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1.
The small organic matter content of mineral soils makes it difficult to obtain 13C and 15N nuclear magnetic resonance (NMR) spectra with acceptable signal-to-noise ratios. Subjecting such samples to hydrofluoric acid removes mineral matter and leads to a relative increase in organic material. The effect of treatment with 10% hydrofluoric acid on bulk chemical composition and resolution of solid-state 13C NMR spectra was investigated with six soils, some associated particle size fractions, plant litter and compost. The treatment enhanced the signal-to-noise ratio of the solid-state 13C NMR spectra. The improvement in spectrum quality was greatest in the clay fraction of soil contaminated with coal ash. The removal of paramagnetic compounds associated with the ash may be the main reason for the improvement. Based on total C, total N, C/N ratio and intensity distribution of the solid-state 13C NMR spectra, no changes in organic matter composition could be detected, except for a possible loss of carbohydrates. After treatment with HF, solid-state 15N NMR spectra of particle size fractions were obtained and indicated that the observable nitrogen is present mostly as peptides and free amino groups. Extraction with hydrofluoric acid is recommended as a routine treatment prior to solid-state 13C and 15N NMR on soil containing little C or N and soil samples containing paramagnetic compounds from natural or anthropogenic sources.  相似文献   

2.
Four soils with a range of clay and silt contents were incubated for 5 a with 15N-labelled (NH4)SO4 and 14C-labelled hemicellulose and then fractionated according to particle size by ultrasonic dispersion and sedimentation. The distribution of labelled and native N between clay, silt and sand fractions was determined and elated to previous results on the C distributions. Between 29% and 48% of the added N was found in organic form. The 15N atom percentage excess decreased in the order: clay > whole soil > silt > sand. For both clay and silt, the enrichment factor for labelled and native N decreased with increasing fraction weight. Clay enrichment was higher for labelled than for native N, the converse being true for silt. The distribution of whole soil labelled organic N was: clay 77–91%, silt 4–11%, and sand <0.5%. Corresponding values for native N were 69–74%, 16–22%, and 1–2%, respectively. All soils had higher proportions of labelled than of native N in the clay, the converse was true for the silt. The C/N ratio of the native silt organic matter was higher and that of clay organic matter lower than whole soil C/N ratios. Differences between the C/N ratio distributions of native and labelled organic matter were small. The relative distribution of labelled N and C was very similar confirming that the turnover of C and N in soil organic matter is closely interrelated.  相似文献   

3.
Transformations of sodium acetate, ammonium sulphate, urea and wheat straw in peat have been studied by determining the distribution of 15N-labelled material, and by 13C and 15N nuclear magnetic resonance spectroscopy (NMR) using cross polarization (CP) and magic-angle spinning (MAS). Samples of an oligotrophic blanket peat were incubated for 6 months at 15°C with 15N ammonium sulphate, 15N urea, 13C15N urea, 15N-labelled wheat straw or 13C sodium acetate. The incubated samples were separated into fractions of >1 mm, 1–0.5 mm, 0.5–0.25 mm, 0.25–0.15 mm, 0.15–0.05 mm, 0.05–0.005 mm and a water-soluble fraction by wet sieving, and were then freeze-dried. The distribution of 15N between the fractions was obtained after isotope-ratio analysis by mass spectrometry, and the 0.5–0.25 mm, 0.05–0.005 mm and water-soluble fractions from the incubations were examined by 13C and 15N NMR. 13C-labelled acetate increased carbohydrate resonances in the 0.05–0.005 mm and soluble material, but an organic acid derived from the substrate was still present 6 months later. Incorporation of 15N from ammonium sulphate into the peat was low, and more than 50% of the added N was detected in the soluble fraction still present as 15NH+4. As carbohydrate and soluble organic matter were detected in the peat, it was concluded that microbial activity and N immobilization were restricted by poor aeration and low pH. Urea, in contrast, interacted with all the fractions examined, with some 15N being incorporated into a range of compounds that included protein, peptides, amides, amino acids and carbamates or lactam derivatives. A small proportion of labelled 15N from wheat straw, orginally present in the > 1 mm and 14.5 mm fractions, had moved into the 0.05–0.005 fraction during incubation and sieving. The 13C spectra suggested that the presence of the straw may have stimulated decomposition of the peat components.  相似文献   

