Agricultural use of microfiltered olive mill wastewater: effects on maize production and soil properties

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1 Aville online t ScienceDirect Agriculture nd Agriculturl Science Procedi 00 (2015) IRLA 2014 Agriculturl use of microfiltered olive mill wstewter: effects on mize production nd soil properties M. Kokkor *, P. Vyrls, Ch. Ppionnou, K. Petrotos, P. Gkoutsidis, S. Leontopoulos nd Ch. Mkridis Deprtment of Agriculturl Engineering Technologists, TEI of Thessly, Lriss, 41110, Greece Deprtment of Biosystems Engineering, TEI of Thessly, Lriss, 41110, Greece Astrct The disposl of olive mill wstewter (OMWW) is considered s one of the most serious environmentl prolems in the Mediterrnen region. This study constitutes prt of holistic OMWW mngement pproch iming t the production of high dded vlue products from OMWW with zero dischrge. OMWW constitutes n orgnic mteril tht could e recycled ck to the soil fter its tretment with microfiltrtion, nd used s liquid fertilizer for plnt production, thus leding to n environmentlly friendly cultivtion method with minor cron footprint, since wstewter would (prtilly or fully) sustitute minerl fertilizers, fresh wter svings, nd lso economic enefits to the frmer. Microfiltered OMWW (MF-OMWW) ws pplied to mize cultivtion in cly lom soil using two rtes of 25 nd 50 Mg h -1, with the ddition of minerl fertiliztion of 200 kg N h -1. Furthermore, tretment of only MF-OMWW pplied t the rtes of 50 Mg h -1 nd n only minerl fertiliztion tretment were used. The four tretments were replicted four times. The results of the 1 st yer experiment showed tht the different mounts of MF-OMWW used hd no significnt effect on soil properties. Mize yield, kernel moisture nd ft content were not significntly influenced y the different tretments, wheres kernel protein, strch, fier nd sh content were significntly ffected. Considering ll qulity nd quntity prmeters studied, the tretment with only minerl fertilizer N ppliction gve similr results with the only MF-OMWW tretment, indicting the potentil of minerl fertilizer full sustitution y MF-OMWW, under the conditions of our study Pulished y Elsevier B.V. Keywords: olive mill wstewter; microfiltrtion; liquid fertilizer; mize yield; kernel qulity; cly lom soil 1. Introduction Olive mill wstewter (OMWW) is y-product of the olive oil extrction process tht consists of vegettion wter, nd wter used in the vrious stges of the oil extrction process [1]. OMWW constitutes serious environmentl prolem in the Mediterrnen re, due to its high polluting lod, minly referring to its high solids * Corresponding uthor. Tel.: ; fx: E-mil ddress: mkokkor@teilr.gr.

2 Author nme / Procedi Agriculture 00 (20145) nd orgnic compounds, high COD content, phytotoxic properties nd resistnce to iodegrdtion cused y its phenolic compounds [2, 3]. As mtter of fct, the pollution effect of 1 m 3 of OMWW is considered equivlent to m 3 of domestic sewge. As olive oil production in Greece is crried out minly y smll or smll medium enterprises, the OMWW produced is usully pplied untreted to nery lnd, in order to void tretment costs. Reserch hs shown tht the ppliction of untreted OMWW to griculturl soil my increse soil orgnic mtter, ville P nd K [4], nd totl N content [5], ut lso it my increse soil electricl conductivity, slinity [5] nd modify the equilirium of useful soil microorgnisms [6]. Moreover, it my result in germintion prolems due to phytotoxic effects of the phenolic compounds contined in the OMWW [7, 8]. Crop response in the OMWW pplictions is lrgely dependent on species sensitivity. Reserch work hs shown tht ryegrss nd proteic pe yields were incresed with untreted OMWW ppliction, wheres clover yield ws negtively ffected [4]. Olive trees nd lso olive fruit yield nd qulity were not ffected y OMWW ppliction [9]. In nother study, lthough mize growth ws not ffected, plnt stress prmeters were found incresed following the untreted OMWW ppliction [5]. On the other hnd, the phenolic compounds contined in the OMWW re nturl ntioxidnts, with commercil nd economic interest. Memrne filtrtion of