The ISME Journal (2 0 1 4 ), 1 -1 2 © 2 0 1 4 International Society for Microbial Ecology All rights reserved 1 7 5 1-7 362 /14 OPEN ww w .nature.com /ism ej ORIGINAL ARTICLE Natural occurrence of microbial sulphur oxidation by long-range electron transport in the seafloor Sairah Y M alkin1,2,4, A lexandra MF Rao1,5, Dorina Seitaj2, Diana Vasquez-Cardenas2,3, Eva-Maria Zetsche1, Silvia Hidalgo-M artinez2, Henricus TS Boschker and Filip JR M eysm an1,2 1Department o f Analytical, Environm ental, and Geo-chemistry, Vrije Universiteit Brussel (VUB), Brussels, Belgium; 2D epartment o f Ecosystem Studies, Boyal Netherlands Institute fo r Sea Besearch (NIOZ), Yerseke, The Netherlands and 3Department o f Marine Microbiology, Boyal Netherlands Institute fo r Sea Besearch (NIOZ), Yerseke, The Netherlands Recently, a novel mode of sulphur oxidation was described in marine sediments, in which sulphide oxidation in deeper anoxic layers was electrically coupled to oxygen reduction at the sediment surface. Subsequent experimental evidence identified that long filamentous bacteria belonging to the family Desulfobulbaceae likely mediated the electron transport across the centimetre-scale distances. Such long-range electron transfer challenges some long-held views in microbial ecology and could have profound implications for sulphur cycling in marine sediments. But, so far, this process of electrogenic sulphur oxidation has been documented only in laboratory experiments and so its imprint on the seafloor remains unknown. Here we show that the geochemical signature of electrogenic sulphur oxidation occurs in a variety of coastal sediment environments, including a salt marsh, a seasonally hypoxic basin, and a subtidal coastal mud plain. In all cases, electrogenic sulphur oxidation was detected together with an abundance of Desulfobulbaceae filaments. Complementary laboratory experiments in intertidal sands demonstrated that mechanical dis­ turbance by bioturbating fauna destroys the electrogenic sulphur oxidation signal. A survey of published geochemical data and 16S rRNA gene sequences identified that electrogenic sulphide oxidation is likely present in a variety of marine sediments with high sulphide generation and restricted bioturbation, such as mangrove swamps, aquaculture areas, seasonally hypoxic basins, cold sulphide seeps and possibly hydrothermal vent environments. This study shows for the first time that electrogenic sulphur oxidation occurs in a wide range of marine sediments and that bioturbation may exert a dominant control on its natural distribution. The ISME Journal advance online publication, 27 March 2014; doi:10.1038/ismej.2014.41 Subject Category: Geomicrobiology and microbial contributions to geochemical cycles Keywords: bioturbation; Desulfobulbaceae; electrobiogeochemistry; electrogenic sulphur oxidation; sulphur oxidizing bacteria Introduction Sulphate reduction is the dom inant m ineralization pathw ay in coastal m arine sedim ents, and leads to an accum ulation of sulphide in deeper sedim ent horizons (Jorgensen, 1982). Various respiratory pathw ays of m icrobial sulphur oxidation have evolved as a m eans of harvesting this stored Correspondence: SY M alkin or FJR Meysman, Analytical, Environm ental, and Geo-chemistry, Vrije U niversiteit Brussel, Pleinlaan 2, Brussels 1050, Belgium. E-mail: smalkin@uga.edu or filip.meysman@nioz.nl 4Current address: Departm ent of Marine Sciences, U niversity of Georgia, Athens, GA, USA. 5Current address: Institut des Sciences de la Mer (ISMER), U niversité du Québec à Rimouski (UQAR), Rimouski, QC, Canada. Received 14 November 2013; revised 4 February 2014; accepted 16 February 2014 chem ical energy (Jorgensen and Nelson, 2004). Recently, a novel sulphur oxidation process, herein called electrogenic sulphur oxidation, was discov­ ered whereby the oxidation of free sulphide in deeper sedim ent horizons was observed to be directly coupled to reduction of oxygen near the sedim ent surface (Nielsen et ah, 2010). Such a spatial separation of redox half-reactions indicates there m ust be a direct pathw ay by w hich electrons originating from sulphide are conducted across centim etre-scale distances to oxygen (Nielsen et al, 2010; Risgaard-Petersen et al., 2012). Experim ental m anipulation revealed that this electrical connec­ tion responded im m ediately (that is, w ithin m inutes) to oxygen depletion in the overlying water, and so the connection was too fast to be explained by diffusion of redox-active shuttles (Nielsen et ah, 2010). M etal-reducing bacteria are Long-range electron transport In th e seafloor SY M alkin e f a/ know n to transport electrons externally via cell surface cytochromes, redox shuttles or conductive pili (Reguera et al., 2005; Gorby et al., 2006; Lovley, 2008; Clarke et al., 2011), and such extracellular electron transport can bridge ~ 100 m icrometer distances in electrode biofilms (Reguera et al., 2006; Logan and Rabaey, 2012). The electron trans­ port associated w ith this electrogenic sulphur oxidation, by contrast, operates on scales of centi­ metres, thereby extending the known length scale of microbially m ediated electron transport by two orders of m agnitude. Electrogenic sulphur oxidation creates a unique geochemical signal in surface sedim ents, w hich is detectable by m icrosensor profiling. A key feature is that the cathodic half-reaction (that is, 0 2 + 4e~ + 4H + ->2H20 ) consumes protons, thereby creating a pH m axim um in the oxic zone. Deeper in the sedim ent, protons are released by an anodic half­ reaction (that is, electrogenic sulphide oxidation; such as V2 H2S + 2H20->V2S0t~ + 4 e ~ + 5 H + ) creat­ ing a broad pH m inim um near the sulphide horizon, separated from the oxic zone by a suboxic zone ranging from several m illim etres to approxim ately 2 cm wide. In laboratory experim