Characterisation of the biodegradability of post-treated digestates via the chemical accessibility and complexity of organic matter Géraldine Maynaud, Céline Druilhe, Mylène Daumoin, Julie Jimenez, Dominique Steyer, Michel Torrijos, Anne-Marie Pourcher, Nathalie Wéry
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Géraldine Maynaud, Céline Druilhe, Mylène Daumoin, Julie Jimenez, Dominique Steyer, et al.. Characterisation of the biodegradability of post-treated digestates via the chemical accessibil- ity and complexity of organic matter. Bioresource Technology, Elsevier, 2017, 213, pp.65-74. 10.1016/j.biortech.2017.01.057. hal-01606007
HAL Id: hal-01606007 https://hal.archives-ouvertes.fr/hal-01606007 Submitted on 26 May 2020
HAL is a multi-disciplinary open access L’archive ouverte pluridisciplinaire HAL, est archive for the deposit and dissemination of sci- destinée au dépôt et à la diffusion de documents entific research documents, whether they are pub- scientifiques de niveau recherche, publiés ou non, lished or not. The documents may come from émanant des établissements d’enseignement et de teaching and research institutions in France or recherche français ou étrangers, des laboratoires abroad, or from public or private research centers. publics ou privés. Version postprint errors maybediscoveredwhichcould affect content,and the al review oftheresultingproofbe manu The manuscript. the of version early this providing are we acce been has that manuscript unedited an of file PDF a is This 2017.01.057 matter, organic of complexity and pos of biodegradability the of Characterisation N., Wéry, A-M., Please 27January2017 cite this article as: Maynaud, G., Druilhe, C., Daumoin, January2017 24 2016 2December Accepted Date: Revised Date: S0960-8524(17)30094-9 Received Date: BITE17552 To appearin: Reference: DOI: PII: Dominique Patureau,MichelTorrijo Géraldine Maynaud,CélineDruilh ical accessibilityandcomplexityoforganicmatter Characterisation of the biodegradability of post-treated digest Accepted Manuscript post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057 Bioresource Technology http://dx.doi.org/10.1016/j.biortech.2017.01.057 fore it is published in its fin fore itispublishedinits Comment citer cedocument: e, MylèneDaumoin,JulieJimene s, Anne-MariePourcher,Natha Bioresource Technology
al form. Please note that during the production process during the form. Pleasenotethat al ates via the chem- the via ates M., Jimenez, J., Patureau, D., Torrijos, M., Pourcher, (2017), doi: l legaldisclaimers that app pted for publication. As a service to our customers our to service a As publication. for pted t-treated digestates via the chemical accessibility chemical the via digestates t-treated script will undergo copyediting, typesetting, and typesetting, copyediting, undergo will script lie Wéry z, http://dx.doi.org/10.1016/j.biortech. ly to the journalpertain. Version postprint post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, Here, the organic matter stability Here,compared bet matter wasthe organic digestateTheismatter organicstability keyof a Abstract Tel: 51 42 4 *Corresponding68 E-ma 86; author. +33 c b a Patureau GéraldineMaynaud mattercomplexity and accessibility organic of biodegradability post-tr Characterisation the of of with biodegradableorganic significantmatter a eas phaseaftersolidfractions obtained con separation slowly composted digestateswhichcomprised accessi biodegradability complexityorganic matter. of and complexityPost-treatmentsprese matter. organicof biodegradabilityfluorescenceandspectroscopy, was usingassessedcomplexitywerematter organicofch typeslinearbothbiodegrada ofcorrelation between highlighted complexitythe organic between matter relationship Université France BretagneLoire, AvenueEtangs,INRA, des LBE, F-11100 102 Narbonne, Irstea, UR OPAALE, 17 avenue de Cucillé, CS64427, R Cucillé, avenue UR 17 CS64427, OPAALE,Irstea, de Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057 a , Michel, Torrijos .
