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Biol Fertil Soils (2000) 32 : 222–227 Q Springer-Verlag 2000

ORIGINAL PAPER

C. Paredes 7 A. Roig 7 M.P. Bernal


M.A. Sánchez-Monedero 7 J. Cegarra

Evolution of organic matter and nitrogen during co-composting


of olive mill wastewater with solid organic wastes

Received: 14 June 1999

Abstract Four olive mill wastewater (OMW) com-


posts, prepared with three N-rich organic wastes and
Introduction
two different bulking agents, were studied in a pilot Great amounts of olive mill wastewater (OMW) are
plant using the Rutgers system. Organic matter (OM) produced in Mediterranean countries, where this waste
losses during composting followed a first-order kinetic causes a great environmental impact. OMW is com-
equation in all the piles, the slowest being the OM mi- posed of the tissue water of the fruit, the water used for
neralisation rate in the pile using maize straw (MS). the different steps of oil production, olive pulp, muci-
The highest N losses through NH3 volatilisation oc- lage, pectin, oil, etc., suspended in a relatively stable
curred in the mixtures which had a low initial C/N ratio emulsion.
and high pH values during the process. Such losses Several methods have been proposed for OMW dis-
were reduced considerably when MS was used as the posal, based on evaporation ponds, thermal concentra-
bulking agent instead of cotton waste (CW). N fixation tion and different physico-chemical and biological
activity increased during the bio-oxidative phase before treatments, as well as its direct application to agricul-
falling during maturation. This N fixation capacity was tural soils as an organic fertiliser (Martínez Nieto and
higher in piles with a lower NHc 4 -N concentration. Only Garrido Hoyos 1994). However, very little research has
the composts prepared with OMW, CW and poultry been performed into the composting of OMW. Tomati
manure or sewage sludge reached water-soluble or- et al. (1995) found that by composting OMW with
ganic C (CW) and NHc 4 -N concentrations and CW/Norg wheat straw a material can be obtained with a high lev-

and NHc 4 /NO 3 ratios within the established limits which el of humification and without phytotoxic effects. Par-
indicate a good degree of compost maturity. Increases edes et al. (1996b) studied the mineralisation and hu-
in the cation-exchange capacity, the percentage of hum- mification of the organic matter (OM), the N losses and
ic acid-like C and the polymerisation ratio revealed that the biological N fixation during composting of OMW
the OM had been humified during composting. The sludge with maize straw (MS) or cotton waste as bulk-
germination index indicated the reduction of phytotox- ing agents. Also, Galli et al. (1997) studied the micro-
icity during composting. biological aspects of OMW-wheat straw composting,
and Paredes et al. (1999) composted agroindustrial
Key words Olive mill wastewater 7 Composting 7 wastes with or without OMW, and found that the addi-
Organic matter degradation 7 Nitrogen fractions 7 tion of OMW produced a greater degradation of OM,
Humification higher pH and electrical conductivity (EC) values and
greater losses of total N (NT) than the pile without
OMW.
For OMW to be co-composted, it has to be absorbed
on a solid substrate, such as lignin-cellulosic wastes,
and be provided with a N source, since this liquid waste
has a high moisture content and C/N ratio. In this way,
C. Paredes 7 A. Roig 7 M.P. Bernal (Y) it is possible to transform OMW into organic fertilisers
M.A. Sánchez-Monedero 7 J. Cegarra free of phytotoxicity, which can improve soil fertility
Department of Soil and Water Conservation and Organic Waste and plant production. Therefore, the aim of the present
Management, Centro de Edafología y Biología Aplicada del
Segura, CSIC, PO Box 4195, 30080 Murcia, Spain
work was to study the co-composting of OMW with sol-
e-mail: pbernal6natura.cebas.csis.es id organic wastes, paying special attention to the evolu-
Tel.: c34-68-215717, Fax c34-68-266613 tion of OM and N.
223

