Solid-State and Multidimensional Solution-State NMR of Solid Phase Extracted and Ultrafiltered Riverine Dissolved Organic Matter

In this study we used multidimensional solution-state NMR to elucidate the differences in the chemical composition of solid phase extracted and ultrafiltered DOM isolates. DOM was isolated from water sampled from an oligotrophic river, the River Tagliamento (Italy). The recovery of total DOM was up...

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Bibliographic Details
Published in:Environmental science & technology 2003-07, Vol.37 (13), p.2929-2935
Main Authors: Kaiser, Edith, Simpson, Andre J, Dria, Karl J, Sulzberger, Barbara, Hatcher, Patrick G
Format: Article
Language:English
Subjects:
dissolved organic matter
Earth sciences
Earth, ocean, space
Environmental Monitoring - methods
Exact sciences and technology
Filtration
Geochemistry
Hydrology
Hydrology. Hydrogeology
Magnetic Resonance Spectroscopy
Matter & antimatter
Mineralogy
NMR
Nuclear magnetic resonance
Organic Chemicals - analysis
Organic chemistry
Silicates
Soil and rock geochemistry
Solubility
Spectrum analysis
Water geochemistry
Water Pollutants, Chemical - analysis
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Summary:In this study we used multidimensional solution-state NMR to elucidate the differences in the chemical composition of solid phase extracted and ultrafiltered DOM isolates. DOM was isolated from water sampled from an oligotrophic river, the River Tagliamento (Italy). The recovery of total DOM was up to 42% with both isolation techniques. In addition to 1- and 2-D solution-state NMR, we also applied 1-D solid-state 13C NMR spectroscopy for DOM characterization. 13C NMR spectroscopy only produced broad overlapping resonances, thus allowing a bulk characterization of DOM composition. However, it demonstrated that the bulk chemical composition of the two DOM fractions exhibited minor spatial-temporal changes. The 2-D experiments (TOCSY, HMQC) showed that the solid phase extracted hydrophobic DOM contained predominantly aliphatic esters, ethers, and hydroxyl groups, whereas the ultrafiltered DOM was comprised partially of peptides/protein, with further evidence for a small amount of aliphatic/fatty acid material. Sugars were present in both DOM fractions. The results show the two isolation techniques selected for different suites of compounds within the bulk DOM pool.
ISSN:0013-936X
1520-5851
DOI:10.1021/es020174b