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

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 spectroscopy for amore »« less

Authors:

^[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.

Publication Date:: Tue Feb 20 00:00:00 EST 2018

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

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

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.

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                    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.  https://doi.org/10.1016/j.scitotenv.2018.02.121

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                    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.  https://doi.org/10.1016/j.scitotenv.2018.02.121.  https://www.osti.gov/servlets/purl/1463852.

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@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         = {Tue Feb 20 00:00:00 EST 2018},

  month        = {Tue Feb 20 00:00:00 EST 2018}

}

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Similar Records

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

Abstract

Citation Formats

ATTEMPTS TO IMPROVE SOLID STATE 13 C NMR SPECTRA OF WHOLE MINERAL SOILS journal, August 1988

Assessing the extent of decomposition of natural organic materials using solid-state 13C NMR spectroscopy journal, January 1997

An In-Situ ATR-FTIR Study: The Surface Coordination of Salicylic Acid on Aluminum and Iron(III) Oxides journal, May 1994

Spectroscopic characterization of the structural and functional properties of natural organic matter fractions journal, July 2002

Soft X-ray Spectromicroscopy Study of Mineral-Organic Matter Associations in Pasture Soil Clay Fractions journal, May 2014

Properties of Fe-Organic Matter Associations via Coprecipitation versus Adsorption journal, November 2014

C-1s NEXAFS Spectroscopy Reveals Chemical Fractionation of Humic Acid by Cation-Induced Coagulation journal, March 2007

Determination of chemical-structural changes in vitrinite accompanying luminescence alteration using C-NEXAFS analysis journal, May 1998

Formation of soil organic matter via biochemical and physical pathways of litter mass loss journal, September 2015

Cross polarization-single pulse/magic angle spinning (CPSP/MAS): A robust technique for routine soil analysis by solid-state NMR journal, August 2014

Applicability of solid-state 13C CP/MAS NMR analysis in Spodosols: chemical removal of magnetic materials journal, December 1999

Stabilisation of soil organic matter by interactions with minerals as revealed by mineral dissolution and oxidative degradation journal, December 2003

Complexes of fulvic acid on the surface of hematite, goethite, and akaganeite: FTIR observation journal, April 2006

Adsorption and desorption of natural organic matter on iron oxide: mechanisms and models journal, January 1994

Changes in water extractable organic matter during incubation of forest floor material in the presence of quartz, goethite and gibbsite surfaces journal, August 2011

C 1s K-edge near edge X-ray absorption fine structure (NEXAFS) spectroscopy for characterizing functional group chemistry of black carbon journal, October 2011

Quantitative solid-state 13C NMR with signal enhancement by multiple cross polarization journal, February 2014

Organic carbon and sulphur compounds in wetland soils: insights on structure and transformation processes using K-edge XANES and NMR spectroscopy journal, July 2003

Dissolved organic matter sorption by mineral constituents of subsoil clay fractions journal, October 2000

Innershell Absorption Spectroscopy of Amino Acids journal, April 2002

Nano-scale investigation of the association of microbial nitrogen residues with iron (hydr)oxides in a forest soil O-horizon journal, October 2012

13C NMR studies of organic matter in whole soils: I. Quantitation possibilities journal, March 1995

N-15 and C-13 CPMAS and solution NMR studies of N-15 enriched plant material during 600 days of microbial degradation journal, April 1995

13C and 15N NMR spectroscopy as a tool in soil organic matter studies journal, November 1997

Soil phosphorus supply controls P nutrition strategies of beech forest ecosystems in Central Europe journal, September 2017

Spatial complexity of soil organic matter forms at nanometre scales journal, March 2008

Iron Oxide Removal from Soils and Clays by a Dithionite-Citrate System Buffered with Sodium Bicarbonate journal, January 1958

Radiocarbon Dating for Determination of Soil Organic Matter Pool Sizes and Dynamics journal, January 1997

Variable-Amplitude Cross-Polarization MAS NMR journal, October 1993

Analysis of non-cellulosic polysaccharides helps to reveal the history of thick organic surface layers on calcareous Alpine soils journal, July 2012

Organic matter losses in German Alps forest soils since the 1970s most likely caused by warming journal, June 2016

ATHENA , ARTEMIS , HEPHAESTUS : data analysis for X-ray absorption spectroscopy using IFEFFIT journal, June 2005

