample 1 – 3. For the samples amended with additives
plastic bags (Samples 4 – 7) proceeded very that were supposed to enhance biodegradability,
well. In terms of visual assessment, Samples almost no biodegradation was observed after 12
4 and 5 exhibited the highest degree and rate weeks of composting. SEM images did not reveal
of decomposition (70 %). Samples 6 and 7 were qualitative changes in the appearance of Sample
decomposed to about 80 % of their initial condition. 1 and 3. Only slight changes can be observed at
The CP (Sample 8) completely degrade implying Sample 2 (Fig. 3 B). Sample 2 shows certain erosion
that the conditions required for biodegradation of surface.
to occur in sampling environment were present SEM analysis exhibited the microbial activity of
(Vaverková et al., 2014). degradation on the bioplastic Samples 4 – 7 (Fig. 5 – 8).
The surface structure of the material had lost its
smoothness, and cracks were evident. The samples
showed a significant change in the structure. SEM
images confirmed the biodegradation process

1: Location of the Central Composting Plant in Brno

352 D. Adamcová, M. Radziemska, J. Zloch, H. Dvořáčková, J. Elbl, J. Kynický, M. Brtnicky, M. D. Vaverková

2: Sample 1 - Surface of the original sample (A) compared to the composted sample (B)

3: Sample 2 - Surface of the original sample (A) compared to the composted sample (B)

4: Sample 3 - Surface of the original sample (A) compared to the composted sample (B)
Sem Analysis and Degradation Behavior of Conventional and Bio-Based Plastics During Composting 353

5: Sample 4 - Surface of the original sample (A) compared to the composted sample

6: Sample 5 - Surface of the original sample (A) compared to the composted sample (B)

7: Sample 6 - Surface of the original sample (A) compared to the composted sample (B)
354 D. Adamcová, M. Radziemska, J. Zloch, H. Dvořáčková, J. Elbl, J. Kynický, M. Brtnicky, M. D. Vaverková

8: Sample 7 - Surface of the original sample (A) compared to the composted sample (B)

that happened over the bioplastic film with additives do not biodegrade any faster than
the presence of cracks and loss of filmy nature. non‑additive containing plastics. Manufacturers of
After the termination of the testing process in real these additives claim that if at least 1 – 5 % (by weight)
conditions, the bioplastic sample showed visual of their additive is added to plastics products,
modifications, and broke into pieces when touched these will fully biodegrade when disposed of in
upon. Sample 6 and 7 significantly degraded microbe‑rich environments. These claims are
as apparent by visual detection. This fact was not supported by the findings of study by Gómez
additionally confirmed by the figures from the SEM and Miche (2013). Moreover, for conventional
analysis (Sample 6 B and Sample 7 B see Fig. 7 and plastics with additive no significant conversion was
8). The reduction on mechanical properties is one of observed over the entire period of study.
the main consequences of the degradation process An experimental investigation was conducted
occurring during composting, this process also by Leejarkpai et al. (2011). It was observed
favored the microorganism’s action. This effect could that the swelling at the starch granules occurs
be explained since the loss in mechanical properties throughout the surface of the PE / starch due to
after 12 composting weeks produced a brittle water absorption by the granules. However, almost
material consisting in broken pieces with a high all surface of the PE / starch remained relatively
defects density, such as cracks and porous structure, unchanged suggesting that only a small degree
permitting the easy access of microorganisms to of swelling had occurred (Leejarkpai et al., 2011).
the polymer bulk. The optical inspection of Samples Additionally, in this study SEM examination,
4 – 7 (Fig. 5 – 8) revealed these defects. SEM images confirmed the biodegradation of biodegradable
of bioplastics before and after composting showed plastics material. The results also prove that both
substantial changes in the surface of the material. PE and PE / starch are non-biodegradable plastics
whereas Polylactic acid is a biodegradable plastic.
In a different study, Selke et al. (2015) examined
DISCUSSION the effect of biodegradation-promoting additives
Composting seems to be the most promising on the biodegradation of PE and polyethylene
for waste management options for biodegradable terephthalate (PET). Biodegradation was evaluated
plastics because the composting process is designed in compost, anaerobic digestion, and soil burial
to degrade wastes. There are, however, obstacles environments. None of the additives tested
that make many communities reluctant to accept significantly increased biodegradation in any of these
plastic bags for composting. Various studies environments. Thus, no evidence was found that these
have shown that new biodegradable polymers additives promote and/or enhance biodegradation of
do biodegrade under controlled composting PE or PET polymers. The finding provides evidence
conditions (Gómez and Miche, 2013; Unmar and that anaerobic and aerobic biodegradation are not
Mohee, 2008; Leejarkpai et al., 2011; Vaverková et al., recommended as feasible disposal routes for plastics
2012; Bahramian et al., 2016; Castellani et al., 2016). containing any of the biodegradation-promoting
However, the biodegradability of plastics is additives (Selke et al., 2015).
a complex process and is influenced by the nature of
each plastic (Selke et al., 2015).
The results of Gómez and Miche (2013) study
indicate that conventional plastics containing
 Sem Analysis and Degradation Behavior of Conventional and Bio-Based Plastics During Composting 355

CONCLUSION
The experimental samples were placed in the compost pile operated by the Central Composting
Plant in Brno, and were checked and visually assessed during the experiment which lasted 12
weeks. The goal of the experiment was to test the biodegradation of the above-described samples in
real composting conditions. After the expiration of the experimental period it was found out that
the samples with the additive (Samples 1 – 3) had not been decomposed, their color had not changed
and that no degradation neither physical changes had occurred. SEM analysis of the samples was
done in order to analyze microstructure and morphology of specimens, validating dispersion results.
SEM images showed the biodegradation indicators such as fractures, breaches, cavities, and holes on
the surface (Samples 4 – 7). It can be concluded that samples certified as compostable have degrade
in real composting conditions. Selected Samples (4 – 7) showed significant erosion on surface when
subjected to the SEM analysis. Samples labeled (by their producers) as 100 % degradable (Samples
1 – 3) did not show any visual signs of degradation.

Acknowledgements
The research was financially supported by the IGA FA MENDELU No. TP 5/ 2017.

We would like to express our great appreciation to Dr. Agnieszka Ostrowska (Analytical Centre of
Warsaw University of Life Sciences – SGGW) for her assistance and her willingness to provide her
time so generously in preparing SEM images.

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356 D. Adamcová, M. Radziemska, J. Zloch, H. Dvořáčková, J. Elbl, J. Kynický, M. Brtnicky, M. D. Vaverková

Contact information
Dana Adamcová: dana.adamcova@mendelu.cz
Maja Radziemska: maja_radziemska@sggw.pl
Jan Zloch: xzloch@mendelu.cz
Helena Dvořáčková: helena.dvorackova@mendelu.cz
Jakub Elbl: jakub.elbl@mendelu.cz
Jindřich Kynický: jindrich.kynicky@mendelu.cz
Martin Brtnický: martin.brtnicky@mendelu.cz
Magdalena Daria Vaverková: magda.vaverkova@uake.cz