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Response of CH4 emission of paddy fields to land management practices at a microcosmic cultivation scale in China
Jing-An Shao et al. J Environ Sci (China). 2005.
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The terrestrial ecosystem may be either a source or a sink of CH4 in rice paddies, depending, to a great extent, on the change of ecosystem types and land use patterns. CH4 emission fluxes from paddy fields under 4 cultivation patterns (conventional plain culture of rice (T1), no-tillage and ridge culture of rice (T2), no-tillage and ridge culture of rice and wheat (T3), and rice-wheat rotation (T4)) were measured with the closed chamber technique in 1996 and 1998 in Chongqing, China. The results showed that differences existed in CH4 emission from paddy fields under these land management practices. In 1996 and 1998, CH4 emission was 71.48% and 78.82% (T2), 65.93% and 57.18% (T3), and 61.53% and 34.22% (T4) of that in T1 during the rice growing season. During the non-rice growing season, CH4 emission from rice fields was 76.23% in T2 and 38.69% in TI. The accumulated annual CH4 emission in T2, T3 and T4 in 1996 decreased by 33.53%, 63.30% and 65.73%, respectively, as compared with that in T1. In 1998, the accumulated annual CH4 emission in T1, T2, T3 and T4 was 116.96 g/m2, 68.44 g/m2, 19.70 g/m2 and 11.80 g/m2, respectively. Changes in soil physical and chemical properties, in thermal and moisture conditions in the soil and in rice plant growth induced by different land use patterns were the dominant causes for the difference in CH4 emission observed. The relative contribution of various influencing factors to CH4 emission from paddy fields differed significantly under different land use patterns. However, the general trend was that chlorophyll content in rice leaves, air temperature and temperature at the 5 cm soil layer play a major role in CH4 emission from paddy fields and the effects of illumination, relative humidity and water layer depth in the paddy field and CH4 concentration in the crop canopy were relatively non-significant. Such conservative land use patterns as no-tillage and ridge culture of rice with or without rotation with wheat are thought to be beneficial to reducing CH4 emission from paddy fields and are, therefore, recommended as a significant solution to the problems of global (climatic) change.
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[Effects of rice plants on methane emission from paddy fields]
[Article in Chinese]
Zhongjun Jia et al. Ying Yong Sheng Tai Xue Bao. 2003 Nov.
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Methane emission from rice paddy fields is the net result of the combination of many processes, i.e., CH4 production, CH4 oxidation and CH4 transportation in paddy soil. Rice plants play a key role in the CH4 emission from paddy fields, particularly in all the processes involved. The positive and negative effects of rice plants on CH4 emission from paddy fields are well recognized as the main factors influencing the temporal variation of CH4 emission flux in paddy field. Process-based studies about the effects of rice plants on methane emission from paddy fields were summarized, and different roles of rice plants on this emission were discussed. Root exudates and litters of rice plants could serve as the substrate for methanogenesis and enhance the CH4 production of paddy soils, resulting in a high CH4 emission peak, particularly in rice late growing season. Rhizospheric CH4 oxidation induced by rice root-excreted oxygen constitutes a main biogenic sink of CH4, which could account for 36-90% of CH4 produced in paddy soil over the entire growing season of rice. Up to 80% and more of CH4 released from rice field during a growing season could be emitted by rice plant-mediated transport. The fully developed aerenchyma of rice plants could be of importance in CH4 emission during rice growing seasons, and responsible for the CH4 emission peak observed at rice early growing season.
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[Characteristics of CO2, CH4 and N2O emissions from winter-fallowed paddy fields in hilly area of South China].
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Effect of substrate concentration on carbon isotope fractionation during acetoclastic methanogenesis by Methanosarcina barkeri and M. acetivorans and in rice field soil
Dennis Goevert et al. Appl Environ Microbiol. 2009 May.
