Structural studies on soil nitrogen by Curie-point pyrolysis ? gas chromatography/mass spectrometry with nitrogen-selective detection

Schulten, H.‐R.; Sorge, C.; Schnitzer, M.

doi:10.1007/bf00336555

Cited by 50 publications

(30 citation statements)

References 35 publications

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“…Heterocyclic-N structures of SOM were recently identified by Schulten et al (1995b). Cultivation increased the relative heterocyclic-to-peptide ratio, suggesting that the annual addition of 150 kg N ha -1 for 25 yr resulted either in the incorporation of fertilizer-N into heterocyclic compounds of SOM, or in the preferential decomposition and crop uptake of N derived from soil peptides.…”

Section: Turnover Of Som In Aggregatesmentioning

confidence: 99%

“…The identification of the pyrolysis products was based on determinations of thermal properties (Schulten 1987;Leinweber et al 1992), accurate mass measurements using high resolution mass spectrometry (Hempfling et al 1988;Hempfling and Schulten 1990), Curie-point gas chromatography-mass spectrometry (Hempfling and Schulten 1991;Schnitzer and Schulten 1992;Schulten et al 1995b), extensive National Institute of Science and Technology, Wiley library searches, and pyrolysis-mass spectrometry investigations of model polymers. The coefficient of variation for mass signals above 0.2% relative abundance of the summed spectra was 6%.…”

Section: Analysis Of Organic Componentsmentioning

confidence: 99%

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Age, turnover and molecular diversity of soil organic matter in aggregates of a Gleysol

Monreal¹,

Schulten²,

Kodama³

1997

Can. J. Soil. Sci.

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Monreal, C. M., Schulten, H.-R. and Kodama, H. 1997. Age, turnover and molecular diversity of soil organic matter in aggregates of a Gleysol. Can. J. Soil Sci. 77: 379-388. We used an integrated approach to describe soil organic matter (SOM) dynamics through known inorganic and organic components in aggregates of adjacent forested and cultivated Gleysolic soil. Mineral and SOM components were examined in water stable macroaggregates (>250 µm), microaggregates 1 (50-250 µm) and microaggregates 2 (<50 µm) fractions. SOM was characterized by pyrolysis-field ionization mass spectrometry (Py-FIMS), and soil minerals by X-ray diffraction analysis. The mean residence time of organic-C (OC) was determined using radiocarbon dating. OC turnover was determined using the natural abundance of native 13 C and that derived from corn residue. We found that OC in macroaggregates was young (<100 yr), turned over in 14 yr, and consisted of OM typical of that found in tissues of plants and soil organisms. Chemical classes of compounds in macroaggregates consisted mainly of carbohydrates, lignin monomers and phenols, lignin dimers, lipids (alkanes, alkenes, n-alkyl esters), fatty acids, sterols, suberin and aliphatic and aromatic N compounds. The fast turnover time of OC in larger size aggregates supports the hypothesis that the initial decline in SOM after breaking native land is associated with losses of SOM stored in macroaggregates. OC in microaggregates 1 was young (<100 yr) and turned over in 61 yr. OC in microaggregates 2 was old, turned over in 275 yr, and consisted of highly humified macromolecules. Pyrolyzable SOM products representing plant and microbial components like lignin dimers, sterols, suberin and fatty acids were absent from microaggregates 2 containing old OC. The turnover time of OC correlated directly with the amount of smectite and Al extracted with ammonium oxalate, inversely with non-expandable phyllosilicates, and weakly with the total clay content of aggregates. Thermolabile and thermostable molecular components in aggregates indicated degree of association between SOM and clay minerals. Carbohydrates, peptides and alkylaromatics appeared to be less affected by abiotic stabilization reactions. The distribution, allocation and dynamics of soil OC and chemical structures in SOM within aggregate fractions is not well understood. Carbon dynamics were characterized in humic acid fractions, whole soil and particle size fractions (Campbell et al. 1967;Hsieh 1992;Gregorich et al. 1995); kinetically described in simulation models for rapidly cycling (seconds to months) and more stable pools of organic matter (years to thousands of years) (Monreal and McGill 1989;Jenkinson and Rayner 1977;Parton et al. 1987 For personal use only.

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Section: Turnover Of Som In Aggregatesmentioning

confidence: 99%

Section: Analysis Of Organic Componentsmentioning

confidence: 99%

Age, turnover and molecular diversity of soil organic matter in aggregates of a Gleysol

Monreal¹,

Schulten²,

Kodama³

1997

Can. J. Soil. Sci.

