Resources, Conservation and Recycling 70 (2013) 919

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Resources, Conservation and Recycling

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Recycled wastes of tomato and hemp bres for biodegradable pots:

Physico-chemical characterization and eld performance
Evelia Schettini a , Gabriella Santagata b, , Mario Malinconico b , Barbara Immirzi b ,
Giacomo Scarascia Mugnozza a , Giuliano Vox a
a
b

Department of Agricultural and Environmental Science (DiSAAT) University of Bari, Via Amendola 165/a, 70126 Bari, Italy
Institute of Chemistry and Technology of Polymers, CNR, Via Campi Flegrei 34, Comprensorio Olivetti, 80078 Pozzuoli, Napoli, Italy

a r t i c l e

i n f o

Article history:
Received 24 January 2012
Received in revised form 30 October 2012
Accepted 2 November 2012
Keywords:
Agro-food industry waste
Polysaccharides
Renewable by-products
Eco-sustainability
Mechanical properties
Transplanting

a b s t r a c t
Wastes and by-products of agro-food industries and papertextile manufacturing companies, such as
tomato peels and seeds, and hemp, were glued with sodium alginate in order to produce biodegradable pots for plant transplanting in agriculture, thus aiming both to reduce such wastes and also to
ght the accumulation of plastic pot wastes produced in plant nurseries. Laboratory tests performed on
polysaccharide lms and biocomposites based sheets prepared with the same materials developed for
preparing the pots, were carried out in order to understand the chemico-physical correlations between
resin, ionic crosslinking agent, reinforcing bres and water. To this aim, mechanical tests, water vapour
permeability tests, water up-take evaluations and morphological analysis were carried out. It was found
a strong physical interaction between sodium alginate and calcium ions in the development of a threedimensional network. The crosslinked structure was able to physically entrap the reinforcement bres by
means of hydrogen bonding, as evidenced by scanning electron microscopy (SEM) and energy-dispersive
X-ray spectroscopy (EDS) analysis. SEM analysis performed on fracture surfaces of the biocomposites
evidenced that the bres were well embedded inside the three-dimensional network, even if their dispersion needed some improvements; EDS analysis revealed the presence of calcium in rather all the
selected internal micro-zones, thus suggesting a well structured network. In order to assess the agronomic performance of the novel biodegradable pots in seedling transplanting activity, the pots were
tested in real eld condition during 2009 at the experimental farm of the University of Bari, Italy. From
the analysis of the young plants transplanted in the eld, it was inferred that the biodegradable containers had enhanced the roots plants development and the plant growing, avoiding transplant shock and
root deformation. After the using time, they completely degraded into the soil within 2 weeks.
2012 Elsevier B.V. All rights reserved.

1. Introduction
The agro-food industries and the papertextile manufacturing companies produce huge amount of wastes and by-products
handled as material of negative impact both in terms of the environmental concern, due to the increasing of pollutant disposal,
and in terms of the industrial sustainability due to the high costs
related to their management. In Europe, for example, the agro-food
processing industries produce about 250 million tonnes per year of
by-products and wastes (AWARENET, 2004), whereas only in Italy,

Corresponding author at: Institute of Chemistry and Technology of Polymer

(ICTP), National Council of Research (CNR), Via Campi Flegrei, 34-80078 Pozzuoli,
NA, Italy. Tel.: +39 081 8675214; fax: +39 081 8675230.
E-mail address: santagata@ictp.cnr.it (G. Santagata).
0921-3449/$ see front matter 2012 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.resconrec.2012.11.002

the paper and textile industries generate each year about 37 million
tonnes of wastes (OECD/Eurostat, 2005).
In the past most of the edible scraps were often recovered
as raw material for the production of animal feed, compost and
fertilizer; otherwise they were discarded in common dumps.
Recently, in order to reduce the trash collection and disposal
fees, new methods and policies for waste handling and treatment
have been introduced (Riggi and Avola, 2010) to recover, recycle
and convert the by-products and wastes into upgraded products
(Federici et al., 2009; Laufenberg et al., 2003; Rousu et al., 2002).
A valid example of this policy is represented by the European
tomato industries that produce and process each year about
10 million tonnes of tomatoes; the deriving wastes, quantied
in approximately 0.1 million tonnes per year, are made up of
processing residues, brous parts, seeds and peels, containing high
amounts of polysaccharides, such as pectin and other important
chemicals like carotenoids, especially lycopene, whose antioxidant

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E. Schettini et al. / Resources, Conservation and Recycling 70 (2013) 919