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Methanosarcina is the only acetate-consuming genus of methanogenic archaea other than Methanosaeta and thus is important in methanogenic environments for the formation of the greenhouse gases methane and carbon dioxide. However, little is known about isotopic discrimination during acetoclastic CH(4) production. Therefore, we studied two species of the Methanosarcinaceae family, Methanosarcina barkeri and Methanosarcina acetivorans, and a methanogenic rice field soil amended with acetate. The values of the isotope enrichment factor (epsilon) associated with consumption of total acetate (epsilon(ac)), consumption of acetate-methyl (epsilon(ac-methyl)) and production of CH(4) (epsilon(CH4)) were an epsilon(ac) of -30.5 per thousand, an epsilon(ac-methyl) of -25.6 per thousand, and an epsilon(CH4) of -27.4 per thousand for M. barkeri and an epsilon(ac) of -35.3 per thousand, an epsilon(ac-methyl) of -24.8 per thousand, and an epsilon(CH4) of -23.8 per thousand for M. acetivorans. Terminal restriction fragment length polymorphism of archaeal 16S rRNA genes indicated that acetoclastic methanogenic populations in rice field soil were dominated by Methanosarcina spp. Isotope fractionation determined during acetoclastic methanogenesis in rice field soil resulted in an epsilon(ac) of -18.7 per thousand, an epsilon(ac-methyl) of -16.9 per thousand, and an epsilon(CH4) of -20.8 per thousand. However, in rice field soil as well as in the pure cultures, values of epsilon(ac) and epsilon(ac-methyl) decreased as acetate concentrations decreased, eventually approaching zero. Thus, isotope fractionation of acetate carbon was apparently affected by substrate concentration. The epsilon values determined in pure cultures were consistent with those in rice field soil if the concentration of acetate was taken into account.
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FIG. 1.
Catabolism of acetate in pure…

FIG. 2.
Isotope enrichment during acetoclastic methanogenesis…

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Anaerobic incubation of rice field…

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Carbon isotope fractionation during consumption…
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Effect of temperature on carbon and electron flow and on the archaeal community in methanogenic rice field soil.
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Pathway of CH4 formation in anoxic rice field soil and rice roots determined by 13C-stable isotope fractionation
Ralf Conrad et al. Chemosphere. 2002 Jun.
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In anoxic rice fields methane is produced by either reduction of CO2 or cleavage of acetate. We measured the delta 13C-values of CH4 and CO2, acetate and organic carbon during time course experiments with anoxic methanogenic soil and root samples and used these values to calculate the fractions of CH4 (and acetate) produced from CO2 reduction. Comparison with radiotracer and/or inhibitor studies constrained the kinetic fractionation factors used for calculation. The fractionation factors for the conversion of CO2 to CH4 and of acetate to CH4 were on the order of alpha = 1.07 (epsilon = -70%) and epsilon > or = - 20%, respectively. The pathway of CH4 production changed with time of anoxic incubation. Anoxic slurries of rice field soil first produced CH4 predominantly (>50%) from CO2, then predominantly (>80%) from acetate and finally (after about one month) according to the theoretically expected ratio (33% CO2 and 67% acetate). Anoxic rice roots, on the other hand, initially produced CH4 exclusively from CO2, followed by contribution of acetate of about 40-60%. Rice roots also produced acetate that partially originated (< or = 1 30%) from reduction of CO2 as determined by calculation of isotopic fractionation using fractionation factors from the literature. The results demonstrate that there is quite some variability in pathways of CH4 production, and also indicate that isotopic fractionation factors may be different in different habitats and change with time.
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[Effects of rice plants on methane emission from paddy fields].
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North American terrestrial CO 2 uptake largely offset by CH 4 and N 2 O emissions: toward a full accounting of the greenhouse gas budget
Hanqin Tian et al. Clim Change. 2015.