Deep soil organic matter—a key but poorly understood component of terrestrial C cycle journal, May 2010

Vertical distribution, age, and chemical composition of organic carbon in two forest soils of different pedogenesis journal, October 2002

Is demineralization with dilute hydrofluoric acid a viable method for isolating mineral stabilized soil organic matter? journal, October 2017

Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle journal, February 1976

Improvement of 13C and 15N CPMAS NMR spectra of bulk soils, particle size fractions and organic material by treatment with 10% hydrofluoric acid journal, June 1997

Intimate association between O/N-alkyl carbon and iron oxides in clay fractions of forest soils journal, October 2005

Chemical Heterogeneity of Organic Soil Colloids Investigated by Scanning Transmission X-ray Microscopy and C-1s NEXAFS Microspectroscopy journal, December 2005

Differenzierung der Eisenoxide des Bodens durch Extraktion mit Ammoniumoxalat-Lösung journal, January 1964

Nuclear Magnetic Resonance Spectroscopy and Its Key Role in Environmental Research journal, August 2012

Environmental Nuclear Magnetic Resonance Spectroscopy: An Overview and a Primer journal, December 2017

The removal of magnetic materials from surface soils - a solid state 13C CP/MAS NMR study journal, January 1994

The use of spin counting for determining quantitation in solid state 13C NMR spectra of natural organic matter journal, May 2000

Soil Organic Matter Composition in the Subhumid Ethiopian Highlands as Influenced by Deforestation and Agricultural Management journal, January 2002

Carbon K-Edge NEXAFS and FTIR-ATR Spectroscopic Investigation of Organic Carbon Speciation in Soils journal, January 2005

Carbon (1s) NEXAFS Spectroscopy of Biogeochemically Relevant Reference Organic Compounds journal, January 2009

Soil organic matter stabilization in acidic forest soils is preferential and soil type-specific journal, August 2008

Organic carbon distribution, speciation, and elemental correlations within soil microaggregates: Applications of STXM and NEXAFS spectroscopy journal, November 2007

Small-scale spatial distribution of phosphorus fractions in soils from silicate parent material with different degree of podzolization journal, September 2017

Micro-scale heterogeneity of soil phosphorus depends on soil substrate and depth journal, June 2017

CP-MAS-13C-NMR-Spektren organischer Lagen einer Tangelrendzina journal, January 1985

Relationship between macropores and soil organic carbon fractions under long‐term organic manure application journal, January 2020

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

ATTEMPTS TO IMPROVE SOLID STATE ¹³ C NMR SPECTRA OF WHOLE MINERAL SOILS
journal, August 1988

Assessing the extent of decomposition of natural organic materials using solid-state 13C NMR spectroscopy
journal, January 1997

An In-Situ ATR-FTIR Study: The Surface Coordination of Salicylic Acid on Aluminum and Iron(III) Oxides
journal, May 1994

Spectroscopic characterization of the structural and functional properties of natural organic matter fractions
journal, July 2002

Soft X-ray Spectromicroscopy Study of Mineral-Organic Matter Associations in Pasture Soil Clay Fractions
journal, May 2014

Properties of Fe-Organic Matter Associations via Coprecipitation versus Adsorption
journal, November 2014

C-1s NEXAFS Spectroscopy Reveals Chemical Fractionation of Humic Acid by Cation-Induced Coagulation
journal, March 2007

Determination of chemical-structural changes in vitrinite accompanying luminescence alteration using C-NEXAFS analysis
journal, May 1998

Formation of soil organic matter via biochemical and physical pathways of litter mass loss
journal, September 2015

Cross polarization-single pulse/magic angle spinning (CPSP/MAS): A robust technique for routine soil analysis by solid-state NMR
journal, August 2014

Applicability of solid-state 13C CP/MAS NMR analysis in Spodosols: chemical removal of magnetic materials
journal, December 1999

Stabilisation of soil organic matter by interactions with minerals as revealed by mineral dissolution and oxidative degradation
journal, December 2003

Complexes of fulvic acid on the surface of hematite, goethite, and akaganeite: FTIR observation
journal, April 2006

Adsorption and desorption of natural organic matter on iron oxide: mechanisms and models
journal, January 1994

Changes in water extractable organic matter during incubation of forest floor material in the presence of quartz, goethite and gibbsite surfaces
journal, August 2011

