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Biodegradability and Compostability of Lignocellulosic Based Composite Materials
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Biodegradability and Compostability of Lignocellulosic
Based Composite Materials
Sudhakar Muniyasamy1, Andrew Anstey2, Murali M. Reddy1, Manju Misra1,2 and Amar Mohanty1,2,*
1
Bioproducts Discovery & Development Centre (BDDC), Department of Plant Agriculture, Crop Science Building, University of Guelph,
Guelph, N1G 2W1, Ontario, Canada
2
School of Engineering, Thornbrough Building, University of Guelph, Guelph, N1G 2W1, Ontario, Canada
Received April 9, 2013; Accepted August 14, 2013; Published online August 14, 2013
ABSTRACT: Lignocellulosic composites have attracted interest from both academia and industry due to their
beneficial environmental and sustainability attributes. The lignocellulosic industry has seen remarkable
improvements in the development of composites for high performance applications. Both biodegradable as
well as non-biodegradable polymers are used in the design and engineering of lignocellulosic composites.
Biodegradability studies of lignocellulosic composites in soil and composting environments help in planning
their end-life management. Biodegradability tests are complex and dependent on the environment in which
the testing is carried out. Due to this, standards have been developed by international agencies such as the
American Society for Testing and Materials (ASTM) and International Organization for Standardization (ISO)
to adopt and test plastic materials in both composting and soil environments. The first part of this intended
review article deals with the classification of lignocellulosic composites, biodegradation and composting
concepts, biodegradability testing standards, and factors affecting biodegradation. A comparative analysis
of ASTM and ISO biodegradability standards in terms of testing methodology and results interpretation is
provided.. A special focus is given to the biodegradation mechanisms found in polymers and their composites.
The second part of this review article is devoted to biodegradation studies of lignocellulosic composites
under composting conditions and soil environments. The effect of filler type, environmental conditions, and
compatibilization on the biodegradation of lignocellulosic composites is discussed in detail. Also, a special
section on the biodegradability of lignin-based materials is given.
KEYWORDS: Biodegradation, compostability, lignocellulose, biocomposites
1 INTRODUCTION lignocellulosic fibers have a major role to play, and

the polymer composite industry is undergoing a
Lignocellulosic fibers are increasingly being used as remarkable transformation in adopting lignocellu-
fillers and/or reinforcing agents in the design and losic fibers. This approach will also help the agricul-
development of polymer composites. The renewabil- tural community, as most of the lignocellulosic fibers
ity, low cost, rigidity and low abrasiveness of these used in composites can be obtained from agricultural
fillers have made them attractive natural materials in by-products. Forestry resources like wood also play
the plastic industry. Furthermore, increased consumer a significant role in lignocellulosic fiber-based com-
demands for materials for high performance applica- posite uses.
tions have led manufacturers to adopt technological Lignocellulosic fibers can be classified as primary
advances to meet these demands. Rising oil prices, and secondary fibers based on their usage and utili-
depleting natural resources and increased environ- zation. Primary fibers are fibers from purpose-grown
mental concerns can be circumvented through the plants, including jute, sisal, kenaf, flax and hemp.
use of annually renewable materials. In this regard, Secondary fibers are fibers obtained as by-products of
*Corresponding author: mohanty@uoguelph.ca
DOI: 10.7569/JRM.2013.634117
J. Renew. Mater., Vol. 1, No. 4, November 2013 © 2013 Scrivener Publishing LLC 253
Sudhakar Muniyasamy et al.: Biodegradability and Compostability of Lignocellulosic DOI: 10.7569/JRM.2013.634117
plants, including agro-residues, coir fibers, and pine- 2 LIGNOCELLULOSIC MATERIALS

