Science of the Total Environment 662 (2019) 1–7

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Science of the Total Environment

journal homepage: www.elsevier.com/locate/scitotenv

Three different methods for turning olive pomace in resource: Benefits of

the end products for agricultural purpose
Adele Muscolo ⁎, Teresa Papalia, Giovanna Settineri, Federico Romeo, Carmelo Mallamaci
Department of AGRARIA Mediterranea University, Feo di Vito, 89122 Reggio Calabria, Italy

H I G H L I G H T S G R A P H I C A L A B S T R A C T

• Three different clean processes were

used to transform olive waste in by-
products.
• We produced compost, digestate and
olive pomace-sulphur-bentonite based
pads.
• All the by-products had beneficial ef-
fects on soil fertility.
• All by-products fell into limits for the
marketability established by legislation.
• The best effects on soil were in the order
compostNolive waste-S-padsNdigestate.

a r t i c l e i n f o a b s t r a c t

Article history: In Mediterranean countries the olive oil industry produces, yearly, a huge quantity of pollutant wastes in a short time
Received 13 December 2018 that are phytotoxic for their high content of phenols and wax that affect soil and groundwater quality. With the use
Received in revised form 15 January 2019 of biological processes, we can transform these wastes into fertilizers for a sustainable agriculture. We used three dif-
Accepted 17 January 2019
ferent methods anaerobic digestion, aerobic digestion, and crude agricultural waste management system to produce
Available online 18 January 2019
organic fertilizers. The obtained compounds were chemically analysed to verify if their characteristics fell into the
Editor: Jay Gan marketability limits permitted by the current Italian regulation. Their effects on soil were subsequently assessed. Re-
sults evidenced that all the by-products obtained were suitable as fertilizers. They were able to increase soil organic
Keywords: matter, microbial biomass, and nutrients with beneficial effects on soil fertility, but at different extent. The best ef-
Aerobic digestion, anaerobic digestion fects were in the order: compost, olive pomace-sulphur-bentonite pelletized and digestate. Considering that the
Compost three different methodologies dispose different amounts of olive pomace (90% in aerobic digestion, 12% in anaerobic
Digestate digestion and 5% in sulphur bentonite pelletized) in different time (4 months for compost, 1 month for anaerobic
Olive wastes digestion and 1 day for sulphur-bentonite pelletized) and processing set-up, each method can be differently compet-
Sulphur-bentonite
itive for environment and/or agriculture. Aerobic digestion has economic advantage over other alternatives and has
the greatest fertilizer effect even if the production time is longer than the other two. Digestate, coming from anaer-
obic digestion, reduces the environmental impact of greenhouse gas emissions it is rich in nutrients and can be ob-
tained in a shorter time than compost. Olive pomace-sulphur-bentonite pelletized represents a crude waste
management systems that reduce greenhouse gas emission in the atmosphere producing fertilizers able to generate,
mainly in alkaline soils, a soluble zone of nutrients while minimizing leaching losses to the environment.
© 2019 Elsevier B.V. All rights reserved.

1. Introduction

⁎ Corresponding author. In Mediterranean countries the most common wastes come from the
E-mail address: amuscolo@unirc.it (A. Muscolo). olive sector that produces, yearly, a huge quantity of residues in a short

https://doi.org/10.1016/j.scitotenv.2019.01.210
0048-9697/© 2019 Elsevier B.V. All rights reserved.
2 A. Muscolo et al. / Science of the Total Environment 662 (2019) 1–7

