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Degradation Behaviour of Poly (Lactic Acid) Films and Fibres in Soil Under Mediterranean Field Conditions and Laboratory Simulations Testing
Degradation Behaviour of Poly (Lactic Acid) Films and Fibres in Soil Under Mediterranean Field Conditions and Laboratory Simulations Testing
Degradation Behaviour of Poly (Lactic Acid) Films and Fibres in Soil Under Mediterranean Field Conditions and Laboratory Simulations Testing
a r t i c l e i n f o a b s t r a c t
Article history: Long-term degradation/disintegration behaviour, indicative of the biodegradation in soil behaviour of
Received 25 November 2010 poly(lactic acid) films and fibres, was studied in natural Mediterranean soil environment during an
Received in revised form eleven-month trial in the experimental field. In parallel, simulated soil burial experiments were car-
21 December 2010
ried out under controlled laboratory conditions. The degradation/disintegration behaviour of PLA was
Accepted 23 December 2010
analysed using visual inspection, mechanical testing, DSC and FTIR analysis. The influence of the thick-
Available online 22 January 2011
ness and the type of the materials (film vs. fibre) on disintegration was investigated under the given mild
conditions. For comparison purposes, degradation/disintegration of PLA film was also studied under low
Keywords:
Biodegradation
temperature composting conditions (house composting). During long-term exposure under natural soil
Biodegradable materials environment dominated by complex and uncontrolled biotic–abiotic conditions and Mediterranean cli-
Agricultural films matic conditions and under house composting conditions, PLA film samples of different thicknesses were
Poly(lactic acid) partially, to a rather low degree, degraded mechanically or slightly disintegrated. The results showed that
Composting degradation behaviour of bio-based polymers like poly(lactic acid) in a real soil environment is a complex
Biodegradation in soil phenomenon, following different patterns regarding morphological changes.
© 2010 Elsevier B.V. All rights reserved.
0926-6690/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.indcrop.2010.12.031
E. Rudnik, D. Briassoulis / Industrial Crops and Products 33 (2011) 648–658 649
The degradation of PLA films in Costa Rican soil was investigated standard respirometric testing methods (Briassoulis and Dejean,
by Ho et al. (1999). The average soil temperature and moisture con- 2010). The field experimental degradation results were monitored
tent were 27 ◦ C and 80%, respectively. The average degradation rate through systematic sampling, measurements and analysis of sev-
of PLA films in the soil of banana field was 7675 Mw (average-weight eral key properties of the materials in the lab and confirmed by
molecular weight)/week. Films of poly(l-lactide) (PLLA) were simulated soil burial and composting conditions.
buried in outdoor environment in south Finland during two years
(Gallet et al., 2001). No lactic acid was observed during the first 2.2. Full-scale field experiments
year of soil burial. Urayama et al. (2002) found only a 20% decrease
in molecular weight of PLA (l-rich) plates after 20 months in soil. Biodegradation studies under real Mediterranean field condi-
Injection moulded tensile bars composed of native starch (0–70%), tions were carried out at the experimental field of the Agricultural
poly(d,l-lactic acid) (95% L) (PLA, 13–100%) and poly(hydroxyester- University of Athens in Spata. The latitude of the site is 37◦ 58 49 N,
ether) (PHEE, 0–27%) were buried in soil for 1 year in order to longitude 23◦ 54 49 E and altitude 119 m. The soil in Spata is clay
study the effects of starch and PHEE on rates of biodegradation loam. The detailed soil characteristics of the field at the experimen-
(Shogren et al., 2003). Rates of weight loss increased in the order tal site are given elsewhere (Rudnik and Briassoulis, 2011).