Analytical methods
Materials and methods
The composted samples were analysed for EC and pH in a 1 : 10
Experimental procedure (w/v) water-soluble extract, while the dry matter content was as-
sessed by drying at 105 7C for 12 h and OM by determining the
Four different mixtures of OMW were prepared with three or- loss on ignition at 430 7C for 24 h (Navarro et al. 1993). NT and
ganic wastes rich in N: poultry manure (PM), sewage sludge from organic C (Corg) were determined by automatic microanalysis
a treatment plant of municipal wastewater (SS), and an industrial (Navarro et al. 1991), as were water-soluble organic C (CW), 0.1-
waste from orange juice extraction, containing pulp, seeds and M-NaOH-extractable organic C (CEX) and fulvic acid-like C
peel of this fruit (OIW). To these wastes were added two bulking (CFA), the latter after precipitation of the humic acid-like C
agents: a waste from cotton gin (CW) and MS (Table 1). The con- (CHA) at pH 2.0 (Sánchez-Monedero et al. 1996). The CHA was
centration of potentially toxic heavy metals of SS was below the calculated by subtracting the CFA from the CEX. NHc 4 -N was ex-

limits set by the EU directive for SS use in agricultural soils tracted with 2 M KCl from the frozen subsamples and determined
(Council of the European Communities 1986) (data not shown). by a colorimetric method based on Berthelot’s reaction (Sommer
CW and MS had similar hemicellulose and lignin contents (ap- et al. 1992), adding sodium citrate to complex divalent cations.
proximately 25% for both parameters), whereas the cellulose NO3–-N was determined by ion chromatography in a 1 : 20 (w/v)
content was higher in CW than in MS (40.4% and 32.0%, respec- water extract. N fixation was assayed by gas chromatography ac-
tively). cording to Cacciari et al. (1989) in a compost sample (1 g dry
The mixtures were prepared in the following proportions on a weight) incubated for 72 h at 30 7C in 0.9% NaCl (25 ml). After
fresh weight basis (dry weight basis in brackets), where OMW1 HNO3/HClO4 digestion, P was determined colorimetrically as a
and OMW2 indicate waste water from two different olive mills: molybdovanadato phosphoric acid and K by flame photometry.
1. Pile 1 : 36% PMc64% CWc1.9 l OMW1 kg –1 (12 : 84 : 4). The cation-exchange capacity (CEC) was determined with
2. Pile 2 : 33% SSc67% CWc0.9 l OMW1 kg –1 (9 : 88 : 3). BaCl2–triethanolamine (Lax et al. 1986). The germination index
3. Pile 3 : 78% OIWc22% CWc2.1 l OMW2 kg –1 (35 : 53 : 12). (GI) was calculated using seeds of Lepidium sativum L. (Zucconi
4. Pile 4 : 47% SSc53% MSc1.8 l OMW1 kg –1 (15 : 80 : 5). et al. 1981). Losses of OM and NT were calculated from the initial
Piles 1 and 3 were watered with OMW until days 18 and 52, re- (X1) and final (X2) ash contents according to the equations of
spectively, whereas in the two other piles the OMW was added Paredes et al. (1996a).
only on the first day. OM loss (%)p100–100 [X1(100–X2)]v[(X2(100-X1)]
The mixtures (about 2000 kg) were composted in a pilot plant
in trapezoidal piles (1.5 m high with a 2!3-m base). The Rutgers NT loss (%)p100–100 [(X1N2)v(X2N1)]
static pile composting system was used, involving on-demand ven- where N1 and N2 are the initial and final NT concentrations, re-
tilation through temperature feedback control (Finstein et al. spectively.
1985). The air was blown from the base of the pile through the
holes of three PVC tubes of 3 m length and 12 cm diameter. The
timer was set for 30 s of ventilation every 15 min, and the ceiling
temperature for continuous air blowing was 55 7C. Piles 1, 2, 3 and Results and discussion
4 were turned after 13, 27, 66 and 49 days, respectively, in order
to improve both the homogeneity of the material and the fermen- OM degradation
tation process. The bio-oxidative phase of composting was consid-
ered finished when the temperature of the piles was stable and
close to that of the atmosphere, then the air-blowing was stopped OM mineralisation was substantial in all mixtures dur-
to allow the composts to mature over a period of 2 months. Four ing the bio-oxidative phase (Fig. 1a,b), whereas it was
samples per mixture were selected at different stages of the com- low during the maturation phase (0.4%, 0%, 3.1% and
posting process: 11.2% for piles 1, 2, 3 and 4, respectively), which indi-
1. From the initial non-decomposed mixture (I).
2. From the thermophilic phase (T).
cated product stability after the bio-oxidative stage.
3. At the end of the bio-oxidative phase (E). The degradation of OM during composting, as de-
4. From the mature compost (M). termined by the OM lost, followed a first-order kinetic
The samples were taken by mixing six subsamples taken from six equation:
points in the pile, spanning the whole profile (from the top to the
bottom of the pile). Each sample was divided into two parts, one OM losspA (1-e – kt)

of which was immediately frozen and kept for NHc 4 -N and NO3 -N
analysis, while the other subsample was air-dried and ground to where A is the maximum degradation of OM (%), k the
0.5 mm for analysis. rate constant (days –1) and t the composting time (days).