ents, the develop­ m ent of this characteristic geochemical fingerprint has been used as a sign of electrogenic sulphur oxidation activity (Nielsen et al., 2010; Pfeffer et al., 2012; Risgaard-Petersen et al., 2012). Compelling evidence indicates that electrogenic sulphur oxidation is likely carried out by long filam entous bacteria. First, in sedim ents w ith the geochemical signature of this process, detailed m icroscopic investigation revealed high densities of long m ulticellular filam entous bacteria, belonging to the family Desulfobulbaceae, w hich were span­ ning the entire length of the suboxic zone (Pfeffer et al., 2012). Second, w hen a thin wire was passed horizontally through the suboxic zone, the electric circuitry was effectively ‘cut’, as indicated by an im m ediate decrease in sedim ent oxygen consum p­ tion by a factor of 2, and a decrease in the signature pH maximum. This experim ent identified that the electron conduction occurred along a continuous structure spanning the suboxic zone (Pfeffer et al., 2012). Thirdly, w hen sedim ent was experim entally incubated w ith filters of various pore sizes w hich were inserted horizontally, the geochemical signa­ ture of electrogenic sulphur oxidation developed only in cores that had filters w ith pore sizes large enough for Desulfobulbaceae filaments to penetrate (Pfeffer et al., 2012). Taken together, these experi­ ments provide strong evidence that electrogenic sulphur oxidation is carried out by Desulfobulbaceae filaments. The capacity of Desulfobulbaceae filaments to oxidize su lp h u r by long-range electron transport represents an entirely novel m icrobial lifestyle (Pfeffer et al., 2012). By conducting electrons across centim etre-scale distances, these filam entous bacteria appear capable of enabling a The ISME Journal previously unrecognized strategy for resource competition in marine sediments (Nielsen et al., 2010; Risgaard-Petersen et al., 2012). Yet until now, electrogenic sulphur oxidation has only been induced in laboratory experim ents that have used sieved and hom ogenized sedim ent from a deep sedim ent horizon obtained from one particular location in the Baltic Sea (Nielsen et al., 2010; Pfeffer et al., 2012; Risgaard-Petersen et al., 2012). Our objective here is to identify w hether electrogenic su lp h u r oxidation, together w ith D esulfobulbaceae filam ents, are found in natural m arine sedim ents. We further aim to identify major environm ental constraints on the occurrence and distribution of electrogenic sulphur oxidation in m arine sedim ents. Given the high growth rate and densities of these bacteria observed in laboratory experim ents (Pfeffer et al., 2012; Risgaard-Petersen et al., 2012), we hypothesize that electrogenic sulphur oxidation is a com petitively successful strategy in natural m arine sedim ents and therefore may be w idespread in nature. Materials and methods Site descriptions The laboratory experim ents of Nielsen et al. (2010) and Pfeffer et al. (2012) suggested that electrogenic sulphur oxidation may be com petitively successful in coastal m arine sedim ents w ith high rates of sulphide generation linked to high rates of organic m atter m ineralization. Our site selection therefore targeted four different coastal seafloor habitats in the southern North Sea area, three of w hich were in depositional areas and were particularly rich in organic matter. We exam ined intact sedim ents collected from these sites for geochemical evidence of electrogenic sulphur oxidation and for the presence of Desulfobulbaceae filaments. Our first site was Rattekaai Salt M arsh (RSM), an intertidal area heavily loaded w ith organic matter, including large periodic deposits of macroalgal detritus, w hich supports high rates of sulphate reduction (Oenema, 1988; Pallud and Van Cappellen, 2006; Table 1). We sam pled the un-vegetated sedim ents in an intertidal drainage channel. At low tide, sulphiderich porewater seeps out from these creek sediments. Large bioturbating anim als were absent from these seepage areas, likely excluded by high levels of porew ater sulphide. Our second site was Station 130 in the Belgian Coastal Zone (BCZ), a subtidal site at 12 m water depth (Table 1). This site is characterized by high accum ulation rates of m uddy deposits w hich generate intense sulphate reduction and free sulphide was previously detected below a suboxic zone of several centim etres (Gao et al., 2009). A m onthly survey in 2011 revealed that large bioturbating m acrofauna is generally absent from this site (Braeckman et al., 2014), and no m acro­ fauna was detected in our collected sedim ent cores. Long-range electron transport In the seafloor SY M alkin e ta / 3 Table 1 The geochemical fingerprint of electrogenic sulphur oxidation was observed at three sites in the coastal North Sea under field conditions Site nam e RSM, Oosterschelde, The N etherlands Station 130, BCZ Coordinates N E N E MLG, Holpervoet and Den Osse N basins, The Netherlands E OSF, The Netherlands Dates o f sam pling 5T 26' 04° 10' 5T 16' 02° 54' 51“ 46' 03c 56' 21" 22 June 2011 11" 25 February 2013 13" 10 October 2011 19" 1 M arch 2013 24" 3 November 2011 16" 22 January 2012 24 February 2012 N 5T 26' 52" 17 May 2011 E 04° 05' 47" 15 August 2011 OPD (mm) 0.7 ±0.1 1.3 10.4 0 .710.1 1.2 10.8 0 .9 1 0 .2 1 .4 1 0 .4 1.8 10.4 1.610.3 1.5 10.3 DOU Current density 0 2 consum ed by (m m ol m ~ 2 d ^ 1) cathodic reaction (%) (m A m ~ 2) 30 .3 1 3 .6 19.912.2 32.3115.0 24.8120.9 44.1116.1 13.914.1 22.2 19.5 4 .8 1 1 .6 3 .5 1 0 .5 2 9 .9110.7 7.3 14.0 25.2 12.6 4 .6 1 1 .8 24.8 15.5 16.1 110.4 27.0116.2 22.7110.1 8.2 1 4 .3 19.11 7.1 5 .3 1 2 .9 14.01 7.9 29.5125.3 33.71 30.6 NA NA Abbreviations: BCZ, Belgian Coastal Zone; DOU, diffusive oxygen uptake across the sediment-water interface; MLG, Marine Lake Grevelingen; OPD, Oxygen