Respirometric activity CH and Comment citer cedocument: a ,Céline Druilhe a , Anne-Marie , Pourcher
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MylèneDaumoin 4 yields in batch tests showed a yields tests in positive showed batch parameter for its use in itsuse for agriculture. parameter tained aremainingoftained substantial part b,c ily accessible fraction comprisingfractionilyaccessible bility(R Biodegradabilitylow for was ween 14 post-treated ween digestatesand post-treated 14 nted a significanta thented on effect and biodegradabilityand was , and , Nathalie Wéry emical extractions combined with emicalcombined extractions mostly anti-correlated with mostly anti-correlated eated digestateseated thevia chemical il address: [email protected]:il ble complex molecules. Inversely,molecules.ble complex b, c b, ennes, F-35044, ennes, France F-35044, ,France , Julie , Jimenez 2 =0.8). The accessibilityThe =0.8). and a*
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1 Version postprint post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, CODtot: Total chemicalTotal(gO CODtot: demand oxygen CO (gO BOD:oxygendemand Biological potentialBMP:Biomethane (NLCH biodegradabilityBDana:Anaerobic CODtot) (% AerobicBDaero: CODtot) biodegradability(% AT AD:digestion Anaerobic Abbreviations Keywords: todigestates help valorizati should optimize their simplerpost effectmolecules.Understanding of the (mmO rate OUR: uptake Oxygen OM:Organicmatter OFMSW:wastemunicipalOrganicof fraction solid O organicextractableCODtot) NEOM: Non (% matter MSW:Municipalwaste solid fraction MH: (%BDaero) biodegradable slowly easilyMB:fraction (%BDaero) biodegradable DRI DOM: dissolved organicmatter 2 Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057 : Oxygen 4 2 : Cumulativeoxygen in (gOfour days uptake 24 : Carbon dioxide :O Average digestate; biodegradability; complexity; biodegradability;digestate; anaerobic Comment citer cedocument: 2 uptake rate in the 24 h of maximum activityin hmaximum24 of uptake rate the (mgO
2 h -1 4 kg kg 2 kg -1 -1 VS) VS) VS) VS) -1 VS) 2 kg -1 on. on. 2 kg VS) VS) -treatment on theon -treatment biodegradability of -1 VS) digestion;respirometry 2 h -1 kg -1 VS) VS)
2
Version postprint post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, which(Tam ideallycaninorganic fertilizer replace potentialdigestateorganicThe fu isfertilizer. a methaneinto (CH Introduction 1. VS: Volatilesolid solidTotal TS: CODtot) SolubleSPOM: particularextractable from fraction Slowly (% SEOM: organicextractableCODtot) matter RT:time Retention ReadilyREOM:organicextractableCODtot) (% matter PoorlyCODtot) (% PEOM: matter organic extractable landfully prior toapplication.to be The assessed fulfil also standards, current landbefore are generallyapplication recommended a Consequently,assuch post-treatments solid-liquid which compounds ca cellulosic process the digestion containpresentbiodegradability residual compl and times,when2010).applicationAt (Tegliad al., et digestateassessment value theof agronomic and of theon CH focus optimization of
Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057 Anaerobic digestionis Anaerobicbiological (AD) a treatment To be used as anas be To organicstabilityused b fertilizer, or Comment citer cedocument: 4 ). It can thus produce energy, It digestatecanproduce whilethethus ). i.e.
efficiency safetyal., 2011). et (Teglia and 4 production from rarely from organicthebut productionwaste on lly fermented nutrient-rich llyfermented material biodegradability of organic residues biodegradability residues organicof igestate is not fullycanit igestateisnot stabilized, bone et al., al., 2010).bone et Many studies separation, separation, composting, drying or ex organic elements such assuch exorganic ligno- elements its valorisation through land land itsvalorisation through extractable (% matter organic nnot degrade (Bayard et al.,(Bayard et degrade 2015). nnot nd the fertilizer produced should thefertilizernd produced iodegradabilityhasdigestate a of
thatconverts waste organic is regarded as a regardeda as is