Table 1 Analysis of the starting materials: two different olive mill orange industry waste (OIW) (dry weight basis). EC Electrical
wastewaters (OMW1 and OMW2), cotton waste (CW), maize conductivity, OM organic matter, Corg organic C, NT total N, n.d.
straw (MS), poultry manure (PM), sewage sludge (SS) and not determined

OMW1 a OMW2 a CW MS PM SS OIW

pH (H2O) 5.5 5.2 7.1 7.2 7.6 6.8 3.6


EC (S m –1) 0.53 0.66 0.41 0.30 0.89 0.42 0.25
OM (%) 1.3 2.5 82.8 77.4 66.5 67.3 94.1
Corg (g kg –1) 9.2 17.2 422.8 386.6 348.0 354.0 451.4
NT (g kg –1) 0.2 0.4 21.0 7.0 54.6 65.9 19.6
C/N 46.0 43.0 20.1 55.2 6.4 5.4 23.0
–1
NHc 4 -N (mg kg ) n.d. n.d. 530 154 27595 7980 709
P (g kg –1) 0.1 0.1 1.8 0.7 19.2 38.7 1.5
K (g kg –1) 1.2 4.1 17.4 8.3 21.3 9.5 18.7
a
Data of OMW in w/v (g l –1 or mg l –1)
224

Table 2 Parameter values of the first-order equation describing


OM degradation (SE in parentheses). A Maximum degradation
of OM (%), k rate constant, t composting time, pile 1 PM c CW
c OMW, pile 2 SS c CW c OMW, pile 3 OIW plus CW c
OMW, pile 4 SS c MS c OMW; for other abbreviations, see Ta-
ble 1

A(%) k(days –1) Residual F


mean
square

Pile 1 55.0 (1.4) 0.0598 (0.0046) 4.03 658.54 **


Pile 2 68.4 (1.6) 0.0594 (0.0056) 13.48 402.15 **
Pile 3 66.5 (2.2) 0.0377 (0.0037) 12.72 414.16 **
Pile 4 72.5 (19.8) 0.0226 (0.0046) 32.34 128.91 **

** P~0.01

uct of A!k. The use of MS as bulking agent (pile 4)


instead of CW (pile 2) substantially reduced the OM
degradation rate, since the value of k was approximate-
ly 2.5 times lower for pile 4 than for pile 2, although
both had a similar value of A. This reduced decomposi-
tion rate may have been due to the greater particle size
of the MS compared with the CW. Ajwa and Tabatabai
(1994) also found that C from MS mineralised more
slowly in soil than that from other plant wastes.
The decomposition of OM brought about an in-
crease in pH and EC in all piles (Table 3), as a conse-
quence of the degradation of acid-type compounds
such as those with carboxylic and phenolic groups and
the mineralisation of organic compounds, such as pro-
teins, amino acids and peptides to inorganic com-
pounds, such as NH3. After that, the pH showed a gen-
eral decrease which, as shall be seen later, is associated
with the beginning of the nitrification process. The C/N
ratio fell sharply in all the mixtures at the beginning of
decomposition, before stabilising and reaching values
of between 9.4 and 12.0 after the maturation phase.
Fig. 1 Organic matter (OM) losses during composting of piles 1
These final values suggested that all the composts had
[poultry manure (PM) c cotton gin wastes (CW) c olive mill reached an acceptable degree of maturation, since all
waste (OMW)], and 2 [sewage sludge (SS) c CW c OMW] (a), the C/N ratios were ~12, the limit accepted for mature
and piles 3 [orange industry waste (OIW) c CW c OMW] and 4 compost (Bernal et al. 1998). The CW concentration de-
(SS c MS c OMW) (b). Lines represent curve-fitting creased during the composting process (Table 3) be-
cause of the high proportion of easily biodegradable or-
ganic compounds (sugars, amino acids, peptides, etc.)
Curve fitting of the experimental data gave the param- in this fraction. The CW level of the composts ranged
eter values shown in Table 2. All equations were signif- from 0.89% to 3.31%, so that only composts 1 and 2
icant at P~0.01, although the OM degradation kinetics could be considered as sufficiently mature according to
of piles 1, 2 and 3 fitted this equation better than the the threshold value of ~1.7%, suggested by Bernal et
results obtained for pile 4, as shown by the lower F and al. (1998) as representing a good degree of maturity.
higher residual mean square values of the latter. These The CW/Norg ratio also fell during the process to reach
A values were within the range found by Bernal et al. in all cases, except pile 3, values ~0.7, the value consid-
(1996) in a composting study of sweet sorghum bagasse ered as indicating a mature compost (Hue and Liu
with sewage sludge or animal manure (68.3% and 1995).
60.2% OM), whereas only the pile prepared with sweet
sorghum bagasse and sewage sludge gave a value of k
close to that of pile 4. N transformation
The rate of OM decomposition was greater when
PM (pile 1) or SS (pile 2) was used as the N source, as The NT concentration increased in all the piles, proba-
is demonstrated by the higher value of k and the prod- bly as a consequence of a concentration effect due to
225