Penetration Depth; OSF, Oosterschelde sand flats; RSM, Rattekaai Salt Marsh. Values indicate means of between 2 and 4 replicate cores. Reported error is standard deviation between replicate cores. Our third site was M arine Lake Grevelingen (MLG), a seasonally stratified coastal m arine system in the Delta area of The N etherlands w hich experiences bottom water hypoxia and anoxia in the summ er in its deep basins (Table 1). We collected sedim ents from the deepest area of two steep-sided basins (Holpervoet basin at 23 m; Den Osse basin at 35 m water depth). These basins rapidly accum ulate organic rich deposits ( > 2 cm per year) due to focussing of detrital material. At the time of sam pling (winter), the water colum n was fully oxygenated, but even so, m acrofauna is never abundant in these seasonally anoxic sedim ents and no m acrofauna was present in our retrieved sedi­ m ent cores. The fourth site was an intertidal sand flat in the Oosterschelde tidal inlet (Delta area, The Netherlands). Unlike the first three sites, the Oosterschelde Sand Flats (OSF) support high rates of bioturbation, most notably by the lugworm Arenicola marina (Coosen et al., 1994). Free sulphide concentrations are low to non-detectable (< 2 0 p m o ll_1) in at least the top 2.5 cm of the sedim ent. All sites were visited on two or three occasions (Table 1). The intertidal sedim ent samples (that is, RSM and OSF) were collected by m anually inserting core tubes (4 cm diameter) in the sedim ent at low tide. The sedim ent from MLG was retrieved w ith a Uwitec gravity corer (6 cm diameter). On the first occasion, sedim ent from the BCZ was collected w ith a Reineck box corer followed by careful subsam pling w ith a 10 cm diam eter core tube. On the second occasion, sedim ent from this site was collected w ith a Uwitec gravity corer. Retrieved cores were closely inspected and only cores w ith an undisturbed sedim ent surface were kept for the study. M icroprofiling was either conducted im m ediately on-board the sailing vessel (BCZ and MLG in 2011 only), or sedim ent cores were returned to a nearby laboratory where m icroprofiling was conducted under clim ate-controlled conditions. Microprofiling was conducted betw een 2 and 12 h after core collection under darkened conditions. The intertidal sedim ents from RSM and OSF were kept in the dark for at least 6 h prior to m icroprofiling to ensure there was no effect of photosynthesis on the pH profiles. Microelectrode profiling and reactive transport modelling Sedim ent profiling was performed using commer­ cial m icrosensors operated w ith a m otorized m icro­ m anipulator (Unisense A.S., Aarhus, Denmark). Sedim ent was brought level to the core liner surface. Cores were placed in an aquarium containing water collected from the study site and held at in situ tem perature and constantly bubbled w ith air. During m icrosensor profiling, an airstream was additionally provided at the water surface upstream of the sedim ent cores to ensure constant water flow over the sedim ent, estim ated at 2 - 4 c m s -1 at 0.5cm above the sedim ent surface. Oxygen and H2S m icroelectrodes had a tip diam eter of 50 pm, and pH m icrosensors had a tip diam eter of 100 or 200 pm. Vertical oxygen m icroprofiles were recorded at 100 pm steps, beginning at least 1m m above the sedim ent-w ater interface. A tw o-point 0 2 calibra­ tion was m ade in air-saturated seawater and the anoxic zone of the sedim ent (100% and 0%, respectively). Vertical H2S and pH m icroprofiles were m ade concurrently, recorded at 200 pm steps in the oxic zone, and 200 or 400 pm steps below. For H2S, a five-point standard curve was m ade using Na2S standards. ZH2S was calculated from H2S based on pH m easured at the same depth using the R package AquaEnv (Hofmann et al., 2010). For pH, a three-point calibration using NBS standard buffers was made, followed by a salt correction w ith TRIS buffer (Dickson et al., 2007). pH m easurem ents were perform ed w ith a Ag/AgCl reference electrode and values are reported on the total scale. Porosity was determ ined from water content and dry density m easurem ents upon drying to constant weight at 60 °C. The ISME Journal Long-range electron transport In th e seafloor SY M alkin e f a/ Reactive transport m odelling was used to calculate reaction rates from the m icrosensor data (Table 1). The diffusive oxygen uptake (DOU) of the sedim ent was calculated from the oxygen depth profile near the sedim ent-w ater interface using Fick’s first law as below: Ji=q>/{ 1 - 2lnç>)Df(S, T)dC i/dx where q> is the m easured porosity, the term (1 —2ln <p) is a correction for sedim ent tortuosity (Boudreau, 1996), and D¡ is the diffusion coefficient for oxygen calculated at salinity (S) and tem perature (T) calculated using the R package marelac (Soetaert et al., 2012). The m axim um concentration gradient, dC¡/dx, was calculated as the linear slope im m edi­ ately below the sedim ent-w ater interface. The cathodic proton consum ption (CPC) is the proton consum ption corresponding to the cathodic half-reaction, 0 2 + 4e~ + 4H + ->2H20 . The CPC was calculated as the sum of the upw ard and dow nw ard alkalinity fluxes im m ediately above and below the pH m axim um in the oxic zone. A lkalinity fluxes were calculated as the sum of the fluxes of the major individual porew ater com pounds that contribute to the alkalinity: 7 t A = / h C 0 3- + 2 /co2- + 7 b (OH)“ + / h s~ + / oh 7h + The spéciation of individual ions (carbonate, borate, sulphide and water equilibria) were calcu­ lated from H2S and pH m icrosensor data using the R package AquaEnv (Hoffman et al., 2010). For this calculation, we assum ed a constant depth profile for dissolved inorganic carbon and borate. The contribution of other m acronutrients (ammonium, silicate) to alkalinity fluxes are likely small and were not considered