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The terrestrial ecosystems of North America have been identified as a sink of atmospheric CO2 though there is no consensus on the magnitude. However, the emissions of non-CO2 greenhouse gases (CH4 and N2O) may offset or even overturn the climate cooling effect induced by the CO2 sink. Using a coupled biogeochemical model, in this study, we have estimated the combined global warming potentials (GWP) of CO2, CH4 and N2O fluxes in North American terrestrial ecosystems and quantified the relative contributions of environmental factors to the GWP changes during 1979-2010. The uncertainty range for contemporary global warming potential has been quantified by synthesizing the existing estimates from inventory, forward modeling, and inverse modeling approaches. Our "best estimate" of net GWP for CO2, CH4 and N2O fluxes was -0.50 ± 0.27 Pg CO2 eq/year (1 Pg = 1015 g) in North American terrestrial ecosystems during 2001-2010. The emissions of CH4 and N2O from terrestrial ecosystems had offset about two thirds (73 %±14 %) of the land CO2 sink in the North American continent, showing large differences across the three countries, with offset ratios of 57 % ± 8 % in US, 83 % ± 17 % in Canada and 329 % ± 119 % in Mexico. Climate change and elevated tropospheric ozone concentration have contributed the most to GWP increase, while elevated atmospheric CO2 concentration have contributed the most to GWP reduction. Extreme drought events over certain periods could result in a positive GWP. By integrating the existing estimates, we have found a wide range of uncertainty for the combined GWP. From both climate change science and policy perspectives, it is necessary to integrate ground and satellite observations with models for a more accurate accounting of these three greenhouse gases in North America.
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References
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Bioelectrochemical methane (CH 4) production in anaerobic digestion at different supplemental voltages
Kwang-Soon Choi et al. Bioresour Technol. 2017 Dec.
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Microbial electrolysis cells (MECs) at various cell voltages (0.5, 0.7 1.0 and 1.5V) were operated in anaerobic fermentation. During the start-up period, the cathode potential decreased from -0.63 to -1.01V, and CH4 generation increased from 168 to 199ml. At an applied voltage of 1.0V, the highest methane yields of 408.3ml CH4/g COD glucose was obtained, which was 30.3% higher than in the control tests (313.4ml CH4/g COD glucose). The average current of 5.1mA was generated at 1.0V at which the maximum methane yield was obtained. The other average currents were 1.42, 3.02, 0.53mA at 0.5, 0.7, and 1.5V, respectively. Cyclic voltammetry and EIS analysis revealed that enhanced reduction currents were present at all cell voltages with biocatalyzed cathode electrodes (no reduction without biofilm), and the highest value was obtained with 1V external voltage.
Keywords: Acetate; Anaerobic digestion; CO(2) conversion; Methane; Microbial electrolysis cell.
Copyright © 2017 Elsevier Ltd. All rights reserved.
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A review on the applications of microbial electrolysis cells in anaerobic digestion.
Yu Z, et al. Bioresour Technol. 2018. PMID: 29444757 Review.
Upflow anaerobic sludge blanket reactor--a review.
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Environmental and vegetation controls on the spatial variability of CH 4 emission from wet-sedge and tussock tundra ecosystems in the Arctic
Katherine Rose McEwing et al. Plant Soil. 2015.
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Aims: Despite multiple studies investigating the environmental controls on CH4 fluxes from arctic tundra ecosystems, the high spatial variability of CH4 emissions is not fully understood. This makes the upscaling of CH4 fluxes from plot to regional scale, particularly challenging. The goal of this study is to refine our knowledge of the spatial variability and controls on CH4 emission from tundra ecosystems.
Methods: CH4 fluxes were measured in four sites across a variety of wet-sedge and tussock tundra ecosystems in Alaska using chambers and a Los Gatos CO2 and CH4 gas analyser.
Results: All sites were found to be sources of CH4, with northern sites (in Barrow) showing similar CH4 emission rates to the southernmost site (ca. 300 km south, Ivotuk). Gross primary productivity (GPP), water level and soil temperature were the most important environmental controls on CH4 emission. Greater vascular plant cover was linked with higher CH4 emission, but this increased emission with increased vascular plant cover was much higher (86 %) in the drier sites, than the wettest sites (30 %), suggesting that transport and/or substrate availability were crucial limiting factors for CH4 emission in these tundra ecosystems.
Conclusions: Overall, this study provides an increased understanding of the fine scale spatial controls on CH4 flux, in particular the key role that plant cover and GPP play in enhancing CH4 emissions from tundra soils.