OMWW my led to significnt decrese of its orgnic lod nd suspended solids content [2, 10], nd lso to seprte polyphenols from the mss of wste [1, 11, 12]. OMWW tretment with microfiltrtion (MF) hs shown tht polyphenols cn e effectively seprted in the permete [1]. Polyphenols my then e successfully removed with the use of suitle resins [13, 14]. As result, the recovered polyphenols, my e utilized in the phrmceuticl, cosmetic nd food industry, nd the remining effluent will hve decresed phytotoxic properties, nd thus it my e more sfely used in griculture. Reserch on the gronomic effects of treted OMWW ppliction to griculturl soil is limited. OMWW treted with ctivted chrcol nd clcium hydroxide resulted in significntly improved seed germintion of Itlin ryegrss [15]. Incresed productivity of mize nd whet ws oserved following the ddition of OMWW processed, y liming nd storge in pond, nd microilly, respectively [16, 17]. This pper descries the gronomic effects of 1 yer ppliction of treted OMWW, y microfiltrtion nd resin, for polyphenols removl, to mize cultivtion, with prticulr regrds to crop yield nd qulity, nd soil properties. 2. Mterils nd methods 2.1. Microfiltered olive mill wstewter (MF-OMWW) A smple of pproximtely 10 Mg of OMWW ws collected from Alevizos olive mill, locted in Pyrgetos villge, Lriss, centrl Greece. Initilly, the rw OMWW ws centrifuged t 1200 rpm using rotry finisher ering stinless screen with holes of 150 μm dimeter. As second step, the treted OMWW ws microfiltered using cermic microfiltrtion memrne of 200 nm pore size to seprte the polyphenols (permete) from oil sustnces. Finlly, the permete produced in the second step ws treted with the XAD4 mcroporous resin, which hs the ility to retin selectively the polyphenols [14], iming to minimize ny phytotoxic effects. Some qulity properties of the produced MF-OMWW re presented in Tle 1. Tle 1. Microfiltered olive mill wstewter qulity properties. Prmeter Vlue ph 4.73 EC (ms cm -1 ) 9.91 TSS (%) 4.15 Aville P (mg L -1 ) 1680 Extrctle K (mg L -1 ) 1440 NH 4-N (mg L -1 ) 86

3 Author nme / Procedi Agriculture 00 (2014) Field experiment A field experiment ws undertken on cly lom soil (41% snd, 20% silt, 39% cly) t the experimentl frm of Technologicl Eductionl Institute of Lriss, Greece, in Topsoil qulity properties re presented in Tle 2. Tle 2. Topsoil properties t the eginning of the experiment. Prmeter Vlue ph 7.3 EC (ms cm -1 ) Orgnic mtter (%) 1.4 CCO 3 (%) 1.8 Totl N (%) 0.08 Olsen P (mg kg -1 ) 6,5 Extrctle K (g kg -1 ) Extrctle Mg (g kg -1 ) MF-OMWW ws pplied using two rtes of 25 nd 50 Mg h -1, with the ddition of minerl fertiliztion of 200 kg N h -1. Furthermore, tretment of only MF-OMWW pplied t the rtes of 50 Mg h -1 nd n only minerl fertiliztion tretment of 200 kg N h -1 were used. Ech tretment ws pplied to n individul plot of 60 m 2 (6 m x 10 m, including 8 plnt rows), using complete rndomized lock design with four replictes. Mize (Ze mys) ws used s the monitoring crop. Crop sowing ws t the rte of 8.6 seeds m -2, nd took plce on My 25, To ensure germintion, 30 mm ws pplied y sprinkler irrigtion t sowing nd n dditionl irrigtion of 50 mm ws pplied lter for seedling estlishment. Wter nd MF-OMWW were pplied through drip irrigtion system, employing four mnifolds. Ech mnifold supplied set of four plots with one drip lterl per two djusted plnt rows. The volume of required wter controlled y flow meter instlled t upstrem of ech mnifold. The 20-mm dimeter emitting pipe used, is commonly utilized for field crop irrigtion, with pressure compensting emitters t 1 m spcing, dischrging 3.6 liters per hour. MF-OMWW ws pplied through the drip system utilizing 120 L tnk connected to the min line nd mnipulting throttling vlve to crete differentil pressure level. Ech tretment received wter nd MF- OMWW filtered through 1" conventionl mnul clening disk filters of 150 mesh. A preliminry 120 mesh screen filtrtion ws operted on the min pipeline of the system. The secondry filters were clened fter ech MF- OMWW ppliction. Mnul flushing of the lterls ws performed every third week. Five pplictions of MF- OMWW took