time (November–February) (Azbar et al., 2004; Hansen, 2018). Despite in the agro-food market with economic benefit for the enterprises
the absence of toxic compounds or pathogens these agricultural wastes themselves.
can cause environmental pollution for their high content of polyphe-
nols, wax, volatile solids (138–150 kg/ton olive oil) acidic pH, and 2. Materials and methods
high electric conductivity (Belligno et al., 2005; Doula et al., 2012;
Duarte et al., 2014; Muscolo et al., 2017a, 2017b). 2.1. Raw material
In general, for each ton of olive oil production, about 1560 kg of or-
ganic pollutants (dry basis) are produced (IMPEL, 2003). The polluting Olive pomace, used in the following biological transformation pro-
load related to the disposal of 1 m3 of olive waste is proved to be equiv- cesses, was obtained from a traditional two phases olive oil extraction
alent to 100–200 m3 of urban wastes (corresponding to waste amount process in November 2017 from Mediterranea Foods s.r.l. farm
produced by 100,000 people) (PROSODOL, 2012). However, olive Rizziconi-Reggio Calabria, Italy. The chemical characteristics of olive
wastes are yet rich in minerals and organic compounds except sulphur, pomace were detected as reported in Muscolo et al. (2017a) and are
representing a possible source of nutrients for plant growth and devel- shown in Table 1.
opment. Italy is the second European oil producer country with 90% of
the entire oil production located in Southern Italy: Sicily, Calabria and 2.2. Aerobic digestion
Puglia (Doula et al., 2012). In Italy there are about 6180 olive oil mills
that produce oil based on the national legislative frameworks, which in- 300 L of 90% of pulp and kernel of olives and 10% of straw were
clude that the waste treatment must be done by the industries them- composted in bins, three independent times (replicates) as reported
selves. The majority of factories are small domestic enterprises that in Muscolo et al. (2018). Composting parameters were: mesophilic
don't know risks, solutions and technologies for the treatment of these phase 8 days at 29 °C, thermophilic phase 20 days at 50 °C and
wastes, while the more informed industries are generally not inclined mesophilic phase 92 days at 27 °C. Temperature, moisture and oxygen
to adopt new technologies if the cost is elevated. Thus, in the majority levels were monitored daily. Water was added, when necessary to
of the cases, these wastes are disposed untreated in the environment maintain the moisture at 50%. Mixtures were turned over every day to
(rivers, sea, land, lagoons/ponds) causing serious damage to soil (phys- maintain the oxygen percentage N15% for assuring the aerobic decom-
ical and chemical properties, microbial community and activity) and position of organic matter. After 4 months the whole decomposition
groundwater (Karaouzas et al., 2011; Ashraf et al., 2014). and stabilization of the organic mixture was accomplished. Compost
For the above considerations, their removal represents nowadays, an was air dried sieved at 2 mm and homogenized.
ecological challenge (Souilem et al., 2017) brought to light from the in-
creasing awareness that the climatic change is a waste management 2.3. Crude agricultural waste management
problem (Lackner and Jospe, 2017). Numerous efforts have been done,
up to now, to find several chemical, physical and biological methods The manufacturing process to obtain pellets of 3/4 mm diam. was
for the treatment of olive wastes, which include lagoons, ultrafiltra- performed by Steel Belt System s.r.l. as described in detail in Muscolo
tion/reverse osmosis (Jalo et al., 2018), flocculation-clarification et al. (2017a).
(Zouari, 1998; Roig et al., 2006), thermal concentration and evaporation The mixture constituted from 85% of liquid S, 10% of bentonite clay
(Vitolo et al., 1999; Paraskeva and Diamadopoulos, 2006), incineration (as support and carrier), and of 5% olive pomace was introduced in a
and combustion (Vitolo et al., 1999), combustion and gasification special patented rotary pastillator, which deposited the liquid pads on
(Caputo et al., 2003), but all the above mentioned methods are not a heat exchanger in continuous steel tape for solidification step.
only expensive but are also in part negative for the environment and
human health because of the release of different air pollutants like 2.4. Anaerobic digestion
dust, biomass ash, fly ash/char and greenhouse gaseous (Mishra et al.,
2015). Several research groups have been working on alternative uses This research was carried out in collaboration with Uliva Srl soc.
of these organic residues (Fernández-Bolaños et al., 2006; Salomone Agricola, owners of the biogas plant. Biogas energy plant has an installed
et al., 2015; Valenti et al., 2017) by utilizing biological processes that power of 998 kWel. The digester (U) with a total volume of 4240 m3 was
can represent a safe and sanitizing transformation of these wastes into filled with olive waste 30%, citrus pulp 30% and in minor amount (40%)
organic fertilizers for a sustainable agriculture (Morillo et al., 2009). In with animal manure and maize silage as reported in Panuccio et al.
view of the above considerations, we compared three different biologi-
cal methods: anaerobic digestion, aerobic digestion, and crude agricul- Table 1
tural waste management system (sulphur-bentonite processing Chemical properties of olive pomace used in the production of digestate, compost and
procedure) to transform these wastes in fertilizers. The comparison pads. The data are the mean of three replicates ± standard error.
was made on the basis of physico-chemical characteristics of the ob-
Chemical properties Olive pomace
tained by-products and on the fertilizer power of each of them in re-
pH 5.0 ± 0.1
spect to the time spent on and the amount of wastes used in each
Bulk density (Kg/m3) 608 ± 3.9
single process. The obtained compounds (digestate, compost and olive E.C (mS/cm) 12.0 ± 1.1
pomace-sulphur-bentonite pelletized) were chemically analysed to Moisture (%) 86.7 ± 3.2
verify if their characteristics fell within the parameters established by C (%) 59.52 ± 1.9
the Italian regulations in force. The by-products obtained by waste Total N (%) 1.86 ± 0.6
C/N 32.0 ± 1.9
transformation process can be used as natural soil amendments, only Na+ (mg g−1 dw) 1.85 ± 0.5
if they meet the standard limit values (organic matter N40%, C/N b 30, NH+ 4 (mg g
−1
dw) 0.26 ± 0.03
pH range 6–8.5, absence of pathogens, low levels of heavy metals, and K+ (mg g−1 dw) 39.22 ± 2.3
of inert and glass materials) as reported in the Official Gazette, 1997). Mg2+(mg g−1 dw) 2.23 ± 0.4
Ca2+ (mg g−1 dw) 2.53 ± 0.7
The fertilizer effects of the by-products have been assessed and com-
Cl− (mg g−1 dw) 3.83 ± 0.5
pared each other's on soil properties 90 days after their addition. The NO− −1
2 (mg g dw) 0.001 ± 0.0001
main aim of this work was to find sustainable and cost-effective NO− 3 (mg g
−1
dw) 0.02 ± 0.001
3− −1
methods for both small family-owned companies and medium-sized PO4 (mg g dw) 2.06 ± 0.4
2− −1
enterprises. The specific aim was to develop inexpensive and sustain- SO4 (mg g dw) nd
Water soluble phenols (mg TAEg−1 d.w) 1.84 ± 0.4
able systems for waste disposal to make by-products that can be used
 A. Muscolo et al. / Science of the Total Environment 662 (2019) 1–7 3

