Application of DRIFTS, 13 C NMR, and py-MBMS to Characterize the Effects of Soil Science Oxidation Assays on Soil Organic Matter Composition in a Mollic Xerofluvent

Margenot, Andrew J.; Calderón, Francisco J.; Magrini, Kimberly A.; Evans, Robert J.

doi:10.1177/0003702817691776

Application of DRIFTS, ¹³ C NMR, and py-MBMS to Characterize the Effects of Soil Science Oxidation Assays on Soil Organic Matter Composition in a Mollic Xerofluvent

Journal Article · Tue Dec 20 04:00:00 EST 2016 · Applied Spectroscopy

DOI:https://doi.org/10.1177/0003702817691776· OSTI ID:1371652

Margenot, Andrew J.; Calderón, Francisco J.; Magrini, Kimberly A.; Evans, Robert J.

Chemical oxidations are routinely employed in soil science to study soil organic matter (SOM), and their interpretation could be improved by characterizing oxidation effects on SOM composition with spectroscopy. We investigated the effects of routinely employed oxidants on SOM composition in a Mollic Xerofluvent representative of intensively managed agricultural soils in the California Central Valley. Soil samples were subjected to oxidation by potassium permanganate (KMnO4), sodium hypochlorite (NaOCl), and hydrogen peroxide (H2O2). Additionally, non-oxidized and oxidized soils were treated with hydrofluoric acid (HF) to evaluate reduction of the mineral component to improve spectroscopy of oxidation effects. Oxidized non-HF and HF-treated soils were characterized by diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS), 13C cross polarization magic angle spinning (CP-MAS) nuclear magnetic resonance (NMR) spectroscopy, and pyrolysis molecular beam mass spectrometry (py-MBMS), and for particle size distribution (PSD) using laser diffractometry (LD). Across the range of soil organic carbon (OC) removed by oxidations (14-72%), aliphatic C-H stretch at 3000-2800 cm-1 (DRIFTS) decreased with OC removal, and this trend was enhanced by HF treatment due to significant demineralization in this soil (70%). Analysis by NMR spectroscopy was feasible only after HF treatment, and did not reveal trends between OC removal and C functional groups. Pyrolysis-MBMS did not detect differences among oxidations, even after HF treatment of soils. Hydrofluoric acid entailed OC loss (13-39%), and for H2O2 oxidized soils increased C:N and substantially decreased mean particle size. This study demonstrates the feasibility of using HF to improve characterizations of SOM composition following oxidations as practiced in soil science, in particular for DRIFTS. Since OC removal by oxidants, mineral removal by HF, and the interaction of oxidants and HF observed for this soil may differ for soils with different mineralogies, future work should examine additional soil and land use types to optimize characterizations of oxidation effects on SOM composition.

Research Organization:: National Renewable Energy Laboratory (NREL), Golden, CO (United States)

Sponsoring Organization:: USDOE Office of Energy Efficiency and Renewable Energy (EERE)

DOE Contract Number:: AC36-08GO28308

OSTI ID:: 1371652

Report Number(s):: NREL/JA-5100-68308

Journal Information:: Applied Spectroscopy, Journal Name: Applied Spectroscopy Journal Issue: 7 Vol. 71; ISSN 0003-7028

Publisher:: Society for Applied Spectroscopy

Country of Publication:: United States

Language:: English

References (49)