4.
Investigating the biogeochemistry of plant material decomposition in soil has been restricted by difficulties extracting and identifying organic compounds. In this study the decomposition of 13C- and 15N-labelled Lolium perenne leaves mixed with mineral soil has been investigated over 224 days of incubation under laboratory conditions. Decomposition was followed using short-term rates of CO2 evolution, the amounts of 13C and 15N remaining were determined by mass spectrometry, and 13C and 15N solid-state nuclear magnetic resonance (NMR) spectroscopy was used to characterize chemically the plant material as it decomposed. After 224 days 48% of the added 13C had been lost with a rapid period of C02 evolution over the first 56 days. The fraction of cross-polarization magic angle spinning (CP MAS) 13C NMR spectra represented by O-alkyl-C signal probably in carbohydrates (chemical shift, 60–90 p.p.m.) declined from 60 to 20% of the spectrum (chemical shift, 0–200 p.p.m.) over 224 days. The rate of decline of the total 13C exceeded that of the 60–90 p.p.m. signal during the first 56 days and was similar thereafter. The fraction of the CP MAS 13C NMR spectra represented by the alkyl- and methyl-C (chemical shift, 10–45 p.p.m.) signal increased from 5 to 14% over the first 14 days and was 19% after 224 days. CP MAS 13C NMR of 13C- and 15N-L. perenne contained in 100-μm aperture mesh bags incubated in the soil for 56 days indicated that the remaining material was mainly carbohydrate but there was an increase in the alkyl- and methyl-C associated with the bag's contents. After 224 days incubation of the labelled 13C- and 15N-L. perenne mixed with the soil, 40% of the added N had been lost. Throughout the incubation there was only one signal centred around 100 p.p.m. detectable in the CP MAS 15N NMR spectra. This signal corresponded to amide 15N in peptides and may have been of plant or microbial origin or both. Although there had been substantial interaction between the added 15N and the soil microorganisms, the associated redistribution of 15N from plant to microbial tissues occurred within the amide region. The feasibility of following some of the component processes of plant material decomposition in soil using NMR has been demonstrated in this study and evidence that microbial synthesis contributes to the increase in alkyl- and methyl-C content of soil during decomposition has been represented.  相似文献   

5.
The availability of C and N to the soil microbial biomass is an important determinant of the rates of soil N transformations. Here, we present evidence that changes in C and N availability affect the 15N natural abundance of the microbial biomass relative to other soil N pools. We analysed the 15N natural abundance signature of the chloroform‐labile, extractable, NO3–, NH4+ and soil total N pools across a cattle manure gradient associated with a water reservoir in semiarid, high‐desert grassland. High levels of C and N in soil total, extractable, NO3–, NH4+ and chloroform‐labile fractions were found close to the reservoir. The δ15N value of chloroform‐labile N was similar to that of extractable (organic + inorganic) N and NO3– at greater C availability close to the reservoir, but was 15N‐enriched relative to these N‐pools at lesser C availability farther away. Possible mechanisms for this variable 15N‐enrichment include isotope fractionation during N assimilation and dissimilation, and changes in substrate use from a less to a more 15N‐enriched substrate with decreasing C availability.  相似文献   

6.
DFT calculations are a powerful tool to support NMR studies of xenobiotics such as decomposition studies in soil. They can help interpret spectra of bound residues, for example, by predicting shifts for possible model bonds. The described bound‐residue models supported the hypothesis of a free amino side chain already suspected by comparison with the experimental data of the standards. No match was found between the calculated shifts of amide bondings of the amino side chains (free or substituted) and the experimental NMR shifts of a previous study. In the present paper, first‐principles quantum chemical calculations were used to support and check the interpretation of the 15N cross polarization‐magic angle spinning nuclear magnetic resonance (15N‐CPMAS NMR) spectra of simazine and its metabolites. Density functional theory (DFT) calculations were performed using Gaussian 03 and the nuclear magnetic shielding tensors were calculated using the Gauge‐Independent Atomic Orbital (GIAO) method and B3LYP/6–311+G(2d,p) model chemistry. Good agreement was reached between the calculated and measured chemical shifts of the core nitrogens and the lactam and lactim forms of the hydroxylated metabolites could be clearly distinguished. The calculated spectra showed that these metabolites exist preferentially in the lactam form, an important fact when considering the possible interactions of such hydroxylated metabolites with the soil matrix. Although the calculated bound‐residue models in the present study only partly matched the experimental data, they were nevertheless useful in helping to interpret the experimental NMR results of a previous study. To get a better match between the calculated and the measured shifts of the side‐chain nitrogens the calculations need to be further developed, taking into account the influence of neighbouring molecules in the solid state. Altogether, quantum chemical calculations are very helpful in the interpretation of NMR spectra. In the future, they can also be very useful for the prediction of NMR shifts, in particular when it is not possible to measure the metabolites due to a lack of material or in cases where practical experiments cannot be conducted.  相似文献   