activity is well set up (Zhao et al., 2002). Their recovery should be

highly cost-effective (Naviglio et al., 2008), particularly considering
that lycopene cost is about 50,000 D per kg.
Among wastes coming from agro-foodtextile manufacturing,
the bres represent sizeable and functional component. In particular natural bres, such as jute, kenaf, ax, hemp, and agriculture
residues including stalks of most cereal crops, coconut bres,
peanut shells and tomato seeds and peels, are becoming very
attractive as reinforcing bres of biocomposites (Sreekumar et al.,
2008). Natural bres coming from wastes of agro-food industries
and papertextile manufacturing companies provide environmental and technological prots when used to reinforce composites
both in terms of high strength and stiffness performance in low
density materials, and in terms of positive environmental impact
(Uma Devi et al., 2004; Lopez et al., 2012). In this paper, these
bres were employed as mechanical reinforcement of biodegradable polymers in the setting up of biodegradable pots that can be
used for transplanting.
The process of removing a plant from the place where it has
been growing to another growing location, known as transplanting, is a worldwide cultural practice. Growers use pots and cell
trays of different materials, sizes, shapes, and colours, to suit crop
species, growing methods, and marketing strategies (Evans and
Hensley, 2004; Evans and Karcher, 2004). At nurseries and greenhouses, seeds, bulbs, and young plants are allocated in cell trays
or pots containing growing substrate both to start the growth
under uniform cultivation conditions, with a better control of crop
density and uniformity, and to preserve seeds, bulbs, and plants
from soil pests and diseases, if compared to direct seeding in soil,
thus improving the growth of vigorous seedlings and plants. One
of the limitations of un-permeable and rigid containers is that
roots tend to circle the outer perimeter of the root ball, which can
result in reduced plant growth, health, and survival once transplanted (Evans and Karcher, 2004; Struve, 1993). So transplanting
is necessary to allow a more natural development of plants root
structure; anyway, during the transplanting, the roots can be damaged.
Most of the containers used for transplanting are made of
non-renewable oil-based raw materials, such as polystyrene,
polyethylene and polypropylene, with suitable mechanical properties, chemical and microbial degradation resistance, durability,
as well as low costs. After use, plastic pots result contaminated with soil, organic matter and agro-chemicals. Nevertheless
the high costs related to a correct collection, disposal of and
recycling process of post-use plastic pots, determine their wild
neglecting in landll or their uncontrolled combustion with the
subsequent emission of toxic substances both into the atmosphere and into the soil. A valid alternative to the employment
of petroleum based thermoplastic pots may be represented by
the use of biodegradable pots (Evans and Hensley, 2004; Evans
and Karcher, 2004; Horinouchi et al., 2008; Kowalska et al.,
2002; Yamauchi et al., 2006; Wu et al., 2003). Once buried, the
biodegradable pots are subjected to biodegradation process, being
transformed in biomass and inorganic products (e.g., carbon dioxide and water). Biodegradable pots, already produced by worldwide
companies, such as William Sinclair Horticulture Ltd. (Lincoln,
England, http://www.william-sinclair.co.uk/), Enviroarc (Scoresby,
Australia, http://www.enviroarc.net/), Fertil SA (Boulogne Billancourt, France; www.fertilpot.com), and Jiffy Products International
AS (Stange, Norway, http://www.jiffygroup.com/), are made of
plant bre, rice, starch, grasses and vegetable oils, with a lifetime ranging from few months to 12 years. Although being
biodegradable, they generally need a composting site to completely
decompose (Trojanowsky and Huttermann, 2002). Moreover, some
of these pots show unsuitable mechanical performances hindering the roots to pass throughout; in addition they may forth

odd smell and may be not cost effective if compared to plastic

pots.
Recently researches have been focusing the attention on the
development of novel biodegradable and cost-competitive pots or
multiple nurseries. These pots are biocomposites whose continuous phase is characterized by biopolymers coming from renewable
and available origin, such as polysaccharides (Malinconico
et al., 2002; Avella et al., 2007), and whose solid phase, dispersed within the polymeric matrix, is represented by natural
llers and bres coming from wastes of agro-food and tex
2008). The arrangement
tile processing industries (Simkovic,
obtained from the phases combination produces a system with
improved structural, mechanical and chemico-physical performance (Mohanty et al., 2000a; Hatami-Marbini and Pietruszczak,
2007).
Among the wide range of biopolymers, polysaccharides can be
used as binders for pots applications because they are biodegradable, biocompatible and non-toxic polymers, widely available and
renewable (Malinconico et al., 2002; Avella et al., 2007; Schettini
et al., 2007; Kapanen et al., 2008). Moreover, as a consequence of the
presence of polar groups (OH , NH3 + , COO ) on macromolecular
chains and following to the intrinsic physico-chemical properties,
polysaccharides show high afnity with water molecules. As a
matter of fact, they induce the development of hydrogels, i.e., threedimensional water stable networks, structured by means of ionic,
covalent, thermoreversible or pH-reversible crosslinked processes
(Coviello et al., 2007; Russo et al., 2007).
In biodegradable pots carrying out, the natural bres act as a
reinforcement able to enhance the strength and stiffness of the
resulting composite structures. Nevertheless, the mechanical performances of natural bres are poorer if compared to those of
the most widely used competing reinforcing man-made bres.
The conventional bres, such as glass, carbon, and aramid, can be
produced with a denite range of properties, whereas the characteristic properties of natural bres depend on the plant source,
plant age, separating technique, moisture content, etc. (Lewin and
Pearce, 1985).
Anyway, because of low density of natural bres, the specic properties (property-to-density ratio), such as strength and
stiffness, of plant bres are comparable with the ones of glass
bres (Wambua et al., 2003). In literature, the inuence of plant
bres on the mechanical properties of biodegradable polymers has
been widely explored (Cyras et al., 2001; Hepworth and Bruce,
2000).
Moreover the chemical similarity between polysaccharides
and natural bres, consisting mainly of cellulose, resulted in an
increased tensile strength of the reinforced polymers. This nding
has been ascribed to the good adhesion between bre and matrix,
promoted by the similar highly hydrophilic character of both components (Mohanty et al., 2000a).
On the base of the above remarks, in this paper the development,
the implementation, and the eld test of innovative biodegradable pots realized by means of sodium alginate, as polymeric
matrix, and tomato and hemp bres, as natural reinforcing dispersed phase, are investigated. The mechanical performances of
the new biocomposites strictly depend on the physico-chemical
interactions among polymeric matrix and bres (Mohanty et al.,
2000b). To this aim, the hydrogen bonding between the active
functional groups of the biocomposites components (Mohanty and
Misra, 1995) could entail suitable effects (Shinde and Nagarsenker,
2009).
Aim of the paper is both to investigate the functionality,
the physico-chemical and mechanical behaviour of these novel
biodegradable pots in standard and controlled experimental eld
conditions, and to follow the assessment of the biodegradation process of these pots during plant cultivation in soil.

E. Schettini et al. / Resources, Conservation and Recycling 70 (2013) 919

11

Fig. 1. Structure of alginate: -l-guluronic acid (G) -d-mannuronic acid (M) and MG block copolymer (a); schematic drawing of the egg-box model and calcium coordination
to homopolymeric blocks of -l-guluronate residues (b).