apple fibers. There are several types of lignocellulosic AND THEIR COMPOSITES
fibers which are as follows: bast fibers (flax, jute, hemp,
kenaf, etc.), leaf fibers (sisal, pineapple leaf fiber), seed Lignocellulosic materials are materials that contain
fibers (cotton, coir), grass (switchgrass, miscanthus, both lignin and cellulose. They are also known as pho-
etc.), reed fibers (wheat, corn and rice) and other types tomass, due to the fact that they are obtained as a result
(wood and roots) [1]. of photosynthesis. Wood, grasses, plant and agricul-
Lignocellulosic polymer composites have advanced tural residues are the most common resources of ligno-
significantly from the times of simply mixing plastics cellulosic materials. Lignocellulosic materials generally
and fibers and characterizing their properties. Today, lack consistent, uniform and reproducible properties
more and more biobased plastics are being adopted in and composition. However, they offer many advan-
designing lignocellulosic composites, and these devel- tages in the design and engineering of polymer com-
opments are mirrored by a corresponding growth in posites because of their renewability, low abrasiveness,
the market. The worldwide bioplastic industry capac- load bearing capacity, and biodegradable nature [1]. In
ity was projected by European Bioplastics to increase addition, these composites can be cost competitive and
over a 5-year period to 5.8 million tons per year by have applications in various sectors, including the pro-
2016, a significant increase from the 1.2 million tons duction of durable and biodegradable products.
produced in 2011 [2]. Upcoming biobased plastics, Lignocellulosic composites are defined as polymer
such as bio-PE and biobased PET, account for a sig- composites in which lignocellulosic materials are major
nificant portion of the world’s bioplastic production. fillers. They are classified into two types based on their
The biobased PET makes up around 40% of the mar- biodegradability in soil and composting facilities as
ket, and is projected to control 80% of global produc- shown in Figure 1 (as represented on left-hand side):
tion by 2016 [2].
Lignocellulosic fibers are naturally biodegradable 1. Non-biodegradable lignocellulosic composites:
in both soil and composting environments. A biode- Lignocellulosic composites belonging to this cate-
gradable material is one that is able to break down, gory can be made up of both petro and/or renew-
or degrade, through the action of biological factors able polymers, but they are not biodegradable in
such as fungi and bacteria. However, their biodeg- either soil or composting facilities. For example:
radation rate depends on their composition. For polypropylene-natural fiber composites, bio-
example, a high lignin content is detrimental to the based nylon-natural fibers composites, etc.
biodegradation of the fibers in composting environ- 2. Biodegradable lignocellulosic composites:
ments. Biodegradation of plastics and lignocellulosic Lignocellulosic composites belonging to this
composites is a topic of interest for both industry category can be made up of both petro and/
and academia. There are a large number of factors or renewable polymers. They are biodegrad-
that affect the biodegradability and chemical prop- able in either soil or composting facilities. For
erties of such materials, and there exists a suitably example: poly(lactic acid)-natural fiber compos-
extensive infrastructure to standardize the classifi- ites, poly(butylene adipate-co-terephthalate)-
cation of these materials. Both of these factors will natural fiber composites, etc. It is well known
be discussed in great detail throughout this review that PLA is a renewable resource-based polymer,
article. while PBAT is a petro-based polymer.
Non−
biodegradable Based on Based on Lignocellulosic
Lignocellulosic Biodegradability Polymer Matrix Biocomposites
Composites
Lignocellulosic
Composites
Biodegradable Lignocellulosic
Lignocellulosic Whole Green
Composites Composites
Figure 1 Classification of lignocellulosic composites.
254 J. Renew. Mater., Vol. 1, No. 4, November 2013 © 2013 Scrivener Publishing LLC
DOI: 10.7569/JRM.2013.634117 Sudhakar Muniyasamy et al.: Biodegradability and Compostability of Lignocellulosic
In another concept on the origin of polymer matrix, biodegradability of the resulting composites can be
lignocellulosic composites can also be classified into two changed in comparison to the base polymer. Just as
types: lignocellulosic biocomposites and lignocellulosic with pure polymer materials, the true biodegradabil-
whole green composites (Figure 1, right-hand side): ity of polymer composites (in terms of rate of degra-
dation and toxicity for safe disposal in environmental
1. Lignocellulosic biocomposites: Lignocellulosic conditions) must be evaluated using specific standard-
composites belonging to this category are ized testing methods [5, 7]. These tests cover a broad
made up of petro-based polymers, but their scope of conditions in order to accommodate all types
biodegradability in either soil or composting of plastics, and the various environmental conditions
facilities depends on their polymer matrix. For they could be exposed to as plastic waste. Thus, with
example: polypropylene-natural fiber com- continuous development and innovation in the bio-
posites (non-biodegradable), poly(butylene polymer industry, these standard test methods for
adipate-co-terephthalate)-natural fibers com- evaluating the biodegradability of polymeric materi-
posites (biodegradable), etc. als are essential to the future of the plastics industry,
2. Lignocellulosic whole green composites: and will be necessary to reduce the global issue of
Lignocellulosic composites belonging to this plastic pollution.
category are made up of renewable resource-
based polymers, but their biodegradability in
either soil or composting facilities depends on
2.1.1 Definition and Concept
their polymer matrix. For example: poly(lactic Biodegradation is defined as a process in which mate-
acid)-natural fiber composites (compostable), rials undergo chemical changes due to the action of
biobased nylon-based composites (non-biode- enzymes that are secreted by living organisms (bacte-
gradable), etc. ria, fungi and algae). The process of biodegradation is
comprised of two phases, including the initial phase
This intended review article discusses the biode- (primary biodegradation) and the secondary phase
gradability of biodegradable lignocellulosic compos- (ultimate biodegradation). During the initial phase,
ites in both soil and compositing environments as a polymer undergoes significant weight loss, reduc-
mentioned below. tion in molecular weight and fragmentation, and is
degraded into soluble low molecular weight com-
2.1 Biodegradable and Compostable pounds. The second phase of biodegradation is the
Polymeric Materials ultimate conversion of primary degraded low molecu-
lar weight compounds into CO2, water and cell bio-
Because of the dependence of biodegradation on both mass (in aerobic conditions), and CH4, CO2 and cell
polymer structure and environmental factors, a wide biomass (in anaerobic conditions). The primary and
range of tests are required to fully quantify the biodeg- ultimate biodegradation must occur at specific times
radability of a given plastic [3, 4]. To ensure a global with specific rates under biological environmental
standard of plastic biodegradability, standardized conditions (soil, compost, aqueous, anaerobic diges-
testing procedures have been defined by international tate) in order to prevent the accumulation of plastics
organizations, such as the International Organization in the environment.
for Standardization (ISO) [5, 6] and American Society The American Society for Testing and Materials
for Testing and Materials (ASTM) [7]. These organiza- (ASTM) and the International Organization for
tions define and regulate a number of standard tests Standardization (ISO) define:
that are used to properly assess biodegradable poly-
mers and encompass a variety of environmental fac- i. Degradation as “an irreversible process leading
tors. The definition of these biodegradability tests to a significant change of the structure of a mate-
was established by the ISO [5, 6, 8]. For biodegradable rial, typically characterized by a loss of proper-
plastics, these factors include humidity, temperature, ties (e.g., integrity, molecular weight, structure
pH level, oxygen presence, and most importantly, the or mechanical strength) and/or fragmentation.
presence of microorganisms (both in compost and Degradation is affected by environmental condi-
soil). Each factor affects the rate of degradation, and tions and proceeds over a period of time compris-
changing them could have a major effect on the result ing one or more steps” [9, 10].
of the experiment; as a result, these factors must be
According to the ASTM definition [7]:
closely monitored for accurate testing.
Through the addition of natural fiber to the bio- ii. Biodegradable plastic is “a degradable plastic
degradable polymer, the polymer properties and in which the degradation results from the action
of naturally occurring microorganisms such as lifetime of a polymer can be controlled with the use of
bacteria, fungi and algae.” additives or chemicals in order to suit various practical
