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Digestion of cattle manure under mesophilic and thermophilic conditions: characterization of organic matter applying thermal analysis and 1H NMR

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Abstract

Digestion of cattle manure collected from a livestock farm together with bedding material (straw) has been studied under mesophilic and thermophilic conditions in batch reactors. The digestion was carried out for a prolonged period with the aim of evaluating the changes undergone by the organic matter. The mesophilic digestion carried out revealed a greater capacity to produce gas and transform organic matter, while a higher conversion rate, but a lower gas yield, was obtained under thermophilic conditions. Degradation of the organic matter was evaluated by means of thermal analysis and 1H NMR. Stabilisation through anaerobic digestion (either mesophilic or thermophilic) resulted in an increase in the quality of the organic matter, as characterised by an enrichment in thermostable compounds, and an accumulation of long chain aliphatic materials. The experiments performed demonstrated the transformation of organic matter into complex materials under anaerobic conditions with an accumulation of aliphatic components under both types of conditions tested. Degradation through mesophilic digestion, in comparison to the thermophilic process, resulted in a greater destruction of straw particles.

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References

  • Adani F, Genevini P, Tambone F, Montoneri E (2006) Compost effect on soil humic acid: a NMR study. Chemosphere 65:1414–1418

    Article  PubMed  CAS  Google Scholar 

  • Amir S, Hafidi M, Lemee L, Merlina G, Guiresse M, Pinelli E, Revel JC, Bailly JR, Ambles A (2006) Structural characterization of humic acids, extracted from sewage sludge during composting by thermochemolysis–gas chromatography–mass spectrometry. Process Biochem 41:410–422

    Article  CAS  Google Scholar 

  • APHA, AWWA, WPCF (1989) Standard methods for the examination of water and wastewater. In: Di’az de Santos SA (ed) American Public Health Association, American Water Works Association and Water Pollution Control Federation, Madrid, Spain

  • Aursand M, Mabon F, Martin GJ (1998) High-resolution 1H and 2H NMR spectroscopy of pure essential fatty acids for plants and animals. Magn Reson Chem 35:S91–S100

    Article  Google Scholar 

  • Bartoszek M, Polak J, Sułkowski WW (2008) NMR study of the humification process during sewage sludge treatment. Chemosphere 73:1465–1470

    Article  CAS  Google Scholar 

  • Buddrus J, Burba P, Herzog H, Lambert J (1989) Quantification of partial structures of aquatic humic substances by one- and two-dimensional solution 13C nuclear magnetic resonance spectroscopy. Anal Chem 61:628–631

    Article  CAS  Google Scholar 

  • Chachkhiani M, Dabert P, Abzianidze T, Partskhaladze G, Tsiklauri L, Dudauri T, Godon JJ (2004) 16S rDNA characterisation of bacterial and archaeal communities during start-up of anaerobic thermophilic digestion of cattle manure. Bioresour Technol 93:227–232

    Article  PubMed  CAS  Google Scholar 

  • Chang C, Liou G (2007) Stably anodic green electrochromic aromatic poly(amine–amide–imide)s: synthesis and electrochromic properties. Org Electron 8:662–672

    Article  CAS  Google Scholar 

  • Cuetos MJ, Morán A, Otero M, Gómez X (2009) Anaerobic co-digestion of poultry blood with OFMSW: FTIR and TG–DTG study of process stabilization. Environ Technol 30(6):571–582

    Article  PubMed  CAS  Google Scholar 

  • Cuetos MJ, Gómez X, Otero M, Morán A (2010) Anaerobic digestion of solid slaughterhouse waste: study of biological stabilization by Fourier transform infrared spectroscopy and thermogravimetry combined with mass spectrometry. Biodegradation. doi:10.1007/s10532-009-9322-7

  • Dell’Abate MT, Canali S, Trinchera A, Benedetti A, Sequi P (1998) Thermal analysis in the evaluation of compost stability: a comparison with humification parameters. Nutr Cycl Agroecosyst 51:217–224