pure PLA (0%/year) < starch/PLA (0–15%/year) < starch/PHEE/PLA A first set of materials was studied in the experimental field of
(4–50%/year) and increased with increasing starch and PHEE AUA in Spata for a period of 11 months, starting from October 2007
contents. Studies of the microbial communities responsible for till September 2008 (winter–summer period). Samples (size of 1/2
the decomposition of poly(-caprolactone) (PCL), poly(butylene A4 in the case of films and approx. 2 g of mass for fibres) were placed
succinate) (PBS), poly(butylene succinate-co-adipate) (PBSA) and in envelopes of plastic nets and buried in the soil 10–15 cm beneath
poly(lactide) (PLA), were performed in two Japanese soils (Kamiya the surface, in a pattern arranged along 11 lines.
et al., 2007). The PCL, PBS and PBSA films were considerably During the test period, the weather and soil parameters were
degraded within 50 days at 25 ◦ C under upland dark conditions recorded by a data logger (Campbell) with sensors. The following
in one soil, while the PLA film was not degraded at all after 120 parameters were monitored and recorded regularly:
days in soil. In another study (Suyama et al., 1998), no soil bacterial
colonies that degrade PLA were found. • meteorological conditions (air temperature & humidity, total
The aim of the present research work was to offer a better under- irradiation, UV irradiation);
standing and enrich the existing knowledge about the long-term • soil conditions (soil temperature and soil water content).
biodegradation in soil behaviour, of PLA films of various thick-
nesses and of PLA fibres, under real Mediterranean soil conditions. The following two-day irrigation cycle was applied: one day of
The biodegradation behaviour in the natural complex biotic–abiotic irrigation and one day without irrigation. During rain period the
soil environment was studied by full scale field experiments and irrigation was interrupted.
by simulated soil burial experiments under controlled laboratory Samples were taken off every month, or at appropriately modi-
conditions. The biodegradation behaviour was studied through fied time intervals, depending on the evaluation of the results, and
monitoring the evolution of several important degradation sen- analysed following the experimental protocol.
sitive properties along with the disintegration behaviour of the
tested materials, considered as indicators, but not measures, of the 2.3. Laboratory simulations set-up
biodegradation process. The results obtained by the full-scale field
experiments were compared against the results obtained through In parallel to field testing, laboratory biodegradation studies
laboratory simulations of PLA degradation/disintegration in soil were carried out. The laboratory experiments were performed in
and the results of composting of PLA films under farm conditions. two solid environments: in soil using “bioreactors” and under com-
posting conditions. For the simulated laboratory experiments soil
taken from the experimental field in Spata was used. A flexible
2. Experimental studies periodicity of samples recovery during laboratory and field experi-
ments was established according to the degradation/disintegration
2.1. Materials progress, being continuously monitored.
Poly(lactic acid) (PLA) samples in various forms (films with 2.3.1. Laboratory experiments for biodegradation in soil
various thicknesses and fibres) were obtained from commercial The degradation/disintegration studies on biodegradation were
suppliers and used in the experimental studies. According to the carried out in “bioreactors” (4 l plastic boxes containing condi-
suppliers, these materials were made out of Nature Works PLA tioned soil). Each “bioreactor” contained about 2 kg of soil collected
pellets [NatureWorks LLC, http://www.natureworksllc.com/] (no from the experimental field of AUA in Spata and sieved using 2 mm
further information was made available though, for reasons of con- size sieve. Studies were performed at room temperature during an
fidentiality, concerning processing, plasticisers, etc.). Filter paper 11 month-period and water content was periodically adjusted at
(Whatman) and poly(ethylene) (PE) film were used as a positive and a constant level (40%). Samples (films and fibres) were placed in
negative reference, respectively. The characteristics of the materi- envelops of plastic nets and buried in the conditioned soil contain-
als studied are given in Table 1. ing boxes. Two representative PLA films with thickness 30 m and
Biodegradation under real soil conditions in the field was 75 m were chosen for the laboratory studies (PLA 30 and PLA 75).
determined indirectly through the study of the degradation and Filter paper (Whatman) and polyethylene (PE) film were used as a
disintegration of the materials, both used as strong indicators (but positive and negative reference, respectively.