in this study. The concentration gradient dQ/dx for each individual species was estim ated by a noise robust num erical differentiation using the Savitsky-Golay algorithm, optim ized w ith a iV=21 point stencil (Savitsky and Golay, 1964). The current density was calculated from the CPC using a conversion factor of one electron per proton (1A = 1.036 x 10~5m ole~ s _1). The percentage, p, of oxygen consum ed electrochem ically was calculated as P = 25 (CPC/DOU), based on a reaction stoichiom etry that four moles of H + are consum ed per mole of 0 2 by the cathodic reaction. The rem aining part of the oxygen consum ption (1 —p) is attributed to aerobic respira­ tion, w hich does not consum e or release alkalinity. This sim plified m odel assumes that no other biogeochemical reactions are releasing or consuming alkalinity w ithin the oxic zone. In reality, some alkalinity consum ption will take place, associated w ith nitrification, ferrous iron oxidation, calcium carbonate precipitation or direct sulphur oxidation by oxygen (Risgaard-Petersen et al., 2012). The rates of these reactions cannot be estim ated from m icrosensor profiles. However, correcting for these reactions w ould increase the value of p. Accordingly, the p estimates derived here should The ISME Journal be interpreted as conservative, lower bounds on the oxygen that is consum ed electrochemically. Identification of Desulfobulbaceae filaments M icroscopic identification of Desulfobulbaceae filaments was achieved by catalysed reporter deposition-fluorescence in situ hybridization (CARD-FISH; Pernthaler et al., 2002), using a Desulfobulbaceae-specific oligonucleotide probe (DSB706; 5'-ACC CGT ATT CCT CCC GAT-3') labelled w ith horseradish peroxidase (Liicker et al., 2007). Sedim ent samples were fixed w ith a 1:1 (vol/vol) ethanol solution and stored at —20 °C until analysis. H undred m icrolitres of the preserved sample sedim ent slurry was pipetted onto polycar­ bonate m em brane filters (0.2 pm pore size). The retained filam entous cells were perm eabilized w ith lysozyme ( l h at 37 °C) and treated w ith achromopeptidase (30m in at 37 °C). Endogenous peroxidases were inactivated w ith a m ethanol and peroxide solution (30m in at 20 °C), and subsequently hybri­ dized in standard hybridization buffer (46 °C) w ith 45% formamide. CARD-FISH was also performed w ith probes EUB388-I and NONEUB388 (with 10% formamide) as positive and negative controls, respectively. Subsequently, hybridized cells were visualized using epifluorescence microscopy (Axioplan II Imaging, Zeiss, Jena, Germany). Desulfobulbaceae filaments were additionally quan­ tified from suboxic zone (0.3-0.8 cm) sedim ent sections obtained from RSM, BCZ and OSF, using the FISH probe as above. Filam ent length was m easured in 200 random m icroscopic fields. Sedim ent samples from MLG enabled filament identification, but could not be used for enumeration. Specim ens for scanning electron microscopy (SEM) were prepared by isolating filaments w ith a hook m ade from flame-drawn pasteur pipettes under a light microscope ( x 40) and transferring these filaments to polycarbonate filters (pore size 5 pm). Filam ents retained on filters were then transferred through a gradual ethanol gradient (25-100% ), critical point dried w ith liquid C 0 2, m ounted on stubs and coated w ith gold. Images were m ade w ith a JEOL 5600 SEM under lowvacuum, operated at 30 kV. Partial 16S rRNA gene sequences of the Desulfobulbaceae filaments were recovered by constructing 16S rRNA cDNA clone libraries using suboxic zone sections of sedim ents (0.3-0.8 cm) in w hich the geochemical fingerprint of electrogenic sulphide oxidation was detected. RNA was extracted w ith a ZR Fungal/Bacterial RNA M iniprep kit (Zymo Research, Irvine, CA, USA) and reversetranscribed using random prim ers. The 16S rRNA gene was am plified by PCR using general bacterial prim ers (Bac F968.60 and Bac R140.10), cloned into Escherichia coli by one shot chem ical transform a­ tion and sequenced using a genetic analyzer (3130 Genetic Analyzer, A pplied Biosystems, Grand Long-range electron transport In the seafloor SY M alkin e ta / Island, NY, USA). Sequences were aligned w ith the software ARB (Ludwig et al., 2004) against the SILVA database. A phylogenetic tree was con­ structed in ARB by m axim um parsimony, w ith 1000 bootstrap iterations. The software Pintail was used to check for chimeras (Ashelford et al., 2005). Related 16S rRNA gene sequences were obtained by BLAST searches of GenBank. Experiments with bioturbated sediments In addition to the field study, we perform ed two laboratory experim ents to investigate the role of bioturbation on the natural distribution of electro­ genic sulphur oxidation in coastal m arine sedi­ m ents. Sedim ents collected from the heavily bioturbated OSF field site did not show evidence of electrogenic sulphur oxidation or a detectable presence of Desulfobulbaceae filaments on repeated visits (details in Results). In a first experim ent, we tested w hether the geochemical signature of electro­ genic sulphur oxidation could develop in these sediments when bioturbation is removed. Sediments from the sand flats differed from the other three study sites in several ways, including a coarser grain size and lower water content, lower organic C content, lower oxygen consum ption rates and lower free sulphide content to at least 2.5 cm depth. We first tested if these differences, independent of m echanical mixing by bioturbation, inhibited the developm ent of the geochemical signature of elec­ trogenic sulphur oxidation. Sedim ent was collected in May 2011, hom ogenized and defaunated by passing it through a 500 pm sieve. The sedim ents were then repacked into core tubes (4 cm diameter), w ith the sedim ent surface adjusted to be level w ith the top of the core liner. The