(2016) and Muscolo et al. (2017b). The digestate coming from plant was
separated in liquid and solid fractions, chemically characterized as re-
ported in Muscolo et al. (2017b) The chemical characteristics of
digestate, compost and olive-pomace-sulphur-bentonite pelletizedare
shown in Table 2.
2.5. Test of phytotoxicity
Three distinct experiments have been carried out to test the phyto-
toxicity of the obtained by-products following the method of Gariglio
et al. (2002). 10-seeds of Cucumis sativus L for each germination test
were used. The experiments were performed in 9 cm diameter petri
dishes. Compost was used at the concentration of 25, 50, 75 and 100%
w/v, digestate at 10, 25, 50 and 100% w/v and olive-pomace-sulphur-
bentonite pelletized at the concentration of 0.11, 0.22, 0.44, 0.88 and
1.66 mgL−1. The petri dishes were hermetically sealed with parafilm
to prevent evaporation and kept in a growth chamber at a temperature
of 25 ± 1 °C in the dark with a relative humidity of 70%. 6 days after dark
incubation, the numbers of germinated seeds as well as the length of
their roots were recorded. Six replicates were analysed for each treat-
ment. The GI (germination index) which combines measures of relative
seed germination (%) and relative root elongation (%), has been used to
evaluate the toxicity of by-products because germination and root elon-
gation has proven to be the most sensitive parameters, capable of de-
tecting low levels of toxicity which affect the root growth, as well as
high toxicity levels which affect the germination (Tiquia and Tam,
1998), indicating non-phytotoxicity of the by-products when the values
are higher than 60% (Zucconi et al., 1981).
2.6. Soil experiments
Soil was taken from Motta San Giovanni, Loc. Liso, Italy (x:561023,1;
y: 4204908,9; WGS 84 UTM Zone 33 N), the soil is a sandy-loam (11.85%
clay, 23.21% silt, and 64.94% sand) textural class according to FAO soil
classification system (FAO, 1999). The experiment was carried on in
plastic pots (19 cm diameter). The pots have been filled with soil, and
amended with 100 g compost (corresponding to 1.5 q/ha), or 50%
solid digestate fraction, or 0.88 mg olive pomace- sulphur bentonite
pads corresponding to 476 kg sulphur ha−1). The amounts of compost
(A), olive pomace-sulphur bentonite pads (B) and digestate (C), have
been selected on the basis of previous research results that evidenced
Table 2
Chemical properties of compost, digestate, and pads. The data are the mean of three rep-
licates ± standard deviation. Different letters in the same row indicatesignificant differ-
ences among the by-products, (Tukey's test, *p ≤ 0.05).
Chemical properties Compost Digestate Pad
the optimal dose of application for each by-product (Muscolo et al.,
2017a, 2017b, 2018). Non-amended soil was used as control in order
to evaluate in a comparative way the effects of the different amend-
ments on soil chemical and biochemical properties. The experiment
was conducted in glass house to avoid external perturbation (rainfall),
managing the irrigation system to maintain 70% of field capacity. Soil
have been collected 3 months after the treatments. Soils from each pot
were homogenized and sieved (2 mm mesh). The experiment consisted
of 3 pots for each treatment. Soil samples were subdivided in two sub-
samples, one of them was kept at 4 °C for biochemical assays for 24 h
until processing, and the other one was air-dried and sieved (b2 mm).
2.7. Soil chemical analysis
Organic Carbon (OC) was detected following Walkley–Black proce-
dure (1934) and it was converted to organic matter (OM) multiplying
the percentage of C by 1.72; total nitrogen (N) was measured with
Kjeldahl method (Bremner and Mulvaney, 1982). Humic substances
were extracted, dialyzed and fractioned in humic and fulvic acids as re-
ported by Bettany et al. (1980). The C content of humic and fulvic acids
was determined by dichromate oxidation (Nelson and Sommers, 1982).
Phenols were extracted in triplicate with distilled water (Kaminsky and
Muller, 1977, 1978). Total water-soluble phenols (monomeric and
polyphenols) were determined by using the Folin–Ciocalteau reagent,
following the method of Box (1983).Water-soluble phenolic concentra-
tion was expressed as tannic acid equivalents (μg TAE g−1 D.W.). Cat-
ionic exchange capacity (CEC) was determined by using an aqueous
solution of BaCl2 buffered to pH 7.0 to saturate the exchange complex
of soils (Mehlich, 1953).
2.8. Soil biochemical and biological analysis
The amount of microbial biomass C (MBC) was determined follow-
ing the method of Vance et al. (1987) using field moist samples (equiv-
alent to 20 g DW). The filtered soil extracts (both fumigated and
unfumigated samples) were analysed for soluble organic C with the
method of Walkley and Black (1934). MBC was estimated on the basis
of the differences between the organic C extracted from the fumigated
soil and no fumigated soil, and an extraction efficiency coefficient of
0.38 was used to convert soluble C into biomass C (Vance et al., 1987).
Dehydrogenase (DH) activity was determined with von Mersi and
Schinner (1991) method.
Fluorescein diacetate (FDA) reaction was determined according to
Adam and Duncan (2001) procedure.
2.9. Statistical analysis