2. Materials and methods

2.1. Experimental part
2.1.1. Materials
Sodium alginate, purchased from Lianyungang Zhongda Seaweed Industrial Co. Ltd. (XuGou, Lianyungang, Jiangsu, China), was
characterized by 37 1% of guluronic fraction. The weight average
molecular weight (Mw) was equal to 1.2 106 Da and the number average molecular weight (Mn) was equal to 2.3 105 Da. In
aqueous media the guluronate residues of sodium alginate are
able to provide ionic crosslinking process in presence of multivalent cations, such as calcium ions (Draget et al., 2006) (Fig. 1).
Due to the natural presence of calcium into the soil, it is predictable that biocomposites based on sodium alginate, once buried,
undergo to spontaneous ionic crosslinking, thus providing water
resistant biodegradable pots (Immirzi et al., 2009; Malinconico
et al., 2008).
The natural bres used to reinforce the polymeric matrix were
exible and short bres from tomato peels and seeds combined
to more rigid, stiff and long bres from hemp strands (Ashori and
Nourbakhsh, 2010). Hemp bres, consisting of about 70% of cellulose, 15% of hemicelluloses, 5% of lignin and wax and up to 10% of
moisture (Amar et al., 2005), were provided from ASSOCANAPA
(Pistoia, Italy), and were on average 200 m long, 10 m wide
and 5 m thick. Tomato bres were wastes of tomato-processing
industry of Lycopersicon esculentum S. Marzano, tomato cultivar
purchased from Bulsem (Salerno, Italy) (Tommonaro et al., 2008).
The dry matter of tomato peels and seeds was mostly composed of
about 50% of bres and 20% of crude protein, while the remaining
part was characterized by fats and carotenoids, such as lycopene
and -carotenoid. The cell walls of bres contained cellulose, hemicelluloses and pectin, while starch was present as energetic and
preserving plant source (Knoblich et al., 2005). After the extraction
of high added value bioactive molecules, such as polysaccharides,
carotenoids and polyphenols, from peels and seeds, the residual
dried bres were used as received. Tomato bres were on average
80 m long, 10 m wide and 10 m thick (Tommonaro et al., 2008).
Polyglycerol, as plasticizer, was supplied from Solvay (Milan,
Italy) and used as received.
Calcium chloride used to crosslink sodium alginate was provided from Sigma Aldrich (Milan, Italy) and used as received.

2.1.2. Laboratory-scale lms, sheets and pots setting up

In order to identify and characterize the blends to be used for the
pots, two different laboratory-scale lms, based on sodium alginate
and calcium alginate, were prepared to perform physico-chemical
analysis helpful to predict the polymers performance as bonding
agent inside the pots.
The sodium alginate lms (coded A) were prepared by casting
from an aqueous solution obtained by dissolving 2.0 g of sodium
alginate in 100 ml of distilled water (2%, w/v) under stirring at
the temperature of 7075 C. Successively 1.0 g of polyglycerol
(1%, w/v) was added as plasticizer and dissolved under stirring.
The solution was ltered and kept few minutes under vacuum for
degassing. After this treatment, the solution was rstly poured,
avoiding bubble formation, into a polyester mould kept in plane,
in this way assuring the homogeneity of lm thicknesses, and
afterwards placed under ventilated hood for 3 days at room temperature, thus allowing the water evaporation.
The crosslinked calcium alginate lms (coded ACr) were prepared by soaking for 15 min the A lms in a 5% (w/v) aqueous
solution of calcium chloride. The drying process of the ACr
crosslinked lms followed the procedure previously described for
the A un-crosslinked lms.
Prior to testing, all the lms were equilibrated at 45% relative
humidity by storing them in a desiccator over a saturated solution
of calcium nitrate at room temperature.
The pots and the sheets were obtained from the same biocomposites, soaking 50.0 g of aggregate of bres in 100 ml of a 2% (w/v)
sodium alginate water solution. The components were thoroughly
mixed by means of a Brabender Plastograph blender (Rheomix,
Haake Rheometer, Germany) for 30 min at room temperature (cold
process) and at a rate of 16 revolutions per minute (rpm). Successively the paste was used to shape the two different forms (pot and
sheet). The pots were obtained by using a stainless steel device,
appositely produced, made with pots shaped closed moulds (Fig. 2).
After distributing the paste inside the moulds, the device was xed
between the cold plates of a press where the moulds were allowed
to close, left for few minutes for completely ll the cavity with the
wet paste and then opened, in this way providing the wet shaped
pots. A following drying process, carried out in an oven at 40 C
under air ow for 24 h, allowed to remove the water content up
to obtain a nal constant weight. The pots were characterized by
a height of 40 mm, an end base diameter of 40 mm, a top base

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E. Schettini et al. / Resources, Conservation and Recycling 70 (2013) 919

permeability tests, density and porosity tests and morphological

analyses were carried out on the A and ACr laboratory-scale lms.

2.1.3.1. Mechanical test. Youngs modulus, stress and strain at

break were evaluated by means of a dynamometer (model 4301,
Instron, Canton, MA, USA) following the ISO 5893 standard (ISO
5893, 2002). The dumbbell specimens tested were characterized by
a thickness of 75 m for the A lms and of 108 m for the ACr lms,
a width of 4 mm, and a length of about 28 mm. For each composition six specimens were tested. All the measurements were carried
out at room temperature and at crosshead rate of 2 mm min1 . The
values of the Youngs modulus are within 10%, while the stress
values are within 15%, and the elongation at break uctuates in
the range of 20%.
Fig. 2. Stainless steel pots mould.

diameter of 55 mm, a thickness of 4 mm, and a weight of 9.0 g

(Fig. 3).
As concerning the preparation of sheets, about 2.5 g of the wet
paste was distributed into stainless steel moulds of 70 mm2 with
a rubber frame of 3 mm and successively shaped in parallelepiped
sheets by cold pressing. After the drying process, carried out as in
the case of the pots, sheets of about 3 mm thick were obtained.
Three different compositions of biocomposites (both for sheets
and for pots) were prepared varying the percentage of tomato and
hemp bres added to sodium alginate water solution; the rst one
included 100% of tomato bre (coded ATH100), the second one
consisted of 90% of tomato bre and 10% of hemp bre (ATH90) and
the last one contained 70% of tomato bre and 30% of hemp bre
(ATH70). The crosslinked sheets (ATH100Cr, ATH90Cr, ATH70Cr)
were achieved by soaking the sheets for 15 min in a 5% (w/v) deionized water solution of calcium chloride; the drying process of the
crosslinked sheets was the same as described for the pots.
The lms and sheets thickness was determined with an electronic digital micrometre with accuracy of 0.001 mm. The thickness
was measured after the drying and the conditioning at room temperature and 45% relative humidity, averaging the values measured
over 10 different points.
2.1.3. Laboratory lm tests
With the aim to predict and highlight the physico-chemical
behaviour of the pots based on the sodium alginate and calcium alginate polymeric resins, mechanical tests, water vapour

Fig. 3. Experimental biodegradable pot.