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“…These and similarly substituted N-heterocyclic compounds were detected by Cp Py-GC/MS under the same analytical conditions in aquatic humic fractions and dissolved organic matter (Schulten 1999;Schulten et al 2002), in organic precursors of SOM such as microbial biomass and plant residues (Schulten and Schnitzer 1998), re-circulated leachates of municipal solid waste (Franke et al 2006(Franke et al , 2007 and also in whole soils such as Vertisols (Leinweber et al 1999) and Haplaborolls in the Canadian prairies (Leinweber et al 2009b). These Nheterocyclic compounds often were explained by their formation during Cp pyrolysis, as shown for individual amino acids and peptides (Bracewell and Robertson 1984;Schulten et al 1995). Pyrolysis products were reported for lysine (pyridine) (Sorge 1995), hydroxyproline, proline (1H-pyrrole, 1-methyl-) (Nguyen et al 2003), hydroxyproline (1H-pyrrole, 2,5-dimethyl-) (Chiavari and Galletti 1992), alanine, tyrosine (pyridine) (Chiavari and Galletti 1992;Nguyen et al 2003), threonine (pyridine, 5-ethenyl-2-methyl-) (Sorge et al 1993), and phenylalanine (quinoline) (Patterson et al 1973) (pyrolysis product in parenthesis).…”

Section: Resultsmentioning

confidence: 97%

Nitrogen speciation in fine and coarse clay fractions of a Cryoboroll - new evidence from pyrolysis-mass spectrometry and nitrogen K-edge XANES

Leinweber

Jandl²,

Eckhardt³

et al. 2010

Can. J. Soil. Sci.

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Nitrogen speciation in fine and coarse clay fractions of a Cryoboroll Á new evidence from pyrolysis-mass spectrometry and nitrogen K-edge XANES. Can. J. Soil Sci. 90: 309Á318. Soil clay fractions are usually enriched in nitrogen (N), but the chemical identity of this N is largely unknown. Therefore, we investigated organic N in fine and coarse clay of a clay-rich Cryoboroll by Curie-point pyrolysis-gas chromatography/mass spectrometry (Cp Py-GC/MS), Pyrolysis-field ionization mass spectroscopy (Py-FIMS) and synchrotron-based nitrogen K-edge X-ray absorption near edge structure (N-XANES) spectroscopy. The Cp Py-GC-MS revealed 30 structurally different N-containing compounds, such as substituted pyridines, pyrroles; pyrazines, pyrazoles, imidazoles, quinolines, side-chain N-containing benzenes, and single compounds of substituted benzotriazole, purine and indole. These accounted for about 10% of peak area in the Py-GC chromatograms. The Py-FIMS and N-XANES spectra indicated interlayer-NH 4 ' and revealed pyridinic and nitrilic N compounds, but disagreed in the proportions of pyrroles. All three complementary methods confirmed to different extents previous wet-chemical data on N-fractions in these samples, and provided new evidence for about 30 to 40% non-proteinaceous N as major constituent of the so-called ''unknown organic N'' in soil.

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“…But it requires elaborate preparation or derivatization steps prior to analyses involving degradation of the macromolecular structure. In recent years, combinations of analytical pyrolysis with GC, MS or GC/MS have become widely used in determining the molecular structure of various bio-and geopolymers (50,(82)(83)(84)(85)(86)(87)(88)(89)(90). Although it is an ideal technique for the study of recalcitrant polymeric organic matter, even when more than one macromolecule is present, it involves thermal decomposition of chemical structures and provides only partial and sometimes biased molecular information (91).…”

Section: Other N-containing Moleculesmentioning

confidence: 99%

“…While traditional approaches such as elemental analysis and calculations of C/N ratios are still routinely used (12,50), various spectroscopic and biochemical methods have become more popular in the last decade. These latter methods can provide detailed molecular information on the chemical structure(s) of N-containing molecules.…”

Section: Other N-containing Moleculesmentioning

confidence: 99%

Nitrogen and N-Containing Macromolecules in the Bio- and Geosphere: An Introduction

Stankiewicz

Bergen

1998

ACS Symposium Series

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Structural studies on soil nitrogen by Curie-point pyrolysis ? gas chromatography/mass spectrometry with nitrogen-selective detection

Cited by 50 publications

References 35 publications

Age, turnover and molecular diversity of soil organic matter in aggregates of a Gleysol

Age, turnover and molecular diversity of soil organic matter in aggregates of a Gleysol

Nitrogen speciation in fine and coarse clay fractions of a Cryoboroll - new evidence from pyrolysis-mass spectrometry and nitrogen K-edge XANES

Nitrogen and N-Containing Macromolecules in the Bio- and Geosphere: An Introduction

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