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Characterization of organic matter in an interlayer clay-organic complex from soil by pyrolysis methylation-mass spectrometry



Characterization of organic matter in an interlayer clay-organic complex from soil by pyrolysis methylation-mass spectrometry



Geoderma 69(1-2): 105-118



The composition of organic matter in clay-organic complexes isolated from a New Zealand Spodosol has been investigated using the novel analytical combination of (a) labscale (500 mg) off-line pyrolysis, (b) direct inlet (5 mg) off-line methylation with tetramethylammonium hydroxide (TMAH) and pyrolysis-field ionization mass spectrometry (Py-FIMS), and (c) Curie-point pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) with off-line and conventional on-line derivatisation with TMAH. In complex I the organic matter was associated with both external and interlayer surfaces of a swelling clay. Complex II was obtained by removing the external portion with H (sub 2) O (sub 2) , leaving the interlayer organic matter essentially intact. For both complexes, a high proportion of the carbon (64-86%) and nitrogen (76-91%) was volatilized during pyrolysis. Analysis of the pyrolysates showed mono- and dicarboxylic acids, alkanes, alkenes, n-alkylmonoesters, and N-containing compounds to be major constituents. Thermal methylation of the material, prior to (off-line) and during (on-line) pyrolysis gave rise to a wide range (between C (sub 6) and C (sub 35) ) of methyl esters of aliphatic and aromatic acids, methoxy derivatives of phenols and phenolic acids. In accord with previous (super 13) C-nuclear magnetic resonance (NMR) spectroscopic measurements, the organic matter in both complexes was highly aliphatic in composition. Although there was little difference between complex I and complex II in the composition of the aliphatic constituents, complex II was greatly depleted in lignin-derived aromatics. In addition, the interlayer material in complex II had a relatively low thermal stability.

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Accession: 002775840

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DOI: 10.1016/0016-7061(95)00054-2


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