2.1.3.2. Water vapour permeability, density and porosity tests. Water

vapour permeability (WVP) was calculated on the base of the ASTM
standard method E 9680 (ASTM E 9680, 2002) following the
equation:
WVP = WVTR

 L 
p

(1)

where WVTR (g m2 s1 ) is the water vapour transmission rate of

lms, L (m) is the lm thickness, and p (Pa) is the water pressure
difference between both sides of the lm. WVTR assessment consists of evaluating the rate of water vapour diffusion through the
specimen by means of gravimetric measurements, making periodic weightings. For the tests it was used the desiccant method
by which three test specimens for each sample were sealed to the
open mouth of a CEAST metal cup, with a 3000 mm2 exposed area
for the test and lled with silica gel; the metal cups were placed in
an environmental chamber set at air temperature of 23 C and air
relative humidity of 45%.
In order to better explain some peculiar results of chemicophysical properties of the lms and composites, such as
permeability and mechanical performance, the density and porosity of the lms and sheets were evaluated. The tests were carried
out via a liquid displacement method (Bundela and Bajpai, 2008),
using n-hexane as the displacement liquid, due to its ability to
easily penetrate the pores of the sheets without inducing shrinkage, swelling or solubilization of the polymeric matrix (Zhang and
Ma, 1999). A sample of weight W was immersed in a graduated
cylinder containing a known volume (V1 ) of n-hexane. The sample was kept in n-hexane for 10 min, and then a series of brief
evacuationrepressurization cycles were conducted to force the
solvent into the pores of the composite. The cycling was continued until no air bubbles emerged from the sheets. The total
volume of the n-hexane plus the n-hexane-impregnated sheets was
recorded as V2 and the residual n-hexane volume was recorded as
V3 . The n-hexane impregnated sheet was removed from the cylinder. The density of the sheet was expressed as d = W/(V2 V3 ) and
the porosity of the open pores in the composite was obtained with
= (V1 V3 )/(V2 V3 ) 100.
2.1.3.3. Scanning electron microscopy (SEM) analysis. Morphological analysis on the A and ACr sample surfaces was performed by
means of scanning electron microscopy (SEM) (Quanta 200 FEG,
FEI, Eindhoven, The Netherlands).
Air dried samples were xed onto aluminium stubs through carbon adhesive disks and observed with a low-vacuum secondary
electron detector using the accelerating voltage of 5.0 kV. The samples were observed at room temperature and at an internal water
vapour pressure of 66.66 Pa.

E. Schettini et al. / Resources, Conservation and Recycling 70 (2013) 919

13

2.1.4. Laboratory biocomposites tests

The sheets of un-crosslinked and crosslinked biocomposites
were used to perform mechanical and morphological analyses, as
well as water up-take and biodegradation tests.
2.1.4.1. Mechanical tests: exural test and puncture test. In order to
simulate the natural pressure exerted by roots against the pot wall
and bottom, two different mechanical tests were performed: the
exural test, according to ASTM D790 normative (ASTM D790-10,
2010), and the puncture test, an empiric test previously used by
Immirzi et al. (2009). All the mechanical analyses were performed
on six specimens, previously conditioned at room temperature and
at air relative humidity equal to 45%.
Flexural loads combined tensile, compression and shear loads.
The upper surface of each specimen was put into compression, the
central portion experienced shear, and the lower face underwent
tension. The exural samples were cut into specimens of about
3 mm thick, 5 mm wide and 7 mm long; the exural modulus was
determined using an universal testing machine (4504, Instron, Canton, MA, USA) in accordance with ASTM D790 standard (ASTM
D790-10, 2010). Three-point bend testing was performed at a crosshead speed of 1 mm min1 with load cell of 1 kN, to evaluate both
exural strength and exural modulus; each test was performed
until failure occurred. The distance between the span was 48 mm,
so the span to depth ratio, i.e., the length of the outer span divided
by the thickness of the specimen, was 16 which is an acceptable
value to minimize the area of shear stress created along the midline
of the specimen that could invalidate the test (Lee et al., 2009).
The puncture test consisted in penetrating the specimens until
the laceration of the same (Malinconico et al., 2008; Immirzi et al.,
2009). More specically, the samples to test, opportunely cut with a
punch cutter of 42 mm circular section, were trapped in cups xed
on the inferior traverse of the INSTRON instrument (Fig. 4). They
underwent the action of a force exerted by a spherical dart linked
to a steel rod xed on the upper traverse of the apparatus; the
dart, moving down at a xed rate of 2 mm min1 , penetrated the
sample until the rupture of the same. The applied load as a function
of the displacement was recorded; the parameters obtained were
normalized with respect to the of the area of the sphere and with
respect to an estimated value of the displacement of 10 mm.
2.1.4.2. Scanning electron microscopy analysis. Morphological analysis was carried out on cryogenically fractured surfaces of lms and
sheets by means of a SEM (Quanta 200 FEG, FEI, Eindhoven, The
Netherlands) in high vacuum mode, using a secondary electron
detector and an accelerating voltage of 20.0 kV. Before the electron microscopy observation, the fractured surfaces were coated
with AuPd alloy with a SEM coating device (MED 020, Bal-Tec AG,
Tucson, AZ, USA). The coating provided the entire sample surfaces
with a homogeneous layer of the metal of 18 0.2 nm. By means
of energy dispersive X-ray spectroscopy (EDS) it was possible to
perform the chemical analysis of selected microscopic regions. EDS
was performed in the SEM by means of an Oxford Inca Energy 250
System equipped with an INCAx-act LN2-free detector, using an
accelerating voltage of 20.0 kV.
2.1.4.3. Water up-take test. In order to reproduce the mechanical resistance of biodegradable pots in wet soil, pre-weighted dry
sheets were immersed in deionized water for 60 min at room
temperature and weighed every 15 min. The samples tested were
characterized by a length of 20 mm and a width of 15 mm, a weight
of 0.2 g and a thickness of 3 mm for the un-crosslinked samples
while a weight of 0.5 g and a thickness of 5 mm for the crosslinked
samples. Since the ATH100, ATH90 and ATH70 samples were not
crosslinked, the polymer chains were more exible and able to
interact, with water molecules; for this reason it was predictable