Soil carbon fractions based on their degree of oxidation, and the development of a carbon management index for agricultural systems Blair, Gj; Lefroy, Rdb; Lisle, L. Australian Journal of Agricultural Research, Vol. 46, Issue 7 https://doi.org/10.1071/AR9951459	journal	January 1995
Changes in soil organic matter with cropping as measured by organic carbon fractions and 13C natural isotope abundance Lefroy, Rod D. B.; Blair, Graeme J.; Strong, Wayne M. Plant and Soil, Vol. 155-156, Issue 1 https://doi.org/10.1007/BF00025067	journal	October 1993
Comparison of nuclear magnetic resonance methods for the analysis of organic matter composition from soil density and particle fractions Clemente, Joyce S.; Gregorich, Edward G.; Simpson, André J. Environmental Chemistry, Vol. 9, Issue 1 https://doi.org/10.1071/EN11096	journal	January 2012
Soil organic matter–hydrogen peroxide dynamics in the treatment of contaminated soils and groundwater using catalyzed H2O2 propagations (modified Fenton's reagent) Bissey, L.; Smith, J.; Watts, R. Water Research, Vol. 40, Issue 13 https://doi.org/10.1016/j.watres.2006.05.009	journal	July 2006
Sodium hypochlorite oxidation reduces soil organic matter concentrations without affecting inorganic soil constituents Siregar, A.; Kleber, M.; Mikutta, R. European Journal of Soil Science, Vol. 56, Issue 4 https://doi.org/10.1111/j.1365-2389.2004.00680.x	journal	August 2005
The Performance of Visible, Near-, and Mid-Infrared Reflectance Spectroscopy for Prediction of Soil Physical, Chemical, and Biological Properties Soriano-Disla, José M.; Janik, Les J.; Viscarra Rossel, Raphael A. Applied Spectroscopy Reviews, Vol. 49, Issue 2 https://doi.org/10.1080/05704928.2013.811081	journal	August 2013
Direct mass-spectrometric studies of the pyrolysis of carbonaceous fuels Evans, Robert J.; Milne, Thomas A.; Soltys, Michael N. Journal of Analytical and Applied Pyrolysis, Vol. 9, Issue 3 https://doi.org/10.1016/0165-2370(86)80012-2	journal	March 1986
Mechanisms of Hydrogen Peroxide Decomposition in Soils Petigara, Bhakti R.; Blough, Neil V.; Mignerey, Alice C. Environmental Science & Technology, Vol. 36, Issue 4 https://doi.org/10.1021/es001726y	journal	February 2002
Estimating active carbon for soil quality assessment: A simplified method for laboratory and field use Islam, K. R.; Stine, M. A.; Gruver, J. B. American Journal of Alternative Agriculture, Vol. 18, Issue 1 https://doi.org/10.1079/AJAA2003003	journal	March 2003
Critical Evaluation of the Use of Laser Diffraction for Particle-Size Distribution Analysis Eshel, G.; Levy, G. J.; Mingelgrin, U. Soil Science Society of America Journal, Vol. 68, Issue 3 https://doi.org/10.2136/sssaj2004.7360	journal	May 2004
Assessing the Reliability of Permanganate-Oxidizable Carbon as an Index of Soil Labile Carbon Tirol-Padre, A.; Ladha, J. K. Soil Science Society of America Journal, Vol. 68, Issue 3 https://doi.org/10.2136/sssaj2004.9690	journal	May 2004
The mid-infrared reflectance of mineral mixtures (7–14 μm) Thomson, Janice L.; Salisbury, John W. Remote Sensing of Environment, Vol. 45, Issue 1 https://doi.org/10.1016/0034-4257(93)90077-B	journal	July 1993
Old and stable soil organic matter is not necessarily chemically recalcitrant: implications for modeling concepts and temperature sensitivity: SLOW TURNOVER OF LABILE SOIL ORGANIC MATTER Kleber, Markus; Nico, Peter S.; Plante, Alain Global Change Biology, Vol. 17, Issue 2 https://doi.org/10.1111/j.1365-2486.2010.02278.x	journal	January 2011
Sodium hypochlorite separates an older soil organic matter fraction than acid hydrolysis Zimmermann, Michael; Leifeld, Jens; Abiven, Samuel Geoderma, Vol. 139, Issue 1-2 https://doi.org/10.1016/j.geoderma.2007.01.014	journal	April 2007
Mid-infrared spectral interpretation of soils: Is it practical or accurate? Reeves, James B. Geoderma, Vol. 189-190 https://doi.org/10.1016/j.geoderma.2012.06.008	journal	November 2012
Alteration of soil organic matter following treatment with hydrofluoric acid (HF) Rumpel, C.; Rabia, N.; Derenne, S. Organic Geochemistry, Vol. 37, Issue 11 https://doi.org/10.1016/j.orggeochem.2006.07.001	journal	November 2006
Visible, near infrared, mid infrared or combined diffuse reflectance spectroscopy for simultaneous assessment of various soil properties Viscarra Rossel, R. A.; Walvoort, D. J. J.; McBratney, A. B. Geoderma, Vol. 131, Issue 1-2 https://doi.org/10.1016/j.geoderma.2005.03.007	journal	March 2006