not as a quantitative measures) of biodegradation. The approach Each “bioreactor” contained 1 sample of a given film in the
used is a normal approach adopted by researchers in this RTD area, form of 1/2 A4 (for tensile testing) and 5 samples in the form of
including major producers of agricultural biodegradable films. This 2 cm × 2 cm pieces (for mass change measurements).
approach is justified based on the fact that the research objec-
tive concerns testing biodegradability under real soil environment 2.3.2. Composting studies
where it is not possible to measure and quantify biodegradation in The composting studies were performed outdoors using a com-
the way it is measured in the lab under controlled conditions by post bin of 100 l volume with perforated wall for improved air
650 E. Rudnik, D. Briassoulis / Industrial Crops and Products 33 (2011) 648–658
Table 1
Characteristics of the materials studied for biodegradation in soil.
PLA (EarthFirst® PLA)a P1 (Plastic Suppliers Inc.; Sidaplax v.o.f.) Film Thickness: 20 m transparent PLA 20
PLA (EarthFirst® PLA) P1 (Plastic Suppliers Inc.; Sidaplax v.o.f.) Film Thickness: 30 m transparent PLA 30
PLA (EarthFirst® PLA) P1 (Plastic Suppliers Inc.; Sidaplax v.o.f.) Film Thickness: 40 m transparent PLA 40
PLA (EarthFirst® PLA) P1 (Plastic Suppliers Inc.; Sidaplax v.o.f.) Film Thickness: 50 m transparent PLA 50
PLA (EarthFirst® PLA) P1 (Plastic Suppliers Inc.; Sidaplax v.o.f.) Film Thickness: 75 m transparent PLA 75
PLA (NatureWorksTM PLA polymer 2002D) P2 (FOLIETECHNIEK International BV) Film Thickness: approx. 400 m transparent PLA 400
PLA (PLSTD-013NRR-1950) P3 (MiniFIBERS, Inc.) Fibres Length, 19 mm 1.3 denier per filament; white PLA fib
a
Based on IngeoTM resin of NatureWorks® LLC.
circulation. The composting medium was prepared by blending at a rate of 10 ◦ C min−1 from 20 ◦ C to 200 ◦ C, then was held for 1 min
sheep manure and sawdust in a ratio of 5:1 (w/w). Temperatures at 200 ◦ C and cooled at a cooling rate of 10 ◦ C min−1 to 20 ◦ C. The
outside and inside the compost bin were monitored, as well as procedure was repeated twice.
water content. Initial water content was 52%. The composting pro- For the polylactic samples (PLA) the glass transition, crystal-
cess was evaluated systematically by Solvita respiration testing lization, and melting temperatures (Tg , Tc and Tm , respectively),
[Solvita, http://solvita.com/]. For composting studies Whatman cel- as well as the enthalpy of fusion (Hf ), the enthalpy of crystal-
lulose paper was chosen as positive reference. PLA film of 30 m lization (Hc ), and crystallinity (Xc ) were determined. Tm and Hf
thickness (PLA 30) and PLA fibres (PLA fib), were chosen for com- were determined by the first scan, while Tg and Tc were determined
posting studies. Film samples of 1/2 A4 size and fibres of approx. by the second scan. The repeatability of DSC measurements was
2 g were placed in envelopes of plastic nets and buried in the checked for selected samples.
composting medium. The period of the composting studies was The Xc values were calculated according to the following equa-
11 months. tion:
Hc + Hf
2.4. Methods of analysis and testing Xc (%) = 100 × (1)
93
The degradation/disintegration process in soil was followed where Hf is the melting enthalpy, Hc is the crystallization
by visual inspection (digital images), as well as by mechanical enthalpy and 93 (J/g) the melting enthalpy of 100% crystalline PLA
properties testing (tensile properties for films) and FTIR analy- sample (Ahmed et al., 2009).