Fig. 4. Apparatus used for the puncture test: a test cup for puncture test analysis
(a) and the penetrating dart xed on Instron device (b).

that some of the bres could disentangle from the polymeric network owing out from the mat. To take into account this drawback,
all the samples were placed in Petri dish covered with lter papers,
previously dipped in water and weighed.
The sheets were withdrawn from the solutions and their wet
weights were determined after rst blotting with a lter paper
to remove the surface water. The water up-take percentage was
calculated using the equation:
Wst (%) =

W W 
t
d
Wd

100

(2)

where Wst (wt%) is the water sorption of the sheets, Wd and Wt

respectively are the weights of the samples in the dry state and in
the swollen states at different times. For each kind of sample, the
data were averaged on three specimens.
2.1.4.4. Laboratory biodegradation tests. To simulate the biodegradation process undergone by biodegradable pots when buried in
soil for transplanting, biodegradation tests were performed on
biocomposites thick sheet samples. Among the biocomposites,
the ATH100Cr and ATH70Cr crosslinked samples were analysed
since it was expected that the un-crosslinked biodegradable pots,
when buried and regularly watered, endured the crosslinking
process promoted by the calcium ions present in the soil and
naturally available to the polymeric resin. The biodegradation
tests, carried out on a laboratory-scale, followed the standard test
method described in ASTM Standard D5338-98 (2003) regarding
the biodegradation in soil. Following this test, the mineralization
of the sample, i.e., the amount of organic carbon of the material
which is converted into CO2 , was measured. The CO2 production

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E. Schettini et al. / Resources, Conservation and Recycling 70 (2013) 919

Table 1
Densities and porosities of un-crosslinked and crosslinked lms and sheets.

Fig. 5. Experimental biodegradable pots setting up.

measured for a material, expressed as a fraction of the calculated

carbon content, was reported with respect to time, from which
the degree of biodegradability was assessed. The soil used, characterized by a pH equal to 7.76, total solid content equal to 86.83%
and volatile solid content equal to 5.55%, was loaded with salts
and compost, according to the rate of 1 g of compost in 25 g of soil.
The soil was mixed with the test material and the CO2 evolved
was measured. Testing and observation were followed for 60 days.
Crystalline cellulose was used as control.
2.2. The eld test
The biodegradable pots for seedling transplanting were tested
in real eld condition during 2009. The test was carried out inside
a steel-constructed greenhouse (30.00 m 10.00 m), North-South
oriented, at the experimental farm of the University of Bari in
Valenzano (Bari), Italy, having latitude 41 05 N, longitude 16 53 E,
altitude 85 m asl. The greenhouse was covered with an ethylene
vinyl acetate (EVA) lm (PATILUX, Pati Co., Treviso, Italy), having
a thickness of 200 m and the following radiometric coefcients:
solar radiation range (2002500 nm) total transmissivity equal to
90.9%, solar direct transmissivity equal to 56.7%, and long wave
infrared range (LWIR, 750012500 nm) transmissivity equal to
22.5%. Greenhouse temperature was controlled by means of a natural and a forced ventilation system. Ventilation was provided
automatically when inside air temperature exceeded 27 C.
The experiment was conducted in the greenhouse from July
21 to October 30, 2009. Besides the ATH100, ATH90 and ATH70
biodegradable pots, commercial pots made of 100% polystyrene
(coded PS) with drainage holes were tested and used as control.
All the pots were lled with potting soil.
During the period from seeding to seedlings transplanting, from
July 21 to August 25, 2009, the pots were allocated in a steel bench,
characterized by an area of 2.0 m 1.0 m and a depth of 0.3 m.
The bench, covered with an anti root lm (Tenax FL, Tenax SPA,
Vigan, Lecco, Italy), was lled with perlite (Agrilit2, Perlite Italiana srl, Perlite Italiana, Corsico, Milan, Italy) for almost half of its
depth. The bench area was divided in equal parts. The experimental
design was a completely randomized design; the four treatments
(ATH100, ATH90, ATH70 and PS) had four replicates with four pots
per replicate. The pots were allocated inside the perlite for 2/3 of
their height (Fig. 5). On July 21, 2009 three pepper seeds were put
into the growing substrate in each pot. After emergence only one
plant per pot was kept. The irrigation was provided by means of an
intensive fogging system, realized with a PVC irrigation pipe (diameter of 1.6 mm) placed all around the bench with plastic nebulizer
nozzles every 0.5 m. The nozzles watered over 180 . During the