plce etween 1 July nd 8 of August delivering in totl 1200 L for the two 50 Mg h -1 MF-OMWW ppliction rte tretments nd 600 L for the 25 Mg h -1 MF-OMWW ppliction rte tretment. An utomtic wether sttion in the experimentl field mesured solr rdition, ir temperture nd humidity, nd wind speed. These were used to clculte dily reference evportion (ET o ). The irrigtion pplied through the drip system ws scheduled using reference evportion nd growth stge sed crop coefficient, ccording to FAO- 56 methodology [18]. There ws 108 mm of rinfll during the experiment. Totl wtering during the growing seson ws 500 mm with 310 mm pplied through the drip system for ll tretments. Fertilizer nitrogen ws pplied s mmonium nitrte using the fertilizer tnk t rte of 20 g N m -2. All tretments were irrigted t 100% crop evpotrnspirtion (ET c ) during the full seson. Crop production ws determined t hrvest (Septemer 20, 2013) y mesuring fresh nd dry weight of mize ers. Mize ers were hrvested y hnd from 10 mize plnts from the centrl four rows of ech experimentl plot, when their dry mtter content ws on verge 12.5%. Mize ers dry mtter yield ws determined y drying the ers in ventilted oven t 60 C, until constnt weight. After drying, mize kernels were seprted from the rest of the er, grinded, nd then nlysed for protein, strch, sh nd fier content, using n utomtic ner infrred nlyser. Soil smples were collected three dys fter hrvest. Smples were tken from 0-30 cm depth, from ech plot. Soil smples were nlysed for ph, EC, Olsen P, totl N, extrctle K, C, Mg, N, NH 4 -N nd NO 3 -N.

4 Yield (Mg h -1 ) Averge er mss (g) Author nme / Procedi Agriculture 00 (20145) The effect of ech tretment on crop nd soil mesured vriles were ssessed y ANOVA t the level of sttisticl significnce of p<0.05, nd mens were seprted y Duncn s test using the sttisticl progrm SPSS (Edit. 17.0). 3. Results nd discussion 3.1. Crop production Mize yield, which ws determined y mesuring the ers fresh mss, ws not significntly ffected y the different tretments s shown in Fig.1 (left). Averge fresh nd dry mss of mize er re presented in Fig. 1 (right). Although the differences etween the tretments re not sttisticlly significnt, there is trend for etter yield with the MF-OMWW ppliction t the rte of 50 Mg h -1. This finding proly suggests tht other nutrients contined in the MF-OMWW, rther thn N, my hve influenced crop production. As fr s mize kernel qulity is concerned, kernel moisture nd ft content were not significntly influenced y the different tretments, wheres kernel protein, strch, fier nd sh content were significntly ffected (see Fig. 2 nd 3). MF-OMWW ppliction t the rte of 25 Mg h -1 comined with minerl fertilizer N ddition resulted in higher protein nd sh content in comprison to the only MF-OMWW ppliction. The lter, however, resulted in higher strch content. Generlly, in ll tretments, kernel strch content responded in different mnner thn kernel protein nd sh, which is in good greement with other reserch work [19, 20]. Riedell [19] showed tht kernel protein nd minerl P nd K content were higher, wheres strch content ws lower, in plnts grown under higher N input, which my lso pply to the findings in our study. Also, since the er yield ws out 20% higher for the only MF-OMWW tretment compred to the MF-OMWW tretment t the rte of 25 Mg h -1 with the ddition of minerl fertilizer N, the yield (on kg h -1 sis) of protein, strch nd sh, is expected to e similr for the two tretments, which indictes tht crop response to the different tretments ws limited. The importnt thing to note, however, is tht considering ll qulity nd quntity prmeters studied, the tretment with only minerl fertilizer N ppliction gve similr results with the only MF-OMWW tretment, indicting the potentil of minerl fertilizer full sustitution y MF-OMWW, under the conditions of our study Fresh Dry Tretments 80 Tretments Fig.1.Mize yield (ers fresh weight) (left), nd Averge er mss (fresh nd dry) (right) for the different tretments (N: 200 kg N h -1, 25: 25 Mg MF-OMWW h -1, 50: 50 Mg MF-OMWW h -1 ). Columns lelled with the sme letter re not significntly different (P>0.05).