sis. Morphological changes were investigated using the differential
scanning calorimetry (DSC) method. 2.4.3. FTIR analysis
A qualitative surface analysis by attenuated total reflectance
2.4.1. Mechanical testing (ATR) infrared spectroscopy was carried out using a Bruker Tensor
Tensile properties were measured using an Instron 4204 mate- 27 instrument. Resolution: 1 cm−1 , range; 600–4000 cm−1 .
rials testing machine. Cross-speed rate was 10 mm/min. Five
specimens were tested for each film sample. Samples were con- 3. Results and discussion
ditioned at 23 ◦ C and 50% humidity in a climate chamber for 24 h
before testing. 3.1. Meteorological data
2.4.2. DSC method Fig. 1 presents some of the weather data (temperature and rel-
Thermal analysis was carried out using a Perkin Elmer Pyris DSC ative humidity) recorded in Spata during the field experiments for
6 Differential scanning calorimeter. The sample (≈3 mg) was heated the period October 2007–September 2008. Total rainfall ranged
30 80
70
25
60
20
Temperature, oC
50
Humidity, %
15 40
30
10
20
5
10
0 0
Oct Nov Dec Jan Feb Mar Apr May Jun Jul Aug Sep
2007 2007 2007 2008 2008 2008 2008 2008 2008 2008 2008 2008
Temperature Humidity
Fig. 1. Temperature and air humidity data during the period October 2007–September 2008 in Spata (monthly averages).
E. Rudnik, D. Briassoulis / Industrial Crops and Products 33 (2011) 648–658 651
Fig. 2. Photos of PLA 20 (a), PLA 40 (b), PLA 75 (c) and PLA 400 (d) films during biodegradation studies in the experimental field of AUA (period 1: October 2007–September
2008), at different stages of degradation (left to right: November 2007 1-month, March 2008 3-months, May 2008 7-months and September 2008 11-months).
from 10 mm (February 2008), 8–6 mm (October–December 2007) During 11 months of burial in soil, fragmentation and disin-
to 2 mm (March, April, September 2008) and nearly zero mm (Jan- tegration of PLA film samples was observed. The first significant
uary, May, July, August 2008). Soil water content during the period changes were observed after 7 months. It seems that the increase
May 2007–October 2008 was in the range 34–47% (monthly aver- in temperature in May 2008 correlates with the onset of fragmen-
ages). Soil temperature measured at 30 cm below soil surface varied tation of the PLA film samples. Then the extent of fragmentation
in the range 16–21 ◦ C. and disintegration proceeded faster. At the end of 11 months burial
samples disintegration of the materials could be clearly observed
(a strong indication of the associated stage of the biodegradation of
3.2. Field test results the material process). However, the degree of disintegration of the
material was still rather low. Obviously, thickness influences the
3.2.1. Visual observations extent of degradation of PLA films. The thinner the films, the more
Photos of PLA samples recovered during the biodegradation pronounced changes can be observed, in general.
studies in the experimental field of AUA in Spata are shown in Fig. 2 All PLA films became brittle after 1 month of soil burial. Many
for selected PLA 20, PLA 40, PLA 75 and PLA 400 film samples. cracks could be seen in the samples of thin PLA films. It is notewor-
Fig. 3. Photo of filter paper after 1 month (a), PE film (b) and PLA fibres (c) after 11 months of soil burial in the experimental field of AUA in Spata, respectively (period 1:
October 2007–September 2008).
652 E. Rudnik, D. Briassoulis / Industrial Crops and Products 33 (2011) 648–658
Fig. 4. Tensile properties after 1 month of burial in Spata: tensile strength for PLA 3.2.2. Testing of mechanical properties
20 and PLA 50 films (top figure); elongation at break for PLA 20 and PLA 50 films After one month burial in the experimental field, PLA film sam-
(bottom figure). ples of 30, 40, 75 and 400 m thickness were too brittle and they
were broken when trying to cut specimens as a result of the first
thy that during burial in the real soil environment worms and roots stage of the material degradation. Only for PLA 20 and PLA 50 sam-
of plants clearly contributed to degradation (mechanical fragmen- ples it was possible to cut specimens for tensile testing and this only
tation and disintegration) of samples. for the early period of soil burial (first month). The results for the
Filter paper (cellulose) used as positive reference biodegraded tested PLA films are presented in Fig. 4 (the initial values were found
completely after 1 month of burial (Fig. 3a). On the contrary for the to be close to those reported for PLA (98% l-lactide) in Auras et al.