pH 6.32b⁎ ± 0.05 8.4a ± 0.20 6.5b ± 0.18

Analysis of Variance (MANOVA) was used to test the effects of treat-
Bulk density (Kg/m3) 581b ± 9 775a ± 8 nd ments on soil properties for each case study separately. Treatment
E.C (mS/cm) 1.2a ± 0.25 1.3a ± 0.20 0.9a ± 0.10 means were compared using Tukey's test (Sokal and Rohlf, 1981). All
Moisture (%) 46b ± 3 60a ± 7 nd statistical analyses were performed using Systat v. 8.0 software package
C (%) 42.6a ± 2.40 43.2a ± 1.40 2.2b ± 0.14
(SPSS Inc., Evanston, Ill, USA). P values b0.05 were considered significant
Total N (%) 1.95b ± 0.22 5.3a ± 0.20 0.1c ± 0.03
C/N 21.84a ± 1.66 8.1b ± 0.05 22a ± 8.14 as the probability levels.
Na+ (mg g−1 dw) 1.09a ± 0.06 0.9b ± 0.08 0.16c ± 0.04
−1
NH+ 4 (mg g dw) 0.07b ± 0.02 0.04b ± 0.02 0.6a ± 0.10 3. Results and discussion
K+(mg g−1 dw) 17a ± 1.50 0.31b ± 0.02 0.32b ± 0.04
Mg2+ (mg g−1 dw) 1.30a ± 0.06 0.51b ± 0.08 0.46b ± 0.03
Ca2+ (mg g−1 dw) 2.4a ± 0.28 1.51b ± 0.02 0.13c ± 0.01
Olive pomace is characterized by an acidic pH, an electric conductiv-
Cl− (mg g−1 dw) nd 0.75a ± 0.07 0.17b ± 0.01 ity of 12 mS cm−1, moderate levels of total nitrogen (1.86%), a C/N ratio
NO−2 (mg g
−1
dw) nd nd nd of 32, a high percentage of organic carbon (59.52%), a great amount of
NO−3 (mg g −1
dw) 0.01b ± 0.002 0.41a ± 0.03 0.001c ± 0.0001 potassium (39.22 mg g−1), and a high amount of water soluble phenols
−1
PO3−
4 (mg g dw) 0.41a ± 0.04 0.45a ± 0.09 0.10b ± 0.03
−1 (1.84 mg TAET g−1) (Table 1). The chemical properties fall in any case
SO2−
4 (mg g dw) 0.24 ± 0.02 nd nd
S (%) nd nd 85 ± 6 within the ranges commonly reported in literature for these materials
Water soluble phenols 2.31b ± 0.06 5.02a ± 1.00 1.10b ± 0.15 (Mari et al., 2003; Doymaz et al., 2004; Manios, 2004). The olive pomace
(mg TAE g−1 d.w) was used to produce three different by-products: compost, digestate
ON/TN 91a ± 5 99a ± 8 87a ± 3 and olive pomace sulphur-bentonite pelletized, whose chemical com-
−
NH+ 4 -N/NO3 -N 1.30b ± 0.13 0.34c ± 0.07 2.17a ± 0.11
positions are shown in Table 2. The aerobic digestion process, the
4 A. Muscolo et al. / Science of the Total Environment 662 (2019) 1–7

Germination Germination
100 a ab 120
b a a a

Seed germination (%)

Seed germination (%)

80 100 b
c c
80
60 d
60
40
40
20 20
0 0
25 50 75 100 0.11 0.22 0.44 0.88 1.32 1.66

Compost concentrations (%) Pad mg L-1

Germination
120
a
100
Seed germination (%)

80 b b
60

40

20 c

0
10 25 50 100

Digestate concentrations (%)

Fig. 1. Seed germination percentage of Cucumis sativus L. in presence of selected concentrations (% w/v) of compost, olive pomace-sulphur bentonite pads and digestate.

anaerobic digestion process, and the crude agricultural management sulphur-bentonite pelletized. C/N ratio was much higher in olive
system have been repeated three times and the by-products obtained pomace-sulphur-bentonite pads and compost than digestate. Nutrients
from each of the three independent processes had the same chemical were more concentrated in compost than in the other by-products,
characteristics, so that we can affirm that the procedures adopted can while water soluble phenols were contained in the greatest amount in
be standardized as the results are reproducible over time. Our data the digestate. No significant differences in ON/TN ratio have been ob-
showed that pH was slightly acidic in compost, and olive pomace served among the three by-products, while NH4+-N/NO3−- N was the
sulphur-bentonite pelletized, while it was alkaline in digestate. The EC lowest in the digestate and the highest in the olive pomace sulphur-
was low in all the by-products analysed. Organic carbon content, was bentonite pelletized. The test of phytotoxicity, expressed as germination
significantly greater in compost and digestate. Nitrogen content was percentage (Fig. 1) and germination index (Fig. 2) evidenced that the
the greatest in digestate followed by compost and olive pomace compost tested on seed germination at different concentrations were

Germination index
100
a
90
Germination index (%)

80
70
b b
60
50
40
30
20
10
0
Compost Digestate Pad
Treatments

Fig. 2. Global germination index of Cucumis sativus L. in presence of selected concentrations (% w/v) of compost, olive pomace-sulphur bentonite pads and digestate.
 A. Muscolo et al. / Science of the Total Environment 662 (2019) 1–7 5