5 Ash (%) Fier (%) Protein (%) Strch (%) Author nme / Procedi Agriculture 00 (2014) ,, 65 55,, Tretments Tretments Fig. 2. Mize kernels protein (left) nd strch (right) content for the different tretments (N: 200 kg N h -1, 25: 25 Mg MF-OMWW h -1, 50: 50 Mg MF-OMWW h -1 ). Columns lelled with the sme letter re not significntly different (P>0.05) ,, 5 4,, Tretments 2 Tretments Fig. 3. Mize kernels sh (left) nd fier (right) content for the different tretments (N: 200 kg N h -1, 25: 25 Mg MF-OMWW h -1, 50: 50 Mg MF-OMWW h -1 ). Columns lelled with the sme letter re not significntly different (P>0.05) Soil properties No significnt differences etween the different tretments were oserved regrding ll mesured soil properties (ph, EC, ville P, extrctle K, Mg, N, C, totl N, nd NO 3 -N), with the exception of NH 4 -N. Tle 3 summrizes the results for the different tretments. The lck of soil response to the MF-OMWW ppliction is minly ttriuted to the reltively low rtes of ppliction used, nd lso to the fct tht it ws the first yer of ppliction. Other studies, which hve shown increse in soil EC, P nd N content following the ppliction of

6 Author nme / Procedi Agriculture 00 (20145) treted OMWW (using other methods, e.g. lgoon stiliztion), used higher rtes of treted OMWW ppliction [21, 22]. Tle 3. Soil properties following one yer MF-OMWW ppliction to mize cultivtion on cly lom soil. Men vlues per tretment re only represented if sttisticlly differences were found. In this cse, numers followed y different letter re sttisticlly different. Soil properties 50 Mg OMWW kg N Tretments (per h) 25 Mg OMWW kg N ph 6.2 EC (μs cm -1 ) P (mg kg -1 ) 5,9 K (mg kg -1 ) 383,3 Mg (mg kg -1 ) 1336,9 Totl N (%) 0.1 NO 3-N (mg kg -1 ) Mg OMWW 200 kg N NH 4-N (mg kg -1 ) c 4.3c 9.7 N (mg kg -1 ) C (mg kg -1 ) Economic nlysis Although crop nd soil response to one yer MF-OMWW ppliction ws limited, it ws evident tht MF- OMWW ws cple to fully sustitute the fertilizer N pplied, under the conditions of our study. Considering tht tody the price of wter solule mmonium nitrte (which is the fertilizer used in this study) is out 0.46 per kg, nd the fct tht this is fertilizer commonly used y the frmers in the re t the rte of 200 kg N per h, tht leds to svings up to out 267 per h. However, MF-OMWW trnsporttion costs should lso e tken into considertion. The preprtion of MF- OMWW, s descried in this pper, is not considered s n extr cost to the frmer, s it will e performed y the olive mill in order to reclim the high dded vlue polyphenols. As olive mills in Greece re scttered in different res, for trnsporttion distnce of round 50 km etween the olive mill nd the frm, n verge trnsporttion cost is round 5 per Mg of MF-OMWW. Hence, for n ppliction of 50 Mg MF-OMWW per h, the cost ccounts to 250 per h. In this cse, frmers svings re limited (only out 17 per h). However, the ctul svings re expected to e higher following consecutive pplictions, due to potentil soil meliortion. Moreover, in nother cse scenrio, the trnsporttion costs my e chrged to the olive mill. Other work hs shown, tht lnd ppliction of OMWW t mximum nnul rte of 420 m 3 h -1, nd considering n nnul production of 1500 m 3 OMWW nd 10 yer period of trnsporttion equipment use (including the required investment costs: trctor nd triler with tnk), cost less thn per kg processed olive fruit [9]. 4. Conclusions The results of the 1 st yer of MF-OMWW ppliction to mize production suggested tht MF-OMWW could fully sustitute minerl fertilizer N. Crop production ws not enhnced y minerl fertilizer nitrogen ddition to the MF-OMWW treted soil. Soil properties were not negtively ffected y the ppliction of MF-OMWWW. Considering the economics of MF-OMWW ppliction, lthough there ppers to e economic enefits to frmer from the minerl fertilizer sustitution, the trnsporttion costs need to e tken into considertion. Further work is necessry to evlute the effects of MF-OMWW ppliction to griculturl soil in the longer term.

