Cited by 320X-ray Spectroscopy and Fluorescence AnalysisSoil Carbon and Nitrogen DynamicsAdvanced X-ray Imaging Techniques

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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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Lehmann, Johannes, Liang, Biqing, Solomon, Dawit, Lerotic, Mirna, Luizão, Flavio, Kinyangi, James, Schäfer, Thorsten, Wirick, Sue, Jacobsen, Chris·2005·Global Biogeochemical Cycles

DOI 10.1029/2004gb002435

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Abstract

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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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
ORCID: Lehmann, Johannes
Liang, Biqing
Solomon, Dawit
Schäfer, Thorsten
Jacobsen, Chris
Venue: Global Biogeochemical Cycles
Publisher: American Geophysical Union (AGU)
Published: 2005-02-16
Volume: 19
Issue: 1
ISSN: 0886-6236 (ISSN-L)
1944-9224
DOI: 10.1029/2004gb002435
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
Licence: onlinelibrary.wiley.com/termsAndConditions#vor (vor)
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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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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