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Cobalt and Nickel Bioavailability for Biogas Formation
Linköping University, The Tema Institute, Department of Water and Environmental Studies. Linköping University, Faculty of Arts and Sciences.
2012 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Supplementation of trace metals such as Co and Ni may improve anaerobic digestion of organic material for biogas formation. Which trace metals that are needed and the quantity to apply are, at least partly, related to metal speciation and bioavailability. According to the common perception, metals have to be dissolved to be available for microbial uptake. However, the impact of trace metal speciation on bioavailability is still unclear. The purpose of the present study was to investigate the effect of Fe-, Co- and Ni-addition on the biogas process performance of stillage-fed lab-scale biogas tank reactors. Metal speciation was determined by sequential extraction (SE), extraction of acid volatile sulfides (AVS) and continuously extracted metals (AVS-Me). Sulfur forms, which may be associated to metal speciation, were studied with S XANES (sulfur X-ray absorption near edge structure). The effect of different Co- and Ni-concentrations on process microflora composition was examined with quantitative PCR (qPCR) and 454-pyrosequencing.

The results showed that Co- and Ni-supplementation stimulated and stabilized the biogas process performance by increasing methane production and substrate utilization and by establishing low concentrations of volatile fatty acids. 10-20% of the total Co-amount was found in the dissolved phase, which shows that Co was relatively available for microbial uptake. Nickel was entirely associated to organic matter/sulfides and AVS, and was therefore considered to be non-bioavailable. Nevertheless, Ni-supplementation had stimulatory effects on the biogas process performance. This implies that Ni was available for microbial uptake despite its extensive association to sulfides and that other mechanisms than solubility govern the availability of this trace metal. The microbial analyzes revealed that it was primarily the methane producers which were affected by the concentration of Co and Ni. At stimulatory Co- and Ni-concentrations, the archaeal methanogenic community was dominated by aceticlastic Methanosarcinales. At lower Co- or Ni-levels, when biogas process performance was poor, an increase in hydrogenotrophic Methanomicrobiales was observed. This indicates a shift in the methanogenic flora, from being dominated by acetate utilizers to increased importance of hydrogen utilizers, and that the former was more dependent on Co and Ni.

Abstract [sv]

Tillsats av spårmetaller kan förbättra rötning av organiskt material till biogas. Typ och mängd av respektive spårmetall som behöver tillsättas för att uppnå stimulerande effekter, varierar mellan processer. Detta är delvis kopplat till specieringen och biotillgängligheten av metallerna. Endast fria metalljoner och vissa metallkomplex antas vara tillgängliga för mikrobiellt upptag. Det är dock i många fall oklart hur metallernas speciering påverkar biotillgängligheten. Syftet med föreliggande studie var därför att undersöka effekten av tillsats av Fe, Co och Ni för biogasproduktion från drank, en restprodukt i produktion av bioetanol från spannmål, samt att undersöka hur dessa metallers speciering påverkar deras biotillgänglighet. Effekten av tillsatserna av Fe, Co och Ni undersöktes på biogasreaktorer i lab-skala. Metallernas speciering bestämdes genom sekventiell extraktion (SE), extraktion av AVS (acid volatile sulfide) och kontinuerligt extraherade metaller (AVS-Me). Svavelformer med betydelse för metallspeciering studerades med S XANES (sulfur X-ray absorption near edge structure). Effekten av olika Co- och Ni-koncentrationer på processens mikroflora undersöktes molekylärbiologiskt med kvantitativ PCR (qPCR) och 454-pyrosekvensering.

Resultaten visade att Co och Ni stimulerade och stabiliserade biogasprocessen genom ökad metanproduktion, ökad utrötningsgrad samt låga halter av flyktiga fettsyror i det studerade systemet. 10-20% av totala mängden Co återfanns i löst fas, vilket visar att Co var relativt lättillgängligt för mikroorganismerna. Nickel var däremot enbart bundet till organiskt material/sulfider och AVS och kunde alltså betraktas som otillgängligt. Trots detta hade även tillsatsen av Ni stimulerande effekter på biogasprocessen. Det innebär att mikroorganismerna har förmåga att komma åt Ni bundet i svårlösliga sulfidföreningar och att andra mekanismer än löslighet reglerar tillgängligheten av denna spårmetall. De molekylärbiologiska analyserna visade att framför allt de metanbildande mikroorganismerna påverkades av halten av Co och Ni. De halter, som gav välfungerande processer, dominerades helt av acetiklastiska Methanosarcinales. Vid lägre halter av Co eller Ni, då processerna gick sämre, tillkom vätgasutnyttjande metanogener. Det tyder på ett skift i bildningen av metan från att ha dominerats av acetatklyvning till att vätgasutnyttjarna fått större betydelse och att de förra är mer beroende av Co och Ni.

