Comparison of soil organic carbon speciation using C NEXAFS and CPMAS 13C NMR spectroscopy

Prietzel, Jörg; Müller, Svenja; Kögel-Knabner, Ingrid; Thieme, Jürgen; Jaye, Cherno; Fischer, Daniel

doi:10.1016/j.scitotenv.2018.02.121

Title: Comparison of soil organic carbon speciation using C NEXAFS and CPMAS ¹³C NMR spectroscopy

Journal Article · Tue Feb 20 00:00:00 EST 2018 · Science of the Total Environment

DOI:https://doi.org/10.1016/j.scitotenv.2018.02.121· OSTI ID:1463852

^[1];

^[1]; Kögel-Knabner, Ingrid ^[1]; Thieme, Jürgen ^[2]; Jaye, Cherno ^[3]; Fischer, Daniel ^[3]

Munich Univ. of Technology (Germany). Chair of Soil Science and Dept. of Ecology and Ecosystem Management
Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States). Material Measurement Lab.

Here, we compared synchrotron-based C near-edge X-ray absorption fine structure (NEXAFS) and CPMAS ¹³C nuclear magnetic resonance (NMR) spectroscopy with respect to their precision and accuracy to quantify different organic carbon (OC) species in defined mixtures of soil organic matter source compounds. We also used both methods to quantify different OC species in organic surface horizons of a Histic Leptosol as well as in mineral topsoil and subsoil horizons of two soils with different parent material, stage of pedogenesis, and OC content (Cambisol: 15–30 OC mg g^-1, Podzol: 0.9–7 OC mg g^-1). CPMAS ¹³C NMR spectroscopy was more accurate and precise (mean recovery of different C functional groups 96–103%) than C NEXAFS spectroscopy (mean recovery 92–113%). For organic surface and topsoil samples, NMR spectroscopy consistently yielded larger O-alkyl C percentages and smaller alkyl C percentages than C NEXAFS spectroscopy. For the Cambisol subsoil samples both methods performed well and showed similar C speciation results. NEXAFS spectroscopy yielded excellent spectra with a high signal-to-noise ratio also for OC-poor Podzol subsoil samples, whereas this was not the case for CPMAS ¹³C NMR spectroscopy even after sample treatment with HF. Our results confirm the analytical power of CPMAS ¹³C NMR spectroscopy for a reliable quantitative OC speciation in soils with >10 mg OC g^-1. Moreover, they highlight the potential of synchrotron-based C NEXAFS spectroscopy as fast, non-invasive method to semi-quantify different C functional groups in soils with low C content (0.9–10 mg g^-1).

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Research Organization:: Brookhaven National Lab. (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: SC0012704; 28WC406301

OSTI ID:: 1463852

Report Number(s):: BNL-207922-2018-JAAM; TRN: US1902335

Journal Information:: Science of the Total Environment, Vol. 628-629, Issue C; ISSN 0048-9697

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 20 works

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Title: Comparison of soil organic carbon speciation using C NEXAFS and CPMAS ¹³C NMR spectroscopy