Comparison of different methods of obtaining a resilient organic matter fraction in Alpine soils Favilli, Filippo; Egli, Markus; Cherubini, Paolo Geoderma, Vol. 145, Issue 3-4 https://doi.org/10.1016/j.geoderma.2008.04.002	journal	June 2008
Poorly crystalline minerals protect organic carbon in clay subfractions from acid subsoil horizons Mikutta, R.; Kleber, M.; Jahn, R. Geoderma, Vol. 128, Issue 1-2 https://doi.org/10.1016/j.geoderma.2004.12.018	journal	September 2005
Comparison of Permanganate-Oxidizable Carbon and Mineralizable Carbon for Assessment of Organic Matter Stabilization and Mineralization Hurisso, Tunsisa T.; Culman, Steve W.; Horwath, William R. Soil Science Society of America Journal, Vol. 80, Issue 5 https://doi.org/10.2136/sssaj2016.04.0106	journal	September 2016
Molecular characterization of the pyrolysis of biomass Evans, Robert J.; Milne, Thomas A. Energy & Fuels, Vol. 1, Issue 2 https://doi.org/10.1021/ef00002a001	journal	March 1987
Pyrolysis-molecular beam mass spectrometry to characterize soil organic matter composition in chemically isolated fractions from differing land uses Plante, Alain F.; Magrini-Bair, Kim; Vigil, Merle Biogeochemistry, Vol. 92, Issue 1-2 https://doi.org/10.1007/s10533-008-9218-3	journal	July 2008
Determination of black carbon in natural organic matter by chemical oxidation and solid-state 13C nuclear magnetic resonance spectroscopy Simpson, Myrna J.; Hatcher, Patrick G. Organic Geochemistry, Vol. 35, Issue 8 https://doi.org/10.1016/j.orggeochem.2004.04.004	journal	August 2004
Organo-mineral associations in temperate soils: Integrating biology, mineralogy, and organic matter chemistry Kögel-Knabner, Ingrid; Guggenberger, Georg; Kleber, Markus Journal of Plant Nutrition and Soil Science, Vol. 171, Issue 1 https://doi.org/10.1002/jpln.200700048	journal	February 2008
Short- and Long-Term Labile Soil Carbon and Nitrogen Dynamics Reflect Management and Predict Corn Agronomic Performance Culman, Steve W.; Snapp, Sieglinde S.; Green, John M. Agronomy Journal, Vol. 105, Issue 2 https://doi.org/10.2134/agronj2012.0382	journal	January 2013
Stability of organic carbon in deep soil layers controlled by fresh carbon supply Fontaine, Sébastien; Barot, Sébastien; Barré, Pierre Nature, Vol. 450, Issue 7167 https://doi.org/10.1038/nature06275	journal	November 2007
Demineralization of marine and freshwater sediments for CP/MAS 13C NMR analysis Gélinas, Yves; Baldock, Jeff A.; Hedges, John I. Organic Geochemistry, Vol. 32, Issue 5 https://doi.org/10.1016/S0146-6380(01)00018-3	journal	May 2001
Biological indicators of soil quality and soil organic matter characteristics in an agricultural management continuum Veum, Kristen S.; Goyne, Keith W.; Kremer, Robert J. Biogeochemistry, Vol. 117, Issue 1 https://doi.org/10.1007/s10533-013-9868-7	journal	June 2013
Solid-state Carbon-13 Nuclear Magnetic Resonance and Infrared Spectroscopy of Composted Organic Matter Inbar, Y.; Chen, Y.; Hadar, Y. Soil Science Society of America Journal, Vol. 53, Issue 6 https://doi.org/10.2136/sssaj1989.03615995005300060014x	journal	January 1989
Can mid infrared diffuse reflectance analysis replace soil extractions? Janik, L. J.; Merry, R. H.; Skjemstad, J. O. Australian Journal of Experimental Agriculture, Vol. 38, Issue 7 https://doi.org/10.1071/EA97144	journal	January 1998
Permanganate Oxidizable Carbon Reflects a Processed Soil Fraction that is Sensitive to Management Culman, Steven W.; Snapp, Sieglinde S.; Freeman, Mark A. Soil Science Society of America Journal, Vol. 76, Issue 2 https://doi.org/10.2136/sssaj2011.0286	journal	January 2012
SOM fractionation methods: Relevance to functional pools and to stabilization mechanisms von Lützow, Margit; Kögel-Knabner, Ingrid; Ekschmitt, Klemens Soil Biology and Biochemistry, Vol. 39, Issue 9 https://doi.org/10.1016/j.soilbio.2007.03.007	journal	September 2007
Using data mining to model and interpret soil diffuse reflectance spectra Rossel, R. A. Viscarra; Behrens, T. Geoderma, Vol. 158, Issue 1-2 https://doi.org/10.1016/j.geoderma.2009.12.025	journal	August 2010
13C and 15N NMR spectroscopy as a tool in soil organic matter studies Kögel-Knabner, Ingrid Geoderma, Vol. 80, Issue 3-4 https://doi.org/10.1016/S0016-7061(97)00055-4	journal	November 1997
