Fate of carbon and nitrogen in water-stable aggregates during decomposition of 13C15N-labelled wheat straw in situ

When incorporated in soil, plant residues and their decomposition products are in close contact with mineral particles with which they can be bound to form aggregates. We measured the incorporation of carbon (C) and nitrogen (N) derived from crop residues in water-stable aggregate fractions of a silty soil in a field experiment in Northern France using ¹³C¹⁵N-labelled wheat straw (Triticum aestivum L.). Soil samples were taken seven times for 18 months and separated into slaking-resistant aggregate size fractions which were analysed for total C and N contents, and ¹³C and ¹⁵N enrichments. During the early stages of decomposition (approximately 200 days), the enrichment of ¹³C increased rapidly in the macro aggregates (> 250 pm) but decreased thereafter. The macro aggregates represented only < 20% of the soil mass and at any one time, they accounted for <25% of the residual ¹³C in the soil. The proportion of ¹³C recovered in the <50-μm and 50–250-μm fractions increased during decomposition of the residues; at day 574, the 50–250-μm fraction accounted for close to 50% of the residual ¹³C. A greater proportion of ¹⁵N than ¹³C was recovered in the <50-μm fraction. The results indicate that during decomposition in soil, C and N from crop residues become rapidly associated with stable aggregates. In this silty soil the 50–250-μm stable aggregates appear to be involved in the storage and stabilization of C from residues.     

Transformation and binding of 13C and 14C-labelled atrazine in relation to straw decomposition in soil

As a source of organic matter, crop residues affect the behaviour of pesticides in agricultural soils. The fate of [U‐ring‐¹³C] and [U‐ring‐¹⁴C] atrazine (6‐chloro‐N‐ethyl‐N‐isopropyl‐1,3,5‐triazine‐2,4‐diamine) was investigated during laboratory incubation under controlled conditions in a loamy soil amended with wheat straw at two different states of decomposition: no preliminary decomposition or 6 months’ preliminary decomposition. After 3 months, non‐extractable, so‐called ‘bound’, ¹³C‐atrazine residues were recovered in three particle‐size fractions (> 200, 50–200 and < 50 μm), and investigated with solid‐state ¹³C‐NMR spectroscopy. Parallel incubations with [U‐ring‐¹⁴C] atrazine were carried out to quantify the bound residues as well as the extractable and mineralized fractions. The effect of straw residues on atrazine behaviour depended on whether they had been previously decomposed or not. When straw was decomposed for 6 months prior to incubation, atrazine mineralization was enhanced to 50% of the initial ¹⁴C in contrast to 15% of the initial ¹⁴C in soil alone and soil amended with fresh straw. In parallel, atrazine bound residues were formed in greater amount representing up to 20% of the initial ¹⁴C. CP/MAS ¹³C‐NMR on soil size fractions of soil–straw mixtures after incubation with ¹³C‐atrazine showed that bound residues contained mostly triazinic C, corresponding to atrazine or primary metabolites. Non‐humified organic materials recovered in size fractions > 200 and 50–200 μm contained significant amounts of bound residues, especially when straw was added to the soil. CP/MAS ¹³C‐NMR analysis of humic acids obtained from < 50‐μm fractions was difficult due to overlapping of the native carboxyl ¹³C signal with the ¹³C‐atrazine signal.     

Nitrogen in particle size fractions of soils incubated for five years with 15N-ammonium and 14C-hemicellulose

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.     

Nitrogen interactions and crop uptake from fresh and composted 15N-labelled poultry manure

¹⁵N-labelled poultry excrement was obtained by feeding chickens with ¹⁵N-labelled barley grain. The excrement produced was tested for uniformity of ¹⁵N-labelling; only small variations in the ¹⁵N content were found, indicating uniform labelling. The excrement was mixed with straw to produce manures which were used in a pot experiment measuring uptake of labelled and unlabelled N by ryegrass from the mixture in both a fresh form and after a period of composting. Interactions of N pools differed between the two materials. Addition of composted manure to soil caused a larger uptake of unlabelled N by ryegrass, whereas fresh manure caused a smaller plant uptake of unlabelled N. The proportion of plant N coming from labelled N from fresh manure was 25.7% and from composted manure 3.8%. However, the contributions of the two manures to plant uptake of total N were 15.5% and 13.8%, respectively. The fresh manure, being a mixture of excrement and straw, is considered as a two-component material, whereas composted manure is considered as a single component. It was concluded that the increase or decrease in the quantity of unlabelled, soil-derived N in plants after manure addition was related to the amount of energy available in the different manures.     