Place, publisher, year, edition, pages
Linköping: Linköping University Electronic Press, 2012. , 49 p.
Series
Linköping Studies in Arts and Science, ISSN 0282-9800 ; 549
Keyword [en]
Biogas production, bioavailability, cobalt, nickel, sequential extraction, S XANES, 454-pyrosequencing.
Keyword [sv]
Biogasproduktion, biotillgänglighet, kobolt, nickel, sekventiell extraktion, S XANES, 454-pyrosekvensering
National Category
Natural Sciences
Identifiers
URN: urn:nbn:se:liu:diva-73113ISBN: 978-91-7519-989-4 (print)OAI: oai:DiVA.org:liu-73113DiVA: diva2:466545
Public defence
2012-01-19, Vallfarten, Campus Valla, Linköpings universitet, Linköping, 10:15 (English)
Opponent
Supervisors
Available from: 2011-12-16 Created: 2011-12-16 Last updated: 2012-01-31Bibliographically approved
List of papers
1. The feasibility of trace element supplementation for stable operation of wheat stillage-fed biogas tank reactors
Open this publication in new window or tab >>The feasibility of trace element supplementation for stable operation of wheat stillage-fed biogas tank reactors
2011 (English)In: Water Science and Technology, ISSN 0273-1223, E-ISSN 1996-9732, Vol. 64, no 2, 320-325 p.Article in journal (Refereed) Published
Abstract [en]

The aim of this study was to investigate the effect of trace element supplementation on operation of wheat stillage-fed biogas tank reactors. The stillage used was a residue from bio-ethanol production, containing high levels of sulfate. In biogas production, high sulfate content has been associated with poor process stability in terms of low methane production and accumulation of process intermediates. However, the results of the present study show that this problem can be overcome by trace element supplementations. Four lab-scale wheat stillage-fed biogas tank reactors were operated for 345 days at a hydraulic retention time of 20 days (37 degrees C). It was concluded that daily supplementation with Co (0.5 mg L(-1)), Ni (0.2 mg L(-1)) and Fe (0.5 g L(-1)) were required for maintaining process stability at the organic loading rate of 4.0 g volatile solids L(-1) day(-1).

Place, publisher, year, edition, pages
IWA Publishing, 2011
Keyword
biogas, sulfides, trace elements, wheat stillage
National Category
Social Sciences
Identifiers
urn:nbn:se:liu:diva-70229 (URN)10.2166/wst.2011.633 (DOI)000293272500002 ()
Note
©IWA Publishing 2011. The definitive peer-reviewed and edited version of this article is published in Jenny Gustavsson, Bo Svensson and Anna Karlsson, The feasibility of trace element supplementation for stable operation of wheat stillage-fed biogas tank reactors, 2011, Water Science and Technology, (64), 2, 320-325. http://dx.doi.org/10.2166/wst.2011.633 and is available at www.iwapublishing.com. Available from: 2011-08-26 Created: 2011-08-26 Last updated: 2017-12-08
2. Shifts in microbial community structure at Co and Ni nutrient deficiency in biogas tank reactors digesting grain stillage
Open this publication in new window or tab >>Shifts in microbial community structure at Co and Ni nutrient deficiency in biogas tank reactors digesting grain stillage
(English)Manuscript (preprint) (Other academic)
Abstract [en]

From previous studies in our laboratory it was concluded that Co- and Ni-amendment was necessary for stable biogas process operation during anaerobic digestion of grain stillage. In the present study, shifts in microbial community structure were investigated in relation to omission of Co or Ni from the stable biogas processes. The first effect of the stopped Co- or Ni-additions was an increase in volatile fatty acid (VFA) concentrations. Eventually, the methane production ceased in the reactor without Niaddition. Quantitative polymerase chain reaction (qPCR) revealed that Methanosarcinales was the dominating order of methanogens during stable process performance (both Co and Ni supplied) while Methanomicrobiales increased with increasing VFA-concentrations at both Co- and Ni-deficiency. The increase was however more pronounced at Co-limitation. The qPCR results agreed with sequencing data obtained by 454-pyrosequencing, where the dominating sequences belonged to Methanosaeta sp (order Methanosarcinales) at stable conditions, while the proportion of sequences belonging to Methanoculleus sp. (order Methanomicrobiales) increased at reactor instability as a result of decreasing concentration of Co or Ni.