Keywords: Arctic; Climate change; Greenhouse gas emission; Permafrost; Vegetation control.
Figures

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Soil collar vegetation sites at…

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a) CH 4 flux (mg…

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The influence of the interaction…

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The influence of water table…

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CH 4 exchange within arctic…
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Molecular simulation of CH 4/CO 2/H 2 O competitive adsorption on low rank coal vitrinite
Song Yu et al. Phys Chem Chem Phys. 2017.
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The competitive adsorptions of CH4/CO2/H2O on coal vitrinite (DV-8, C214H180O24N2) were computed based on density function theory (DFT) and grand canonical Monte Carlo (GCMC). The adsorption process reaches the saturation state after adsorbing 17 CH4s, 22 CO2s, and 35 H2Os per C214H180O24N2 respectively. The optimal configurations of CH4-vitrinite, CO2-vitrinite, and H2O-vitrinite respectively manifest as aromatic1/T2/rT3 (1 adsorption location, 2 adsorption sites and T here represents sites above the carbon atom and the heteroatom, 3 adsorption orientation and rT here means the orientations of three hydrogen atoms pointing to vitrinite), aromatic/T/v (v represents the orientations perpendicular to the plane of vitrinite), and aromatic/rV/T (rV represents an oxygen atom pointing to the vitrinite surface). The GCMC results show that high temperature is not conducive to the vitrinite's adsorption of adsorbates and the adsorption capacity order is H2O > CO2 > CH4 (263-363 K) in the one-component, binary, and ternary adsorbate systems. The optimal configurations of vitrinite are similar to graphite/graphene, while ΔE is significantly lower than graphite/graphene. Simulation data are in good agreement with the experimental results.
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Socioeconomic determinants of China's growing CH 4 emissions
Rong Ma et al. J Environ Manage. 2018.
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Reducing CH4 emissions is a major global challenge, owing to the world-wide rise in emissions and concentration of CH4 in the atmosphere, especially in the past decade. China has been the greatest contributor to global anthropogenic CH4 emissions for a long time, but current understanding towards its growing emissions is insufficient. This paper aims to link China's CH4 emissions during 2005-2012 to their socioeconomic determinants by combining input-output models with structural decomposition analysis from both the consumption and income perspectives. Results show that changes in household consumption and income were the leading drivers of the CH4 growth in China, while changes in efficiency remained the strongest factor offsetting CH4 emissions. After 2007, with the global financial crisis and economic stimulus plans, embodied emissions from exports plunged but those from capital formation increased rapidly. The enabled emissions in employee compensation increased steadily over time, whereas emissions induced from firms' net surplus decreased gradually, reflecting the reform on income distribution. In addition, at the sectoral level, consumption and capital formation respectively were the greatest drivers of embodied CH4 emission changes from agriculture and manufacturing, while employee compensation largely determined the enabled emission changes across all industrial sectors. The growth of CH4 emissions in China was profoundly affected by the macroeconomic situation and the changes of economic structure. Examining economic drivers of anthropogenic CH4 emissions can help formulate comprehensive mitigation policies and actions associated with economic production, supply and consumption.
Keywords: China's CH(4) emissions; Consumption-based accounting; Income-based accounting; Input-output analysis; Structural decomposition analysis.
Copyright © 2018 Elsevier Ltd. All rights reserved.
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Low O 2 level enhances CH 4-derived carbon flow into microbial communities in landfill cover soils
Ruo He et al. Environ Pollut. 2020 Mar.