Table 3 sulphur-bentonite pelletized and higher than control in soil with

Soil physical and chemical properties of alkaline sandy-loam soils, in pots, amended with digestate (Table 3). Among the soil biological properties considering
compost “A”; sulphur-bentonite + olive pomace, “B”; digestate “C”. Not amended soil was
used as control (CTR). pH, electric conductivity (EC μS/cm); water content (WC, %); water
the CTR as reference point, FDA increased in presence of compost, and
soluble phenols (WSP, μg TAE g−1 dry soil); total organic carbon (TOC %) total nitrogen decreased with the other two treatments, DH increased both with com-
(TN, %), carbon nitrogen ratio (C/N); soil organic matter (SOM, %); fluorescein diacetate post and digestate while decreased with olive pomace sulphur-
(FDA) hydrolysis (fluorescein released, μg g−1 dry soil); dehydrogenase (DH μg INTF bentonite pelletized, MBC increased mainly in presence of compost
g−1 dry soil h−1); microbial biomass (MBC μg C g−1 soil); humic carbon (HC %), fulvic car-
and sulphur-based pads (Table 3). In the control soil a greater HC in re-
bon (FC, %); humic carbon fulvic carbon ratio (HC/FC) and cation exchange capacity (CSC,
cmol(+) Kg−1). The data are the mean of three replicates ± standard deviation. Different spect to FC was found. In soils treated with olive pomace sulphur-
letters in the same row indicate, within each treatment, significant differences (Tukey's bentonite pelletized, and digestate the values of HC and FC were similar
test, p ≤ 0.05). indicating that the mineralization and humification processes were bal-
Treatment CTR A B C
anced. In compost treated soils, prevailed the humification process as
demonstrated by the higher HC in respect to FC value. The CSC was
Texture SL SL SL SL
pH 8.5a ± 0.60 8.0a ± 0.80 7.2a ± 0.40 7.5a ± 0.20
higher in treated soils, especially in presence of digestate, than control.
EC 350c ± 14 450a ± 10 419b ± 12 466a ± 8.00 The concentration of ions changed after the treatments. In respect to
WC 21.5b ± 2.81 27.4a ± 0.79 24.2ab ± 1.70 28.8a ± 1.76 control, Na+ increased with compost and decreased with olive pomace
WSP 14c ± 2.80 45b ± 1.60 41b ± 3.26 96a ± 4.00 sulphur-bentonite pelletized, and digestate, K+ increased only with
TOC 3.1b ± 0.16 4.4a ± 0.15 3.4b ± 0.25 4.6a ± 0.30
compost and digestate. Mg++ increased in all treatments in respect to
TN 0.15 ± 0.01bc 0.22 ± 0.02b 0.33 ± 0.04a 0.13 ± 0.03c
C/N 20.6b ± 0.31 20.0b ± 1.14 10.4c ± 0.49 35.4a ± 4.60 control while calcium decreased. SO4−− increased with compost and
SOM 5.33b ± 0.27 7.57a ± 0.26 5.85b ± 0.43 7.91a ± 0.86 digestate while nitrate and phosphate were found only in soils treated
FDA 42ab ± 1.39 44a ± 1.16 38b ± 1.40 41b ± 3.00 with digestate and in amount greater than in control (Table 4). Cl−
DH 57b ± 2.81 65a ± 1.86 48c ± 3.17 62ab ± 1.95 slightly increased in presence of compost, strongly enhanced with
MBC 835c ± 18 1007b ± 21 1081a ± 44 861c ± 27
digestate (quadrupling its value) while significantly decreased when
HC 0.60a ± 0.05 0.43b ± 0.02 0.66a ± 0.01 0.62a ± 0.03
FC 0.45b ± 0.08 0.26c ± 0.05 0.62a ± 0.03 0.60a ± 0.03 amended with olive pomace sulphur-bentonite pelletized (Table 4).
HC/FC 1.33b ± 0.12 1.65a ± 0.10 1.06c ± 0.04 1.03c ± 0.06 MANOVA analysis, carried on only on the indices of soil quality,
CSC 18.7b ± 1.42 23.10a ± 1.58 22.3ab ± 1.23 23.4a ± 1.36 showed that treatments significantly affected soil biological properties
at different extent (Table 5). SOM, MBC and DH were most positively af-
fected by compost, FDA by olive pomace sulphur-bentonite pelletized
not phytotoxic. The germination index, detected 6 days after germina- and WSP by digestate (F-ratio). In short, our results evidenced a speci-