7.
The contribution of bacteria and fungi to NH4+ and organic N (Norg) oxidation was determined in a grassland soil (pH 6.3) by using the general bacterial inhibitor streptomycin or the fungal inhibitor cycloheximide in a laboratory incubation study at 20°C. Each inhibitor was applied at a rate of 3 mg g?1 oven‐dry soil. The size and enrichment of the mineral N pools from differentially (NH415NO3 and 15NH4NO3) and doubly labelled (15NH415NO3) NH4NO3 were measured at 3, 6, 12, 24, 48, 72, 96 and 120 hours after N addition. Labelled N was applied to each treatment, to supply NH4+‐N and NO3?‐N at 3.15 μmol N g?1 oven‐dry soil. The N treatments were enriched to 60 atom % excess in 15N and acetate was added at 100 μmol C g?1 oven‐dry soil, to provide a readily available carbon source. The oxidation rates of NH4+ and Norg were analysed separately for each inhibitor treatment with a 15N tracing model. In the absence of inhibitors, the rates of NH4+ oxidation and organic N oxidation were 0.0045 μmol N g?1 hour?1 and 0.0023 μmol N g?1 hour?1, respectively. Streptomycin had no effect on nitrification but cycloheximide inhibited the oxidation of NH4+ by 89% and the oxidation of organic N by more than 30%. The current study provides evidence to suggest that nitrification in grassland soil is carried out by fungi and that they can simultaneously oxidize NH4+ and organic N.  相似文献   

8.
A series of humic and fulvic acids isolated from different sources, size‐fractions separated from a humic acid, and three soils of different origin were subjected to CPMAS 13C‐NMR spectroscopy to obtain the distribution of their carbon contents. The relative areas of chemical shift regions in NMR spectra were used to apply a principal component analysis (PCA) to the three sets of samples. The multivariate analysis was successful in efficiently differentiating samples on the basis of the quality of their organic carbon content. The PC biplots based on two principal components distinguished objectively among samples as accurately as it was possible to do by subjective qualitative evaluation of the original spectra. In the case of the soils, a discriminant analysis (DA) was applied to build a classification model that allowed the validation of the three soils according to their origin. Percentage of validation in the classification model is expected to increase when a large number of NMR spectra are accumulated and/or the concentration of organic carbon in samples is enhanced. The multivariate analyses described are likely to become a useful tool to increase the importance of CPMAS 13C‐NMR spectra in the appraisal of natural organic matter variations in heterogeneous natural systems.  相似文献   

9.
A detailed discussion of the quantitative nature of 13C CPMAS NMR spectra as applied to solid samples, such as soil, is given. In particular, the influence of the cross-polarization (CP) time constant (TCH), the relaxation time constant of protons in the rotating frame (T1pH) and the contact time (tc) in the CPMAS experiment are considered. Three distinct quantitation regimes are numerically identified according to sample parameters tCH and T1PH > and the experimental choice of tc: (i) quantitation obtainable from a single CPMAS spectrum; (ii) quantitation obtainable from a series of CPMAS spectra; and (iii) quantitation not possible using CPMAS. Strategies for the measurement of sample parameters TCH and TipH are reviewed. When quantitation is not possible using CPMAS it is necessary to regress to the direct polarization (DP) of 13C nuclei. The sensitivity problems of DPMAS are discussed, as too are general factors that affect the quantitation of 13C data such as spinning sidebands. More specifically in relation to soil samples, the effects on quantitation arising from the presence of paramagnetics and the actual methods for the measurement of signal intensities are covered.  相似文献   