    Article  Google Scholar 

  • Fernández JM, Hockaday WC, Plaza C, Polo A, Hatcher PG (2008) Effects of long-term soil amendment with sewage sludges on soil humic acid thermal and molecular properties. Chemosphere 73:1838–1844

    Article  PubMed  Google Scholar 

  • Flaig W, Beutelspacher H, Rietz E (1975) Chemical composition and physical properties of humic substances. In: Gieseking JE (ed) Soil components, vol 1. Springer-Verlag, Berlin, pp 119–126

    Google Scholar 

  • Font R, Fullana A, Conesa JA, Llavador F (2001) Analysis of the pyrolysis and combustion of different sewage sludges by TG. J Anal Appl Pyrolysis 58–59:927–941

    Article  Google Scholar 

  • France J, Lopez S, Kebreab E, Bannink A, Dhanoa MS, Dijkstra J (2005) A general compartmental model for interpreting gas production profiles. Anim Feed Sci Technol 123–124:473–485

    Article  Google Scholar 

  • Francioso O, Ferrari E, Saladini M, Montecchio D, Gioacchini P, Ciavatta C (2007) TG–DTA, DRIFT and NMR characterisation of humic-like fractions from olive wastes and amended soil. J Hazard Mater 149:408–417

    Article  PubMed  CAS  Google Scholar 

  • Gómez X, Cuetos MJ, García AI, Morán A (2005) Evaluation of digestate stability from anaerobic processes by thermogravimetric analysis. Thermochim Acta 426:179–184

    Article  Google Scholar 

  • Gómez X, Diaz MC, Cooper M, Blanco D, Morán A, Snape CE (2007) Study of biological stabilization processes of cattle and poultry manure by thermogravimetric analysis and 13C NMR. Chemosphere 68:1889–1897

    Article  PubMed  Google Scholar 

  • Gómez X, Cuetos MJ, Tartakovsky B, Martínez-Núñez MF, Morán A (2010) A comparison of analytical techniques for evaluating food waste degradation by anaerobic digestion. Bioprocess Biosyst Eng 33:427–438

    Article  PubMed  Google Scholar 

  • Gómez-Rico MF, Font R, Fullana A, Martín-Gullón I (2005) Thermogravimetric study of different sewage sludges and their relationship with the nitrogen content. J Anal Appl Pyrolysis 74:421–428

    Article  Google Scholar 

  • Guillén MD, Ruiz A (2006) Study by means of 1H nuclear magnetic resonance of the oxidation process undergone by edible oils of different natures submitted to microwave action. Food Chem 96:665–674

    Article  Google Scholar 

  • Hatcher PG (1987) Chemical structural studies of natural lignin by dipolar dephasing solid-state 13C nuclear magnetic resonance. Org Geochem 11:31–39

    Article  CAS  Google Scholar 

  • Haw JF, Maciel GE, Schroeder HA (1984) Carbon-13 nuclear magnetic resonance spectrometric study of wood and wood pulping with cross polarization and magic-angle spinning. Anal Chem 56:1323–1329

    Article  CAS  Google Scholar 

  • Henze M, Harremoes P (1983) Anaerobic treatment of wastewater in fixed film reactors—a literature review. Water Sci Technol 15:1–101

    CAS  Google Scholar 

  • In I, Kim SY (2005) Hyperbranched poly(arylene ether amide) via nucleophilic aromatic substitution reaction. Macromol Chem Phys 206:1862–1869

    Article  CAS  Google Scholar 

  • Keeney DR, Nelson DW (1982) Nitrogen: inorganic forms. In: Miller RH, Keeney DR, Page AL (eds) Methods of soil analysis. Part 2. Chemical and microbiological properties. American Society of Agronomy, Soil Science Society America, Madison, pp 643–698

    Google Scholar 

  • Klammer S, Knapp B, Insam H, Dell’Abate MT, Ros M (2008) Bacterial community patterns and thermal analyses of composts of various origins. Waste Manag Res 26:173–187

    Article  PubMed  Google Scholar 

  • Kolattukudy PE (1980) Biopolyester membranes of plants: cutin and suberin. Science 208:990–1000