iii. Compostable plastic is “a plastic that under- applications. Hydrolytic biodegradation is the mecha-
goes biological degradation during composting to nism for some naturally occurring biopolymers like
yield carbon dioxide, water, inorganic compounds polysaccharides and proteins, plant source polymers
and biomass at a rate consistent with other known such as poly(lactic acid) (PLA), and poly(butylene
compostable materials and leaves no visually distin- succinate) (PBS) and microbially-synthesized poly-
guishable or toxic residues.” mers like poly(3-hydroxybutyrate-co-3-hydroxyvaler-
ate) (PHBV) [13]. Many factors, such as chemical
The aforementioned standard guideline definitions bonds, type of co-polymer, thickness, water uptake and
have been given to establish and identify biodegrad- morphology can influence the rate of hydrolytic degra-
able polymeric materials or products. Based on these dation in enzyme-mediated or non-enzyme-mediated
guidelines, ASTM standards have provided various conditions. Comparing hetero-chain and carbon chain
test methods to evaluate the potential biodegradabil- polymers, the carbon backbone polymers biodegrade
ity of polymeric materials and products in various dis- more slowly [13]. The degradation mechanism of car-
posal environmental conditions such as soil, compost, bon backbone polymers is chemical degradation via
marine water and sewage. In the case of compostable oxidation or oxidative enzyme-mediated degradation.
plastics, the polymeric organic carbon must be con- Several naturally occurring biopolymers, such as natu-
verted into CO2, water and cell biomass within 180 ral rubber and lignin, undergo oxidative biodegrada-
days [11, 12]. tion. The process of oxidative polymer biodegradation
may take years, significantly more time than hydro-
2.1.2 Factors Affecting the Biodegradability lytic biodegradation.
of Plastics
The rate and degree of biodegradation of plas- 2.2.1 Hydrolytic Biodegradation
tics is mainly dependent on various factors such as Hydrolytic biodegradation occurs in polymers that
active microbial species present in environments, contain hydrolyzable groups, such as polysaccharides,
temperature, humidity, oxygen presence, pH level, polyesters and polyamides, when they are exposed to
UV radiation and polymer properties (crystallinity, moisture in biotic environmental conditions. The bio-
hydrophobicity, molecular weight, etc.). The biodegra- degradation of aliphatic polyesters is similar to the
dation behavior of plastics is mainly associated with biodegradation of cellulose and chitin via enzymatic
their chemical structure along with their physical and hydrolytic degradation. It has been reported that a
chemical properties. Both the physical and chemi- group of esterase enzymes is responsible for the hydro-
cal properties of plastics can influence the polymer lytic degradation of aliphatic polyester groups [15].
biodegradation mechanism. Such properties include Esterase enzymes, such as lipase, have been well stud-
surface area, hydrophobic and hydrophilic nature, ied, and are more capable of hydrolyzing aliphatic pol-
chemical nature, molecular weight, molecular weight yesters than aromatic groups [16]. Esterase enzymes are
distribution, crystallinity, crystal structure, glass tran- proven to hydrolyze triglycerol into fatty acid and glyc-
sition temperature, melting temperature and elastic- erol. The main reason for this kind of degradation is that
ity [3]. These physical and chemical properties play the active site of lipase is more in contact with the main
important roles in the polymer biodegradation process chain of the polymer, due to the hydrophilic nature of
in different environmental conditions. the aliphatic polyester, rather than the aromatic polyes-
ter, which is hydrophobic. These enzymatic reactions
2.2 Biodegradation Mechanisms are heterogeneous; the hydrolytic enzymes adsorb onto
the surface of the substrate polymer through the bind-
in Polymers ing site of the molecules, then the hydrolytic enzymes
Polymers contain either a hetero-chain or carbon back- directly contact the ester bond to break it down into
bone. The degradation mechanism of hetero-chain functional group molecules. Each group of hydrolytic
backbone polymers is chemical degradation via hydrol- enzymes has a specific active binding site for substrate
ysis, or enzyme-catalyzed hydrolysis [13]. Hydrolytic molecules, determined by the binding capacities of
biodegradation mainly depends on the hydrolytic the substrate. These enzymes can hydrolyze polymers
enzymes secreted by local microorganisms and the into low molecular weight compounds, which are
physico-chemical properties of the polymer. Through then capable of undergoing bioassimilation processes
this process, polymer biodegradation may occur with the aid of naturally occurring microorganisms.
within a month [14]. The hydrolytic biodegradation It has been shown in extensive studies that biobased
polymers such as starch, cellulose, poly(lactic acid) According to the ASTM D6400 standard specifica-
(PLA), polyhydroxybutyrate (PHB), chitin, protein, and tion [7], in order for the compostable plastics and their
petro-based polyesters like poly(caprolactam) (PCL) products including packaging made from plastics to
and poly(butylene adipate-co-terephthalate) (PBAT) be considered “compostable in municipal and indus-
readily undergo biodegradation under composting trial composting facilities,” the following key require-
conditions [17–19]. ments must be satisfied for labeling and marketing
products.
2.2.2 Oxidative Biodegradation
1. The polymeric carbon must be converted into
Oxidative degradation occurs when polymers contain- CO2, water and cell biomass by the action of
ing oxidizable groups, such as lignin, natural rubber, natural microorganisms such as bacteria and
poly(vinyl alcohol) and polyolefins, are exposed to fungi.
either abiotic or biotic environmental conditions. The 2. The biodegradation rate shall be comparable
oxidized biodegradable compounds are further assim- to the similar biodegradation rates of natural
ilated by microorganisms [20–22]. Lignin is an exam- materials such as leaves, paper, grass and food
ple of a natural polymer that, like cis-polyisoprene, scraps.
cannot biodegrade through a hydrolytic process, but 3. The compostable plastics should be disinte-
instead biodegrades slowly by the oxidative attack of grated during the biological treatments.
extracellular peroxidases produced by fungi and actin- 4. The final quality of compost produced should
omycetes [23]. not have any harmful effects.
Both hydrolytic and oxidative degradation share
the same purpose: to break the polymer into fragments According to ISO/DIS 17088 international stan-
small enough to pass through the cell membrane of dard, the biodegradable plastic is designed for recov-
the active microorganism [19, 24–26]. These fragments ering through aerobic composting process, and the
enter the microorganism and are metabolized. In the following four criteria must be addressed:
case of aerobic biodegradation, this process yields a full
decomposition of the polymer into carbon dioxide and 1. Biodegradation (conversion carbon into
water [3, 27]. In anaerobic biodegradation, carbon diox- CO2, water and cell biomass by natural
ide, water and methane are produced from the polymer. microorganisms).
This process is called mineralization. It is the final step 2. Disintegration of compostable plastics during
in biodegradation, and this means that the active micro- microbial treatment.
organisms utilize carbon sources from the polymeric 3. No negative impacts on these biological
carbon as a nutrient. processes.
4. No toxic effects on the final quality of compost
2.3 Standards for Testing (including in the presence of metal and other
Biodegradability in Composting harmful ingredients).
Environment
European standard EN 13432 is the most relevant
The standards relating to the compostable plastics have standard in all European countries and is valid in all
been developed by various international bodies such EU member states. This standard specifies that the
as CEN (European Committee for Standardization), compostability and anaerobic treatability of packag-
ASTM (American Society for Testing and Materials), ing waste including products produced from plastics
ISO (International Standards Organization) and must have the following characteristics:
the Japan BioPlastics Association. Some of the most
widely adopted standards for biodegradation of poly- 1. Biodegradability
mers are EN 13432, ASTM D6400, ISO/DIS 17088 and 2. Mineralization during biological treatment
JISK 6953. These standards from these organizations (microbial enzymatic process)
are intended to identify the polymeric materials and 3. No adverse effects on biological processing
their related products which undergo biodegradation 4. No harmful effects on the final quality of
to their specified standards. compost
According to the European Directive on packaging
and packaging waste [28], the packaging waste pro- Biodegradable plastics in Japan are identified under
cessed through composting must be biodegradable the GreenPla identification system which is monitored
in nature and it should not hinder any unrecoverable by the Japan BioPlastics Association (JBPA). GreenPla
materials. is the nickname for biodegradable plastics. GreenPla
14855–2 are tests of biodegradation in compost; ISO