10.
Long‐term dynamics of amino acids (AAs), from a bare fallow soil experiment (established in 1928 at INRA‐Versailles, France), were examined in unamended control (Con) plots and plots treated with ammonium sulphate (Amsul), ammonium nitrate (Amnit), sodium nitrate (Nanit) or with animal manure (Man). Topsoil (0–25 cm) from 1929, 1963 and 1997 was analysed for C, N and 15N content and distribution of 18 amino acids recovered after acid hydrolysis with 6 m HCl. With time, soil N, C and AA content were reduced in Con, Amsul, Amnit and Nanit, but increased in Man. However, the absolute N loss was 3–11 times larger in Man than Nanit, Amsul, Amnit and Con, due to the much higher N annual inputs applied to Man. From 1929 to 1997 in Con, Amsul, Amnit and Nanit the whole soil and non‐hydrolysable‐N pool δ15N increased associated with the loss of N (indicative of Rayleigh 15N/14N fractionation). No δ15N change from 1929 to 1997 was found in the hydrolysable AA‐N (HAN) pool. Fertilizer N inputs aided stabilization of soil AA‐N, as AA half‐life in the mineral N fertilizer treatments increased from 34 years in 1963 to 50 years in 1997. The δ15N values of alanine and leucine reflected both source input and 15N/14N fractionation effects in soils. The δ15N increase of ornithine (～6‰) was similar to the whole soil. The δ15N change of phenylalanine in Con (decrease of 7‰) was related to its proportional loss since 1929, whereas for Amsul, Amnit, Nanit and Man it was associated with isotope effects caused by the fertilizer inputs. However, the soil δ15N value of most individual amino acids (IAAs) did not significantly change over nearly 70 years, even with mineral or organic N inputs. We conclude for these bare fallow systems that: (i) δ15N changes in the whole soil and non‐hydrolysable AA pool were solely driven by microbial processes and not by the nature of fertilizer inputs, and (ii) without plant inputs, the δ15N of the HAN pool and (most) IAAs may reflect the influence of plant–soil interactions from the previous (arable cropping) rather than present (fallow) land use on these soil δ15N values.  相似文献   

11.
31P‐NMR spectroscopy on bulk soils is a powerful tool for the identification of the different phosphorus forms in soils and for the evaluation of the dynamics of soil P. Up to now the majority of the papers dealt with liquid state 31P‐NMR spectroscopy on soluble soil organic substances. Only few papers were addressed to the study of the different phosphorus forms directly in bulk soils. In the present paper, some organic and inorganic phosphates of known structures, which are likely to be present in soil systems, were studied by direct polarization (DP) magic angle spinning (MAS) 31P‐NMR spectroscopy in order to understand the electronic factors responsible for chemical shifts of the phosphorus (P) nucleus and to serve as guidelines to assign P resonances in soil spectra. Number of hydrating water molecules, type of counter‐cation, degree of covalence, and spatial conformation of P in phosphate structures were found to affect signal positions in 31P‐NMR spectra. Both hydrating water and increase in degree of covalence of the X‐O‐P bonds (X=H, Na) enhanced the electronic density (ED) around P, thereby producing up‐field shifts in 31P‐NMR spectra. The exchange of the Na+ counter‐cation with NH4+ resulted in an increase of the cation potential (PC) that is a measure of the cation polarizing power, and induced a down‐field shift of P signals, due to a corresponding reduction in ED around the P nucleus. Both NMR down‐ and up‐field shifts were observed in organic phosphates, and were dependent on the spatial orientation of the phosphate groups that may have been fixed anisotropically in the solid state. Based on the factors that influence P chemical shifts for standard phosphates, attempts to assign 31P‐NMR signals in the spectra of five different unperturbed bulk soils were made.  相似文献   