tion, in presence of compost at 25, 50 and 75% showed values higher ficity between treatment and soil properties showing that the effects
than 80%, falling in the class of phytonutrient. These findings are in of the single by-product obtained were differentiated and property-
agreement with the data of the germination index showing values of specific. The most promising treatments for improving soil fertility
88% that confirmed the non phytotoxicity of the compost. Digestate at were in the following order compostN olive pomace-sulphur-
all concentrations was less effective than compost, at 25% we observed bentonite padsN digestate. These results meet the global trend now fo-
a germination percentage of 70% that decreased increasing its concen- cused on looking for sustainable and controlled disposal of these wastes
tration. The germination index was 60%. In presence of olive pomace- with an efficient bio-transformation into useful by-products to avoid
sulphur-bentonite pelletized up to a concentration of 0.88 mg L−1 all soil and groundwater contamination (Doula et al., 2012). This study ev-
seed germinated, increasing the concentration a progressive reduction idenced that is possible to dispose olive pomace by using three different
in germination percentage (~ 40%) was observed. Germination index methods, with the obtainment of final products placeable on the market
was 60%. with positive consequence on the local bio economy, suggesting that the
All the three treatments, even if differently, influenced the soil integration of different methodologies such as recycling, valorisation,
chemical properties, decreasing the pH and increasing the EC in respect and energy-producing processes, to obtain different kind of high
to the control. The EC values in all the treated and untreated soils were added-value products, can represent an economic incoming both for
in any case far from the value of 4 dS/m that is the threshold to define a farm and industrial sectors (Salomone et al., 2017).
soil as saline. The maximum value of EC (corresponded to 0.46 dS/m) All the three processes used were able to bio-convert the olive pom-
was reached by adding digestate (Table 3). Water holding capacity ace in suitable fertilizers, underlying that the proportion of about 30:1 of
was significantly higher in treated soils than control and the greatest C and N in the starting crude waste is a necessary prerequisite for stim-
values of WC have been found in soil treated with compost and ulating the activity of microorganisms both in aerobic and anaerobic
digestate. WSP significantly increased in all the treatments and the processes to obtain stable products. Our results are in agreements
greatest increase was found in soil treated with digestate. Carbon signif- with previous findings of Nayak et al. (2013) and Muscolo et al.
icantly increased in soils amended with compost and digestate in re- (2018) showing how important is the C/N ratio in the starting material
spect to CTR and olive pomace sulphur-bentonite pelletized treated for driving the biotransformation of the biomass. To be sure of stability
soil. Conversely TN increased much more in soil treated with olive and maturity of the compost, digestate and olive pomace-sulphur-
pomace-sulphur-bentonite pelletized followed by compost. With bentonite pelletized we calculated for each by-product the T value
digestate a decrease in TN in respect to the other treatments and control that is the ratio between the C/N in the by-products and the C/N in
was observed. The C/N ratio was similar to control for soil treated with the starting material (olive pomace), T value = the final C/N ratio/the
compost, lower than control in soil amended with olive pomace initial C/N ratio. T value is an index used to evaluate organic matter