14855–1 analyzes the amount of CO2 evolved using a
Compostability general method, while ISO 14855–2 requires the evolved
CO2 to be measured gravimetrically. According to ISO
Biodegradability Disintegration 14855–1, a maximum of 100 grams of sample and 600
grams of inoculum are required for one-test sample
measurements. Conversely, only 10 grams of sample
No toxic effects are required according to ISO 14855–2. According to
the ISO 17088 standard guidelines for a material to be
Material characterization & considered a compostable plastic, the conditions of one
chemical characterization of ISO 14855–1, ISO 14855–2 or ASTM D5338 must be
satisfied (Table 1).
According to the European Norm (EN) standards
13432 and 15351 [28, 35], biodegradability is the abil-
Figure 2 The criteria of compostability. ity of a compostable material to be converted into
CO2 through the action of microorganisms. This
property is measured with the laboratory standard
test method EN 14046. This standard test method is
considers both the treatment and final disposal of similar to the ISO 14855, another biodegradability
the plastics in understanding and certifying the bio- test that applies controlled composting conditions.
degradability. GreenPla is ultimately degraded into For a material to claim complete biodegradability,
water and carbon dioxide. JIS K 6950, 6951, 6953, 6955 it must biodegrade by at least 90% within 180 days.
are the standards used by JBPA [29–33]. The following In the same test, there must be evidence of no visual
are the requirements for GreenPla certification: pollution, such as fragmentation and disintegrability,
in the final compost within 90 days. Table 1 gives a
1. All constituents of the product must be dis- comparison of ASTM, ISO, and EN compostability
closed to JBPA and be on the positive list. standards in terms of mineralization, disintegration
2. Product must pass the JBPA’s standards. and eco-toxicity.
In general, the criteria of compostability are similar 2.3.1 Composting Process and Methods
in all standards and are represented in Figure 2.
According to the US Environmental Protection The composting process of organic materials can be
Agency (EPA), composting is a biological process accomplished using three basic methods: 1) in-vessel
decomposing of organic material in an aerobic envi- methods, 2) aerated static pile methods, and 3) wind-
ronment to convert it into the form of humus-like row methods [37, 38]. In the in-vessel methods, the
material [34]. Organizations such as the ASTM, ISO organic materials are processed in a covered container
and European Normative (EN) are involved in estab- or open channel process. These processes are closely
lishing the standard test methods for materials, sys- monitored to ensure that they are well aerated with
tems, products and services for both producer and proper humidity conditions, and are mechanically agi-
consumer consumption. These standard techniques tated at a frequent, consistent time interval. The aer-
mainly cover the required criteria to claim materials ated static pile method uses forced air to form piles
as environmentally biodegradable and compostable of compostable material. This pile is not mechanically
(Table 1). The ASTM standard D6400 [7] defines turned or mixed. The windrow method uses elongated
compostable plastic as one that undergoes biologi- piles of compostable material which are regularly
cal degradation when exposed to controlled com- mechanically turned. In order to achieve a successful
posting conditions to produce CO2, H2O and new composting process, the composting microorganisms
cell biomass at a consistent rate, and leaves no toxic must proceed with the following phases: i) mesophilic
residues. phase, ii) thermophilic phase, and iii) cooling and mat-
The ISO standards ISO 14855–1 and ISO 14855–2 uration phase [39].
[9, 10] define composting as “autothermic and ther-
mophilic biological degradation of biowaste (organic 2.3.1.1 Mesophilic Phase
waste) in the presence of oxygen under controlled con- The mesophilic phase occurs in the beginning of
ditions by the action of micro- and macro-organisms the composting process and extends up to 45°C.
in order to produce compost.” ISO 14855–1 and ISO Mesophile microorganisms are active during this
Table 1 Comparison of standards relating to specification for compostable plastics [6, 8, 9, 36, 37].
Standard Test Results

