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

Abstract

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 spectroscopymore » 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).« less

Authors:
ORCiD logo [1]; ORCiD logo [1];  [1];  [2];  [3];  [3]
  1. Munich Univ. of Technology (Germany). Chair of Soil Science and Dept. of Ecology and Ecosystem Management
  2. Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)
  3. National Inst. of Standards and Technology (NIST), Gaithersburg, MD (United States). Material Measurement Lab.
Publication Date:
Research Org.:
Brookhaven National Lab. (BNL), Upton, NY (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1463852
Report Number(s):
BNL-207922-2018-JAAM
Journal ID: ISSN 0048-9697; TRN: US1902335
Grant/Contract Number:  
SC0012704; 28WC406301
Resource Type:
Accepted Manuscript
Journal Name:
Science of the Total Environment
Additional Journal Information:
Journal Volume: 628-629; Journal Issue: C; Journal ID: ISSN 0048-9697
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND TECHNOLOGY; 54 ENVIRONMENTAL SCIENCES; Direct non-invasive SOC speciation; Method comparison; Soil organic matter; C functional groups; Organic surface soil; Mineral soil

Citation Formats

Prietzel, Jörg, Müller, Svenja, Kögel-Knabner, Ingrid, Thieme, Jürgen, Jaye, Cherno, and Fischer, Daniel. Comparison of soil organic carbon speciation using C NEXAFS and CPMAS 13C NMR spectroscopy. United States: N. p., 2018. Web. doi:10.1016/j.scitotenv.2018.02.121.
Prietzel, Jörg, Müller, Svenja, Kögel-Knabner, Ingrid, Thieme, Jürgen, Jaye, Cherno, & Fischer, Daniel. Comparison of soil organic carbon speciation using C NEXAFS and CPMAS 13C NMR spectroscopy. United States. doi:10.1016/j.scitotenv.2018.02.121.
Prietzel, Jörg, Müller, Svenja, Kögel-Knabner, Ingrid, Thieme, Jürgen, Jaye, Cherno, and Fischer, Daniel. Tue . "Comparison of soil organic carbon speciation using C NEXAFS and CPMAS 13C NMR spectroscopy". United States. doi:10.1016/j.scitotenv.2018.02.121. https://www.osti.gov/servlets/purl/1463852.
@article{osti_1463852,
title = {Comparison of soil organic carbon speciation using C NEXAFS and CPMAS 13C NMR spectroscopy},
author = {Prietzel, Jörg and Müller, Svenja and Kögel-Knabner, Ingrid and Thieme, Jürgen and Jaye, Cherno and Fischer, Daniel},
abstractNote = {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).},
doi = {10.1016/j.scitotenv.2018.02.121},
journal = {Science of the Total Environment},
number = C,
volume = 628-629,
place = {United States},
year = {2018},
month = {2}
}

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