cores were placed in an aquarium w ith water draw n from the study site and kept at 16 °C in a clim ate-controlled room. The aquarium was continuously bubbled to ensure full aeration, and water was replaced weekly. The potential developm ent of electrogenic sulphur oxi­ dation in these sedim ents was tracked by recording m icrosensor profiles in triplicate sedim ent cores every few days. The first experim ent confirmed that these sedi­ m ents could develop the geochemical signature of electrogenic sulphur oxidation (see Results). Conse­ quently, we then designed a second m anipulation experim ent to test if bioturbation specifically could halt electrogenic sulphur oxidation. Intact sedim ent cores were collected intact from OSF in August 2011. To accommodate bioturbating macrofauna, these cores were 15 cm diam eter and had ~ 2 0 c m sedim ent depth w ith 15 cm overlying water. Cores were incubated in a climate controlled room at 16 °C throughout the experim ent. Cores were first defau­ nated by asphyxia, w hich was achieved by closing the cores w ith an air-tight sealing. After 10 days, the cores were re-opened and dead m acrofauna (mostly the lugworm A. marina) was carefully rem oved from the sedim ent surface. These defaunated sedim ent cores were then incubated w ith fully aerated water, and we refer to this as Day 1 of the experiment. On Day 8, m icrosensor profiles were recorded, and revealed the geochemical signature of electrogenic sulphur oxidation. On Day 10, the dom inant bioturbating anim al (the lugworm A. marina) was collected from the OSF. Two lugworms were re-introduced to each sedim ent core, achieving approximately natural densities (~ 1 0 0 m ~ 2). Extensive m icrosensor profiling was conducted again on Day 15 (referred to as ‘re-faunated’ cores). Vertical m icrosensor profiles were m easured both in areas where the sedim ent was not visibly disturbed, and in areas where the sedim ent was heavily disturbed by the activities of the lugworms (that is, around the feeding pocket and the fecal casts). Extended experimental details are available in Rao et al. (in review). Results A geochemical signal of long-range electron transport in natural sediments The geochemical signature of electrogenic sulphide oxidation was present at three of the four coastal zone habitats investigated in the North Sea area. Represen­ tative microsensor profiles are shown for the three sites where the geochemical signature was found (RSM, BCZ and MLG; Figures la-c), and the one site where it was not found (OSF; Figure Id; all site locations are shown in Figures le and f). Furthermore, the geochemical signature of electrogenic sulphur oxidation was evident on multiple visits at the three sites (RSM, BCZ and MLG), identifying that electro­ genic sulphide oxidation occurs regularly at these sites. These three sites were characterized by high DOU rates (range: 13.9-44.1 at RSM, BCZ and MLG vs 3.5-4.8mmol 0 2m ~ 2d ~ 1 at OSF; Table 1). The first three sites had suboxic zones between 5 and 40 mm wide and typically showed a steep increase in the XH2S concentration below the suboxic zone. At these three sites, at least 5.3-33.7% of the DOU was attributable to electrogenic sulphide oxidation (Table 1). Current densities ranged from 4.6 ± 1.8m A m ~ 2 at BCZ in March 2013 up to 29.9 ± 10.7m A m ~2 at RSM in June 2011. Long Desulfobulbaceae filaments in natural sediments At all sites w ith geochemical evidence of electro­ genic sulphide oxidation, m icroscopic exam ination of the sedim ents revealed long, unbranched, filam entous bacteria (Figure 2a), w hich were subse­ quently identified by CARD-FISH as Desulfobulbaceae (Figure 2b; Supplem entary Figures S i and S2). Enum eration using FISH revealed densities of 82.0 and 122.8 m of filament per cubic centim etre of bulk sedim ent at RSM and BCZ, respectively. No filaments were detected at the OSF reference site, w here there was no geochemical evidence of The ISME Journal Long-range electron transport in the seafloor SY M alkin et al o 5 E 1° E .c 15 Q_ (D ° 20 25 30 - r T 1-- 1-- 1-- 1---1 100 200 300 0 2 or £H2S Omoi L 1) The Netherlands ÍS. MLG BCZ Belgium Figure 1 M icrosensor depth profiles of 0 2 (red), SH2S (blue) and pH (black) show the characteristic biogeochem ical fingerprint of electrogenic su lp h u r oxidation in surface sedim ents from three coastal sites in the North Sea: (a) RSM, (b) BCZ and (c) MLG. In contrast, m icrosensor depth profiles from (d) OSF do not show the characteristic fingerprint. R epresentative m icroprofile curves are illustrated, (e) World map indicating A arhus Harbour, the location w here the electrogenic signature and Desulfobulbaceae filam ents were first found in laboratory incubations (yellow cross), and the present study region (Dutch Delta area; red triangle), (f) Detailed map of individual study site locations (red triangles); full site details are given in Table 1. The w orld map also indicates locations w here the geochem ical signature of long distance electron transport have been found in literature reports (black circles) and locations w here highly sim ilar (^ 9 7 % ) 16S rRNA gene sequences to the Desulfobulbaceae filam ents w ere retrieved from GenBank (blue squares); see D iscussion for details. electrogenic sulphide oxidation. Filam ent fragments up to 8 mm in length (~ 4000 cells) were retrieved from MLG sedim ents by gently dissecting sedim ent under a microscope. SEM images revealed a pattern of evenly spaced external ridges running in parallel along the length of the filam ents isolated from all three sites (Figure 2c; S upplem entary Figures S i and S2). Cell diam eters were 1.25-3.04 pm at RSM, 0 .8 9 -1 .3 7 pm in the BCZ and 2.182.36 pm in MLG based on m easurem ents of 2-5 filam ents m easured using SEM per site. Filam ents w ith larger cell diam eters had more ridges and