Table 4
Cations (mg g−1 dry soil) and anions (mg g−1 dry soil) detected 3 months after the addition of compost “A”; sulphur-bentonite + olive pomace, “B”; digestate “C”. Not amended soil was
used as control (CTR). The data are the mean of three replicates ± standard deviation. Different letters in the same column indicate, within each treatment, significant differences (Tukey's
test, *p ≤ 0.05).

Treatment Na+ K+ Mg2+ Ca2+ Cl− NO−

2 NO−
3 PO3−
4 SO2−
4

b⁎ c b a c b a
CTR 0.122 ± 0.001 0.108 ± 0.004 0.023 ± 0.001 0.858 ± 0.050 0.206 ± 0.007 nd 0.022 ± 0.0004 0.001 ± 0.002 0.339c ± 0.050
0.130a ± 0.005 0.143b ± 0.007 0.029a ± 0.002 0.468b ± 0.011 0.261b ± 0.020 nd nd nd 0.682a ± 0.101
0.117c ± 0.001 0.110c ± 0.010 0.026a ± 0.001 0.401b ± 0.010 0.175d ± 0.010 nd nd nd 0.344c ± 0.073
0.071d ± 0.001 0.290a ± 0.031 0.027a ± 0.004 0.248c ± 0.013 0.860a ± 0.101 nd 0.050a ± 0.0003 0.098a 0.530b ± 0.721
6 A. Muscolo et al. / Science of the Total Environment 662 (2019) 1–7

