Changes in organic components for fallen logs in old-growth Douglas-fir forests monitored by 13C nuclear magnetic resonance spectroscopy

1990 ◽  
Vol 20 (9) ◽  
pp. 1382-1391 ◽  
Author(s):  
Caroline M. Preston ◽  
Phillip Sollins ◽  
Brian G. Sayer

13C cross-polarization magic-angle spinning nuclear magnetic resonance (CPMAS NMR) spectroscopy was used to characterize heartwood from decaying fallen boles of Douglas-fir (Pseudotsugamenziesii (Mirb.) Franco), western hemlock (Tsugaheterophylla (Raf.) Sarg.), and western red cedar (Thujaplicata Donn). The sample decay classes I to V had been previously assigned based on field observations. Solid-state 13C CPMAS NMR spectra were analyzed to determine the proportion of C of the following chemical types: carbohydrate, lignin, aliphatic, and the sum of carboxyl plus carbonyl. For both Douglas-fir and western hemlock, the proportion of carbohydrate C increased slightly in the early stages of decay. This was followed by a substantial increase in lignin C, while carbohydrate C declined to about 10% of total C. By contrast, the spectra for western red cedar generally showed little change with increasing decay class. One exceptional sample of western red cedar class IV was highly decomposed, indicating complete loss of carbohydrate C, and some loss of lignin side-chain C. For all three species, signals from alkyl and carbonyl C were weak, but tended to increase slightly with decomposition, most likely because of the selective preservation of waxes and resins (alkyl C), and oxidation. Accumulation of chitin was not observed, and there was little evidence for lignin decomposition or for formation of humic polymers. 13C CPMAS NMR offers a simple and information-rich alternative to wet chemical analyses to monitor changes in organic components during decomposition of woody litter.

Fuel ◽  
1983 ◽  
Vol 62 (1) ◽  
pp. 103-111 ◽  
Author(s):  
P PAINTER ◽  
D KUEHN ◽  
M STARSINIC ◽  
A DAVIS ◽  
J HAVENS ◽  
...  

2005 ◽  
Vol 35 (8) ◽  
pp. 1821-1831 ◽  
Author(s):  
Chris E Johnson ◽  
Ronald J Smernik ◽  
Thomas G Siccama ◽  
David K Kiemle ◽  
Zhihong Xu ◽  
...  

Nuclear magnetic resonance (NMR) spectroscopy is a useful tool for examining the structural chemistry of natural organic matter. The use of cross-polarization and magic-angle spinning to study 13C functionality (CPMAS 13C NMR) is convenient, but not always quantitative. We used various 13C NMR techniques to examine the structural chemistry of bark and wood of sugar maple (Acer saccharum Marsh.), American beech (Fagus grandifolia Ehrh.), and yellow birch (Betula alleghaniensis Britt.). Spin counting experiments showed that 87%–97% of the 13C in the samples was observable by CPMAS 13C NMR. A comparison of CPMAS and Bloch decay experiments revealed few differences in spectral properties. Together, these results suggest that CPMAS 13C NMR is quantitative for these tissues. We observed little variation in the structural chemistry of wood, either among samples of the same species or among species. Within-species variations in bark chemistry were greater than in wood, probably because of variations in environmental conditions. However, we observed no significant differences in bark chemistry among the species. Bark and wood chemistry differed significantly, with the bark spectra displaying greater contributions from lignin, suberin, waxes, and resins. Hardwood spectra differ from softwood spectra in the aromatic C regions because of the contribution of syringyl units to hardwood lignin. Hardwood bark appears to contain less tannins than softwood bark. Together, the quantitative and qualitative features of CPMAS 13C NMR spectra are useful for studying the ecology of living and detrital wood and bark.


1997 ◽  
Vol 75 (9) ◽  
pp. 1601-1613 ◽  
Author(s):  
Caroline M. Preston ◽  
J. A. (Tony) Trofymow ◽  
Junning Niu ◽  
Brian G. Sayer

Proximate analysis is often used in decomposition studies to characterize the organic components of foliar litter. The percent weight residue remaining after extraction by nonpolar and polar solvents and H3SO4 hydrolysis (Klason lignin, KL) is commonly used as a measure of litter quality and a modelling parameter. While KL is associated with resistance to decay, its nature is not well understood and it has long been suspected that it incorporates nonlignin components. We used solid-state 13C nuclear magnetic resonance (NMR) spectroscopy to characterize litter, extracted residue, and the KL fraction of five species. NMR shows that cutin and condensed tannin are both significant components of litter and its extraction residues, in addition to lignin and carbohydrate. Hydrolysis with H2SO4 removes carbohydrates and amino acids, leaving the KL fraction derived from cutin, tannin, and lignin. Tannin retention in KL was also demonstrated by a hydrolysis study of purified tannins and a brown-rot lignin, using both NMR and the proanthocyanidin assay for condensed tannins. Although the NMR results are qualitative at this stage, it is clear that KL has limited use as a parameter controlling litter decomposition, and that other biopolymers should not be ignored in conceptual models, chemical analysis, and experimental design. Key words: Klason lignin, 13C CPMAS NMR, proximate analysis, litter quality, decomposition, tannin.


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