Skip to content
BY-NC-ND 3.0 license Open Access Published by De Gruyter Open Access March 1, 2003

13C NMR and mass spectrometry of soil organic matter

Galya Ivanova and Edward Randall
From the journal Open Chemistry


Liquid state, high resolution 13C NMR spectroscopy and mass spectrometry were used to study the composition and structure of soil organic matter (SOM) using soil extracts from two long-term experiments at the Rothamsted Experimental Station. Both one- and two-dimensional NMR techniques were applied. 13C NMR sub-spectra of the CHn (n=0...3) groups, obtained by the Distortionless Enhancement by Polarisation Transfer (DEPT) technique, were used for the elucidation of the qualitative and quantitative composition of humic and fulvic acids in the soils. The chemical structure of SOM was further analysed at the molecular level through Fast Atom Bombardment Mass Spectrometry (FABMS) and Gas Chromatography-Mass Spectrometry (GC/MS). Humic and fulvic extract results were not only compared to each other, but also to the solid state 13C NMR results for the complete soil sample.

[1] E.W. Randall, N. Mahieu, G.I. Ivanova: “NMR studies of soil, soil organic matter and nutriens: spectroscopy and imaging”, Geoderma, Vol. 80, (1997), pp. 307–325. in Google Scholar

[2] C.M. Preston: “Applications of NMR to soil organic matter analysis: history and prospects”, Soil Science, Vol. 161, (1996), pp. 144–166. in Google Scholar

[3] H.S. Shin and H. Moon: “An ‘average’ structure proposed for soil fulvic acid by DEPT/QUAT 13C NMR pulse techniques”, Soil Science, Vol. 161, (1996), pp. 250–256. in Google Scholar

[4] J. Lambert, P. Burba, J. Buddrus: “Quantification of Partial Structures in Aquatic Humic Substances by Volume Integration of Two-Dimensional 13C Nuclear Magnetic Resonance Spectra. Comparison of One- and Two-Dimensional Techniques”, Magn. Reson. Chem., Vol. 30, (1992), pp. 221–227. in Google Scholar

[5] L.W. Dennis and R.E. Pabst: Polarisation Transfer and 2D Experiments in NMR of Solutions of Humic Materials and Fossil Fuel Liquids. NMR of Humic Substances and Coal, Ch.6, Chealsea, USA, 1987. Search in Google Scholar

[6] J. Buddrus, B. Burba, H. Herzog, J. Lambert: “Quantitation of partial structures of aquatic humic substances by one- and two-dimensional solution 13C nuclear magnetic resonance spectroscopy”, Anal. Chem., Vol. 61, (1989), pp. 628–631. in Google Scholar

[7] R.M. Ede and G. Brunow: “Application of Two-Dimensional Homo- and Heteronuclear Correlation NMR Spectroscopy to Wood Lignin Structure Determination”, J. Org. Chem., Vol. 57, (1992), pp. 1477–1480. in Google Scholar

[8] H.-R. Schulten: Analytical Pyrolysis, Elsevier, Amsterdam, 1977. Search in Google Scholar

[9] R. Hempfling and H.-R. Schulten: “Chemical characterisation of the organic matter in forest soils by Curie point pyrolysis-GC/MS and pyrolysis-field ionisation mass spectrometry”, Org. Geochem., Vol. 15, (1990), pp. 131–145. in Google Scholar

[10] C.M. Preston, R. Hempfling, H.-R. Schulten, M. Schnitzer, J.A. Trofymov, D.E. Axelson: “Characterisation of the organic matter in a forest soil of coastal British Columbia by NMR and pyrolysis-field ionisation mass spectrometry”, Plant and Soil, Vol. 158, (1994), pp. 69–82. in Google Scholar

[11] M. Schnitzer and H.-R. Schulten: “Analysis of Organic Matter in Soil Extracts and Whole Soils by Pyrolysis-Mass Spectrometry”, Advances in Agronomy, Vol. 55, (1995), pp. 167–217. in Google Scholar

[12] L. Beyer, R. Frund, C. Wachendorf, H. Knicker, C. Sorge, C. Kobbemann, H.-R. Schulten, H.-D. Ludemann, H.-P. Blume: “A simple wet chemical extraction procedure to characterise soil organic matter (SOM): 3. Results of vegetation, crop litter and forest litter in comparison to data as revealed with CPMAS 13C NMR spectroscopy and pyrolysis-field ionisation mass spectrometry”, Commun. Soil Sci. Plant Anal., Vol. 27, (1996), pp. 2243–2264. in Google Scholar

[13] H.-R. Schulten: “The three-dimensional structure of humic substances and soil organic matter studied by computational analytical chemistry”, Fresenius J. Anal. Chem., Vol. 351, (1995), pp. 62–73. in Google Scholar

[14] H.-R. Schulten: “Analytical pyrolysis of humic substances and soils: geochemical, agrocultural and ecological consequences”, J. Analyt. Appl. Pyrolysis, Vol. 25, (1993), pp. 97–122. in Google Scholar

[15] H.-R. Schulten: “The three-dimensional structure of soil organo-mineral complexes studied by analytical pyrolysis”, J. Analyt. Appl. Pyrolysis, Vol. 32, (1995), pp. 111–126. in Google Scholar

[16] G. Calderoni and M. Schnitzer: “Effects of age on the chemical structure of Paleosol humic acids and fulvic acids”, Geochim. Cosmochim. Acta, Vol. 48, (1984), pp. 2045–2051. in Google Scholar

[17] G.I. Ivanova and E.W. Randall: “1H and 13C NMR study of soil organic matter at 14.1 T”, Bulg. Chem. Comm., Vol. 31, (1999), pp. 172–183. Search in Google Scholar

[18] J.A. Baldock, J.M. Oades, A.M. Vassallo, M.A. Wilson: “Incorporation of uniformly labelled 13C-glucose carbon into the organic fraction of soils. Carbon balance and CP/MAS 13C NMR measurements”, Austr. J. Soil Res., Vol. 27, (1989), pp. 725–746. in Google Scholar

[19] R. Frund and H.-D. Ludemann: “The quantitative analysis of solution and CPMAS-C-13 NMR spectra of humic material”, The Science of the Total Environment, Vol. 81/82, (1989), pp. 157–168. in Google Scholar

[20] P. Kinchesh, D.S. Powlson, E.W. Randall “13C NMR studies of organic matter in soils: I. Quantitation possibilities”, Europ. J. Soil Sci., Vol. 46, (1995), pp. 125–138. in Google Scholar

[21] N. Mahieu, D.S. Powlson, E.W. Randall: “Statistical analysis of published carbon-13 CPMAS NMR spectra of soil organic matter”, Soil Sci. Soc. Am. J., Vol. 63, (1999), pp. 307–319. in Google Scholar

[22] M.R. Bendall and D.T. Pegg: “Complete Accurate Editing of Decoupled 13C Spectra Using DEPT and a Quaternary-Only Sequence”, J. Magn. Res., Vol. 53, (1983), pp. 272–296. Search in Google Scholar

[23] J.R. Chapman: Practical Organic Mass Spectrometry, Ch. 5, Ed. J. Wiley & Sons Ltd., England, 1995. Search in Google Scholar

[24] P. Kinchesh, D.S. Powlson, E.W. Randall: “13C NMR studies of organic matter in soils: II. A case study of some Rothamsted soils”, Europ. J. Soil Sci., Vol. 46, (1995), pp. 139–146. in Google Scholar

Published Online: 2003-3-1
Published in Print: 2003-3-1

© 2003 Versita Warsaw

This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Scroll Up Arrow