Table 3 Evolution of the main parameters during initial (I), thermophilic (T), end of bio-oxidative (E) and maturation (M) phases of
the composting process (dry weight basis). CW water-soluble organic C; for other abbreviations, see Tables 1 and 2

Sample Compost- pH EC Corg C/N CW (%) CW/Norg NT NHc4 -N NO3–-N –


4 /NO3
NHc
ing (days) (H2O) (S m –1) (g kg –1) (g kg –1) (mg kg –1) (mg kg –1)

Pile 1
I 0 7.5 0.52 407.2 15.0 2.98 1.25 27.1 3385 ~0.4 n.d.
T 21 8.0 0.65 359.5 11.5 2.74 0.94 31.2 1916 77 24.88
E 49 7.8 0.78 334.3 9.7 2.25 0.70 34.6 861 1511 0.57
M 109 7.4 0.83 337.3 9.7 1.59 0.51 34.7 286 3019 0.10
Pile 2
I 0 7.1 0.44 405.5 21.5 2.35 1.35 19.2 1365 ~0.4 n.d.
T 42 7.8 0.60 334.6 11.0 1.88 0.67 30.4 2130 173 12.31
E 84 7.6 0.73 300.9 10.1 1.40 0.50 29.9 287 1690 0.17
M 144 7.8 0.77 293.6 9.4 0.89 0.32 31.1 314 2739 0.12
Pile 3
I 0 6.0 0.41 425.5 20.5 7.46 3.75 20.8 846 ~0.4 n.d.
T 42 9.5 0.66 371.4 12.3 5.45 1.87 30.2 945 ~0.4 n.d.
E 84 9.7 0.59 352.6 11.5 3.51 1.18 30.7 928 69 13.45
M 144 9.7 0.64 345.3 10.7 3.31 1.05 32.4 583 173 3.37
Pile 4
I 0 6.5 0.42 472.0 31.0 4.79 3.51 15.2 1608 ~0.4 n.d.
T 28 7.7 0.57 408.8 18.5 2.88 1.34 22.2 652 ~0.4 n.d.
E 63 7.4 0.76 415.4 13.9 3.04 1.09 30.0 697 684 1.02
M 123 7.5 0.84 394.3 12.0 2.04 0.67 32.8 661 1749 0.38

the weight reduction of the pile (Table 3). The concen- N fixation activity increased during the bio-oxidative
tration of NHc 4 -N fell during the process; however, only phase before falling during maturation (Fig. 2a–d). N
for piles 1 and 2 did it fall below 400 mg kg –1 after the fixation capacity was higher in piles 3 and 4 because
maturation period, which is the maximum recom- they contained less NHc 4 -N than the other two piles (De
mended value for a mature compost (Zucconi and De Bertoldi et al. 1982), the period of N gain in pile 4 coin-
Bertoldi 1987). Although a substantial quantity of NO3– ciding with the maximum fixation value. Although
was observed in most of the mixtures by the end of the much has been written about N fixation activity in soil,
bio-oxidative phase, maximum values were only little has been published on this topic with respect to
reached after maturation. The addition of PM as a N- composts. N fixation activity has been studied in OMW
rich waste (pile 1) produced the greatest degree of ni- sludge compost (Paredes et al. 1996b) and sawdust
trification, since the resulting compost had the highest compost (Kostov and Lynch 1998).
NO3– concentration (3019 mg kg –1). However, nitrifica-
tion was hardly evident in the pile with OIW (pile 3)
since most of the NHc 4 -N was probably lost through vo- OM humification
latilisation as a result of the high pH observed during