ASTM D6400 Mineralization:
• For products consisting of a single polymer (homopolymer or random copolymer), 60% of the
organic carbon must be converted to carbon dioxide by the end of the 180 day test period when
compared to the positive control.
• For products consisting of more than one polymer (copolymer of either block copolymer or seg-
mented copolymer, blends, and addition of low molecular weight additives), 90% of the organic
carbon must be converted to carbon dioxide by the end of the test period within 180 days, when
compared to the positive control.
• Organic constituents present more than 1% shall be individually tested.
Disintegration:
• No more than 10% of polymer original dry weight may remain after sieving after 84 days in con-
trolled laboratory conditions.
Eco-toxicity:
• There must be no adverse impact on the ability of compost (after testing) to support plant growth
and low levels of heavy metals as described in these standards [28, 36].
ISO 17088 Mineralization:
• For products consisting of a homopolymer, 60% of the organic carbon must be converted to carbon
dioxide within 180 days. For all other polymers (e.g. copolymer or blends), 90% of the organic car-
bon must be converted to carbon dioxide within 180 days.
Disintegration:
• No more than 10% of its original dry mass remains after sieving on a 2 mm sieve after 84 days in
controlled composting test.
Eco-toxicity:
• Low levels of heavy metals as described in these standards [28, 36].
• A minimum of 50% volatile solids (according to APHA 2540G standards).
• Ecotoxicological assessment (plant growth test on two different plant species following modified
OECD guideline).
EN 13432 Mineralization:
• Biodegradation level of at least 90% must be reached in less than 6 months, either from biowaste and
packaging like paper products and biodegradable plastics.
Disintegration:
• No more than 10% of the residues from the packaging waste fragments after sieving on a 2 mm sieve
after 84 days in controlled composting test.
Eco-toxicity:
• Result should show low levels of heavy metals as described in these standards [28, 36].
• Should meet physical chemical analysis of the resulting compost and ecotoxicological assessment
(plant growth test on two different plant species) according to OECD guideline as described in these
standards [28, 36].
stage of composting. At this stage of the composting to the protein degradation and release of NH3, the pH
process, the active mesophilic bacteria and fungi are level starts to rise to a maximum 8–9. The duration of
capable of degrading soluble low molecular weight this phase may occur between a few hours to a few
organic compounds such as starch, monosaccha- days [13].
rides and lipids. During this phase, the bacteria pro-
duce organic acids and the compost starts to slightly 2.3.1.2 Thermophilic Phase
decrease in pH from 5.5 to 5.0. At the same time, the The thermophilic phase occurs when the compost
exothermic degradation process causes the compost reaches temperatures above 40°C. During the thermo-
temperature to rise rapidly. During this period, due philic phase, the higher temperatures accelerate the
breakdown of proteins, fats and carbohydrates like and maturation phase, Actinomycetes grow rapidly.
cellulose, hemicelluloses and other complex structural Anaerobic bacteria may also be present in small num-
compounds. In this phase only, thermophilic bacteria bers in the compost environment. When the oxygen
and fungi are more responsible for the higher degrada- content is rapidly consumed, anaerobic microorgan-
tion of organic materials. At temperatures exceeding isms may develop during the thermophilic phase. It
55–60°C the microbial activity and diversity decrease has been found that various protists and large spe-
dramatically, due to thermophile microorganisms cies of microorganisms, including springtails, milli-
being unable to survive above this temperature. This pedes, mites, ants, beetles, centipedes, spiders, and
phase can range significantly in length, from a few worms are present in the maturation phase of the
days, up to several months. During this phase, the pH compost.
is stabilized to a neutral level.
2.3.3 Composting Conditions
2.3.1.3 Cooling and Maturation Phase
In order to monitor the biodegradability of plastic
As the higher energy compounds have been exhausted materials and their composite materials from natural
by the degradation of thermophilic bacteria, the and synthetic origin under composting conditions,
compost becomes cool and mesophilic bacteria and the following optimization of compost is required for
fungi start to reappear to start the maturation phase. studying in a laboratory setting. The compost inocu-
The mesophiles thrive in low temperatures and will lum is screened to less than 10 mm by sieving and man-
become active once the compost becomes cool. During ually removing and discarding any large inert items
this phase, most of the species may differ from those (pieces of glass, stone, wood, etc.). Table 2 presents
present in the first mesophilic phase. The biological the required physical-chemical properties of compost.
processes decline, but the compost continues to be The total dry solids (weight %) is determined by the
humified and matures. amount of solids present in the compost when meas-
The above three phases have been identified in all ured after drying it at 105°C for 10 hours. The amount
composting processes. Based on these phases, the role of total volatile solids is determined by heating the
of microorganisms and the conditions involved in total dry solids after evaporating the moisture content
organic carbon degradation under composting condi- at 550°C for 30 minutes. It is necessary to characterize
tions have been evaluated. Based on these biological the compost quality, including total nitrogen and car-
organisms, various standard test methods have been bon content, by elemental analysis. The C/N ratio in
established for plastic waste disposal in municipal the mix can be adjusted with ammonium chloride if it
composting and industrial composting conditions. is more than 40% [34].
Among these conditions, studies have shown indus-
trial composting conditions are more favorable for
plastic waste disposal [14].
Table 2 Physical-chemical properties of compost.
2.3.2 Microorganisms Analysis ASTM D6400 Methods
During the composting process, different species of requirements
microorganisms dominate at different composting Total Dry 50–55 APHA 2540D
phases [39–41]. During the mesophilic phase, the solids (%) and 2540E
microorganisms work to degrade any readily avail- pH 7–8 ASTM D12931
able low molecular-weight soluble compounds. At
this stage, the temperature starts to rise and the bac- Moisture (%) 50–55 APHA 2540D
terial growth rate declines. During this stage, mainly and 2540E
thermophilic bacteria of the genus Bacillus are acti- C/N ratio 1:10–1:40 Elemental
vated [42]. When the temperature rises to 55°C and analysis
above, many human and plant pathogens are killed Volatiles More than 30 APHA test
because of the high temperature. Fungi and bacteria solids (%) methods 2540
persist as the majority of the compost microorgan- D and 2540E
isms. Protozoa, larvae, and viruses also play a minor mg CO2 50–150 CO2 evolution test
role in composting. Other heterotrophic bacteria, emission/g
hydrogen-oxidizing bacteria, sulphur-oxidizing volatile solids
bacteria and denitrifying and nitrogen-fixing bacte-
ria are also present in this stage. During the cooling
Table 3 Comparison standards relating to the specification for biodegradation of plastics in soil.
Standard Test Method and Duration Biodegradation condition (mineralization)