    Article  PubMed  CAS  Google Scholar 

  • Kolodziejski W, Frye JS, Maciel E (1982) Carbon-13 nuclear magnetic resonance spectrometry with cross polarization and magic-angle spinning for analysis of lodgepole pine wood. Anal Chem 54:1419–1424

    Article  CAS  Google Scholar 

  • Larghi EL, Kaufman TS (2006) Synthesis of N-methyl-N-formyltyramine, a new b-phenethylamide derivative isolated from Cyathobasis fruticulosa (Bunge) Aellen. J Braz Chem Soc 17. doi:10.1590/S0103-50532006000300026

  • Lopez-Capel E, Abbott GD, Thomas KM, Manning DAC (2006) Coupling of thermal analysis with quadrupole mass spectrometry and isotope ratio mass spectrometry for simultaneous determination of evolved gases and their carbon isotopic composition. J Anal Appl Pyrolysis 75:82–89

    Article  CAS  Google Scholar 

  • Melis P, Castaldi P (2004) Thermal analysis for the evaluation of the organic matter evolution during municipal solid waste aerobic composting process. Thermochim Acta 413:209–214

    Article  Google Scholar 

  • Miranda T, Esteban A, Rojas S, Montero I, Ruiz A (2008) Combustion analysis of different olive residues. Int J Mol Sci 9:512–525

    Article  PubMed  CAS  Google Scholar 

  • Moire L, Schmutz A, Buchala A, Yan B, Stark RE, Ryser U (1999) Glycerol is a suberin monomer. New experimental evidence for an old hypothesis 1. Plant Physiol 119:1137–1146

    Article  PubMed  CAS  Google Scholar 

  • Mondini C, Dell’Abate MT, Leita L, Benedetti A (2003) An integrated chemical, thermal and microbiological approach to compost stability evaluation. J Environ Qual 32:2379–2386

    Article  PubMed  CAS  Google Scholar 

  • Otero M, Calvo LF, Estrada B, García AI, Morán A (2002) Thermogravimetry as a technique for establishing the stabilization progress of sludge from wastewater treatment plants. Thermochim Acta 389:121–132

    Article  CAS  Google Scholar 

  • Rovira P, Vallejo VR (2000) Evaluating thermal and acid hydrolysis methods as indicators of soil organic matter quality. Commun Soil Sci Plan 31:81–100

    Article  CAS  Google Scholar 

  • Rovira P, Kurz-Besson C, Coûteaux M, Vallejo VR (2008) Changes in litter properties during decomposition: a study by differential thermogravimetry and scanning calorimetry. Soil Biol Biochem 40:172–185

    Article  CAS  Google Scholar 

  • Rubiera F, Arenillas A, Pevida C, García R, Pis JJ, Steel KM, Patrick JW (2002) Coal structure and reactivity changes induced by chemical demineralisation. Fuel Process Technol 79:273–279

    CAS  Google Scholar 

  • Sánchez E, Borja T, Weiland P, Travieso L, Martín A (2000) Effect of temperature and pH on the kinetics of methane production, organic nitrogen and phosphorus removal in the batch anaerobic digestion process of cattle manure. Bioprocess Biosyst Eng 22:247–252

    Google Scholar 

  • Sánchez M, Gómez X, Barriocanal G, Cuetos MJ, Morán A (2008) Assessment of the stability of livestock farm wastes treated by anaerobic digestion. Int Biodeterior Biodegrad 62:421–426

    Article  Google Scholar 

  • Seca AML, Cavaleiro JAS, Domingues FMJ, Silvestre AJD, Evtuguin D, Neto CP (2000) Structural characterization of the lignin from the nodes and internodes of Arundo donax reed. J Agric Food Chem 48:817–824

    Article  PubMed  CAS  Google Scholar 

  • Siegrist H, Hunzinker W, Hofer H (2005) Anaerobic digestion of slaughterhouse waste with UF-membrane separation and recycling of permeate after free ammonia stripping. Water Sci Technol 52:531–536

    PubMed  CAS  Google Scholar 

  • Smidt E, Lechner P (2005) Study on the degradation and stabilization or organic matter in waste by means of thermal analyses. Thermochim Acta 438:22–28