PE film used as negative control sample no degradation signs were (2004)). The tensile properties of both PLA samples with different
observed during the field experiments (Fig. 3b). The PE film surface thicknesses decreased significantly after a burial period of just one
was not found to be broken even by the activity of plant roots. month. The tensile strength for the PLA 20 film decreased almost
Fig. 5. FTIR-ATR spectra of PLA 75 film: initial (top) and after 11 months of soil burial (bottom) in Spata.
E. Rudnik, D. Briassoulis / Industrial Crops and Products 33 (2011) 648–658 653
64
62
60
56
54
52
50
48
46
0 1 3 5 7 9 11
Time, months
PLA 20 PLA 30 PLA 40 PLA 50 PLA 75 PLA 400 PLA 30-lab PLA 75-lab
Fig. 6. Glass transition temperatures for PLA films during soil burial in the field in Spata and at laboratory.
to one-third its initial value, from 53.8 to 14.9 MPa, whereas for the ferent climatic conditions. Thus, for example, it has been reported
thicker PLA 50 film, the decrease was half the initial value, i.e. from by Maharana et al. (2009) that non-enzymatic hydrolysis of PLA
53.2 to 24.0 MPa. The elongation at break values was decreased dra- is preceded by an apparently inert first stage of degradation with-
matically for both tested PLA films. This explains the fact that most out weight loss but resulting in random cleavage of polymer chain
PLA film samples were found to be too brittle, after one month of backbone (endo-type degradation) with a concomitant substantial
burial, already with cracks. The tensile properties of the polyethy- decrease in molecular weight, leading to a decrease in mechanical
lene film used as negative control were not affected, as expected. properties such as tensile strength and elongation at break.
The early drastic decrease of the tensile strength and elonga-
tion at break values of the PLA films exposed to Mediterranean 3.2.3. FTIR-ATR analysis
field soil burial conditions (one month exposure) suggests that, FTIR-ATR spectroscopy was used to evaluate chemical modifi-
the first stage of the PLA biodegradation in soil process results in cations occurring on film surface. The FTIR-ATR spectra of PLA 75
severe degradation of the mechanical properties of the material (i.e. before its use and after 11 months burial in the soil under real field
embrittlement), leading to gradual slow disintegration of the mate- conditions are presented in Fig. 5. The two spectra seem similar.
rial. Analogous results were obtained with the PLA films exposed No shifts of characteristic bands or formation of new bands are
to the laboratory simulated soil burial conditions. The decrease of observed. However, the intensity of absorbance at 1748 cm−1 , cor-
the elongation at break was found to be higher than that of the ten- responding to carbonyl C = 0 stretching band, decreased after 11
sile strength in all cases tested under both soil burial conditions. months of soil burial. Similar tendencies are observed in the spec-
This confirms similar research results reported earlier under dif- tra obtained for PLA film of various thicknesses. After 11 months
168
167
166
Melting temperature, oC
165
164
163
162
161
160
159
158
0 1 3 5 7 9 11
Time, months
Fig. 7. Melting temperatures of PLA films and fibres during soil burial in the field in Spata and at laboratory.