ASTM D 5988- Analysis of evolved carbon dioxide from testing Biodegradation: No defined time duration for testing
96/2012 samples with time interval .The recommended materials.
frequency for analysis of carbon is every 3 to Validity of test: More than 70% theoretical CO2
4 days for the first 2 to 3 weeks and every 1 to evolution is observed for a reference material
3 weeks thereafter. This is characterized by (starch or cellulose) within 6 months.
titrations over a 6 month period.
ISO - 17556 Test samples oxygen demand or analysis of Biodegradation: No defined time duration for testing
evolved carbon dioxide over a 6 month period. materials.
Validity of test: (a) Degree of biodegradation is more
than 60% of reference material at plateau phase
or at the end of the test and (b) Biodegradation
values of, or amounts of carbon dioxide evolved
from, the two blanks are within 20% of the mean
at the plateau phase or at the end of the test
2.4 Standards for Testing This test method is designed to achieve an ideal extent
Biodegradability in Soil of biodegradation by providing sufficient aeration and
humidity to the soil environment. This respirometric
Plastics that are biodegradable in soil are defined as biodegradation test method is applicable to test all poly-
“degradable plastics in which the degradation results mers from natural and synthetic origin, copolymers or
from the action of naturally occurring microorganisms mixtures that contain additives such as plasticizers, col-
such as bacteria, fungi and algae” (i.e., real soil condi- orants or water-soluble polymers. Also, this test requires
tions) [43]. that the carbon dioxide output from the reference mate-
Table 3 presents the ASTM and ISO standards that rial should be more than 60% and for blank this should
are available for testing plastics in a soil environment. be 20% during both the plateau phase and at end of the
These test methods cover the determination of both test. Any deviations from these criteria shall be regarded
rate and degree of ultimate aerobic biodegradation of as an invalid test and a new test must be conducted.
polymeric materials in soil.
ASTM D5988–12 specifies a “standard test method
for determining aerobic biodegradation of plastic mate- 3 BIODEGRADATION OF
rials in soil,” and deals with the extent of biodegradation LIGNOCELLULOSIC COMPOSITES
over a time period in the microorganisms present in the
soil-mineralized plastics [11]. This standard determines A significant amount of research studies have been
the extent of aerobic biodegradation in soil using a mea- conducted to investigate the biodegradability of ligno-
surement of evolved carbon dioxide. Carbon dioxide cellulosic fiber-based biocomposites. In this research,
is an end product of biodegradation and evolves over both treated and untreated lignocellulosic fillers were
time. This standard requires the reference material to be used to change or modify the physico-chemical char-
at least 70% biodegraded within six months. Also, this acteristics of the polymer biocomposites. However,
test requires that the carbon dioxide output from blank research has not been well established in terms
samples should be around 20% during both the pla- of the ultimate biodegradability (mineralization).
teau phase and at the conclusion of the test. Such CO2 Biodegradation end products such as CO2, H2O and
emissions from blank samples in a composting test do cell biomass occur in aerobic conditions. In the case
not have threshold values at the conclusion of the test of anaerobic conditions, biodegradation end products
because validation is carried out within 10 days of the like CH4, CO2, H2O and cell biomass are produced [13].
test. Any deviations from these criteria shall be regarded Many studies have discussed the biodegradation of
as an invalid test, and a new test must be conducted. polymer composites in soil or compost, and reported
ISO 17556:2003 specifies “Plastics – Determination of their observation in terms of weight loss and change
the ultimate aerobic biodegradability of plastic materials in mechanical properties. Although useful, such obser-
in soil [44] by measuring the oxygen demand in a closed vations cannot provide an understanding of the com-
respirometer or the amount of carbon dioxide evolved.” plex processes involved in the biodegradation of these
biocomposite materials. There has been a wide range the biodegradation of composites prepared from 70%
of standardized test methods (ISO, ASTM and EN) PLA and 30% cotton cellulose fiber in composting con-
established to estimate the mineralization (aerobic ditions at 58 ± 2°C with a microbial oxidative degrada-
and anaerobic) of polymeric materials. These methods tion analyzer (MODA) system, following the standard
have emerged in part due to the development of more ISO-14855. The cotton fiber PLA composite showed
sensitive test equipment, such as respirometers, fully- higher rates of biodegradability (80% degradation in
closed circuit systems connected with CO2 and CH4 25 days) and was approaching the plateau phase when
sensors which automatically measure the end prod- the experiment concluded at 50 days, while the neat
ucts of these materials under aerobic and anaerobic PLA sample attained 80% degradability in 50 days.
conditions. Because of their suitability for the applica- This study indicated that the biodegradation of PLA
tion, respirometers are very commonly used to test the samples was enhanced by the presence of cellulose fib-
biodegradability of biopolymers and biocomposites. ers. In both studies [47, 48], PLA composites showed
a higher rate of biodegradability than the neat PLA
sample, but Funabashi and Kunioka [46] achieved
3.1 Effect of Fiber Content
neat PLA biodegradability in shorter times (80% 50
Lignocellulosic materials derived from various agro- days) than Way et al. [45] (90% in 90 days). The ana-
industrial, agri-food waste and agro-forestry feed- lyzed results showed that the slower rate of biodegra-
stocks have been widely utilized in the development dation was due to a d-content of 4.5% and 1000 ppm
of polymer composites. These renewable resource- Erucamide processing additive in the PLA of Way et al.
based materials can have a reduced environmental [45], while the PLA used by Funabashi and Kunioka
burden in comparison to non-renewable resource- [46] did not have any additives. The added additive
based plastic materials. The assessment of overall improves the adhesion of the matrix with fillers.
biodegradability of these biocomposites can reveal Pradhan et al. [49] studied and compared the aero-
the final environmental fate of their individual com- bic biodegradability of injection molded PLA-wheat
ponents during composting. Researchers investigated straw and PLA-soy straw biocomposites with 70–30%
the aerobic biodegradability of chemically treated and ratio of polymer to filler, as well as their constituent
untreated maple wood fiber in PLA-fiber composites materials. The study was done under composting con-
(70–30 wt%), in compost conditions according to the ditions, according to the standard ASTM D5338, by
standard procedure of ISO-14855 at a temperature using an acid-base titration procedure. The PLA com-
58 ± 2°C using a respirometric unit [45]. In this study, posites (PLA-untreated soy and PLA-wheat straw)
maple wood fibers were treated sequentially with showed 90% biodegradation in 70 days, while the nat-
several different treatments, including NaOH, NaOH ural biomass (untreated soy straw and wheat straw)
then acetylation, or NaOH then silanation. These attained 90% biodegradation in 45 days, and neat PLA
studies compared the CO2 emission from untreated reached 90% biodegradation in 100 days. This study
and treated wood fiber-PLA composites and charac- showed that the PLA biodegradation was facilitated
terized the composites using analytical techniques to by the natural biomass. The authors suggested that
understand the behavior of treated natural fiber in the these biocomposite strategies can help satisfy the
PLA composite. All treated (NaOH, acetylation and ASTM D6400 standard requirements of 90% degrada-
silane) wood fiber with PLA composites showed a tion in 180 days under composting conditions.
high extent of biodegradation (90% within 75 days), The comparative biodegradability of composites of
compared to the untreated PLA composite (90% in PLA-soy straw (70–30%), PLA-wheat straw (70–30%),
85 days) and neat PLA (90% in 90 days). The author PCL-distiller’s dried grains with solubles (70–30%) and
reported [45] that the higher rate of biodegradabil- PCL-soy meal (70–30%) were studied by Pradhan et al.
ity observed in the treated PLA composites is due to [50] under controlled composting conditions, with the
an enhanced rate of hydrolysis of the PLA polymer procedure adopted to follow ASTM D5338 using an
matrix. The test samples were further characterized acid-base titration procedure. This study showed PLA-
by gel permeation chromatography (GPC) analysis. soy straw and PLA-wheat straw composites attained
In treated (NaOH, acetylation and silane) compos- 90% biodegradability compared to the neat PLA biode-
ites, increasing the porosity of the fibers resulted in an gradability that occurred 50% in 70 days. PCL-distiller’s
increase in the rate and degree of biodegradation in dried grains with soluble and PCL-soy meal composites
the fiber via the removal of surface waxes and inter- showed 30% degradation in 65 days when compared to
nal hemicellulose structures. Most importantly, this the neat PCL degradation which was 25% in 65 days.
study showed that both untreated and treated wood All of the biocomposite results showed improved bio-
fiber-PLA composites are biodegradable in compost- degradation compared to the neat polymer used. The
ing conditions. Funabashi and Kunioka [46] analyzed rate of biodegradability of the PLA- and PCL-based
biocomposites was clearly shown to be better than Recently, studies were carried out by Muniyasamy
those of neat PLA and PCL. An increase in the biodegra- et al. [47] to analyze the aerobic biodegradability of bio-
dation rate was observed in their composites compared composites prepared from the petroleum-based poly-
to the neat polymers PLA and PCL. This higher rate of mer, poly(butylene adipate-co-terephthalate) (PBAT),
biodegradation is attributed to the presence of readily and bioethanol co-products such as water-washed
biodegradable materials such as soy straw, soy meal, distiller’s dried grains with solubles (wwDDGS). The
distiller’s dried grains with solubles and wheat straw. biocomposites were studied for their degradability
Biodegradability studies were carried out [51] on under controlled composting conditions according to
biocomposites prepared from 40% bio-flour (rice husk the standard ASTM D5338 by using a manual acid-base
flour filler) filled with 60% of the biodegradable poly- titration procedure. This study suggested that PBAT-
mer, poly(butylene succinate) (PBS). The authors stud- wwDDGS (70–30 and 80–20 ratios) biocomposites were
ied biodegradation test conditions simulated according sensitive to hydrolytic biodegradation, and the material
to the ASTM D 6003–96 under soil burial and aerobic showed 90% biodegradability in 120 days compared to
composting in municipal solid waste (MSW) for 80 neat PBAT, which achieved 90% biodegradability in
days [51]. These biocomposite materials were evalu- 180 days under the composting conditions used. The
ated in terms of percentage of weight loss, change in rate of biodegradation of PBAT-wwDDGS is similar
their mechanical properties before and after degrada- to that of cellulose and wwDDGS. In addition, ther-
tion, microbial colony count in test samples and surface mogravimetric analysis (TGA) and Fourier transform
morphology of the test samples. Based on the observa- infrared spectroscopy (FT-IR) analysis revealed that the
tions, by increasing the rice husk flour content from 20 biodegradation mechanisms of these PBAT-wwDDGS
to 40 wt% in the PBS matrix, the biodegradability rate biocomposites were hydrolytic. The decrease in ther-
of the biocomposites in terms of weight loss increased mal stability and ester group broadening of the PBAT
in both soil and compost environments, as compared matrix after composting incubation was due to enzy-
to neat PBS polymer. This study showed that bio-flour- matic hydrolysis and biodegradation. The mineral-
based PBS composites can be biodegraded faster in ization of the PBAT, wwDDGS, and PBAT-wwDDGS
compost than in soil environmental conditions. These composites under composting conditions were com-
results were further proven by the microbial colonies pared with standard cellulose as per ASTM D5338. The
present after the above biodegradation tests and mor- mineralization of cellulose has validated the test and
phology studies by scanning electron microscopy of compost quality. These results indicated that the use of
these biocomposite samples. The observed results indi- wwDDGS as a filler in a PBAT matrix can enhance the
cated that PBS biocomposites will have shorter survival biodegradability of the resulting biocomposites rela-
time in compost rather than landfills. tive to PBAT polymer matrix (Figure 3).
110
100
90
80
Biodegradation (%)
70
60
50
40
Cellulose
30
treated DDGS
20 PBAT
80/20 (PBAT/treated DDGS)
10 70/30 (PBAT/treated DDGS)
0
0 20 40 60 80 100 120 140 160 180 200
Incubation time (days)
Figure 3 Biodegradation profiles of hydro-biodegradable plastic materials and filter paper in respirometric compost tests. (From
reference [47] with permission).
In another study, Chiellini et al. [48] showed that method to measure gas emission from the test sam-
composite samples based on starch and poly(vinyl ples contained in a closed chamber. This instrument
alcohol) (PVA) presented a lower ultimate mineral- is highly adaptable to suit different standards (ASTM,
ization in soil and compost experiments. This reduc- ISO and EN). Measurement of the biodegradation rate
tion was caused by the presence of the synthetic PVA in compost (Table 4) confirmed a higher mineraliza-
polymer. Interestingly, this lower biodegradation tion rate for samples containing cellulose fiber (55%
was not observed in composites of starch/cellulose biodegradation in 75 days), and a lower biodegrada-
fiber (55/45 wt%) and starch/PVA/cellulose fiber tion rate for samples prepared without cellulose fibers
(45/10/45 wt%). These biodegradations of biocompos- (40% biodegradation in 75 days). The authors con-
ites were evaluated using micro-oxymax respirometer cluded that the biodegradation of PVA is due to the
system (Columbus Instruments, Columbus, OH). The presence of cellulose, which acts as a promoting agent
micro-oxymax respirometric system is an automated for PVA biodegradation.
Table 4 Biodegradability of natural filler-based biocomposite materials.
Principal components (wt%) Conditions for Results Reference