Table 5 the other two processes, utilize also a great amount of the pollutant sul-
Analysis of variance of the effects of compost “A”; sulphur-bentonite + olive pomace, “B”; phur, through a short processing cycle, that using a crude agricultural
digestate “C” on total phenols (WSP); soil organic matter (SOM); fluorescein diacetate
(FDA); dehydrogenase (DH) and microbial biomass C (MBC). F-ratio and R2 are shown.
waste management systems, reduce the emission of greenhouse gas in
the atmosphere, even if this process uses electricity in the whole pro-
WSP SOM FDA DH MBC duction cycle. The olive-pomace-sulphur-bentonite pelletized contain-
A F-ratio 277.212 104.780 3.661 16.908 175.747 ing high amount of sulphur is able to low soil pH and to generate,
p-value 0.000 0.001 0.128 0.015 0.000 mainly in alkaline soils, a soluble zone of nutrients while minimizing
R2 0.986 0.963 0.478 0.809 0.978
leaching losses to the environment.
B F-ratio 118.424 3.074 12.333 13.541 90.774
p-value 0.000 0.154 0.025 0.021 0.001
R2 0.967 0.435 0.755 0.772 0.958
4. Conclusion
C F-ratio 846.141 24.432 0.274 6.411 17.947
p-value 0.000 0.008 0.628 0.065 0.013
R2 0.995 0.859 0.640 0.616 0.818 The results of this study showed the best strategies for reusing
wastes from the olive oil processing sector, highlighting the differences
among aerobic, anaerobic and crude processes on the final product ben-
efits. Our results showed that the efficiency of the fertilizer was linked to
stabilization during the biological transformation of the biomass (Jara-
the chemical properties of the products, evidencing the order of their ef-
Samaniego et al., 2017). A T values b0.70 is indicative of maturity
ficacy on soil ecosystem (compost N olive pomace sulphur bentonite
(Zhang et al., 2013), the higher the value, the less mature the obtained
pelletized N digestate). Even if the effects on soil ecosystem were differ-
by-product. In our experiment, all the by-products had values minor
ent we can expect an economic-environmental benefit from all the pro-
than 0.70 and in particular compost 0.68, digestate 0.25 and olive
cesses taken into consideration, but at different extent. Compost can be
pomace-sulphur-bentonite pelletized 0.68, evidencing that all of them
made on farm and used on farm so it represents a Km 0 process, sustain-
had a good degree of maturity and stability. Results on soils 3 months
able from an environmental point of view with economic return.
after the application of compost or digestate or olive pomace-sulphur-
Digestate use reduces the costs for its disposal and at the same time rep-
bentonite pelletized evidenced that all the by-products affected posi-
resents a source of income if used/sell as fertilizer. Olive waste pelletized
tively soil fertility increasing soil organic matter, microbial biomass
with S-bentonite come from a crude process with reduced greenhouse
and nutrient amount, compost was the best treatment for soil because
gas emissions and even if utilizes electricity its use as ecological fertilizer
it influenced positively not only the enzymatic soil activities, but also in-
can improve the productivity of soils and lower the alkalinity of soils
creased more than the other two treatments the HC/FC ratio (1.65). The
avoiding the use of other more expensive methods.
ratio between the total humic carbon (HC) and total fulvic carbon (FC),
is a well-recognized index of polymerisation, which evidences the grade
of stabilization of organic matter as already reported by Silva et al. Acknowledgments
(2016).
The stability of compost, digestate and olive pomace-sulphur- Research Project Agrifoodtech PON03pe_00090_2 (modelli
bentonite pelletized was also determined by testing the response of sostenibili e nuove tecnologie per la valorizzazione delle olive e dell'olio
Cucumis sativum L. seeds to their extracts at different concentrations. extravergine di oliva prodotto in Calabria) Funded by The Italian Minis-
Results evidenced that seed germinated in any condition but, increasing try of Education, University and Research. We are especially grateful to
the concentration of each extract the germination progressively and Steel Belt System s.r.l for providing pads of olive waste pelletized with S-
slightly decreased. The greatest decrease was observed with high con- bentonite, Uliva Srl soc. Agricola, for the digestate and Mediterranean
centration of digestate. The data in any case confirmed the stability of Food s.r.l for providing olive wastes.
these by-products as suggested by Tiquia et al. (1996) and Sellami
et al. (2008) and evidenced that they were not phytotoxic because the References
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