3 Version postprint post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, their application, they can be exposed toaeroapplication,theirexposed boththey be can can conditions. organicAsbe direc either residues (CO dioxide theThesemethodsare based oxygenaerobic on (O and (Cossu respirometricbeen tests considered have (>30time-consuming Forthese a days). method reaso anotheret thusle (Raposo laboratoryal., 2011) to al.,the(Schievano2008). et However,residues BMP applied method measuringb common for the anaerobic assessing potentialboth wastof the organicbiogas Thecontent theofbiome al., use 2004). et (Godley includingbiological methods ma organicdry matter, Zach,(BinnerWagl and anaerobic testmethods 1999; incluusingcanevaluated (i)biological be methods solidfractions dried seven digestateof solid and anaerobicaerobicconditions post-treated and 14 of investigate to Thethis are(i) study objectives of digestates. informational.,However, et is conc 2015). scarce Raga,andal.,Barrena Ponsá (Cossu2008; 2008; et its organic for waste treatment,biological before tests havebetweenanaerobic aerobicand repor been theircomplementaryprovideson information charact assessmentaerobic biodegradabilitytheirof under Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057 2 ) production which are related to OM )to related which production are biodegradation Comment citer cedocument:
the biodegradabilityboth the under fractions of digestate obtained after fractionsdigestateof obtained suchcompostingprocesses AD as or ading to large ading to discrepancies.is also It bic and anaerobic and environments. An bic tly applied on land or stored stored land prior on to or tlyapplied erning sucherning on correlations e and and It e digestate. is most the and anaerobicandconditions thus ding aerobic respirometric tests and dingaerobicrespirometric tests and thane potential test (BMP) aims attest(BMP) thane potential 2 digestates (seven composted ordigestates (seven composted ) measurementcarbon uptakeor ) et al., 2009; Bohm et al., et al., Bohm 2009; et Liu2010; Raga, 2008; ScagliaRaga,2008; al., 2010). et tter (OM) and(OM) totaltter organic carbon tedespecially severalbyauthors, test vary one protocolcan from eristics. Furthermore, correlations Furthermore, eristics. ns,alternativeapproachesas such and et al., 2009) and al.,2009) (ii) et non- and iodegradabilityorganicof under controlledunder
4 Version postprint post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, phase separation, 1 dried and composted solid fract composted phaseand solid 1 dried separation, T4S)T2S,A1S, SL2S,T1S, digestate T3S, obt (SL1S, AD sitesFourteen i from 13 digestatesweresampled Sampling 2.1. digestates of Materialmethods 2. and theseof organic residues. help theto could define This stability.digestate characterizationbiodegradability descriOM and and 3Dchemicalfluorescencespectros fractionationsto Thi has wastesbeenal.,2015) et applied. (Jimenez characterizethe to method accessibi both developed post-treatmentsof their impact characteristics on characterizeseparation)(ii) to liquid-solid and t characterisationPhysico-chemical 2.2. digestate of forfurtherkg 50 werehomogenized analyses. each) theirin digestates origins arepresented and Table ther digestiondry,ormesophilic (wet processes or food (FPW (OFMSW), processingfraction waste MSW of municipal wastewatertreatment(WWTP), plant solid various includingwaste,sitestypes treated agrof solidA4C,fractions S composted (A3C, digestateof Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057 Comment citer cedocument:
heir OM in order to better assess OMheir into better theorder better strategies for agriculturalstrategies betterre-use for icultural waste, sewage sludge from a sewageiculturalwaste, from sludge and stability. In this view, astability.recent and view, this In 1. All of the samples collected (about theAll (about ofsamples 1. collected mophilic). The designationThethe mophilic). of s method combinessmethod successive ion of digestate (A2D) and of ion (A2D) 6 digestate copy. The final goalfinalThe copy. was correlating litycomplexityorganic and of s s bingpost-treatmentofthe on effect L1C, O1C,O2C,The M1C). L1C, AD n France: 7 solidfractions nFrance: of 7 waste(MSW),the organic ained following ained solid-liquid ), all ), different accordingto
5 Version postprint post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, 2007). The respirometric device consisted of 10 L respirometric2007). The device ofh consisted 10 thebulk density)accordingdynamic a resp using to biodegradabilityThe freshon measured aerobic was (BDaero)Aerobic 2.3.1. biodegradability assay Residual biodegradability2.3. assays expressedin gO K wasby Then,afterCODtot titrationdetermined µm. samplemeasurements,(CODtot) thedemand was dried sampleh. °Cthis calcination 3 550 dried for at of 105(VS)°Cvolatileatsampleh.The 48 for solid each(TS) the sample, tests.For solidconten total kg) Representative2digestateof w aliquots (about and stablelow value. a fellto Zurich,respirometricThefi testwas Switzerland). every mingases aweremonitored 2 using paramagnet theduringexperiment,oxygen therespirometric con thetoInme substrate. conditions order throughout h airL (360the recirculationexhaust part of of to thetemperaturewaterwhilepreheated a bath the airwithwasrate flow70 of continuous supplied a inertascellat Each maintained bulkingwas agent. Thesewithsubstrate cells. studied werefilled the 2 Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057 Cr 2 O 7 in accordance T90-101. AFNORNFstandard with the 2 kg Comment citer cedocument: -1 -1 VS. All measurements were performed in triplicate.VS.wereperformed measurements All