654 E. Rudnik, D. Briassoulis / Industrial Crops and Products 33 (2011) 648–658
70
60
Crystallinity, %
50
40
30
20
10
0
0 1 3 5 7 9 11
Time, months
PLA 20 PLA 30 PLA 40 PLA 50 PLA 75 PLA fib
Fig. 8. Crystallinity of PLA films and fibres during soil burial in the field in Spata.
of soil burial the carbonyl index decreased from 3.24 to 2.44 and
from 3.6 to 3.5, respectively for PLA 30 and PLA 75 films. The
carbonyl index was calculated as the ratio of the intensity of the
1748 cm−1 carbonyl peak in the FTIR spectrum to a reference peak
(1451 cm−1 ). These changes, i.e. no significant shifts or formation of
new bands suggest that while slow hydrolysis of ester bonds pro-
ceeds, no degradation by-products were emerged on the surface of
the specimens.
Fig. 9. Photos of PLA 30 (a), PLA 75 (b) and PE film (c) samples after 11 months of soil burial at the laboratory.
E. Rudnik, D. Briassoulis / Industrial Crops and Products 33 (2011) 648–658 655
45
40
35
Temperature,ºC
30
25
20
15
10
0
1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41 43 45 47 49
Time, days
Temperature outside Temperature inside 1 Temperature inside 2
biotic–abiotic conditions and mild Mediterranean climatic condi- after 11 months of burial. However, the PLA films become brittle as
tions. For north climatic conditions, it was observed by Gallet et al. in the case of the field experiments and creased with some cracks
(2001) that thermal properties of PLA films (glass transition and indicating initiation of mechanical degradation (hydrolysis stage)
melting temperatures) were affected only during the second year of the material. Similarly, small samples (size 2 cm2 ) destined to
of soil burial in south Finland. This behaviour may be explained by determine mass loss remained optically unchanged. No mass loss
the phenomenon observed by Shi and Palfery (2010) that when the was observed for PLA films during the soil burial trial at the labora-
degrading temperature is below PLA glass transition temperature, tory. No visible degradation traces were seen for the studied fibres
sample degradation is slowed. either. Obviously, PE film used as negative reference did not change
at all.
3.3. Laboratory test results Fig. 10 shows the effects of burial time on the mechanical
properties of PLA 30 and PLA 75 films. Both, tensile strength and
Photos of samples taken during biodegradation under simulated elongation at break decreased during soil burial. For PLA 30 film
soil burial conditions are given in Fig. 9. First changes for filter the tensile strength decreased up to 1/3 the initial value (16.1 MPa)
paper (cellulose) used as positive reference were seen already after after 7 months, while the tensile strength of the thicker PLA 75
1 month. Some small fragments remained in the soil. After 3 months sample decreased to a smaller extent, i.e. up to 5/6 the initial value
of soil burial at the laboratory cellulose disintegrated completely. (48.4 MPa), exhibiting a large variability during its burial in soil
On the contrary PLA 30 and PLA 75 films were not disintegrated period. The elongation at break of the PLA samples suffered a more
Fig. 12. Tensile properties changes during composting for PLA 30 film.
656 E. Rudnik, D. Briassoulis / Industrial Crops and Products 33 (2011) 648–658
Fig. 13. Photos of cellulose (positive control) (a; 1, 3, 7 weeks) and PLA 30 (b; 3 weeks, 8, and 11 months) during composting studies.
drastic reduction, a behaviour analogous to the one observed with 3. Cooling (called second mesophilic phase) and maturation phase.
the samples exposed under real field conditions. From the begin-
ning of the laboratory simulated soil burial the values of elongation The highest temperature is reached during the thermophilic
at break of both PLA films decreased dramatically. After 1 month phase (35–65 ◦ C), when thermophilic bacteria and fungi take over,
of burial the elongation at break decreased already from 17.5% and the degradation rate of the waste increases. After the easily
down to 1.3% and from 3.5% down to 1.8%, for PLA 30 and PLA 75, degradable carbon sources have been consumed, the compost starts
respectively. For the thinner PLA 30 film the effect of soil burial to cool. After cooling, the compost is stable. Mesophilic bacteria and
on the degradation, measured by the tensile properties, is more fungi reappear, and the maturation phase follows.