we estim ated across all sam ples betw een 16 and 58 ridges per filam ent. Desulfobulbaceae clones w ith ^ 9 7 % sequence sim ilarity to the 16S rRNA gene sequences reported from the laboratory incubations of Pfeffer et al. (2012), were found in all field samples that showed the electrogenic sulphur oxidation signature (RSM, BCZ and MLG; Figure 2d). A summ ary of the full clone library com position is given in Supplem entary Figure 4. Sequences have been deposited in GenBank under accession num bers BankI t l 707352:KJ562723-KJ562819. A clone library was The ISME Journal not constructed from OSF sedim ents, where the geochemical signature of electrogenic sulphur oxi­ dation was not observed. However, a previous study of sim ilar bioturbated sedim ents in the Oosterschelde found no Desulfobulbaceae sequences in either the surface-oxidized sedim ent or the deeper sulphate-reducing sedim ent (Miyatake et al., 2013). Effects of bioturbation on geochemical signal The geochemical fingerprint of electrogenic sulphur oxidation was not present in intact sedim ent cores collected from the highly bioturbated sandy sedi­ m ent at OSF collected in May and August 2011. However, sedim ents from OSF that were defaunated by sieving and incubated under darkened laboratory conditions in aerated seawater developed the pH profile indicative of electrogenic sulphur oxidation (Figure 3). The characteristic pH profile indicative of cathodic oxygen consum ption was first evident on Day 5 after hom ogenization, whereby porew ater pH was just beginning to increase at the base of the oxic zone (Figure 3). This pH peak progressively Long-range electron transport in the seafloor et al SY M alkin ^TRSM -B-20^ 59 i-^-n-RSM-B-27 —I RSM-B-22 *----------RSM-B-4 Aarhus (JX091073) 88 Aarhus (JX091072) “ BCZ-B-15 J-MLG-B-27 vI r SM-B-6 0.05 “ Desulfobulbus japonicus * Desulfobulbus propionicus — D esulfovibrio alkaliphilus Desulfocapsa sulfexigens 81 -------------------------- -C " Desulfobacter postgatei ' Desulfonema magnum Desulfovibrio desulfuricans Figure 2 Identification of filam entous Desulfobulbaceae bacteria present in intact sedim ent from sites described in Figure 1 and Table 1. (a) A bundant long filam entous bacteria taken from near the surface of sedim ent and gently teased apart w ith forceps, (b) Identification of the filam ents belonging to Desulfobulbaceae using CARD-FISH (DSB 706 probe), (c) SEM image of a bacterial filam ent isolated from the sedim ent. All images show n here are from MLG. See Supplem entary m aterial for images from RSM and BCZ. (d) Phylogenetic tree of Desulfobulbaceae 16S rRNA sequences recovered from intact sedim ent described in Figure 1. Closely related sequences of filam entous Desulfobulbaceae from A arhus Bay and other isolated bacteria are also included. Scale bar shows 5% sequence divergence and bootstrap support is indicated on tree branches. increased over the days of incubation, w ith a m axim um subsurface pH observed on Day 20. At the start of the incubation, before the onset of cathodic oxygen consum ption, the DOU declined from 6.3 ±0.7 at Day 1 to 3.7 ± 0.1 mmol 0 2m -2 d -1 at Day 5. After Day 5, in concert w ith the develop­ m ent of a pH m axim um in the oxic zone, there was an increase in DOU. Between Day 5 and Day 20, DOU increased from 3.7 ±0.1 to 5.4 ±0.2 mmol 0 2m _2d _1, representing a 51% increase in oxygen uptake. Over this same period (Days 5-20), the estim ated electrical current density increased from 0.5 ±0.3 up to 9.5 ± 1 .4 m A m " 2. The percentage of sedim ent DOU attributed to cathodic reactions increased from 0% on Day 1 to 22.4 ± 1.2% on Day 5, and up to 51.6 ±3.7% on Day 20. Although CARD-FISH was not performed during this particular experiment, subsequent analysis of sedim ent collected from OSF and sieved and incubated following the same procedures, The ISME Journal Long-range electron transport in the seafloor SY M alkin et al a pH 6.0 7.5 9.0 6.0 I .1. I .1 1 °5 - F I I I 7.5 I I I 9.0 6.0 I I I I 7.5 I I I 9.0 6.0 I I I I 7.5 I I I 9.0 6.0 I I I I 7.5 I I I 9.0 6.0 I I I I 7.5 I I I 9.0 I I I F E 10- E £ 15 H 25Day 1 Day 5 Day 30- Day 13 1 r i i i i i i 0 100 250 0 100 250 0 100 Day 20 Day 47 i i i i i i i 250 0 100 250 0 100 d 60 -i 250 0 100 20 30 250 I H 2S or 0 2 (pm ol iL- 1 )\ 7 12 -i 10 T3 'e ■a: o E 5 ^E 3 o Q 50- - 6 E 8 < E 6 40 - ^30Q. 4 20- 2 10- 4 3 1 10 20 30 40 Time from S tart (d) 50 0 10 20 30 40 50 Time from S tart (d) 0 10 40 50 Time from S ta rt (d) Figure 3 (a) A subset of m icrosensor profiles from sedim ent collected from a heavily bioturbated sedim ent from an OSF that has been artificially defaunated and incubated w ith well-oxygenated overlying water. Despite a low concentration of free sulphide, developm ent of a geochemical signature of long-range electron transport is evident from Day 5 onwards, (b) DOU during the incubations, average of n = 3, plotted w ith standard error about the mean, (c) Current density calculated from these sedim ents and (d) percentage, p, of oxygen flux that is attributable to cathodic oxygen uptake. confirmed the presence of Desulfobulbaceae filaments w henever the geochemical signature of electrogenic sulphur oxidation was present (Supplem entary Figure 3). To test if infauna specifically can inhibit the geochemical signature of electrogenic sulphide oxidation, we performed a second m anipulation experiment, w here fauna were first removed by asphyxiation and subsequently reintroduced. W hen intact sedim ent cores were retrieved from the OSF field site and im m ediately profiled, these sedim ents did not exhibit evidence of electrogenic sulphur oxidation (Figure 4a). In defaunated sedim ents, the geochemical signature of electrogenic sulphur oxidation again developed w ithin 8 days of exposure to aerated seawater (Figure 4b). The deep burrowing lugworm A. marina was