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Purpose
Data management strategies of pyrolysis results and NMR acquisition modes were examined in humic acids (HAs) from control soils and fire-affected soils. The information supplied by dipolar dephasing (DD) 13C NMR spectroscopy and Curie-point pyrolysis were used to assess chemical structures hardly recognizable and measurable, or of unclear interpretation, when using 13C NMR under standard acquisition pulses (cross-polarization/magic angle spinning, CPMAS).Materials and methods
The HAs were isolated from two forest soils under Pinus halepensis and Pinus sylvestris in control and burned sites affected by medium or severe-intensity wildfires. For NMR analyses, during DD acquisition conditions, a 180° 13C pulse was inserted to minimize phase shifts. Curie-Point pyrolysis was carried out at 510 °C for 5 s, and the pyrolysis fragments were analyzed by GC/MS. The total abundances of the major pyrolysis products were compared by an update of the classical Van Krevelen’s graphical-statistical approach, i.e., as surface density values in the space defined by the compound-specific H/C and O/C atomic ratios.Results and discussion
The DD 13C NMR experiments displayed significant differences in the HA spectral profiles as regards to the standard CPMAS 13C NMR acquisition conditions, mainly in the chemical shift region of alkyl structures as well as for tannin- or carbohydrate-like O-alkyl structures. In fact, the comparison between DD and CPMAS solid-state NMR suggested shortening of alkyl chains and generation of carbohydrate-derived, unsaturated structures—viz. furans—which adds to the aromatic domain. Pyrolytic results showed fire-induced specific changes in HAs chemical structure and its molecular diversity. The changes were evident in the location and sizes of the different clusters of pyrolysis compounds defined by their atomic ratios.Conclusions
The DD 13C NMR provided specific information on the fate of aliphatic structures and the origin of unsaturated HA structures, which could be helpful in differentiating “inherited” from “pyrogenic” aromatic structures. This is further confirmed by the analysis of the molecular assemblages of pyrolytic products, which showed accumulation of condensed polyaromatic domains in the HAs after the high-intensity fire, accompanied by a recalcitrant alkyl hydrocarbon domain. Medium-intensity fire led to aromaticity increase due to a selective accumulation of lignin-derived phenols concomitant to the depletion of aliphatic hydrocarbon constituents.Aglime application can promote carbon dioxide (CO2) emissions from acid soils. However, the controlling mechanisms are still poorly understood, particularly the role of fertiliser-ammonium oxidation. This study therefore assessed the effects of aglime on soil inorganic C (SIC)– and soil organic C (SOC)–derived CO2 emissions from acid soils amended with ammonium.
Materials and methodsAmmonium at three N rates [0% (A0), 0.005% (A1), and 0.2% (A2) w/w] and labelled aglime (Ca13CO3,13C 5.94% aa) at three rates [0% (L1), 0.067% (L1), and 0.392% (L2) w/w] were applied to two contrasting acid soils (Nariva series, Mollic Fluvaquents; and Piarco series, Typic Kanhaplaquults) and incubated in 1-l media bottles for 23 days. A calcareous soil (Princes Town series, Aquentic Eutrudepts, carbonate δ13C of ??4.79‰) was included as a control that only received ammonium at the three rates.
Results and discussionThe application of ammonium at the A2 rate significantly (p?<?0.05) increased cumulative SIC-CO2 emissions by 15.8 and 27.1% in comparison to the A0 rate for the Nariva and Piarco soils, respectively, when they were limed at the L2 rate. The lower rate of ammonium (A1), however, had no effect on these emissions, which suggests that enough acidity may not have been generated at this rate to significantly enhance the release of SIC-CO2. Furthermore, no effect of ammonium rates was observed on SIC-CO2 emissions from the calcareous soil, which refutes the hypothesis that this amendment plays a greater role in regulating these emissions from calcareous soils compared with acid soils. Also, in contradiction to another hypothesis, the aglime-induced priming effect on SOC decomposition was more apparent in the low-C Piarco soil. This effect was also significantly (p?<?0.05) greater at the L2 rate (above the lime requirement for Piarco), which demonstrates the negative impact that over-liming could have on the sequestration of C in this soil. Our results also showed that ammonium addition may also help to reduce the magnitude of the aglime-induced priming effect in the Piarco soil when it is not over-limed.
ConclusionsOverall, the findings of this study suggest that ammonium fertiliser broadcast at conventional rates may not serve as a significant regulator of SIC-CO2 emissions from highly to moderately acidic soils amended with aglime. Our findings also indicate a need to consider nitrogen management as an important factor regulating the effects of aglime on SOC-CO2 emissions.
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