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CH4 oxidation in landfill cover soils plays a significant role in mitigating CH4 release to the atmosphere. Oxygen availability and the presence of co-contaminants are potentially important factors affecting CH4 oxidation rate and the fate of CH4-derived carbon. In this study, microbial populations that oxidize CH4 and the subsequent conversion of CH4-derived carbon into CO2, soil organic C and biomass C were investigated in landfill cover soils at two O2 tensions, i.e., O2 concentrations of 21% ("sufficient") and 2.5% ("limited") with and without toluene. CH4-derived carbon was primarily converted into CO2 and soil organic C in the landfill cover soils, accounting for more than 80% of CH4 oxidized. Under the O2-sufficient condition, 52.9%-59.6% of CH4-derived carbon was converted into CO2 (CECO2-C), and 29.1%-39.3% was converted into soil organic C (CEorganic-C). A higher CEorganic-C and lower CECO2-C occurred in the O2-limited environment, relative to the O2-sufficient condition. With the addition of toluene, the carbon conversion efficiency of CH4 into biomass C and organic C increased slightly, especially in the O2-limited environment. A more complex microbial network was involved in CH4 assimilation in the O2-limited environment than under the O2-sufficient condition. DNA-based stable isotope probing of the community with 13CH4 revealed that Methylocaldum and Methylosarcina had a higher relative growth rate than other type I methanotrophs in the landfill cover soils, especially at the low O2 concentration, while Methylosinus was more abundant in the treatment with both the high O2 concentration and toluene. These results indicated that O2-limited environments could prompt more CH4-derived carbon to be deposited into soils in the form of biomass C and organic C, thereby enhancing the contribution of CH4-derived carbon to soil community biomass and functionality of landfill cover soils (i.e. reduction of CO2 emission).
Keywords: Landfill cover soils; Methane oxidation; Methane-derived carbon; Methanotrophs; Oxygen concentration; Stable isotope probing.
Copyright © 2019 Elsevier Ltd. All rights reserved.
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Soil microorganisms as controllers of atmospheric trace gases (H2, CO, CH4, OCS, N2O, and NO).
Conrad R. Microbiol Rev. 1996. PMID: 8987358 Free PMC article. Review.
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Seasonal variation in CH 4 emissions and production and oxidation potentials at microsites on an oligotrophic pine fen
S Saarnio et al. Oecologia. 1997 Apr.
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Temporal and spatial variation in CH4 emissions was studied at hummock, Eriophorum lawn, flark and Carex lawn microsites in an oligotrophic pine fen over the growing season using a static chamber method, and CH4 production and oxidation potentials in peat profiles from hummock and flark were determined in laboratory incubation experiments. Emissions were lowest in the hummocks, and decreased with increasing hummock height, while in the lawns and flarks they increased with increasing sedge cover. Statistical response functions with water table and peat temperature as independent variables were calculated in order to reconstruct seasonal CH4 emissions by reference to the time series for peat temperature and water table specific to each microsite type. Mean CH4 emissions in the whole area in the snow-free period of 1993, weighted in terms of the proportions of the microsites, were 1.7 mol CH4 m-2. Potential CH4 production and oxidation rates were very low in the hummocks rising above the groundwater table, but were relatively similar when expressed per dry weight of peat both in the hummocks and flarks below the water table. The CH4 production potential increased in autumn at both microsites and CH4 oxidation potential seemed to decrease. The decrease in temperature in autumn certainly reduced in situ decomposition processes, possibly leaving unused substrates in the peat, which would explain the increase in CH4 production potential.
Keywords: Key words Methane; Microsites; Oligotrophic fen; Oxidation; Production.
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Saarnio S, et al. Oecologia. 1999. PMID: 28307757
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Montes F, et al. J Anim Sci. 2013. PMID: 24045493 Review.
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Methane-oxidizing bacteria in a Finnish raised mire complex: effects of site fertility and drainage.
Jaatinen K, et al. Microb Ecol. 2005. PMID: 16283115
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Martian CH(4): sources, flux, and detection
T C Onstott et al. Astrobiology. 2006 Apr.