pronounced as compared with thicker PLA 75 film. The tensile prop- Temperature profiles, i.e. temperature outside as well as tem-
erties of the PE film were not affected during the simulated soil perature inside the compost bin (2 sensors) measured during
burial laboratory experiments. It is noteworthy that after 7 months biodegradation of PLA 30 films under home/farm type Mediter-
simulated burial under laboratory conditions PLA samples were ranean composting conditions in the present study are shown
too brittle to determine mechanical properties. It was difficult to in Fig. 11 (daily averages). Water content was in the range
cut the specimens for mechanical testing. In general, PLA samples 45–60%. The highest temperature was recorded during the
buried in soil under real field conditions degraded faster than those first week of composting then the second mesophilic phase
tested under laboratory conditions. This is indicated by the faster proceeded.
decrease of the elongation at break values of most PLA films buried Solvita respirometric tests confirmed the temperature profile
in the field under Mediterranean conditions that become too brittle of the compost medium. Solvita compost maturity test index at the
to cut specimens even after only one month of burial. This explains beginning of the experiments was 3, indicating active compost with
also the higher degree of disintegration observed for the samples the fresh ingredients. After 7 weeks of composting the condition of
exposed under real filed conditions as compared to the samples the compost changed and the compost was moving past the active
exposed to the simulated laboratory conditions. phases of the decomposition and was ready for curing (value of
The measurement of biodegradation through the BOD based Solvita maturity index increased to 5).
respirometric method confirmed that the tested PLA materials were The tensile properties of PLA 30 film samples taken during vari-
almost not degraded at 30 ◦ C after 20 days of incubation (Rudnik ous composting phases are presented in Fig. 12. The tensile strength
and Briassoulis, 2011). Biodegradation of PLA films and fibres was of the PLA 30 film did not change significantly during 7 weeks of
at a rather low level of about 10%. Further, PLA fibres degraded more composting except during the last week when the tensile strength
slowly in comparison with PLA films. reduced to 2/3 the initial value. However, a major decrease in elon-
gation at break, down to 1/8 the initial value, was observed already
after 1 week of composting. Then the low elongation at break value
3.4. Composting studies results
reaches a plateau.
The exposure of the PLA films to home composting conditions
Composting refers to a biodegradation process of a mixture of
revealed that the elongation at break values decrease drastically
organic substrates carried out by a microbial community composed
and abruptly already after 1 week of exposure, while the tensile
of various populations in aerobic conditions and in solid phase
strength values decrease gradually and only after one month of
(Rudnik, 2008; Diaz et al., 2007). The exothermic process produces
exposure. It is noteworthy that the high sensitivity of the elon-
energy in the form of heat, which results in an increase of the tem-
gation at break property follows the same pattern under both
perature in the mass. Composting process proceeds in three phases
Mediterranean soil and composting environments, with a dras-
(Rudnik, 2008; Diaz et al., 2007):
tic reduction of the elongation at break during the early stage of
biodegradation. It appears that during the first stage, the prelimi-
1. Mesophilic phase. nary steps of the hydrolysis mechanism induce degradation of the
2. Thermophilic phase. mechanical properties of the material leading to serious embrit-
E. Rudnik, D. Briassoulis / Industrial Crops and Products 33 (2011) 648–658 657
tlement under both, soil and composting conditions. This early Acknowledgments
embrittlement phenomenon, affecting predominantly the elonga-
tion at break value, has also been observed and reported for several The work has been carried out under the project BIODESOPO
biodegradable materials exposed to open field conditions during funded by the European Commission (Marie Curie Fellowship of
their useful life-time, through monitoring of the evolution of their Dr. Ewa Rudnik).
mechanical properties before their burial in soil (i.e. degradation Dr. Ewa Rudnik expresses her thanks to Mr. D. Giannopoulos for
under UV radiation, etc.) (Briassoulis, 2006, 2007). his help during experiments.
Photos taken during composting are shown in Fig. 13. First
changes due to degradation can be observed for filter paper (cellu-
lose) already after 1 week of composting. Then degradation process References
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