C 1s K-edge near edge X-ray absorption fine structure (NEXAFS) spectroscopy for characterizing functional group chemistry of black carbon
journal, October 2011

Quantitative solid-state 13C NMR with signal enhancement by multiple cross polarization
journal, February 2014

Organic carbon and sulphur compounds in wetland soils: insights on structure and transformation processes using K-edge XANES and NMR spectroscopy
journal, July 2003

Dissolved organic matter sorption by mineral constituents of subsoil clay fractions
journal, October 2000

Innershell Absorption Spectroscopy of Amino Acids
journal, April 2002

Nano-scale investigation of the association of microbial nitrogen residues with iron (hydr)oxides in a forest soil O-horizon
journal, October 2012

13C NMR studies of organic matter in whole soils: I. Quantitation possibilities
journal, March 1995

N-15 and C-13 CPMAS and solution NMR studies of N-15 enriched plant material during 600 days of microbial degradation
journal, April 1995

13C and 15N NMR spectroscopy as a tool in soil organic matter studies
journal, November 1997

Soil phosphorus supply controls P nutrition strategies of beech forest ecosystems in Central Europe
journal, September 2017

Spatial complexity of soil organic matter forms at nanometre scales
journal, March 2008

Iron Oxide Removal from Soils and Clays by a Dithionite-Citrate System Buffered with Sodium Bicarbonate
journal, January 1958

Radiocarbon Dating for Determination of Soil Organic Matter Pool Sizes and Dynamics
journal, January 1997

Variable-Amplitude Cross-Polarization MAS NMR
journal, October 1993

Analysis of non-cellulosic polysaccharides helps to reveal the history of thick organic surface layers on calcareous Alpine soils
journal, July 2012

Organic matter losses in German Alps forest soils since the 1970s most likely caused by warming
journal, June 2016

ATHENA , ARTEMIS , HEPHAESTUS : data analysis for X-ray absorption spectroscopy using IFEFFIT
journal, June 2005

Deep soil organic matter—a key but poorly understood component of terrestrial C cycle
journal, May 2010

Vertical distribution, age, and chemical composition of organic carbon in two forest soils of different pedogenesis
journal, October 2002

Is demineralization with dilute hydrofluoric acid a viable method for isolating mineral stabilized soil organic matter?
journal, October 2017

Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle
journal, February 1976

Improvement of 13C and 15N CPMAS NMR spectra of bulk soils, particle size fractions and organic material by treatment with 10% hydrofluoric acid
journal, June 1997

Intimate association between O/N-alkyl carbon and iron oxides in clay fractions of forest soils
journal, October 2005

Chemical Heterogeneity of Organic Soil Colloids Investigated by Scanning Transmission X-ray Microscopy and C-1s NEXAFS Microspectroscopy
journal, December 2005

Differenzierung der Eisenoxide des Bodens durch Extraktion mit Ammoniumoxalat-Lösung
journal, January 1964

Nuclear Magnetic Resonance Spectroscopy and Its Key Role in Environmental Research
journal, August 2012

Environmental Nuclear Magnetic Resonance Spectroscopy: An Overview and a Primer
journal, December 2017

The removal of magnetic materials from surface soils - a solid state 13C CP/MAS NMR study
journal, January 1994

The use of spin counting for determining quantitation in solid state 13C NMR spectra of natural organic matter
journal, May 2000

Soil Organic Matter Composition in the Subhumid Ethiopian Highlands as Influenced by Deforestation and Agricultural Management
journal, January 2002

Carbon K-Edge NEXAFS and FTIR-ATR Spectroscopic Investigation of Organic Carbon Speciation in Soils
journal, January 2005

Carbon (1s) NEXAFS Spectroscopy of Biogeochemically Relevant Reference Organic Compounds
journal, January 2009

Soil organic matter stabilization in acidic forest soils is preferential and soil type-specific
journal, August 2008

Organic carbon distribution, speciation, and elemental correlations within soil microaggregates: Applications of STXM and NEXAFS spectroscopy
journal, November 2007

Small-scale spatial distribution of phosphorus fractions in soils from silicate parent material with different degree of podzolization
journal, September 2017

Micro-scale heterogeneity of soil phosphorus depends on soil substrate and depth
journal, June 2017

CP-MAS-13C-NMR-Spektren organischer Lagen einer Tangelrendzina
journal, January 1985

Relationship between macropores and soil organic carbon fractions under long‐term organic manure application
journal, January 2020