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Recent observations have detected trace amounts of CH(4) heterogeneously distributed in the martian atmosphere, which indicated a subsurface CH(4) flux of ~2 x 10(5) to 2 x 10(9) cm(2) s(1). Four different origins for this CH(4) were considered: (1) volcanogenic; (2) sublimation of hydrate- rich ice; (3) diffusive transport through hydrate-saturated cryosphere; and (4) microbial CH(4) generation above the cryosphere. A diffusive flux model of the martian crust for He, H(2), and CH(4) was developed based upon measurements of deep fracture water samples from South Africa. This model distinguishes between abiogenic and microbial CH(4) sources based upon their isotopic composition, and couples microbial CH(4) production to H(2) generation by H(2)O radiolysis. For a He flux of approximately 10(5) cm(2) s(1) this model yields an abiogenic CH(4) flux and a microbial CH(4) flux of approximately 10(6) and approximately 10(9) cm(2) s(1), respectively. This flux will only reach the martian surface if CH(4) hydrate is saturated in the cryosphere; otherwise it will be captured within the cryosphere. The sublimation of a hydrate-rich cryosphere could generate the observed CH(4) flux, whereas microbial CH(4) production in a hypersaline environment above the hydrate stability zone only seems capable of supplying approximately 10(5) cm(2) s(1) of CH(4). The model predicts that He/H(2)/CH(4)/C(2)H(6) abundances and the C and H isotopic values of CH(4) and the C isotopic composition of C(2)H(6) could reveal the different sources. Cavity ring-down spectrometers represent the instrument type that would be most capable of performing the C and H measurements of CH(4) on near future rover missions and pinpointing the cause and source of the CH(4) emissions.
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Yung YL, et al. Astrobiology. 2018. PMID: 30234380 Free PMC article. Review.
Ultraviolet-radiation-induced methane emissions from meteorites and the Martian atmosphere.
Keppler F, et al. Nature. 2012. PMID: 22678286
Evolution of water reservoirs on Mars from D/H ratios in the atmosphere and crust.
Donahue TM. Nature. 1995. PMID: 7700352
Hydrogeologic controls on episodic H2 release from precambrian fractured rocks--energy for deep subsurface life on earth and mars.
Sherwood Lollar B, et al. Astrobiology. 2007. PMID: 18163873
Hydrothermal systems on Mars: an assessment of present evidence.
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The energetics of supported metal nanoparticles: relationships to sintering rates and catalytic activity
Charles T Campbell. Acc Chem Res. 2013.
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Transition metal nanoparticles on the surfaces of oxide and carbon support materials form the basis for most solid catalysts and electrocatalysts, and have important industrial applications such as fuel production, fuels, and pollution prevention. In this Account, I review my laboratory group's research toward the basic understanding of the effects of particle size and support material on catalytic properties. I focus on studies of well-defined model metal nanoparticle catalysts supported on single-crystalline oxide surfaces. My group structurally characterized such catalysts using a variety of ultrahigh vacuum surface science techniques. We then measured the energies of metal atoms in these supported nanoparticles, using adsorption calorimetry tools that we developed. These metal adsorption energies increase with increasing size of the nanoparticles, until their diameter exceeds about 6 nm. Below 6 nm, the nature of the oxide support surface reaches also greatly affects the metal adsorption energies. Using both adsorption calorimetry and temperature programmed desorption (TPD), we measured the energy of adsorbed catalytic intermediates on metal nanoparticles supported on single crystal oxide surfaces, as a function of particle size. The studies reveal correlations between a number of characteristics. These include the size- and support-dependent energies of metal surface atoms in supported metal nanoparticles, their rates of sintering, how strongly they bind small adsorbates, and their catalytic activity. The data are consistent with the following model: the more weakly the surface metal atom is attached to the nanomaterial, the more strongly it binds small adsorbates. Its strength of attachment to the nanomaterial is dominated by the number of metal-metal bonds which bind it there, but also by the strength of metal/oxide interfacial bonding. This same combination of bond strengths controls sintering rates as well: the less stable a surface metal atom is in the nanomaterial, the greater is the thermodynamic driving force for it to sinter, and the faster is its sintering rate. These correlations provide key insights into how and why specific structural properties of catalyst nanomaterials dictate their catalytic properties. For example, they explain why supported Au catalysts must contain Au nanoparticles smaller than about 6 nm to have high activity for combustion and selective oxidation reactions. Only below about 6 nm are the Au atoms so weakly attached to the catalyst that they bind oxygen sufficiently strongly to enable the activation of O₂. By characterizing this interplay between industrially important rates (of net catalytic reactions, of elementary steps in the catalytic mechanism, and of sintering) and their thermodynamic driving forces, we can achieve a deeper fundamental understanding of supported metal nanoparticle catalysts. This understanding may facilitate development of better catalytic nanomaterials for clean, sustainable energy technologies.