Sample

Density (g/cm3 )10%

Porosity (%)20%

A
ACr
ATH100
ATH90
ATH70
ATH100Cr
ATH90Cr
ATH70Cr

0.43
0.38
0.29
0.27
0.22
0.28
0.21
0.19

21.7
29.2
23.8
25.7
27.4
27.1
32.7
36.1

period from seeding to seedlings transplanting, the irrigation was

provided 3 times per day for 4 min at a time. On August 25, 2009 the
seedlings together with the biodegradable pots were transplanted
in the soil, without transplant shock. The control plants, i.e., the
plants grown inside the PS containers, were transplanted following
the procedure of removing the plastic pots. Peppers were harvested
on October 30, 2009.
Air temperature and relative humidity were continuously measured inside the greenhouse during the cultivation period by means
of a Hygroclip-S3 sensor (Rotronic, Zurich, Switzerland); the data,
measured with a frequency of 60 s, were averaged every 15 min and
stored in a data logger (CR10X, Campbell, Logan, USA).
3. Results and discussion
3.1. Laboratory lms and biocomposites evaluation
A signicant increase in thickness was recorded upon crosslinking lms and sheets in calcium chloride solution. The thickness of
the A and ACr samples was respectively about 75 m and 108 m,
with an increase of 44% upon cross-linking; the thickness of the
ATH100, ATH90 and ATH70 sheets was about 3 mm, while the
ATH100Cr, ATH90Cr and ATH70Cr sheets showed a thickness of
about 5 mm, with an increase of about 67%. This thickness increasing may be explained considering that the crosslinking process
of alginate molecules, responsible of tie points development and
stabilizing, often referred in literature as egg-box type process
(Grant et al., 1973), occurred during the samples soaking in water
solutions of calcium chloride; sodium alginate lm swelled while
crosslinked, i.e., it up-took some water during the formation of
three-dimensional stable network of calcium alginate. For this reason the conformation of crosslinked polymeric backbone attained
in wet condition did not change after drying and reconditioning process (Russo et al., 2007, 2010). This outcome induced the
increasing of free volume and consequently of the macromolecular
chain mobility, inuencing in unusual way some physico-chemical
properties of both crosslinked lms and biocomposites (Lee et al.,
2009). The hypothesis of free volume increasing was supported by
the evaluation of biocomposites porosity. The results, reported in
Table 1, could highlight the analysis of some atypical behaviours of
lms and sheets. In particular, the increasing of both free volume
and porosity of crosslinked samples could better explain the permeability results of the ACr lm and the mechanical performances
of crosslinked sheets.
The mechanical properties, analysed by means of the tensile
test method, and the permeability of the A and ACr lms are
reported in Table 2. As a result of the stiffness rising due to the
crosslinked network formation, the increasing of Young modulus
and the dropping off of elongation at break were evidenced in
the ACr samples. As concerning permeability data, it was possible to observe that the ACr lms experienced higher permeability
with respect to the A lms. In literature it is reported that generally crosslinked lms afforded lower water vapour permeability if
compared to un-crosslinked ones, since the tie points produced

E. Schettini et al. / Resources, Conservation and Recycling 70 (2013) 919

15

Table 2
Mechanical properties and water vapour permeability of the sodium alginate (coded A) and calcium alginate (coded ACr) laboratory lms.
Film

Young modulus (MPa)

10%

Tensile stress at break (MPa)

15%

Tensile strain at break (%)

20%

Permeability (ng s1 m1 Pa1 )

A
ACr

2170
4270

74
98

18
4

0.072
0.128

during the development of the three-dimensional network represented a hindrance to the permeation of molecules (Crank and
Parker, 1968). Nevertheless in this research it was found the opposite result. A plausible explanation to this unusual outcome could
be found both in the increasing of free volume of the crosslinked
ACr lms and in their enhanced porosity with respect to the uncrosslinked samples (Table 1), that allowed water molecules to
easily cover a straight pathway throughout the lms surface (Russo
et al., 2007, 2010; Lee et al., 2009).
The SEM analyses of the A and ACr lm surfaces were reported
in Fig. 6: the micrograph of the A lm (Fig. 6a) showed a tracked
but homogeneous and smoothed surface, typical of a quite regular
chain distribution, while the micrograph of the ACr lm (Fig. 6b)
showed an indented and rough surface, with zones of higher material agglomeration, characteristic of a well structured crosslinked
network.

In Table 3 the data related to exural properties of the tested

sheets are detailed; both set of the un-crosslinked and crosslinked
samples showed a general increase of the mechanical parameters
when hemp bres were added to tomato peels. The mechanical
enhancement was expected, as it is known that bres, due to their
increased aspect ratio (length/diameter) compared to non brous
ller, can improve mechanical properties of composites (Girons
et al., 2011). In the case of the un-crosslinked samples, when the
nominal hemp bre weight fraction increased beyond a critical
point, as in the case of the ATH70 sample, a slight lowering of
both Young modulus and stress at break were observed. This outcome could be due to the irregular dispersion of bres inside the
polymeric matrix, responsible of the voids concentration rising in
the biocomposite, as conrmed by the porosity values reported in
Table 1. Generally, the stiffness of bre reinforced plastic composites depends on the properties of the constituent bres, the
matrix and the load transfer capability between the matrix and
bres through the shear stress (Luo and Netravali, 1999). If voids
are produced in the composites, in the matrix or between the bre
and matrix, they signicantly weaken the load transfer capability,
due to the stress concentration around them (Luo and Netravali,
1999). Moreover, by increasing the concentration of hemp bre,
their wettability due to the physical interaction among hydroxyl
groups of both resin and bre, decreased, in this way reducing the
strength of adhesion holding polymeric resin and bres together
(Lee et al., 2009) and, consequently, allowing their mechanical performance fading.
Concerning the crosslinked biocomposites, it was possible to
evidence a general reduction of rigidity and strength with respect
to the corresponding un-crosslinked samples (Table 3). It is known,
from previous studies (Gleghorn et al., 2008) that when alginate
is cross-linked, it loses its adhesive properties since most of its
active carboxylated and hydroxyl groups are strongly engaged in
physical interaction with calcium ions (Russo et al., 2007); therefore the bonding strength between the matrix and the bres is
substantially reduced and, consequently, the mechanical parameters are negatively affected. Moreover, as previously described
for the ACr samples, the three-dimensional network of crosslinked
biocomposites, obtained in wet condition, did not undergo conformational changing or drastic shrinking after drying process;
this experimental nding implies both the enhancing of the sheets
porosity, as shown in Table 1, and the increasing of free volume of
crosslinked biocomposites; as a consequence, the macromolecular
chain mobility was increased and the exural mechanical properties underwent a fading (Russo et al., 2007, 2010).
Anyway, in crosslinked samples, a slight rising of stiffness was
observed passing by ATH100Cr to ATH70Cr samples; the higher

Table 3
Flexural properties of the laboratory biocomposites sheets.

Fig. 6. Scanning electron micrograph of the A surface sample (a) and of the ACr
surface sample (b).

Sheets

Young modulus (MPa)

10 MPa

Tensile stress at break (MPa)

0.2 MPa

ATH100
ATH90
ATH70
ATH100Cr
ATH90Cr
ATH70Cr

63.62
97.08
81.70
48.05
62.51
78.21

0.71
1.20
0.92
0.46
0.68
0.85

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E. Schettini et al. / Resources, Conservation and Recycling 70 (2013) 919

Table 4
Maximum load and displacement of the biocomposites sheets evaluated by the
puncture test.