then re-introduced and caused extensive sedim ent overturning, removing sedim ent from the feeding pocket and expelling sedim ent and organic waste as fecal casts on the sedim ent surface. In sedim ent patches that were not m echanically disrupted by the burrow ing lugworms, the electrogenic signature persisted, though w ith attenuated pH extremes (Figure 4c). In sedim ent patches that were directly overturned by lugworm bioturbation, the electrogenic signature disappeared entirely (Figure 4d). The ISME Journal Discussion Our results provide evidence that electrogenic sulphur oxidation, previously reported from labora­ tory incubations (Nielsen et al., 2010; Pfeffer et al., 2012; Risgaard-Petersen et al., 2012), occurs under natural conditions in the seafloor. We observed evidence of electrogenic sulphur oxidation, together w ith Desulfobulbaceae filaments, in a variety of coastal m arine sedim ents (that is, a salt m arsh drainage channel, a subtidal site recovering from seasonal hypoxia, a coastal area of high m ud deposition). These sedim ents were characterized by high DOU and high organic m atter content. In the narrow oxic zone (0.7-2.0 mm depth), a pH m axim um was observed under dark conditions, indicative of cathodic oxygen consum ption. Below this depth, there was a suboxic zone where oxygen and sulphide were not detectable, w hich was typically 5-15 mm deep (although sometimes extending deeper). Below the suboxic zone, these sedim ents exhibited a steep sulphide gradient, indicating high sulphide production. Repeated visits to these three study sites identified that electrogenic sulphur oxidation is a regularly occur­ ring, although not necessarily perm anent, feature at these field sites. Long-range electron transport in the seafloor et al SY M alkin asphyxiation fauna re-introduction re-aeration I u Cl) c(/) c5 Cl) .Ç £ T<D 1) intact defaunated lightly disturbed heavily disturbed CO d pH 9 pH 6 ts 300 0 2 or IH 2S (^M) 0 2 or IH 2S (^M) 300 0 0 2 or SH2S (hM) 100 200 300 0 2 or IH 2S (hM) Figure 4 Effect of sedim ent disturbance by fauna on electrogenic su lp h u r oxidation. Microprofiles of 0 2 (red), £H 2S (blue) and pH (black and grey) are show n from sedim ent cores collected from the intertidal OSF. Different shades are used for replicate profiles for pH and £H 2S for image clarity, whereas a single m edian profile is show n for 0 2. (a) Profiles from intact sedim ent cores, (b) Profiles from defaunated sedim ent cores, (c) Profiles from re-faunated sedim ent cores, in areas that were not visibly disrupted by m echanical disturbance caused by the re-introduced lugworms. (d) Profiles from re-faunated sedim ent cores, in areas that were not visibly disrupted by m echanical disturbance caused by the re-introduced lugworms. Our observation of the geochemical signature of electrogenic sulphur oxidation always coincided w ith the presence of Desulfobulbaceae filaments that were closely related (that is, ^ 9 7 % 16S rRNA gene sequence similarity) to those previously reported from the laboratory incubations of Pfeffer et al. (2012). Desulfobulbaceae filaments from the suboxic zone of our study sites revealed densities of 82.0 and 122.8m filam ent per cubic centimetre sedim ent at RSM and BCZ, respectively, and no filaments were found at the reference site OSF. These densities are sim ilar to those reported in Pfeffer et al. (2012) (127 m c m -3) and support the hypothesis that the long-range electron transport associated w ith electrogenic sulphur oxidation is m ediated by the Desulfobulbaceae filaments (Pfeffer et al., 2012). The filam entous bacteria retrieved from the three electrogenic sulphur oxidation study sites (RSM, BCZ and MLG) were long and unbranched, and retrieved fragments could exceed eight m illim etres in length. The unusual m orphological feature of raised ridges running in parallel along the length of the filaments, observed previously in laboratory incubations, were also prom inent in the Desulfobulbaceae filaments isolated in this study. Pfeffer et al. (2012) reported filament diameters betw een 0.4 and 0.7 pm w ith fewer than 20 ridges per filament, whereas we herein report filam ent diameters betw een 0.9 and 3.0 pm w ith 16-58 ridges per filament. It rem ains to be seen if these morphological differences represent genotypic or phenotypic variation. A cosm opolitan distribution of electrogenic sulphur oxidation is supported by a num ber of published datasets in w hich the geochemical finger­ print of this process is evident, but has not been formally recognized (Figure Id). Shadow subsurface pH maxima, characteristic of cathodic oxygen con­ sum ption, have been reported from in situ m icro­ sensor profiling in the Santa Barbara (Cai et al., 2000) and Santa M onica Basins (Reimers et al., 1996). These basins are perm anently hypoxic, support high rates of sulphate reduction, and are devoid of bioturbating fauna. Similar pH profiles were also reported from a site situated w ithin an oyster aquaculture park in the Thau lagoon (Medi­ terranean Sea, France; Dedieu, 2005) and from sedim ents near a fish farm in Pillan fjord (Chile; M ulsow et al., 2006), both of w hich experience high The ISME Journal Long-range electron transport In th e seafloor SY M alkin e f a/ organic m atter loading and having little or no burrow ing infauna. Seasonally hypoxic sedim ents from Tokyo Bay have also dem onstrated m icropro­ file evidence of cathodic oxygen consum ption (Sayama, 2011), sim ilar to those reported here from MLG. At a site characterized by high sulphide fluxes and devoid of large bioturbating infauna on the MidA tlantic ridge, high rates of sulphide oxidation were detected w hich could not be attributed to any other know n sulphide removal process, such as sulphur oxidation by large nitrate-accum ulating bacteria (Schauer et al., 2011). One explanation is that electrogenic sulphur oxidations is responsible for the observed sulphide removal, however, direct evidence is needed to confirm this possibility. Gene sequence archives also support a cosm opo­ litan distribution of the conductive filamentous bacteria in locations w ith high rates of sulphide generation, via high organic m atter loading or sulphide seepage, and a paucity of bioturbating animals. 