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Structural requirements and reaction pathways in dimethyl ether combustion catalyzed by supported Pt clusters
Akio Ishikawa et al. J Am Chem Soc. 2007.
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The identity and reversibility of the elementary steps required for catalytic combustion of dimethyl ether (DME) on Pt clusters were determined by combining isotopic and kinetic analyses with density functional theory estimates of reaction energies and activation barriers to probe the lowest energy paths. Reaction rates are limited by C-H bond activation in DME molecules adsorbed on surfaces of Pt clusters containing chemisorbed oxygen atoms at near-saturation coverages. Reaction energies and activation barriers for C-H bond activation in DME to form methoxymethyl and hydroxyl surface intermediates show that this step is more favorable than the activation of C-O bonds to form two methoxides, consistent with measured rates and kinetic isotope effects. This kinetic preference is driven by the greater stability of the CH3OCH2* and OH* intermediates relative to chemisorbed methoxides. Experimental activation barriers on Pt clusters agree with density functional theory (DFT)-derived barriers on oxygen-covered Pt(111). Measured DME turnover rates increased with increasing DME pressure, but decreased as the O2 pressure increased, because vacancies (*) on Pt surfaces nearly saturated with chemisorbed oxygen are required for DME chemisorption. DFT calculations show that although these surface vacancies are required, higher oxygen coverages lead to lower C-H activation barriers, because the basicity of oxygen adatoms increases with coverage and they become more effective in hydrogen abstraction from DME. Water inhibits reaction rates via quasi-equilibrated adsorption on vacancy sites, consistent with DFT results indicating that water binds more strongly than DME on vacancies. These conclusions are consistent with the measured kinetic response of combustion rates to DME, O2, and H2O, with H/D kinetic isotope effects, and with the absence of isotopic scrambling in reactants containing isotopic mixtures of 18O2-16O2 or 12CH3O12CH3-13CH3O13CH3. Turnover rates increased with Pt cluster size, because small clusters, with more coordinatively unsaturated surface atoms, bind oxygen atoms more strongly than larger clusters and exhibit lower steady-state vacancy concentrations and a consequently smaller number of adsorbed DME intermediates involved in kinetically relevant steps. These effects of cluster size and metal-oxygen bond energies on reactivity are ubiquitous in oxidation reactions requiring vacancies on surfaces nearly saturated with intermediates derived from O2.
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Chin YH, et al. J Am Chem Soc. 2011. PMID: 21919447
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Reactivity of chemisorbed oxygen atoms and their catalytic consequences during CH4-O2 catalysis on supported Pt clusters
Ya-Huei Cathy Chin et al. J Am Chem Soc. 2011.