1.6

1.4

Sheets

Maximum load (N)

10%

Displacement (mm)
5%

ATH100
ATH90
ATH70
ATH100Cr
ATH90Cr
ATH70Cr

8.7
10.5
14.8
10.4
11.2
15.0

3.59
4.07
4.75
3.22
3.98
4.02

Water up-take (%)

1.2

0.8

0.6

0.4
ATH100

ATH90

ATH70

ATH100Cr

ATH90Cr

ATH70Cr

0.2

0.0
0

10

20

30
40
Dipping time (min)

50

60

70

200.0
180.0
160.0
140.0

Water absorpition (%)

concentration of longer and stiffer bres, such as hemp strands,

together with the strong three-dimensional network, probably
induce the attainment of improved matrix/bre interfacial region,
responsible of the increasing of exural strength (Luo and Netravali,
1999).
Table 4 shows the results of the puncture tests reporting a signicant increase of the resistance to break when hemp bres were
added, both in the un-crosslinked samples and in the crosslinked
ones. The larger aspect ratio of bres, compared to the tomatoes powder, was the main reason of such increase. The inuence
of polymer cross-linking became evident at high bres content
(ATH70Cr), where the break resistance of the sample was much
higher, as occurred in the exural tests. The enhanced displacement measured for the un-crosslinked samples was probably due
to the presence of voids and points of discontinuity provided by
irregular dispersion of higher un-wettable hemp bre concentration. To explain the reduced sensitivity of the puncture test to
cross-linking, in comparison to the exural test, it is important
to consider the different way to apply loads in both the mechanical tests: for the puncture test a local mechanical solicitation is
applied on the sample, whereas in the exural test tensile, compressive and shear stresses are exerted on the lower face, upper
surface and central portion of the specimen, respectively. In Table 5
the weighting increases of the biocomposites as a consequence of
their swelling in water at different times are reported; the nal
water uptake of the sheets, Wst = 60 min (%), calculated by Eq. (2),
are reported too. The swelling kinetics of the samples, Wst = 60 min
(%), and the water up-take percentage, Wst (%), are shown in Fig. 7
as a function of sampling time. The un-crosslinked samples and
the crosslinked ones behaved in different way with two different
kinetics of water absorption (Fig. 7a): the un-crosslinked samples swelled following a slow and regular prole during all the
experimental time, reaching a swelling plateau after 45 min; the
crosslinked samples, on the other hand, experienced a faster kinetic
of water uptaking mainly during the rst minutes of water dipping,
absorbing most of the water and reaching the swelling equilibrium
after the rst 30 min. This probably suggests that all the available binding sites of crosslinked polymeric networks were easily
and swiftly engaged in hydrogen bonding with water. In addition,
it is worthwhile to underline that the water absorption percentage was about 130% for the un-crosslinked samples, and in the
range of 150190% for the crosslinked samples, as shown in Fig. 7b.
These experimental results were in agreement with the previous

1.0

120.0
100.0
80.0
ATH100

ATH90

ATH70

ATH100Cr

ATH90Cr

ATH70Cr

60.0
40.0
20.0

0.0
0

10

20

30
40
Dipping time (min)

50

60

70

Fig. 7. Water up-take percentage (a) and water absorption percentage (b) as a
function of the dipping time of the sheets of un-crosslinked and crosslinked biocomposites.

hypothesis related to the increasing of free volume of crosslinked

polymer. The thickness rising measured on dried and reconditioned
biocomposites suggests that the three-dimensional network was
formed and stabilized during the swelling phenomena, inducing
the increasing of free volume and hence the availability of binding
sites to water molecules. Moreover, the analysis of Table 1 showed
that a particular enhancing of porosity was recorded in the case
of crosslinked samples when hemp bres were added to tomato
peels. For these reasons the water uptaking process of crosslinked
biocomposites resulted enhanced if compared to the water absorption of untreated samples. Moreover, the conformational stability
of crosslinked structures allowed water molecules to easily cover

Table 5
Water up-take values of the laboratory biocomposites sheets; Wd : weight of the sample in the dry state (t = 0 min); Ws : weight of the sample in the swollen states evaluated
every 15 min.
Sample

Wdt = 0 min (g)

Wst1 = 15 min (g)

Wst2 = 30 min (g)

Wst3 = 45 min (g)

Wst4 = 60 min (g)

Wst (%) evaluated by Eq. (2)

ATH100
ATH90
ATH70
ATH100Cr
ATH90Cr
ATH70Cr

0.220
0.190
0.210
0.550
0.580
0.490

0.358
0.331
0.335
0.750
0.930
0.953

0.482
0.420
0.455
1.330
1.450
1.380

0.500
0.425
0.488
1.350
1.450
1.400

0.502
0.435
0.490
1.350
1.470
1.400

128
129
133
145
153
186

E. Schettini et al. / Resources, Conservation and Recycling 70 (2013) 919

17

25

biodegradability (%)

20
ATH100Cr

ATH70Cr

15

10

0
0

10

20

30

40

50

60

biodegradation time (days)

Fig. 9. Biodegradation (%) in soil of the ATH100Cr and ATH70Cr sheets as a function
of time.

Fig. 8. Scanning electron micrograph of ATH100 fracture surface (a) and of

ATH100Cr fracture surface (b).

the straight pathway of biocomposites network, hastily engaging

most of the free binding sites and swiftly reaching the swelling
plateau.
The SEM micrograph of fractured surface of the ATH100 sample highlighted a smooth and regular coating of polymeric matrix
on tomato bre surface and, at same time, an irregular distribution of bres (Fig. 8a). The SEM micrograph of fractured surface of
the ATH100Cr sample showed a rough fracture surface with the
presence of voids dispersed throughout the biocomposite surface,
probably due to the irregular distribution of bres among macromolecular chains, exchanged with zones of regular polymer matrix
diffusion (Fig. 8b). Table 6 reports the chemical elemental analysis, by EDS, of four selected microscopic regions. EDS revealed the
presence of calcium in rather all the selected internal micro-zones;
this result suggests the formation throughout the whole sample of
stable tie points responsible of free volume development, as previously described. This effect is also detectable in SEM micrographs

Table 6
Chemical elemental analysis by energy dispersive X-ray spectroscopy (EDS).
Spectrum