    Article  CAS  Google Scholar 

  • Smidt E, Parravicini V (2009) Effect of sewage sludge treatment and additional aerobic post-stabilization revealed by infrared spectroscopy and multivariate data analysis. Bioresour Technol 100:1775–1780

    Article  PubMed  CAS  Google Scholar 

  • Smidt E, Tintner J (2007) Application of differential scanning calorimetry (DSC) to evaluate the quality of compost organic matter. Thermochim Acta 459:87–93

    Article  CAS  Google Scholar 

  • Sosanwo OA, Fawcett AH, Apperley D (1995) 13C CPMAS NMR spectra of tropical hardwoods. Polym Int 36:247–259

    Article  CAS  Google Scholar 

  • Sung S, Liu T (2003) Ammonia inhibition on thermophilic anaerobic digestion. Chemosphere 53:43–52

    Article  PubMed  CAS  Google Scholar 

  • Tambone F, Genevini P, D’Imporzano G, Adani F (2009) Assessing amendment properties of digestate by studying the organic matter composition and the degree of biological stability during the anaerobic digestion of the organic fraction of MSW. Bioresour Technol 100:3140–3142

    Article  PubMed  CAS  Google Scholar 

  • Vamvuka D, Troulinos S, Kastanaki E (2006) The effect of mineral matter on the physical and chemical activation of low rank coal and biomass materials. Fuel 85:1763–1771

    Article  CAS  Google Scholar 

  • Van Soest PJ, Robertson JB, Lewis BA (1991) Methods for dietary fiber, neutral detergent fiber, and nonstarch polysaccharides in relation to animal nutrition. J Dairy Sci 74:3583–3597

    Article  PubMed  Google Scholar 

  • Vivas N, Nonier MF, Pianet I, de Vivas Gaulejac N, Bouquet É (2006) Structure of extracted lignins from oak heartwood (Quercus petraea Liebl., Q. Robur L.). CR Chim 9:1221–1233

    Article  CAS  Google Scholar 

  • Walkey A, Black IA (1934) An examination of the Degtjareff method for determining soil organic matter and a proposed modification of the chromic acid titration method. Soil Sci 37:29–38

    Article  Google Scholar 

  • Xia Z, Yoshida T, Funaoka M (2003) Enzymatic degradation of highly phenolic lignin-based polymers (lignophenols). Eur Polym J 39:909–914

    Article  CAS  Google Scholar 

  • Xu F, Sun JX, Sun RC, Fowler P, Baird MS (2006) Comparative study of organosolv lignins from wheat straw. Ind Crop Prod 23:180–193

    Article  CAS  Google Scholar 

  • Yasuda S, Hamaguchi E, Asano K (1999) Ready chemical conversion of acid hydrolysis lignin into water-soluble lignosulfonates. III. Successive treatment of acid hydrolysis lignin and lignin model compounds by phenolation and aryl-sulfonation. J Wood Sci 45:245–249

    Article  CAS  Google Scholar 

  • Zhu Y, Chai X, Li H, Zhao Y, Wei Y (2007) Combination of combustion with pyrolysis for studying the stabilization process of sludge in landfill. Thermochim Acta 464:59–64

    Article  CAS  Google Scholar 

  • Zwietering MH, Jongenburger I, Rombouts FM, van’t Riet K (1990) Modelling the bacterial growth curve. Appl Environ Microbiol 56:1875–1881

    PubMed  CAS  Google Scholar 

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Acknowledgments

The authors wish to thank collaboration of the WWTP of León-SALEAL (mancomunidad municipal para el saneamiento integral de León y su alfoz).

They also would like to thank Dr Margarida Gairí (NMR Facility at Parc Cientific de Barcelona) for access to 600 MHz spectrometer.

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Gómez, X., Blanco, D., Lobato, A. et al. Digestion of cattle manure under mesophilic and thermophilic conditions: characterization of organic matter applying thermal analysis and 1H NMR. Biodegradation 22, 623–635 (2011). https://doi.org/10.1007/s10532-010-9436-y

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  • DOI: https://doi.org/10.1007/s10532-010-9436-y

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