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Kinetic and isotopic data and density functional theory treatments provide evidence for the elementary steps and the active site requirements involved in the four distinct kinetic regimes observed during CH(4) oxidation reactions using O(2), H(2)O, or CO(2) as oxidants on Pt clusters. These four regimes exhibit distinct rate equations because of the involvement of different kinetically relevant steps, predominant adsorbed species, and rate and equilibrium constants for different elementary steps. Transitions among regimes occur as chemisorbed oxygen (O*) coverages change on Pt clusters. O* coverages are given, in turn, by a virtual O(2) pressure, which represents the pressure that would give the prevalent steady-state O* coverages if their adsorption-desorption equilibrium was maintained. The virtual O(2) pressure acts as a surrogate for oxygen chemical potentials at catalytic surfaces and reflects the kinetic coupling between C-H and O═O activation steps. O* coverages and virtual pressures depend on O(2) pressure when O(2) activation is equilibrated and on O(2)/CH(4) ratios when this step becomes irreversible as a result of fast scavenging of O* by CH(4)-derived intermediates. In three of these kinetic regimes, C-H bond activation is the sole kinetically relevant step, but occurs on different active sites, which evolve from oxygen-oxygen (O*-O*), to oxygen-oxygen vacancy (O*-*), and to vacancy-vacancy (*-*) site pairs as O* coverages decrease. On O*-saturated cluster surfaces, O*-O* site pairs activate C-H bonds in CH(4) via homolytic hydrogen abstraction steps that form CH(3) groups with significant radical character and weak interactions with the surface at the transition state. In this regime, rates depend linearly on CH(4) pressure but are independent of O(2) pressure. The observed normal CH(4)/CD(4) kinetic isotope effects are consistent with the kinetic-relevance of C-H bond activation; identical (16)O(2)-(18)O(2) isotopic exchange rates in the presence or absence of CH(4) show that O(2) activation steps are quasi-equilibrated during catalysis. Measured and DFT-derived C-H bond activation barriers are large, because of the weak stabilization of the CH(3) fragments at transition states, but are compensated by the high entropy of these radical-like species. Turnover rates in this regime decrease with increasing Pt dispersion, because low-coordination exposed Pt atoms on small clusters bind O* more strongly than those that reside at low-index facets on large clusters, thus making O* less effective in H-abstraction. As vacancies (*, also exposed Pt atoms) become available on O*-covered surfaces, O*-* site pairs activate C-H bonds via concerted oxidative addition and H-abstraction in transition states effectively stabilized by CH(3) interactions with the vacancies, which lead to much higher turnover rates than on O*-O* pairs. In this regime, O(2) activation becomes irreversible, because fast C-H bond activation steps scavenge O* as it forms. Thus, O* coverages are set by the prevalent O(2)/CH(4) ratios instead of the O(2) pressures. CH(4)/CD(4) kinetic isotope effects are much larger for turnovers mediated by O*-* than by O*-O* site pairs, because C-H (and C-D) activation steps are required to form the * sites involved in C-H bond activation. Turnover rates for CH(4)-O(2) reactions mediated by O*-* pairs decrease with increasing Pt dispersion, as in the case of O*-O* active structures, because stronger O* binding on small clusters leads not only to less reactive O* atoms, but also to lower vacancy concentrations at cluster surfaces. As O(2)/CH(4) ratios and O* coverages become smaller, O(2) activation on bare Pt clusters becomes the sole kinetically relevant step; turnover rates are proportional to O(2) pressures and independent of CH(4) pressure and no CH(4)/CD(4) kinetic isotope effects are observed. In this regime, turnover rates become nearly independent of Pt dispersion, because the O(2) activation step is essentially barrierless. In the absence of O(2), alternate weaker oxidants, such as H(2)O or CO(2), lead to a final kinetic regime in which C-H bond dissociation on *-* pairs at bare cluster surfaces limit CH(4) conversion rates. Rates become first-order in CH(4) and independent of coreactant and normal CH(4)/CD(4) kinetic isotope effects are observed. In this case, turnover rates increase with increasing dispersion, because low-coordination Pt atoms stabilize the C-H bond activation transition states more effectively via stronger binding to CH(3) and H fragments. These findings and their mechanistic interpretations are consistent with all rate and isotopic data and with theoretical estimates of activation barriers and of cluster size effects on transition states. They serve to demonstrate the essential role of the coverage and reactivity of chemisorbed oxygen in determining the type and effectiveness of surface structures in CH(4) oxidation reactions using O(2), H(2)O, or CO(2) as oxidants, as well as the diversity of rate dependencies, activation energies and entropies, and cluster size effects that prevail in these reactions. These results also show how theory and experiments can unravel complex surface chemistries on realistic catalysts under practical conditions and provide through the resulting mechanistic insights specific predictions for the effects of cluster size and surface coordination on turnover rates, the trends and magnitude of which depend sensitively on the nature of the predominant adsorbed intermediates and the kinetically relevant steps.
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