16S rRNA gene sequences that were highly sim ilar 97%) to the Desulfobulbaceae at our field sites have been detected at cold seeps on the Hikurangi Margin (Baco et al., 2010) and the Nile Deep Sea Fan (Griinke et al., 2011) in areas devoid of fauna; in organic rich cohesive sedim ent of a subtropical mangrove swam p (Liang et al., 2007); and at a sewage im pacted site in the Bay of Cadiz (Köchling et al., 2011). Previous laboratory experim ents have show n that sulphur oxidation by long-range electron transport can play a dom inant role in oxygen consum ption and can exert a strong im print on the overall sulphur cycling and pH dynamics in sedim ents (Nielsen et al., 2010; Risgaard-Petersen et al., 2012). Our observations show that this process likely has a sim ilarly profound effect on m ineral cycling in some natural coastal sedim ents. We observed pH values as high as 8.8 in the oxic zone, and as low as 6.1 in the suboxic zone (Figure 1). These pH extremes lead to dissolution of metal sulphides and calcium carbonate w ithin the deep suboxic zone, followed by re-precipitation of iron (hydr)oxides and carbonate near the sedim ent-w ater interface (Risgaard-Petersen et al., 2012). High alkalinity effluxes have been reported from m uddy sites on the BCZ, including Station 130 (Braeckman et al., 2014), and such effluxes are consistent w ith cathodic oxygen consum ption and elevated carbo­ nate dissolution induced by electrogenic sulphur oxidation. Current densities estim ated at the three field sites dem onstrating electrogenic sulphur oxidation (15-23 m A m -2) are comparable w ith the values observed in previous laboratory experim ents (Nielsen et al., 2010; Risgaard-Petersen et al., 2012) and are sim ilar to those reported from the anodes of sedim ent batteries colonized by natural microbial com m unities (Tender et al., 2002; Ryckelynck et al., 2006). We estim ated that a m inim um of 5.3-33.7% of the DOU in these sedim ents was due to electro­ genic sulphur oxidation, substantiating that this The ISME Journal process can be a dom inant biogeochemical process in natural m arine sedim ents. Our data further suggest that bioturbation may exert a major control on the natural distribution of electrogenic sulphur oxidation in coastal m arine sediments. In heavily bioturbated sediment from OSF, the geochemical signature of electrogenic sulphide oxidation was not detected under field conditions, but could be induced in laboratory experiments, as long as bioturbation was excluded. In these sediments, a seed population of Desulfobulbaceae bacteria m ust have existed, from w hich these filam ents w ere able to proliferate w hen burrow ing anim als are rem oved. We observed that sedim ent overturning by bioturbation caused a clear disru p tio n of the electrochem ical signal. This m ay arise from a direct breakage of the bacterial filam ents, in a m anner sim ilar to the previously described cutting experim ents of Pfeffer et al. (2012). In addition, sedim ent overturning m ay halt electrogenic su lp h u r oxidation by depositing an anoxic layer of sedim ent on top of the sedim ent surface, thereby depriving the resident filam entous bacteria from access to electron acceptors. In summary, we have shown that electrogenic sulphur oxidation is found in intact coastal marine sedim ents under natural conditions. We found this process, together w ith the Desulfobulbaceae fila­ ments, in three depositional sedim ent areas (a salt marsh, a subtidal coastal m ud plain and a hypoxic marine basin). These sediments were collectively characterized as being rich in organic matter, and consequently supporting high rates of sulphate reduction, and having an oxygenated overlying water column. These sedim ents were furthermore subject to little biomechanical mixing by macrofauna, which appears to be a key control on the distribution of electrogenic sulphur oxidation in natural settings. Until now, the occurrence of electrogenic sulphur oxidation has not been accounted for in studies of natural marine sediments. Given its w idespread distribution, electrogenic sulphur oxidation may be a key process in the biogeochemistry and microbial ecology of the seafloor. Conflict of Interest The authors declare no conflict of interest. Acknowledgements We th a n k U B raeckm an for p ro v id in g d ata on the m acro fau n a d istrib u tio n in BCZ, R D asseville (U Gent) for h elp w ith SEM, V C onfurius for assistan ce w ith clone lib raries an d S E ng elh ard (NIOZ) for h elp w ith CA RD-FISH im ages. We th a n k th ree an onym ous review ers for th e ir com m ents. T his research w as fin an cially su p p o rte d by th e B russels In stitu te for R esearch an d In n o v atio n (H oloFlow project: SYM, EMZ), th e D arw in C enter for B iogeosciences (DS, DV-C, HTSB), th e R esearch F o u n d atio n - F lan d ers (FW O -O dysseus grant Long-range electron transport In the seafloor SY M alkin e ta / FJRM), th e N eth erlan d s O rganisation for S cientific R esearch (NWO-VIDI grant FJRM) an d the E uro p ean R esearch C ouncil (ERC S tarting grant FJRM). References A sh elford KE, C h u zhanova NA, Fry JC, Jones AJ, W eightm an AJ. (2005). 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To view a copy of this license, visit http://creativecommons.org/ licenses/by-nc-nd/3.0/ Supplementary Information accompanies this paper on The ISME Journal website (http://www.nature.com/ismej) The ISME Journal