-1
), thus ensuring homogeneous ),thus homogeneous ensuring smixedwith actingringsPall plastic Prior to total chemical to Prior oxygen g measured wast of drying by100 content was measured after contentwasmeasured nally halted when nallyO halted the asure the asure O Lh 40 °C by means of a water bath and°Cwaterbath a means by 40 of ere used to all ereused theperform analytical eration system also included a included rapid erationsystem also irometrical.,et (Berthemethod ermetically sealed stainless ermeticallysealed steel centrations of thecentrationsoutlet ofinlet and digesting 1 g of TS withgH TS 1 of digesting digestates (between 2 and4(between2 kg digestates -1 ic analyser (Magnos 206, ABB,ic(Magnos analyser 206, . The incoming air was. ground toground a 500 size particleof 2 2 uptake rate uptakerate (OUR) CODtotwere results 2 uptakerate 2 SO
4 and 6 Version postprint post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, associated withassociatedtheallof biodegrada disappearance thirdlyand consumption, the of (iii) stabilization that(MH) the toOM be be has slowlybiodegradable OURto andexponentialgrowthassumed decrease corr and OM biomassthe(MB) biodegradable growth easily OURmax, a risevalue, (2005): firstly a peak to (i) conceptual typicalA approach b profiles hasof OUR (BOD(gO BDaero(%CODtot)= according Equational., CODtot, et 1 (Liu 2015). to couldexpresse aerobicbiodegradabilitybe (BDaero) maximum activityin averagehthe of OUR 24 (Ponsa ATsubstrate: O (BOD) Thetheofoxygendigestate demand biological thevalues2represented3) or cumulative (i=1, O second and during theoffirst, th the rising phase andvaluesMB2MB3peak: the the MB1, represented c andsimplifiedMHestimation thepeaks.wasMB A of singletypicalatypical a profiles peak,OURwith p endogenousrespiration. todiffeDuring study, this characterisedvaluethecumulative O cumulativeO and carriedthe MHestimation M could MB ofbe out: Onthe the biomass. respirationtheseof of p basis 2 Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057 classicalindi the uptakeduring Two test. aerobic 2 4 consumption duringconsumption risinguntil thephase, OURmax, related to therelated to cumulative O Comment citer cedocument:
2 2 kg -1 2 VS) x/ VS)CODtot(gO 100) uptake during the decrease phase, from OURmax phase,decreasefrom uptakeduring the 2 uptake in four inandfour daysDRIuptake OURconstantlow and value a at ird peak respectively, and the respectively, MHi peakird and 2 revious assumptions, a simplified a assumptions, revious consumption during consumption decreasing the associated withassociatedof the biodegradation rent OUR profilesOURrent wereobtained: rofiles with two or three rofilesO or with two
ble OM and OM the endogenous ble ces were also calculated for each werealsoces calculated for d as theas betweenratio and BOD d een al. et bydescribed Trémier hydrolysed before hydrolysedbiological before Bvalue representedthe corresponded to thetocorrespondedcumulative et al., 2010). Moreover, the al., 2010). et Moreover, n performed for each for n separated performed espond the biodegradation to of umulative O umulative , secondly , in a the break (ii) 2 kg -1 VS) (1) while the MHwhile the 2 consumption consumption 24 related to thetorelated 2 uptake
7 Version postprint post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, respectively.The CH and displacementgas chromatographymethod (Perkin gas and twice production compositionwereestimated andconstant a under darkdigestate Each shaking. w and stoppers aluminiumi gas-tightsealsrubber and withsolutionin flushedflaskwas N (2.5g L bicarbonatesolution gfresh 200following of weres digestate protocol: inocul fresh Thison wasdigestate measured without to Antest wasquantify batch re used anaerobic the (BDana)Anaerobic 2.3.2. biodegradability assay calculations,MBidescribed MHi and wereexpressed and thefirst, thirdphasesecond peak,respecti of theend at theofexperimentproduction was i taken theanaerobic analyscurves of tests werenotbatch (2) = (CH BDana(%CODtot) al. Liuet (2015). CH biodegradabilityas Anaerobic expressed was (BDana) hPa). 1013 inNL CH Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057 4 yieldCODtot and theof studied in digestate, acco Due to thelow frequencyDue CH of 4 kg -1 of VS under standard temperaturestandardcondunder VS of pressure and Comment citer cedocument: 4 yield wasyield calculated experimentalresult using the 4 yield(NLCH -1 ) inmLflasks.ensure anaerobic 500 conditions,) To