Bulk Chemical Characteristics of Dissolved Organic Matter in the Ocean Benner, R.; Pakulski, J. D.; Mccarthy, M. Science, Vol. 255, Issue 5051 https://doi.org/10.1126/science.255.5051.1561	journal	March 1992
Organic carbon and nitrogen in fine soil fractions after treatment with hydrogen peroxide Leifeld, Jens; Kögel-Knabner, Ingrid Soil Biology and Biochemistry, Vol. 33, Issue 15 https://doi.org/10.1016/S0038-0717(01)00127-4	journal	January 2001
Diffuse reflectance infrared fourier transform (DRIFT) spectroscopy in soil studies Nguyen, Tt; Janik, Lj; Raupach, M. Soil Research, Vol. 29, Issue 1 https://doi.org/10.1071/SR9910049	journal	January 1991
Improvement of 13C and 15N CPMAS NMR spectra of bulk soils, particle size fractions and organic material by treatment with 10% hydrofluoric acid Schmidt, M. W. I.; Knicker, H.; Hatcher, P. G. European Journal of Soil Science, Vol. 48, Issue 2 https://doi.org/10.1111/j.1365-2389.1997.tb00552.x	journal	June 1997
Comparison of chemical fractionation methods for isolating stable soil organic carbon pools Helfrich, M.; Flessa, H.; Mikutta, R. European Journal of Soil Science, Vol. 58, Issue 6 https://doi.org/10.1111/j.1365-2389.2007.00926.x	journal	December 2007
Organic matter bound to mineral surfaces: Resistance to chemical and biological oxidation Mikutta, Robert; Kaiser, Klaus Soil Biology and Biochemistry, Vol. 43, Issue 8 https://doi.org/10.1016/j.soilbio.2011.04.012	journal	August 2011
13C- and 15N-NMR spectroscopic examination of the transformation of organic nitrogen in plant biomass during thermal treatment Knicker, H.; Almendros, G.; González-Vila, F. J. Soil Biology and Biochemistry, Vol. 28, Issue 8 https://doi.org/10.1016/0038-0717(96)00078-8	journal	August 1996
Aromatization of organic matter induced by the presence of clays during flash pyrolysis-gas chromatography–mass spectrometry (PyGC–MS) Faure, Pierre; Schlepp, Laurence; Mansuy-Huault, Laurence Journal of Analytical and Applied Pyrolysis, Vol. 75, Issue 1 https://doi.org/10.1016/j.jaap.2005.02.004	journal	January 2006
Stabilization of Soil Organic Matter: Association with Minerals or Chemical Recalcitrance? Mikutta, Robert; Kleber, Markus; Torn, Margaret S. Biogeochemistry, Vol. 77, Issue 1 https://doi.org/10.1007/s10533-005-0712-6	journal	January 2006
Evaluation of pre-treatment procedures for improved interpretation of mid infrared spectra of soil organic matter Yeasmin, Sabina; Singh, Balwant; Johnston, Cliff T. Geoderma, Vol. 304 https://doi.org/10.1016/j.geoderma.2016.04.008	journal	October 2017
Use of specific peaks obtained by diffuse reflectance Fourier transform mid-infrared spectroscopy to study the composition of organic matter in a Haplic Chernozem Demyan, M. S.; Rasche, F.; Schulz, E. European Journal of Soil Science, Vol. 63, Issue 2 https://doi.org/10.1111/j.1365-2389.2011.01420.x	journal	February 2012
Stabilization of soil organic matter isolated via oxidative degradation Eusterhues, Karin; Rumpel, Cornelia; Kögel-Knabner, Ingrid Organic Geochemistry, Vol. 36, Issue 11 https://doi.org/10.1016/j.orggeochem.2005.06.010	journal	November 2005
Applicability of solid-state 13C CP/MAS NMR analysis in Spodosols: chemical removal of magnetic materials Dai, K'o H.; Johnson, Chris E. Geoderma, Vol. 93, Issue 3-4 https://doi.org/10.1016/S0016-7061(99)00072-5	journal	December 1999
The removal of magnetic materials from surface soils - a solid state 13C CP/MAS NMR study Skjemstad, Jo; Clarke, P.; Taylor, Ja Soil Research, Vol. 32, Issue 6 https://doi.org/10.1071/SR9941215	journal	January 1994
Persistence of soil organic matter as an ecosystem property Schmidt, Michael W. I.; Torn, Margaret S.; Abiven, Samuel Nature, Vol. 478, Issue 7367 https://doi.org/10.1038/nature10386	journal	October 2011

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Application of DRIFTS, 13 C NMR, and py-MBMS to Characterize the Effects of Soil Science Oxidation Assays on Soil Organic Matter Composition in a Mollic Xerofluvent

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References (49)

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Application of DRIFTS, ¹³ C NMR, and py-MBMS to Characterize the Effects of Soil Science Oxidation Assays on Soil Organic Matter Composition in a Mollic Xerofluvent