12.
The dynamics of incorporation of fresh organic residues into the various fractions of soil organic matter have yet to be clarified in terms of chemical structures and mechanisms involved. We studied by 13C‐dilution analysis and CPMAS‐13C‐NMR spectroscopy the distribution of organic carbon from mixed or mulched maize residues into specific defined fractions such as carbohydrates and humic fractions isolated by selective extractants in a year‐long incubation of three European soils. The contents of carbohydrates in soil particle size fractions and relative δ13C values showed no retention of carbohydrates from maize but rather decomposition of those from native organic matter in the soil. By contrast, CPMAS‐13C‐NMR spectra of humic (HA) and fulvic acids (FA) extracted by alkaline solution generally indicated the transfer of maize C (mostly carbohydrates and peptides) into humic materials, whereas spectra of organic matter extracted with an acetone solution (HE) indicated solubilization of an aliphatic‐rich, hydrophobic fraction that seemed not to contain any C from maize. The abundance of 13C showed that all humic fractions behaved as a sink for C from maize residues but the FA fraction was related to the turnover of fresh organic matter more than the HA. Removal of hydrophobic components from incubated soils by acetone solution allowed a subsequent extraction of HA and, especially, FA still containing much C from maize. The combination of isotopic measurements and NMR spectra indicated that while hydrophilic compounds from maize were retained in HA and FA, hydrophobic components in the HE fraction had chemical features similar to those of humin. Our results show that the organic compounds released in soils by mineralization of fresh plant residues are stored mainly in the hydrophilic fraction of humic substances which are, in turn, stabilized against microbial degradation by the most hydrophobic humic matter. Our findings suggest that native soil humic substances contribute to the accumulation of new organic matter in soils.  相似文献   

13.
Soils from A horizons of Eutrochrepts under spruce forest (Sf), mixed deciduous forest (Df), permanent grassland (Gp), and arable rotation (Ar) were fractionated into clay- (<2 μm), silt-(2–20 μm) and sand- (20–2000 μm) sized separates. 13C NMR spectroscopy was used to compare SOM composition across size separates and between land-use regimes. CPMAS 13C NMR spectroscopy showed that the intensity of signals assigned to carbohydrates (representing most O-alkyl C) and lignin (phenolic and methoxyl C) declined with decreasing particle size. Concurrently, alkyl C and C-substitution of aromatic C increased in the order sand, silt, clay. The amount of alkyl C correlated well with microbial resynthesis of carbohydrates. Solution 13C NMR spectra suggested that humic acids (HA) extracted from the size separates were richer in carboxyl C and aromatic C than the bulk size separates. Also HA reflected increasing percentage of alkyl C with decreasing particle size. O-alkyl C were lower in silt HA than in clay HA whereas aromatic C tended to peak in silt HA. These results suggested that sand-sized separates were enriched in plant residues (primary resources) whereas clay-sized separates were dominated by products of microbial resynthesis (secondary resources). Silt was rich in selectively preserved and microbially transformed primary resources. 13C NMR spectroscopy showed only small differences in SOM composition between land-use regimes, except that silt and silt HA from Ar were richer in aromatic C than those from the other plots. But enrichment factors (E= content in fraction/content in whole soil) revealed differences in the distribution of C species across the size separates. Relatively high Earomatic (0.9) and Eo-alkyl (1.0) for sand from Gp indicated high amounts of plant residues, probably due to intense rhizodeposition and to occlusion of plant debris within aggregates. Low Earomatic (0.3) and Eo-alkyl (0.3) for sand from Ar suggested depletion of primary resources, which could be attributed to disintegration of soil aggregates upon cultivation. A pronounced enrichment of alkyl C in Ar clay-sized separates (Ealkyl= 3.1) suggested large amounts of microbial carbon. Microbial products attached to clay surfaces by a variety of physico-chemical bondings appeared more stable against mineralization induced by cultivation than plant residues sequestered in aggregates.  相似文献   

14.
Organic matter mineralization of forest litter is catalysed by the action of different extracellular enzymes produced by microorganisms. Coupling enzyme activities with data on the general macromolecular structure of organic matter, provided by cross‐polarization magic angle spinning 13C nuclear magnetic resonance (13C CPMAS NMR), allows researchers new insights into organic matter degradation processes. In this paper, the effect of the temperature of incubation on the degradation processes was evaluated in three distinct layers (OhLn, OhLv and OhLf) of an evergreen oak litter (Quercus ilex L.), located in the Mediterranean area of south‐eastern France. We studied degradation phenomena by a combination of 13C CPMAS NMR and microbiological analysis. In order to determine the microbial activity of litter layers, three enzyme activities (laccase, cellulase and butyrate esterase) were measured in a 6‐month mesocosm study. Results showed an increase in the alkyl C to O‐alkyl‐C ratio and an increase of the phenolic C and carboxyl C regions, indicating a preferential degradation of polysaccharides. The aromaticity also increased with litter depth and degradation, and humification processes were more elevated at 30°C. anova showed significant effects (P < 0.001) of increased temperature, depth and time of degradation on microbiological variables. Further information is needed about the variations in temperature and temperature‐litter response and soil functions to link fundamental understanding of carbon stabilization, climate change and global C cycling.  相似文献   