7 Author nme / Procedi Agriculture 00 (2014) Acknowledgements This reserch hs een co-finnced y the Europen Union (Europen Socil Fund - ESF) nd Greek ntionl funds through the Opertionl Progrm "Eduction nd Lifelong Lerning" of the Ntionl Strtegic Reference Frmework (NSRF) - Reserch Funding Progrm: ARCHIMEDES III. Investing in knowledge society through the Europen Socil Fund. References [1] Petrotos KB, Lellis T, Kokkor MI, Gkoutsidis PE. Purifiction of olive mill wstewter using microfiltrtion memrne technology. J Mem Sepr Tech 2014; 3:50-5. [2] Zirehpour A, Jhnshhi M, Rhimpour A. Unique memrne process integrtion for olive oil mill wstewter purifiction. Sep Purif Technol 2012; 96: [3] Zglis DP, Arvniti EC, Ppdkis VG, Prskev CA. Sustinility nlysis nd enchmrking of olive mill wstewter tretment methods. J Chem Technol Biotechnol 2013; 88: [4] Montemurro F, Dicono M, Vitti C, Ferri D. Potentil Use of Olive Mill Wstewter s Amendment: Crops Yield nd Soil Properties Assessment. Commun Soil Sci Pln 2011; 42: [5] Belqziz M, Lkhl EK, Mouod H.D, El Hdrmi I. Lnd spreding of olive mill wstewter: effect on mize (Ze Mys) crop. J Agron 2008; 7:297-8 [6] Brer AC, Mucieri C, Cvllro V, Ioppolo A, Spgn G. Effects of olive mill wstewter on soil properties nd crops, review. Agr Wter Mnge 2013; 119:43-10 [7] Mekki A, Dhoui A, Sydi S. Polyphenols dynmics nd phytotoxicity in soil mended y olive mill wstewters. J Environ Mnge 2007; 84:134 6 [8] Mssoudinejd MR, Armn K, Aghyni E. Ecologicl risk ssessment to olive mill wstewter (OMW) with iossy on plnt species. Eco Env & Cons 2014; 20:229-5 [9] Chrtzoulkis K, Psrrs G, Moutsopoulou M, Stefnoudki E. Appliction of olive mill wstewter to Cretn olive orchrd: effects on soil properties, plnt performnce nd the environment. Agr Ecosyst Environ 2010; 138: [10] Russo C. A new memrne process for the selective frctiontion nd totl recovery of polyphenols, wter nd orgnic sustnces from vegettion wters (VW). J Memr Sci 2007; 288: [11] Cssno A, Conidi C, Drioli E. Comprison of the performnce of UF memrnes in olive mill wstewters tretment. Wter Res 2011; 45: [12] Rhmnin N, Jfri SM, Glnkis CM. Recovery nd removl of phenolic compounds from olive mill wstewter. J Am Oil Chem Soc 2014; 91:1-18 [13] Weisz GM, Schneider L, Schweiggert U, Kmmerer DR, Crle R. Sustinle sunflower processing I. Development of process for the dsorptive decoloriztion of sunflower [Helinthus nnuus L.] protein extrcts. Innov Food Sci Emerg Technol 2010; 11: [14] Petrotos KB, Gkoutsidis PE, Kokkor MI, Ginkidou KG, Tsgrelis AG. A study on the kinetics of olive mill wstewter (OMWW) polyphenols dsorption on the commercil XAD4 mcroporous resin. Deslin Wter Tret 2013; 51: [15] Brer AC, Mucieri C, Ioppolo A, Milni M., Cvllro V. Effects of olive mill wstewter physic-chemicl tretments on polyphenol tement nd Itlin ryegrss (Lolium multiflorum Lm.) germinility. Wter Res 2014; 52:275-6 [16] Moretis D, Stmti FE, Nikolidis NP, Klogerkis N. Olive mill wstewter irrigtion of mize: Impcts on soil nd groundwter. Agr Wter Mnge 2011; 98: [17] Cereti CF, Rossini F, Federici F, Qurtino D, Vssilev N, Fenice M. Reuse of microilly treted olive mill wstewter s fertilizer for whet (Triticum durum Desf.). Bioresource Technol 2004; 91:135-5 [18] Allen RG, Pereir LS, Res D, Smith M. Crop Evpotrnspirtion: Guidelines for Computing Crop Wter Requirements. Irrigtion nd Dringe Pper 56, Rome: United Ntions Food nd Agriculture Orgniztion (FAO); 1998 [19] Riedell W.E. Nitrogen fertilizer pplictions to mize fter lflf: grin yield, kernel composition, nd plnt minerl nutrients. J Plnt Nutr 2014; 37: [20] Urielrre M, Below FE, Moose SP. Grin composition nd productivity of mize hyrids derived from the Illinois protein strins in response to vrile nitrogen supply. Crop Sci 2004; 44: [21] Sierr J, Mrtí E, Gru A, Cruñs R. Effects of the gronomic use of olive oil mill wstewter: Field experiment. Sci Totl Environ 2007; 378:90-4. [22] Komintss K, Zhrki D. Pre-tretment of olive mill wstewters t lortory nd mill scle nd susequent use in griculture: Legisltive frmework nd proposed soil qulity indictors. Resour Conserv Recy 2012; 69:82-7.