biodegradation
PLA/maple wood fibre (70/30) Compost Acetyl treatment of the maple wood fibers increases [45]
ISO-14855 their porosity, which enhanced hydrolytic
biodegradation of the PLA.
PLA/cotton cellulose fibers Compost Cotton cellulose fibers accelerated the biodegradabil- [46]
(70/30) ISO-14855 ity of PLA.
PLA/soy straw (70/30) Compost Untreated soy straw and wheat straw promoted the [49]
(ASTM D5338) biodegradability of PLA.
PLA/soy straw (70/30); Compost All the biocomposites showed improved degradation [50]
PLA/wheat straw (70/30);PCL/ (ASTM D5338) compared to the neat biodegradable polymer used.
distiller’s dried grains with
soluble (DDGS) (70/30);
PCL/soy meal (70/30)
Distiller’s dried grains with Compost (ASTM PBAT/DDGS biocomposite showed similar [47]
soluble (DDGS)/(aliphatic D5338) biodegradability to DDGS and cellulose. PBAT
and aromatic co-polyester) degradability increased with the incorporation of
PBAT (30/70) water washed DDGS into biocomposite system.
Poly(ethylene sebacate)/ Compost (ASTM Within 30 days, the biocomposite products showed [52]
cellulose fiber (85/15) D5338) 100% biodegradability
49% Starch /45% corn Compost (ASTM Approached plateau phase after 65% biodegradation [48]
fiber/5%inorganic fillers/ D5338) in 75 days.
1% Arabic gum
45% Starch/7% poly(vinyl Compost (ASTM PVA biocomposite approached a plateau phase after [48]
alcohol)/45% corn fiber/3% D5338) 55% biodegradability in 75 days.
inorganic filler
80% Starch/16% poly(vinyl Compost (ASTM Approached a plateau phase after 40% [48]
alcohol)/3% inorganic filler/ D5338) biodegradability in 75 days.
1% Arabic gum
96%Starch/3%inorganic Compost (ASTM Approached a plateau phase after 40% biodegrad- [48]
filler/1% Arabic gum D5338) ability in 75 days.
49% Starch /45% corn fiber/ Soil (ASTM 90% biodegradability was observed within 130 [48]
5% inorganic fillers/ D5988) days and these materials satisfied the soil
1% Arabic gum biodegradability criteria as per ASTM standard
requirements.
45% Starch/7% poly(vinyl Soil (ASTM 90% biodegradability observed within 130 days and [48]
alcohol)/45% corn fiber/ D5988) these materials satisfied soil biodegradability
3% inorganic filler criteria as per ASTM standard requirements.
Fernandes et al. [52] studied the biodegradation of fiber. When the above research studies were con-
biocomposite materials prepared from hexanoylated cluded, the orange fibers appeared to be more stable
cellulose fibers and the biodegradable polyester for years, and the authors argued that these natural
matrix, poly(ethylene sebacate) (PES). The biodegra- fibers may slowly degrade and favor the hydrolytic
dation studies were carried out according to the stan- degradation of the polymer matrix. These suggestions
dard methods ISO 14855 and EN 14046 to determine comply with the other study carried out by Modelli
the ultimate aerobic biodegradability of these biocom- et al. [56], in which the biodegradability of chemically-
posites in controlled composting conditions. In these modified flax fibers and starch powder were tested in
test conditions, PES showed 100% biodegradation soil conditions. The chemically-modified flax fibers
within 15 days, while the unmodified cellulose fibers showed slow biodegradation compared to the starch
required about 25 days to degrade 100%. Composite powder in 180 days; after this long induction time,
samples of PES/15% hexanoylated cellulose fibers they started to mineralize faster as they underwent
were completely degraded, i.e., 100% degraded within hydrolytic biodegradation.
28 days of testing, while a slower biodegradation rate
of 60% was observed in the hexanoylated cellulose 3.2 Effect of Compatibilizer
fiber alone within 30 days of testing. The results con-
cluded that PES/15% hexanoylated cellulose fibers Natural fiber reinforced polymer composites require
experienced slower degradation compared to PES adequate fiber-matrix adhesion to realize their full
matrix due to the effect of surface acylation by hex- potential of superior performance [57]. Poor interfa-
anoyl chloride, which imparted a comparatively non- cial adhesion results in poor mechanical properties
polar characteristic to the surface of the cellulose fiber in the final products. In order to overcome this weak-
as compared to untreated cellulose fiber. ness, suitable compatibilizers can be used in engineer-
Alvarez et al. [53] prepared biocomposites of sisal ing high performance biocomposites. Compatibilizers
fiber (15%) into Mater-Bi®. Mater-Bi is a commercially are also referred to as coupling agents or additives that
available biodegradable material and is a proprietary are capable of modifying interfacial adhesion during
thermoplastic starch. These materials with and with- melt blending of the polymeric matrix with hydroxyl
out sisal fiber were tested in soil burial conditions groups on the surface of fiber. The use of compatibiliz-
for 400 days. Degradation was measured in terms of ers in lignocellulosic polymer composites may affect
their weight loss followed by microscopic analysis. their rate of biodegradability. In this regard, research-
Researchers noticed that the sisal fiber played a sec- ers investigated [24] the biodegradation of PLA/corn
ondary role in this soil burial test, thereby decreasing starch/natural fiber (coir)-based composites with and
the biodegradation rate. In this test Mater-Bi and com- without the coupling agent, maleic anhydride (MA)
posite showed 40 and 33 wt% degradation, respec- (1% wt). The biodegradation of the PLA composite
tively. The authors concluded that Mater-Bi favors was studied in the presence of compost for a 90 day
microbial degradation compared to the Mater-Bi/ incubation period, with the conditions of the proce-
sisal fiber biocomposite, and the higher weight loss dure following the test method ISO 14855. The CO2
of Mater-Bi is mainly due to its amorphous struc- emission was evaluated through a manual titration
ture (destructed starch), which is easily accessible to method. At the end of the 90 day incubation, the bio-
the matrix by microorganisms. The sisal fiber plays a degradability of the PLA biocomposite, PLA and corn
minor role, which slows down the biodegradation of starch were assessed. Corn starch attained a higher
biocomposite materials. level of biodegradation (87%) than neat PLA (55%)
Bastioli [54] studied how the presence of starch in 90 days. The compatibilized composite (PLA/corn
influenced the rate of biodegradability of Mater-Bi in starch/coir/maleic anhydride) had lower biodegra-
a composting environment using ASTM D 5338–92. dation (54%) than the uncompatibilized composite
Contrary to the previous research [53], e.g., biocom- (which showed 59% biodegradation) in a 90 day test
posites of sisal fiber (15%) in Mater-Bi when exposed period. The researchers concluded that the natural
to soil burial, only partial degradation was observed. fiber plays a secondary role to the corn starch in the
These experimental results clearly indicated that a biodegradation of the PLA composite. The presence
composting environment is more suitable to enhance of the maleic anhydride inhibits the microbial growth
the biodegradability of such materials soil environ- in the compatibilized composite, compared to the
ments. Imam et al. [55] studied the biodegradation uncompatibilized composite. The research also con-
of biocomposite materials with a poly(vinyl alcohol) cluded that compost is the most suitable environment
matrix polymer, and starch and orange fiber fillers, for the biodegradation of these PLA/cornstarch/
using a soil burial test. The authors concluded that natural fiber-based composite materials. Tserki et al.
starch was a more biosusceptible material than orange [58] studied the commercial polyester Bionolle® 3020,
obtained from the Showa Highpolymer Company, authors found that there was no PLA biodegradation
Japan, containing succinic acid (40%), adipic acid in the soil or compost at room temperature conditions,
(10%) and 1,4 butanediol (50%), grafted with 7phr while the reference cellulose materials achieved 75%
maleic anhydride (MA). The biodegradation experi- biodegradation in 45 days in both conditions. When
ments of Bionolle-grafted-MA/cellulose fiber com- the same PLA test materials were exposed to indus-
posite were carried out in a soil burial environment for trial composting conditions at temperature 58°C,
90 days. This test was approached to study the effect of 90% biodegradation was achieved within 100 days.
compatibilizers and the thickness of the test specimens Therefore, it was concluded that industrial compost-
(1 and 3 mm) in soil burial conditions. Based on the ing provides a much more suitable environment for
weight loss observation of the compatibilized compos- the thermophilic bacteria and fungi that are involved
ites of varying thickness, the experimental results sug- in the biodegradation of PLA compared to soil burial,
gested that thickness was a very predominant factor home compost and aqueous conditions, where meso-
in controlling the degradation rates. The weight loss philic bacteria and fungi are predominant.
of 1 mm thick polyester Bionolle 3020 was 28% over 90 Researchers studied the biodegradability of
days, compared to only 10% in the 3mm thick Bionolle poly(butylene succinate) (PBS) biocomposites with a
3020 over the same period. The 1 mm thick Bionolle- rice husk flour (RHF) filler in soil and composting con-
grafted-MA/40% cellulose fiber composite showed a ditions [51]. They observed a higher biodegradability
48% weight loss, which was larger in comparison to in the PBS biocomposite than in the neat PBS, and the
the 3 mm Bionolle-grafted-MA/40% cellulose fiber biodegradation rate was enhanced with the addition
composite, which experienced only 29% weight loss of the rice husk flour. The PBS/RHF biocomposite
in the same 90 day period test duration. The authors showed 18% weight loss in compost, while the PBS/
concluded that with the incorporation of 40% cellulose RHF biocomposite had 13% weight loss in soil condi-
fibers into the polymer matrix, the biodegradation rate tions in 80 days. The neat PBS showed 6% weight loss
was steadily increased. These results also suggested in compost, while the neat PBS experienced weight
that sample thickness plays a major role, because as loss of 3% in soil in 80 days. These comparison studies
the sample thickness increased, the rate of biodegra- demonstrated that the RHF promoted the biodegrada-
dation decreased due to the lower ratio of surface area tion of the PBS matrix in both the soil and compost
to mass. The authors also concluded that the compati- environments. A comparison of the effects of environ-
bilizer did not have much influence on the biodegra- mental conditions revealed a higher rate of biodegra-
dation of compatibilized composites. dation in compost compared to soil, due to the larger
The compatibilization of lignocellulosic polymer amount of microbial colonies present in the compost.
composites is mainly used to increase potential dura- Biodegradation studies of aliphatic polyesters (PCL,
bility and mechanical performance. The potential tox- PHBV, PBS, and PLA) with abaca fibers were inves-
icity of compatibilized biocomposites has not been tigated by Termite et al. [62] using a soil burial test. In
well studied in natural environmental conditions this study, there was no weight loss observed for PLA
such as soil, compost, and aqueous solutions [59]. in 180 days. The other composites demonstrated bio-
Further detailed study is needed to ensure that the degradability, in the order of PCL>PHBV>PBS in 180
degradation products and intermediates of such bio- days. In another study, composites of the biodegrad-
composites will not have any negative effect on living able polyester PBS filled with agricultural residues,
organisms in these environments. The potential eco- such as rice husk [63], were exposed to biodegradation
toxicity of biocomposite degradation products can be tests in an Azospirillum brasilense BCRC 12270 liquid
verified using plant growth tests or seed germination culture medium. It was observed that the degree of
tests as prescribed in ASTM and ISO standards. biodegradation increased with an increasing rice husk
content. To conclude, these various biodegradability
3.3 Effect of Environmental Conditions studies demonstrated that a composting environment
is most suitable for the disposal of bioplastic materials
According to an investigation carried out on the bio- in a short time (within six months). Figure 3 summa-
degradation of PLA filled with cornstarch (up to 60%) rizes the conditions in which bioplastics biodegrade in
[60], there was no degradation observed in the PLA different types of biological waste treatments. It is con-
matrix in a soil burial test. The only weight loss that sidered that there are four types of waste treatments:
occurred in the composite was due to the degradation home composting, industrial composting, anaerobic
of the starch. In another study [61], the PLA biodeg- digestion and incineration. The ultimate mineraliza-
radation test was studied and compared to reference tion of bioplastics is mainly dependent on the envi-
cellulose materials in soil and compost conditions at ronmental conditions (temperature, oxygen and active
room temperature (30°C) conditions for 200 days. The microorganisms) and the waste treatment options
Temp- Anaerobic Anaerobic