15.
The uptake of labelled and unlabelled N by wheat was measured in pot and field experiments with 15N-labelled fertilizer. Soils from two sites on the same series were used in the pot experiment; one had been bare-fallowed for 22 years and contained 1.6% organic C, the other had been under grass for many years and contained 3.8% organic C. Fertilizer N increased the uptake of unlabelled soil N in both soils, i.e. there was a positive ‘added nitrogen interaction’ (ANI). There was no ANI in the field experiment. A simulation model is used to show how positive ANIs can arise as a result of ‘pool substitution’—labelled inorganic fertilizer N standing proxy for unlabelled inorganic soil N that would otherwise have been immobilized. In the low-organic fallow soil, pool substitution accounted for the whole of the observed ANI and fertilizer N did not enhance either gross or net mineralization of soil N. Pool substitution also operated in the high organic grassland soil, but here net mineralization of soil N increased with increasing additions of fertilizer, giving rise to a ‘real’ ANI in addition to the larger ‘apparent’ ANI caused by pool substitution. This increase in net mineralization is probably caused by a decrease in immobilization of N as fertilizer N additions increase, not by an increase in gross mineralization of soil N. For pool substitution to operate, fertilizer N and soil inorganic N must occupy the same pool. This occurred in the pot experiment but not in the field experiment, where fertilizer and soil inorganic N remained separate and there was no ANI. When pool substitution occurs, fertilizer use efficiency is predictably lower as measured by the isotopic method than as measured by the conventional non-isotopic procedure.  相似文献   

16.
Pot experiments were carried out to examine the effects of slow-release fertilizer formulations on estimates of N2-fixation determined by the isotope dilution method. Soybeans were used as the N2-fixing plants, with non-nodulated soybeans and maize as the non-fixing controls. The 15N-fertilizer formulations used were (15NH4)SO4, K15NO3, gypsum-pelleted K15NO3, (15NH4)2SO4 + glucose, ground plant material enriched with 15N or 15N-oxamide. The estimate of the amount of N2 fixed by the nodulated soybean plants depended upon both the control plant and the fertilizer formulation used. Maize took up N later than non-nodulated soybean and estimates of soil N-pool (soil “A” value + fertilizer N added) calculated from the enrichment of this control were about twice as large as those calculated from the enrichment of non-nodulated soybean receiving the same fertilizer treatment. As a consequence, estimates of N2-fixation relative to this control were lower than those relative to non-nodulating soybean (mean 140 mg N per pot compared with 292 mg N per pot). With unstablilized 15N salts errors were sufficient to produce negative estimates of fixation relative to maize. Even with a “well-matched” control (non-nodulated soybean) estimates of fixation varied with fertilizer formulation.  相似文献   

17.
The decrease of NMR visibility of the C signal in soil samples due to the association between organic carbon (OC) and the topsoil mineral surface was investigated. CPMAS 13C‐NMR spectra were obtained for soil particle‐size fractions (< 2 μm, 2–20 μm, > 20 μm) and bulk soils from an agricultural topsoil (Chernozem) that had received three different amendments (no fertilization, mineral fertilization (NPK), mineral (NPK) and organic (cattle manure) fertilizations) at Bad Lauchstädt, Germany. The soil organic carbon content of the three soils depended on the degree of soil fertilization. There was no constant relationship between the total NMR signal intensity and the total amount of organic carbon (TOC) for all size fractions. Indeed, a key role played in the C signal intensity by the paramagnetic ferric ion from the clay content in soil fractions and bulk soils was confirmed. Thus, we describe the variations of C signal intensity by taking into account the distribution of clay‐associated OC and non‐associated OC pools. Depending on the amendment, the C signal visibility was weakened by a factor of 2–4 for the clay‐associated OC. This estimation was rendered possible by combining mineral specific surface area (SSA) measurements with the N2 gas adsorption method (BET method) and determination of TOC and iron concentrations. This approach contributes to the quantitative evaluation of the CPMAS 13C‐NMR detection.  相似文献   