composting (Table 3). The NHc 4 /NO3 ratio fell during The humification ratio, expressed as (CEX/Corg)!100,
the composting process in all the piles; after the matu- and the humification index, calculated as (CHA/
ration period values ranged from 0.10 to 3.37, meaning Corg)!100, showed little variation during the compost-
that only composts 1 and 2 could be considered suffi- ing process (Table 4), so that they could not be consid-
ciently mature according to the maximum ratio of 0.16 ered as good indicators of the humification process.
suggested by Bernal et al. (1998). This coincides with the findings of Iglesias-Jiménez and
In general, NT losses were substantial during the Pérez-García (1992) in a study of city refuse com-
bio-oxidative stage (Fig. 2a–d), but practically non-exis- posts.
tent during the maturation stage. NT losses in all the The humification process was best revealed by the
mixtures were below those frequently observed during general increases in percentage of humic acid-like C
composting (50% N) (Witter and López-Real 1987). (PHA) [PHAp(CHA/CEX)!100], CEC and CHA/CFA and
The use of MS considerably reduced N losses, an effect CEC/Corg ratios throughout the composting process
also noted by Mahimairaja et al. (1994) in composts of (Table 4). However, the established values of CEC
PM and different lignocellulosic wastes. This reduction 1 60 mEq 100 g –1 (Harada and Inoko 1980) and CEC/
was probably due to the higher initial C/N ratio of Corg 1 1.9 mEq g –1 (Iglesias-Jiménez and Pérez-García
pile 4 (Table 3), so that the NHc 4 -N formed would have 1992) cannot be used as maturity indicators in this ex-
been rapidly immobilised within the microbial biomass. periment, since these values were exceeded at the be-
Indeed, decreases in NHc 4 -N were observed during the ginning of the experiment. Also, the final values of PAH
thermophilic step (Table 3) although there were no and the CHA/CFA ratio depended on the origin of the
losses of NT in the same period (Fig. 2d). wastes used. Similar findings were observed by Bernal
226

Fig. 2 N losses and biological


N fixation during composting
of piles 1 (a), 2 (b), 3 ( c) and
4 (d). NT Total N, N2 final NT
concentration; for other ab-
breviations, see Fig. 1

Table 4 Evolution of humification indices, cation-exchange ca- acid-like C, CHA/CFA ratio of humic acid-like C/fulvic acid-like C,
pacity (CEC) and germination index (GI) during I, T, E and M GI germination index; for other abbreviations, see Tables 2 and
phases of the composting process (dry weight basis). HR Humifi- 3
cation ratio, HI humification index, PHA percentage of humic

Sample HR (%) HI (%) PHA (%) CHA/CFA CEC a CEC/Corg GI (%)


(mEq 100 g –1) (mEq g –1)

Pile 1
I 17.67 8.54 48.33 0.94 106.5 2.05 13.2
T 19.02 10.72 56.39 1.30 140.1 2.71 29.8
E 20.35 10.99 53.99 1.17 161.2 3.04 45.2
M 16.58 8.72 52.60 1.11 168.4 3.14 76.9
Pile 2
I 14.27 6.98 48.93 0.96 94.2 1.88 38.6
T 12.68 5.39 42.43 0.74 260.1 4.76 66.1
E 13.33 6.48 48.59 0.95 235.4 4.41 83.2
M 10.88 4.62 42.44 0.74 233.2 4.48 94.4
Pile 3
I 28.42 7.14 25.13 0.34 99.3 1.99 0
T 21.57 11.59 53.74 1.16 129.7 2.57 40.9
E 11.85 5.86 49.47 0.98 174.3 3.29 62.9
M 14.49 7.79 53.70 1.16 197.1 3.68 58.9
Pile 4
I 30.28 18.93 62.53 1.67 84.8 1.61 19.5
T 25.23 15.29 60.60 1.54 114.4 2.32 77.9
E 27.38 17.70 64.63 1.83 131.8 2.52 83.6
M 26.14 16.38 62.62 1.69 152.3 2.88 91.3
a
Ash-free material
227

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