erature Bacteria, no fungi Bacteria & fungi
50–60°C Chemical pulp

Chemical pulp
Mechanical pulp
Starch
Starch
PLA PLA
starch/PCL starch/PCL
PHA PHA
thermophilic industrial
digestion composting PBAT
≤35°C Chemical pulp mesophilic home Chemical pulp

Starch digestion composting Mechan. pulp
starch/PCL Starch
PHA starch/PCL
PHA
PBAT
Figure 4 Materials which are biodegradable in four types of biological waste treatment. (From reference [64] with permission).
(composting and anaerobic digestion), which are rep- redox potential of MnP is lower than that of lignin per-
resented in Figure 4. oxidase [65]. Until recently, white-rot fungi were the
only organisms known to be capable of biodegrading
lignin efficiently by their active extracellular enzymatic
4 BIODEGRADATION OF LIGNIN- process [11]. Currently, research on lignin biodegrada-
BASED MATERIALS tion is mainly focused on the following aspects: lignin
biodegradation by white-rot and litter-decomposing
The biodegradation behavior of plant mass is very fungi, and the biochemical pathway mechanisms of
much dependent upon its lignin content, and the peroxidases, purification, production and characteriza-
microbial population of its environmental systems. tion of ligninolytic and cellulolytic enzymes secreted by
Lignin provides physical, chemical and biological white-rot fungi.
protection for the growing of plant wood, straw and Sudhakar et al. [13] studied and made a comparison
husks. Lignin does not degrade easily by either abi- of the CO2 emission profiles of oxo-biodegradable mate-
otic or biotic processes due to its inertness, and it tends rials. These materials included natural rubber, pine nut
to accumulate in the environment. However, lignin shell lignin (PNSL) with synthetic linear low density
undergoes slow biodegradation under composting polyethylene (LLDPE), and a low density polyethylene
conditions. The biodegradation of lignin occurs in a (LDPE)/lignin composite. The analysis was conducted
two-step process. The first step involves the reduc- according to the ASTM D-5988 biodegradation test in
tion of the molecular weight of the lignin, leading soil. The study revealed that oxo-biodegradable materi-
to biodegradable low molecular weight compounds als undergo slow rates of biodegradation (conversion of
[65, 66]. The second step is the microbial assimilation organic carbon to CO2) in soil. The authors suggested
of the low molecular weight compounds produced in that the biodegradation processes of the LDPE/lignin
the first step. The first step requires a specific micro- composite in soil involve microbial populations and
bial enzymatic process, including peroxides in order to biochemical pathways that are similar to those observed
breakdown the C-C chains of lignin through non-specific in lignin and natural rubber biodegradation.
free radical reactions, and produce low molecular com- The degradation of wood in natural environments
pounds which are biodegradable by microorganisms. It such as soil and other outdoor places is mainly caused
has been shown that a large number of peroxide group by fungi. The degradation of wood hard substances
enzymes are capable of removing lignin from lignocellu- is mainly through the fungi organized hypae, which
losic materials without affecting their cellulose compo- usually helps fungal penetration capacity. It has been
nents. Manganese peroxidase (MnP) has been implicated identified as Trichoderma reesei, which is capable of
as a particularly important enzyme formed by white-rot producing cellulases which hydrolyze the cellobiose
fungus during the delignification of kraft pulps [61]. and other short cello-oligosaccharide into glucose. In
This enzyme forms a complex with acids and diffuses spite of this, Trichoderma reesei does not have the capa-
away from the enzyme to oxidize lignin. However, the bility to produce other enzymes to degrade lignin
substances. The best known family of white-rot fungi, Studies have shown [71] that specific microbial actin-
such as Trametes versicolar, are capable of degrading omycetes species and fungi are capable of degrading
both lignin and carbohydrates components of wood in 55% mass loss of rubber sheets in 70 days. Tsuchii et al.
the same proportional rate [67]. [72] found that the actinomyces, Nocardia sp. (strain
The degradation of poly aromatic hydrocarbon 835A) is capable of degrading NR rubber efficiently
(PHAs) is mainly caused by litter composting fungi in in the synthetic medium in the absence of any other
soil conditions. The PHAs are natural and anthropogenic carbon sources. Ikram et al. [73] studied the soil bio-
hydrocarbon which contains two or more fused benzene degradation of natural rubber gloves at ambient tem-
rings. Due to their large presence, bioaccumulation and perature. They showed NR gloves reached 54 and
carcinogenic nature, PHAs are a serious concern as an 94% weight loss after 4 and 48 weeks respectively.
environmental burden. The following lignolytic fungi The authors later concluded that NR biodegradation
are known to biodegrade PHAs: Phanerochaete chryso- is mainly dependent upon the soil nutrients such as
sporium, Bjerkandera adusta, and Pleurotus ostreatus. nitrogen and phosphorous. The natural rubber in
The enzymes involved in the biodegradation of PHAs a higher content of nitrogen (100 mg/l), phospho-
include lignin peroxidase, versatile peroxidase, manga- rous (150 mg/l) system showed a 61.5% weight loss,
nese-peroxidase, and laccase [68]. whereas in the low content of nitrogen (10mg/l), phos-
The organic material can contaminate it with dioxins phorous (15mg/l) system showed only 23.6% after 24
and dibenzofurans, extremely toxic dioxins and dibenzo- weeks. Moreover, the microbial colonies on the natural
furans which are formed during bleaching in pulp indus- rubber also decreased in the lower content of nitrogen
tries. It is common and among the most toxic pollutants and phosphorous present as expected. These authors
encountered in the soil environment. The white-rot fungi have identified a higher number of bacterial popu-
Phanerochaete sordida has been considered the most effi- lation (12317/mg) on the NR gloves than fungi (441/
cient organism at mineralizing these toxic compounds in mg) and actinomycete population (297/mg). In studies,
nature. As a result, white-rot fungi are attractive candi- Linos et al. [74, 75] compared the biodegradability of
dates for use in bioremediation applications [69]. natural rubber and synthetic rubber in the presence
Interestingly, in nature, white-rot fungi possess of Pseudomonas aeruginosa under aqueous medium.
the unique ability to degrade lignin to carbon diox- Results showed natural rubber was 26% mineralized
ide [65] in order to have access to the cellulose mol- in six weeks, compared was 21% mineralization for
ecule, which is a carbon source for white-rot fungi. synthetic rubber. The authors concluded that natural
Recently, researchers have started to understand the and synthetic rubbers undergo a similar rate of bio-
enzymatic mechanism by which the degradation of degradation, and the slight changes may be due to the
lignin is accomplished [65]. Furthermore, 14C-labeled antioxidants used in the synthetic rubber. The micro-
techniques have been used to better understand new bial species Nocardia and P. aeruginosa were shown
features in lignin biodegradation. This technique has [74, 75] in which the breakdown of cis-polyisoprene
helped make it possible to determine the fate of the chain was found due to oxidative microbial enzymes.
mineralized components of lignin, and lignin solubi- The evidence suggests that bacteria initiate free-radical
lization after microbial assimilation. The 14C-labeling chain peroxidation by oxidative biodegradation
techniques also help in replacing carbons on either mechanisms.
aromatic rings or propane side chains [67].
Nonisotopic methods are limited to qualitative lig-
nin degradation studies due to their limited ability to 6 CONCLUSION
provide rough estimation of degradation [67].
Besides white-rot fungi, there are many types of Lignocellulosic composites made from both bioplas-
actinomycetes and eubacteria that are able to degrade tics and fossil plastics are advancing in a multitude
extracted lignin. Most of the bacterial strains belong- of applications, including in both durable and single-
ing to these genera are only capable of solubilizing use products, due to their renewability, low cost, low
and modifying lignin and have limited ability to min- relative density and biodegradability (in the case of
eralize the lignin [70]. some lignocellulosic composites). The end life man-
agement of these lignocellulosic composites depends
on their biodegradability in their optimal disposal
5 BIODEGRADATION OF NATURAL environment. The biodegradability of a lignocel-
RUBBER lulosic composite mainly depends on its polymer
matrix. Many studies have shown that lignocellulosic
The microbial biodegradation of natural rubber (NR) composites are biodegradable if they are made up of
occurs in active microbial environmental conditions. a biodegradable polymer matrix. The composition of
lignocellulosic fibers used as fillers also influences Biodegradable Composite: A polymer composite that
the biodegradation behavior of their composites. degrades by the action of biological agents such as
Also, the rate of biodegradation of lignocellulosic bacteria, fungi.
composites depends on many other environmental Biotic: Components of an environment which are liv-
factors, such as moisture, humidity, temperature and ing and affect the ecosystem. For example: bacteria
microbial population. This review article has empha- and fungi.
sized the variability of the biodegradation behavior Compostability: The ability of a material to undergo
of lignocellulosic composites in composting and soil degradation by the action of biological agents such as
environments. The international standards concern- bacteria, fungi, etc., at the same rate as that of known
ing testing and labeling of biodegradable plastics in compostable materials, such as cellulose, and without
composting conditions and soil environments were leaving toxic residues.
also explained, and are essential to ensure that bio- Composting Rates: The rate of degradation required
composite materials are developed intelligently. The by polymers as per the compostability testing stand-
validation criteria for biodegradability of lignocel- ards. For example, ASTM D6400 requires 60% of the
lulosic composites and polymeric materials such as organic carbon present in single polymer to be con-
mineralization percentage, disintegration and eco- verted to carbon dioxide by the end of the 180 day test
toxicity as per different testing methods vary between period.
different standards. Composting Pile: The pile of organic masses in which
the aerobic breakdown of the substrate occurs.
Inoculum: Medium containing microbial species.
ACKNOWLEDGEMENTS ISO: International Organization for Standardization
Lignocellulosic: Plant biomass composed of cellulose,
The authors are thankful to the Ontario Ministry of
hemicellulose and lignin.
Agriculture, Food, and Rural Affairs (OMAFRA)-New
Mesophile: Microorganisms that grow best in moder-
Directions and Alternative Renewable Fuels “Plus”
ate temperature, neither too hot nor too cold, typically
Research Programs; to the OMAFRA-University
between 20 and 45°C.
of Guelph Bioeconomy-Industrial Uses Program;
Mesophilic Digestion: Digestion of waste at elevated
to the Ontario Research Fund (ORF) Research
temperatures up to 45°C in the presence of mainly
Excellence (RE) Round-4 from the Ontario Ministry
mesophilic microorganisms.
of Economic Development and Innovation (MEDI),
OECD: Organization of Economic Co-operation and
the Natural Sciences and Engineering Research
Development
Council of Canada (NSERC) Individual Discovery
Oxygen Demand: The amount of dissolved oxygen
Grants to MM and AKM; AUTO21-NCE (Canada’s
needed by microorganisms in soil biodegradation
automotive R&D program); the Hannam Soybean
testing.
Utilization Fund (HSUF) and the Grain Farmers of
PLA: Poly(lactic acid)
Ontario (GFO) fund for supporting research on vari-
PHAs: Polyhydroxyalkanoates
ous aspects of biobased materials at the University of
PHB: Polyhydroxybutyrate
Guelph’s Bioproducts Discovery and Development
PHBV: Poly(hydroxybutyrate-co-hydroxyvalerate)
Centre (BDDC).
PCL: Polycaprolactone
PBAT: Poly(butylene adipate-co-terephthalate)
GLOSSARY: PBS: Poly(butylene succinate)
PE: Polyethylene
Abiotic: Components of an environment which are PP: Polypropylene
non-living chemical and physical factors that affect PET: Poly(ethylene terephthalate)
the ecosystem. For example: sunlight, temperature, NR: Natural rubber
oxygen, etc. Thermophile: Microorganisms that live and grow
Adsorption: The adhesion of particles from a fluid to a in hot environments that would kill most other
surface due to attractive forces. organisms.
ASTM: American Society for Testing and Materials Thermophilic Digestion: Digestion of waste at ele-
Biocomposite: Polymer composite consisting of either vated temperatures of up to 70°C in the presence of
a filler or polymer matrix that is derived from biologi- mainly thermophilic microorganisms.
cal resources. Whole Green Composites: Polymer composites that
Biodegradability: The ability of a material to undergo are made up of renewable resource-based polymers
degradation by the action of biological agents such as and fillers. Their biodegradability depends on the type
bacteria, fungi, etc. of polymer matrix used.
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Biodegradability and Compostability of Lignocellulosic Based Composite Materials

Article · August 2013

Compostability and biodegradation of bioplastics and biocomposites View project

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KEYWORDS: Biodegradation, compostability, lignocellulose, biocomposites

1 INTRODUCTION lignocellulosic ﬁbers have a major role to play, and

*Corresponding author: mohanty@uoguelph.ca

plants, including agro-residues, coir ﬁbers, and pine- 2 LIGNOCELLULOSIC MATERIALS

Figure 1 Classiﬁcation of lignocellulosic composites.

14855–2 are tests of biodegradation in compost; ISO

Standard Test Results

Standard Test Method and Duration Biodegradation condition (mineralization)

Table 4 Biodegradability of natural ﬁller-based biocomposite materials.

Principal components (wt%) Conditions for Results Reference

Temp- Anaerobic Anaerobic

50–60°C Chemical pulp

≤35°C Chemical pulp mesophilic home Chemical pulp

REFERENCES and composites in composting and culture environ-

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