Near‐edge X‐ray absorption fine structure (NEXAFS) spectroscopy for mapping nano‐scale distribution of organic carbon forms in soil: Application to black carbon particles
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Small‐scale heterogeneity of organic carbon (C) forms in soils is poorly quantified since appropriate analytical techniques were not available up to now. Specifically, tools for the identification of functional groups on the surface of micrometer‐sized black C particles were not available up to now. Scanning Transmission X‐ray Microscopy (STXM) using synchrotron radiation was used in conjunction with Near‐Edge X‐ray Absorption Fine Structure (NEXAFS) spectroscopy to investigate nano‐scale distribution (50‐nm resolution) of C forms in black C particles and compared to synchrotron‐based FTIR spectroscopy. A new embedding technique was developed that did not build on a C‐based embedding medium and did not pose the risk of heat damage to the sample. Elemental sulfur (S) was melted to 220°C until it polymerized and quenched with liquid N 2 to obtain a very viscous plastic S in which the black C could be embedded until it hardened to a noncrystalline state and was ultrasectioned. Principal component and cluster analysis followed by singular value decomposition was able to resolve distinct areas in a black carbon particle. The core of the studied biomass‐derived black C particles was highly aromatic even after thousands of years of exposure in soil and resembled the spectral characteristics of fresh charcoal. Surrounding this core and on the surface of the black C particle, however, much larger proportions of carboxylic and phenolic C forms were identified that were spatially and structurally distinct from the core of the particle. Cluster analysis provided evidence for both oxidation of the black C particle itself as well as adsorption of non‐black C. NEXAFS spectroscopy has great potential to allow new insight into black C properties with important implications for biogeochemical cycles such as mineralization of black C in soils and sediments, and adsorption of C, nutrients, and pollutants as well as transport in the geosphere, hydrosphere, and atmosphere.
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The formation of carboxyl groups or other functional groups with a negative charge in the pH range of soils can be the result of two principally different processes: (1) surface oxidation of the biochar particles themselves and (2) adsorption of highly oxidized organic matter onto biochar surfaces.
“This formation of carboxyl groups or other functional groups with a negative charge in the pH range of soils can be the result of two principally different processes: (1) surface oxidation of the biochar particles themselves and (2) adsorption of highly oxidized organic matter onto biochar surfaces (Lehmann et al. 2005).”
From Biochar physicochemical properties: pyrolysis temperature and feedstock kind effects (2020) · cites this paper as Lehmann et al. 2005
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- Authors
- Lehmann, J., Liang, B., Solomon, D., Lerotic, M., Luizão, F., Kinyangi, J., Schäfer, T., Wirick, S., & Jacobsen, C.
- Affiliations
- Cornell University (US)
- Stony Brook University (US)
- Instituto Nacional de Pesquisa da Amazonia INPA Manaus Brazil
- Forschungszentrum Karlsruhe Institute für Nukleare Entsorgung (INE) Karlsruhe Germany
- Venue
- Global Biogeochemical Cycles
- Publisher
- American Geophysical Union (AGU)
- Published
- 2005-02-16
- Volume
- 19
- Issue
- 1
- ISSN
- 0886-6236 (ISSN-L)
- 1944-9224
- OpenAlex
- W2100546837
- Cited by
- 319
- References
- 65
- Citations by year
- 2026: 5 · 2025: 7 · 2024: 9 · 2023: 13 · 2022: 27 · 2021: 23 · 2020: 19 · 2019: 9 · 2018: 16 · 2017: 23 · 2016: 16 · 2015: 20 · 2014: 17 · 2013: 16 · 2012: 15
- FWCI
- 12.16
- Type
- journal article
- Language
- en
- Open access
- bronze
- doi.org
- Locations
- Global Biogeochemical Cycles (publishedVersion)
- Funders
- National Science Foundation (DE-AC02-98CH10886, 9510499, 9605045)
- U.S. Department of Energy (DE‐FG02‐, DEAC-02-98CH10886, -AC02-98 CH 10886, DE-AC02-)
- State University of New York
- Biological and Environmental Research (DE-AC02-98CH10886)
- Brookhaven National Laboratory (AC-02-98CH10886, DE-AC02- 98CH10886)
- Topics
- Physical Sciences › Physics and Astronomy › Radiation › X-ray Spectroscopy and Fluorescence Analysis
- Life Sciences › Agricultural and Biological Sciences › Soil Science › Soil Carbon and Nitrogen Dynamics
- Physical Sciences › Physics and Astronomy › Radiation › Advanced X-ray Imaging Techniques
- Keywords
- black carbon, soil organic carbon, NEXAFS spectroscopy, scanning transmission X-ray microscopy, carbon oxidation, aromatic carbon, biomass-derived carbon, carbon adsorption
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