18.
This study was conducted to investigate the influence of land-use systems (grassland and cropland) and of long-term no-till cropping systems [bare soil, oat/maize (O/M), pigeon pea+maize (P+M)] on the composition of organic N forms in a subtropical Acrisol. Soil samples collected from the 0- to 2.5-cm layer in the study area (Eldorado do Sul RS, Brazil) were submitted to acid hydrolysis and cross-polarization magic angle spinning (CPMAS) 15N and 13C nuclear magnetic resonance (NMR) spectroscopies. The legume-based cropping system P+M contained the highest contents of non-hydrolysable C and N, hydrolysable C and N, amino acid N and hydrolysed unknown N. The relative proportion of non-hydrolysable N was higher in bare soil (30.0%) and decreased incrementally in other treatments based on the total C and N contents. The amino acid N corresponded to an average of 37.2% of total N, and was not affected by land use and no-till cropping systems. The non-hydrolysable residue contained lower O-alkyl and higher aromatic C concentrations, as revealed by CPMAS 13C NMR spectroscopy, and higher C:N ratio than the bulk soil. No differences in the bulk soil organic matter composition could be detected among treatments, according to CPMAS 13C and 15N NMR spectra. In the non-hydrolysable fraction, grassland showed a lower concentration of aromatic and a higher concentration of alkyl C than other treatments. From CPMAS 15N NMR spectra, it could be concluded that amide N from peptide structures are the main organic N constituent. Amide structures are possibly protected through encapsulation into hydrophobic sites of organic matter and through organomineral interaction.  相似文献   

19.
Two soils differing in ammonium fixation capacity were incubated for 127 days with 15N-ammonium sulphate. In a gley soil with high NH+4-fixing capacity caused by smectites with a charge up to 0.8 per formula unit, the major part of the added ammonium was first fixed by minerals and then released slowly during incubation. The proportion of labelled N in the nitrate fraction increased during the first weeks and then decreased permanently. In contrast, in a histosol with low NH+4-fixing capacity, the exchangeable fraction contained most of the labelled NH+4, this being highly available to microorganisms and therefore subject to nitrification. About 50% of the added 15NH4 was lost from the histosol in 127 days, but only about 20 per cent was lost from the gley soil.  相似文献   

20.
The isotope dilution method for measuring gross rates of N mineralization, immobilization, and nitrification was applied to intact soil cores so that the effects of soil mixing were avoided. Soil cores were injected with solutions of either 15NH4+ or 15NO4?; gross mineralization rates were calculated from the decline in “N enrichment of the NH: pool during a 24-h incubation; gross nitrification rates were calculated from the decline in 15N enrichment of the NO?3 pool; gross rates of NH4+ and NO3? consumption were calculated from disappearance of the 15N label. The assumptions required for application of this method to intact cores are evaluated. Sensitivity analysis revealed that homogeneous mixing of added “N with ambient pools was not a necessary assumption but that bias in distribution of added label, coincident with a non-random distribution of microbial processes, would cause significant errors in rate estimates. Rate estimates were also sensitive to errors in initial 15N and 14N pool size estimates, In a silt loam soil from a grassland site, abiotic processes consumed over 30% of the added 15NH4+ within minutes of adding the label to sterilized soil. Extracting a subset of soil cores at the beginning of an incubation is recommended for obtaining initial pool size estimates. Gross immobilization is probably stimulated by addition of inorganic 15N substrate and, therefore, is overestimated by the isotope dilution method. As an alternative method, a non-linear equation is given for calculating the gross immobilization rate from the appearance of 15N in chloroform-labile microbial biomass; but incomplete extraction of biomass N may result in low estimates. Details of the isotope dilution methodology (injection rates, concentrations, experimental artefacts, etc.) are described and discussed. When care is taken to understand the underlying assumptions and sources of error, the isotope dilution method provides a powerful tool for measuring gross rates of microbial transformations of soil nitrogen in intact soil cores.  相似文献   

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