National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-73110 (URN)
Available from: 2011-12-16 Created: 2011-12-16 Last updated: 2011-12-16Bibliographically approved
3. Bioavailability and chemical forms of Co and Ni in the biogasprocess: an evaluation based on sequential and acid volatile sulfide extractions
Open this publication in new window or tab >>Bioavailability and chemical forms of Co and Ni in the biogasprocess: an evaluation based on sequential and acid volatile sulfide extractions
Show others...
(English)Manuscript (preprint) (Other academic)
Abstract [en]

Several previous studies report stimulatory effects on biogas process performance after trace element supplementation. However, the regulation of the bioavailability in relation to chemical speciation (e.g. the role of sulfide) is not fully understood. The objective of the present study was to determine the effect of sulfide on the chemical speciation and bioavailability of Co and Ni in lab-scale semi-continuously fed biogas tank reactors, digesting grain stillage. The chemical forms and potential bioavailability of Co and Ni in the reactors were determined by sequential extraction (SE), and analysis of acid volatile sulfide (AVS) together with simultaneously extracted metals (AVS-Me). The results for metal speciation analysis demonstrated that Ni was completely associated to the organic  matter/sulfide fraction and AVS, suggesting low potential Ni-bioavailability. Cobalt was predominantly associated to organic matter/sulfide and AVS, but also to more soluble fractions which are considered to be more bioavailable. Process performance data showed that both Co and Ni were available for microbial uptake. Although the actual bioavailability of Co could be explained by association to more bioavailable chemical fractions as determined by SE, AVS and AVS-Me analysis, the complete association of Ni with organic matter/sulfides and AVS shows that Ni was taken up despite its expected low bioavailability. Thus, the results of the present study imply that Ni-sulfide precipitation does not prevent microbial uptake in the studied biogas reactors.

National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-73111 (URN)
Available from: 2011-12-16 Created: 2011-12-16 Last updated: 2011-12-16Bibliographically approved
4. Sulphur K-edge XANES and acid volatile sulphide analyses of changes in chemical speciation of S and Fe during sequential extraction of trace metals in anoxic sludge from biogas reactors
Open this publication in new window or tab >>Sulphur K-edge XANES and acid volatile sulphide analyses of changes in chemical speciation of S and Fe during sequential extraction of trace metals in anoxic sludge from biogas reactors
2012 (English)In: Talanta: The International Journal of Pure and Applied Analytical Chemistry, ISSN 0039-9140, E-ISSN 1873-3573, Vol. 89, 470-477 p.Article in journal (Refereed) Published
Abstract [en]

The effect of sequential extraction of trace metals on sulphur (S) speciation in anoxic sludge samples from two lab-scale biogas reactors augmented with Fe was investigated. Analyses of sulphur K-edge X-ray absorption near edge structure (S XANES) spectroscopy and acid volatile sulphide (AVS) were conducted on the residues from each step of the sequential extraction. The S speciation in sludge samples after AVS analysis was also determined by S XANES. Sulphur was mainly present as FeS (~60% of total S) and reduced organic S (~30% of total S), such as organic sulphide and thiol groups, in the anoxic solid phase. Sulphur XANES and AVS analyses showed that during first step of the extraction procedure (the. removal of exchangeable cations), a part of the FeS fraction corresponding to 20% of total S was transformed to zero-valent S, whereas Fe was not released into the solution during this transformation. After the last extraction step (organic/sulphide fraction) a secondary Fe phase was formed. The change in chemical speciation of S and Fe occurring during sequential extraction procedure suggests indirect effects on trace metals associated to the FeS fraction that may lead to incorrect results. Furthermore, by S XANES it was verified that the AVS analysis effectively removed the FeS fraction. The present results identified critical limitations for the application of sequential extraction for trace metal speciation analysis outside the framework for which the methods were developed.

Place, publisher, year, edition, pages
Elsevier, 2012
Keyword
Sequential extraction, Biogas, Sulphur speciation, Sulphur K-edge XANES, Acid volatile sulphide, Trace metals
National Category
Natural Sciences
Identifiers
urn:nbn:se:liu:diva-73112 (URN)10.1016/j.talanta.2011.12.065 (DOI)000301278000068 ()
Note
funding agencies|Swedish Energy Agency||Available from: 2011-12-16 Created: 2011-12-16 Last updated: 2017-12-08Bibliographically approved

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