2 for a fewseconds. flasksa The for with weresealed 4 4 measurements (twice a week), themeasurements(twicekinetic week), a kg -1 VS) x 100) / x CODtot(gO(0.35 VS)x 100) vely. Followingvely.thepreviously
uspended in 200 mL of sodiummL in ofuspended 200 ed. Onlycumulativeed. the CH sidualCH nto account. account. nto ncubated at 37 °Cat for ncubated days 40 in 37 the as tested inBiogas tested as duplicate. ation for 40 ationdays40 the for using a weekwatera a using in%BDaero. the betweenofratio themean rdance with the Equation 2 rdanceof Equation 2 with the Elmer Clarus®580), Elmer 4 production in production digestate. itions°C and (0 s and expressed sand 2 4 kg
the -1
VS)) 8 Version postprint post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, sequential acid extractions (25 mL of H mLof sequential acidextractions (25 °C rpm, and (iv) 30 h300 atpoorly extractibleOM NaOHmL sequentialstrongof basic(30 extractions °C minrpm, and 15 (iii) slowly30 300 at extractib NaOH salineNaClmLof basic (30 extractions and 10 300 rpm, (ii)°C (REOM) readily extractibleand OM CaClmL extractionsof (30 werethenextractible soluble (SPO obtained: OM (i) gsample.fract Four wereperformed 0.5 on dried of th mm grindedand was to and 1 particle dried size, according characterised JimenwasOrganic matter to extractionssequentialChemical 2.4.1. Organicmattercharacterisation 2.4. Fluorescence 2.4.2. spectroscopy analysis %aseachof ResultsareCODtot expressed fraction. ISO accordance15705:2002with inthestandard orde totalresidues (COD) The ofoxygen chemical demand at filtered µm. 0.45 recoveredwas OM bythe centrifugation solubilised extractedfromthe sample subtractingOM thetotal rpm.°C 30 300 at the non-extractibleand Finally, Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057
Comment citer cedocument: 2 solution 10 mM) of themin mM) 10 of remaining15 solution pellet for
2 SO 4 72% (w:w)) of theremaining h 72% of 3 (w:w)) pelletfor OM (NEOM)calculatedwas OM by le OM (SEOM) produced after fourafter le (SEOM) OM produced e following e sequential extractions from the initial OM. At eachAt from theinitial step, OM. (PEOM)after produced two ions of decreasing accessibility ionsdecreasing of M) produced after four sequentialafter four M) produced . . (18600 g at 4 °C for g°C at min) 20 and4 for (18600 0.1 M)theremaining pellet of 4 0.1 for ez et al. (2015). Firstly,al. et (2015). sample the ez produced after foursequentialafter produced r tocontent characterise r OM the mM) of the mM) of remaining pelletfor and extracts and in was measured at 30 at
9 Version postprint post-treated digestates via thechemical accessibility and complexity of organic matter. Bioresource A.-M., Wéry, N.(Auteur decorrespondance) (2017). Characterisation ofthebiodegradability of Maynaud, G.,Druilhe, C.,Daumoin,M., Jimenez,J., Patureau,D., Torrijos,M.,Pourcher, Where: influorescencepresented zonesSupplementar is the Anexample and Equations according4. spectof to 3 givenina “i” zone biochemicalcorrespondingto family-ty fluorescence al.(2014), al.Muller et (2014)and the et spectra nmto inwithnm from wavelengths 600 varied 10 200 The be fluorescencequantified. w used spectrometer theextractedfractions spectroscopyto applied was the procedure Similarto bydeveloped alet Jimenez multipleB variablescorrelations includingbetween were analyticalprocessed using comp principal data using(BDaero)biodegradabilities wereinvestigated respirometryAT (BOD, CorrelationstheCH between Statisticalanalysis 2.5. Technology, 213, 65–74. DOI : 10.1016/j.biortech.2017.01.057 i i P zone(nm²): a S(i) the areaof i, COD V UA mg COD L % = % f f (i) (%): the fluorescence proportion of a zonea(%): the proportion of (i) i. fluorescence (i) (U.A. mg L COD (U.A. (i)
sample (mg L Comment citer cedocument: P 100 × -1 = i ):the sample, theconcentrationCOD of was calculated fromvolumesthe fluorescence calculated was zone 4 and DRI and -1 (4) ):i,thetheofrawzone volume 4 yieldthe each and from of obtained parameters