Spectrum 1
Spectrum 2
Spectrum 3
Spectrum 4

71.13
52.16
69.09
37.43

28.87
45.75
29.62
52.96

Na

Ca

0.60

1.49
1.28
6.64

2.96

of ATH90Cr and ATH70Cr samples (data not reported) (Russo et al.,

2007, 2010).
In Fig. 9 the percentages of biodegradation of the ATH100Cr
and ATH70Cr samples as a function of the time are reported; it
was opportunely selected and followed the biodegradation pattern
of the ATH70Cr samples due to the higher concentration of hemp
bres with respect both the ATH100Cr and ATH90Cr samples. During the rst 60 days of permanence in testing soil, it was observed
that the ATH100Cr samples degraded faster than the ATH70Cr samples; in particular the ATH100Cr samples achieved about 20% of
biodegradation whereas the ATH70Cr sample reached 15%. This
nding could be ascribed to the different kind of bres used. Tomato
peels and seeds are short bres based on pectin, starch and cellulose, whose hydrophilic hydroxyl groups along polymeric chains
are easily available to microbial population (Knoblich et al., 2005).
As a matter of fact, being short sized, tomato bres supply a higher
contact surface to soil microorganisms, thus providing a relative
faster biodegradation. On the other hand, hemp bres are longer
and mostly based on microcrystalline cellulose (Amar et al., 2005)
and for these reasons the hydrophilic macromolecular chains are
not easily susceptible to microorganism attack.
Moreover it is worthwhile to highlight the sizeable difference
between the biodegradation rates of lms and crosslinked biocomposites. The lms are based on amorphous polymeric structure
easily available to soil bacteria ora, whereas the biocomposites, due to the presence of cellulose based bres, show a more
structured chemical arrangement able to hinder and to slow the
microbial attack. Moreover, if equivalent exposed surfaces of lms
and biocomposites are considered, it is possible to detect a faster
biodegradation of the lm surface, since in biocomposites microorganisms rstly mineralize the polymeric matrix and following
transform the bres, as shown by Immirzi et al. (2007).
3.2. Field test result
During the rst stage of use, when the seedlings were grown
from the seeds before the transplant, all the biodegradable pots
showed sufcient mechanical resistance to guarantee material
functionality. All the biodegradable pots remained intact throughout the entire period of 35 days from seeding to seedlings
transplanting: the parts of the pots in contact both with the perlite and the air did not show visual biodegradation. In this period
the pots were subjected to a mean greenhouse air temperature of
31.6 C and to a mean greenhouse relative humidity of 53.8%.
The biodegradable pots allowed the development of the root
structure with good branching structure and the development of

18

E. Schettini et al. / Resources, Conservation and Recycling 70 (2013) 919

Fig. 10. Roots development in the ATH100 and ATH90 biodegradable pots and in the polystyrene pot (PS) at seedlings transplanting.

secondary branching, with which the plants up took water and

nutrients. At the transplant, a signicantly dense network of root
hairs developed in ATH100 pots, a dense one in ATH70 pots and a
less dense network in ATH90 pots (Fig. 10). In PS pots, used as control, long roots dominated the root system, reducing overall root
development (Fig. 10). The different pots signicantly inuenced
the seedlings height. The highest seedlings were those grown inside
the ATH100 pots (0.119 m) and inside PS pots (0.115 m); shorter
seedlings were grown inside the ATH90 (0.099 m) and ATH70 pots
(0.100 m) suggesting that the presence of the ller probably inuenced the seedlings growth.
After the transplant, the biodegradable containers degraded
completely in 16 days allowing the passage of the roots through
the containers walls and the growth of the plants. The roots spread
in a radial fashion; no root rot or similar symptoms were observed.
At the end of crop cycle, the different pots inuenced pepper
height. The mean plant height was 0.76 m for the plants grown
inside the ATH90 pots, 0.73 m inside the ATH100 and ATH70 pots.
The control plants were characterized by a mean plant height of
0.67 m.

4. Conclusion
The research showed that wastes and by-products of agro-food
industries and papertextile manufacturing companies, such as
natural bres, may be converted in upgraded products used as
reinforcing solid phase of biocomposites designed for the production of innovative biodegradable pots to be employed for
transplanting process in agriculture. The wastes and by-products,
recycled by means of cost-friendly processes, are environmentally friendly, fully biodegradable and easily available. In addition
biodegradable pots overstay and degrade into the soil with a consequent positive environmental impact, in this way representing
a valid eco-sustainable alternative to the traditional oil-derived
containers, very often cause of environmental pollution, since the
improper post-using discarding.
The use of the biodegradable pots implies the drastic reduction
of man labour related to the pots recovering, cleaning and plants
transplanting.
The eco-friendly methodology of preparation, involving a cold
process, entails low productive costs. Moreover the reduction of
the costs related to the correct disposal of the wastes generated by
agro-food industries and papertextile manufacturing companies
must be considered.
The research showed that the mechanical properties of the biocomposites made of tomatoes seeds and peels, combined to hemp
bres and bound together into the cross-linked alginate network,
are very interesting for the selected application. Laboratory testing was performed on lms and sheets, to well understand the
inuence of water and calcium uptake on the structure of the
materials. It was found a correlation between cross-linking, water
diffusion and mechanical performance. SEM analysis on fracture

surface showed that the bres dispersion needed some improvement, while EDS analysis following the calcium prole, evidenced a
quite regular diffusion of the cross-linker inside the biocomposite.
In terms of horticultural performance, the biodegradable pots
did not cause damage to the plants during the test period but
allowed to develop very dense and active root hair; moreover,
during the transplanting operations, no transplant shock and root
deformation were detected.
Future research should be addressed towards the use of further wastes of agro-food industries such as processing residues of
hazelnuts, citrus fruits, olive oil and wine.
Acknowledgements
The authors shared programming and editorial work equivalently within the areas of their expertise.
M. Malinconico, B. Immirzi and G. Santagata kindly acknowledge
the nancial support of CNR-MISM Program Sviluppo di imballaggi
da fonti rinnovabili per una logistica sostenibile (20072011).
The authors thank Mr. Giuseppe Narciso (CNR) for supporting in
Scanning Electron Microscopy, Mr. Vincenzo di Liello (CNR) for supporting in pots preparation and Dr. Okay Rukaesih, Head of Centre
of Textile in Jawa Barat (Indonesia), for sustaining in biodegradation
tests.
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