Jump to ContentJump to Main Navigation
Show Summary Details
More options …

Open Chemistry

formerly Central European Journal of Chemistry


IMPACT FACTOR 2018: 1.512
5-year IMPACT FACTOR: 1.599

CiteScore 2018: 1.58

SCImago Journal Rank (SJR) 2018: 0.345
Source Normalized Impact per Paper (SNIP) 2018: 0.684

ICV 2018: 163.25

Open Access
Online
ISSN
2391-5420
See all formats and pricing
More options …
Volume 1, Issue 1

Issues

Volume 13 (2015)

13C NMR and mass spectrometry of soil organic matter

Galya Ivanova
  • Institute of Organic Chemistry with Centre of Phytochemistry, Bulgarian Academy of Sciences, 1113, Sofia, Bulgaria
  • Email
  • Other articles by this author:
  • De Gruyter OnlineGoogle Scholar
/ Edward Randall
Published Online: 2003-03-01 | DOI: https://doi.org/10.2478/BF02479254

Abstract

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.

Keywords: soil organic matter; 13C NMR; DEPT; FABMS; GC/MS; Rothamsted soils

  • [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. http://dx.doi.org/10.1016/S0016-7061(97)00057-8CrossrefGoogle Scholar

  • [2] C.M. Preston: “Applications of NMR to soil organic matter analysis: history and prospects”, Soil Science, Vol. 161, (1996), pp. 144–166. http://dx.doi.org/10.1097/00010694-199603000-00002CrossrefGoogle 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. http://dx.doi.org/10.1097/00010694-199604000-00006CrossrefGoogle 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. http://dx.doi.org/10.1002/mrc.1260300306CrossrefGoogle 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. 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. http://dx.doi.org/10.1021/ac00181a027CrossrefGoogle 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. http://dx.doi.org/10.1021/jo00031a028CrossrefGoogle Scholar

  • [8] H.-R. Schulten: Analytical Pyrolysis, Elsevier, Amsterdam, 1977. 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. http://dx.doi.org/10.1016/0146-6380(90)90078-ECrossrefGoogle 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. http://dx.doi.org/10.1007/BF00007919CrossrefGoogle 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. http://dx.doi.org/10.1016/S0065-2113(08)60540-4CrossrefGoogle 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. http://dx.doi.org/10.1080/00103629609369701CrossrefGoogle 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. http://dx.doi.org/10.1007/BF00324293CrossrefGoogle 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. http://dx.doi.org/10.1016/0165-2370(93)80035-XCrossrefGoogle 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. http://dx.doi.org/10.1016/0165-2370(94)00864-WCrossrefGoogle 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. http://dx.doi.org/10.1016/0016-7037(84)90385-5CrossrefGoogle 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. 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. http://dx.doi.org/10.1071/SR9890725CrossrefGoogle 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. http://dx.doi.org/10.1016/0048-9697(89)90121-6CrossrefGoogle 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. http://dx.doi.org/10.1111/j.1365-2389.1995.tb01819.xCrossrefGoogle 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. http://dx.doi.org/10.2136/sssaj1999.03615995006300020008xCrossrefGoogle 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. Google Scholar

  • [23] J.R. Chapman: Practical Organic Mass Spectrometry, Ch. 5, Ed. J. Wiley & Sons Ltd., England, 1995. 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. http://dx.doi.org/10.1111/j.1365-2389.1995.tb01820.xCrossrefGoogle Scholar

About the article

Published Online: 2003-03-01

Published in Print: 2003-03-01


Citation Information: Open Chemistry, Volume 1, Issue 1, Pages 10–27, ISSN (Online) 2391-5420, DOI: https://doi.org/10.2478/BF02479254.

Export Citation

© 2003 Versita Warsaw. This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License. BY-NC-ND 3.0

Comments (0)

Please log in or register to comment.
Log in