Following the decomposition of ryegrass labelled with 13C and 15N in soil by solid-state nuclear magnetic resonance spectroscopy

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.     

Immobilization and remineralization of N following addition of wheat straw into soil: determination of gross N transformation rates by N-ammonium isotope dilution technique

N dynamics in soil where wheat straw was incorporated were investigated by a soil incubation experiment using ¹⁵N-labelled nitrate or ¹⁵N-labelled wheat straw. The incubated soils were sampled after 7, 28, 54 days from the incorporation of wheat straw, respectively, and gross rates of N transformations including N remineralization and temporal changes in the amount of microbial biomass were determined.Following the addition of wheat straw into soils, rapid decrease of nitrate content in soil and increase of microbial biomass C and N occurred within the first week from onset of the experiment. Both the gross rates of mineralization and immobilization determined by ¹⁵N-ammonium isotope dilution technique were remarkably enhanced by the addition of wheat straw, and gradually decreased with time. Remineralization rate of N derived from ¹⁵N-labelled nitrate, and mineralization rate of N derived from ¹⁵N-labelled wheat straw was estimated by ¹⁵N isotope dilution technique using non-labelled ammonium. Remineralization rates of N derived from ¹⁵N-labelled nitrate were calculated to be 0.71 mg N kg⁻¹ d⁻¹ after 7 days, 0.55 mg N kg⁻¹ d⁻¹ after 28 days, and 0.29 mg N kg⁻¹ d⁻¹ after 54 days.Nearly 10% of the ¹⁵N-labelled N originally contained in the wheat straw was held in the microbial biomass irrespective of the sampling time. The amount of inorganic N in soil which was derived from ¹⁵N-labelled wheat straw ranged between 1.93 and 2.37 mg N kg⁻¹.Rates of N transformations in soil with ¹⁵N-labelled wheat straw were obtained by assuming that the k value was equal to the ¹⁵N abundance of biomass N, and the obtained values were considered to be valid.     

Distribution of 14C between particle size fractions and carbohydrates separated from a peat incubated with 14C-glycine

Samples of fresh Sphagnum peat from a raised bog were amended with ¹⁴C-labelled glycine. The distribution of ¹⁴C between particle size fractions obtained by wet sieving (sieve sizes 1, 0.5, 0.25, 0.15 and 0.05mm) was determined immediately on control (unincubated) samples and after 1, 6 and 12 months incubation at 10°C. The recovery of glycine in solution was almost 100%. During the incubation with ¹⁴C-glycine, ¹⁴CO₂ was released within the first 20 weeks, equivalent to 51.5% of the added ¹⁴C, but thereafter very little ¹⁴CO₂ was evolved. After 26 weeks a substantial amount of ¹⁴C was distributed amongst all the fractions, but the greatest incorporation (4.47%) occurred in the finest fraction (0.005–0.05 mm). Labelling of the other particle size fractions was <2.3% of added ¹⁴C. Carbohydrate accounted for 23% of ¹⁴C in the finest fraction and the sugars, rhamnose, arabinose, xylose, mannose, galactose and glucose all became labelled. Rhamnose showed the greatest, and arabinose, galactose and xylose the least, increase in specific activity; glucose and mannose had intermediate values. It was concluded that the finest fraction in peat contains a significant proportion of the microbially-synthesized material.     

Interaction of 15N-labelled ammonium nitrate,urea and ammonium sulphate with soil N during growth of wheat (Triticum aestivum L.) under field conditions

The effects of ¹⁵N-labelled ammonium nitrate, urea and ammonium sulphate on yield and uptake of labelled and unlabelled N by wheat (Triticum aestivum L. cv. Mexi-Pak-65) were studied in a field experiment. The dry matter and N yields were significantly increased with fertilizer N application compared to those from unfertilized soil. The wheat crop used 64.0–74.8%, 61.5–64.7% and 61.7–63.4% of the N from ammonium nitrate, urea and ammonium sulphate, respectively. The fertilizer N uptake showed that ammonium nitrate was a more available source of N for wheat than urea and ammonium sulphate. The effective use of fertilizer N (ratio of fertilizer N in grain to fertilizer N in whole plant) was statistically similar for the three N fertilizers. The application of fertilizer N increased the uptake of unlabelled soil N by wheat, a result attributed to a positive added N interaction, which varied with the method of application of fertilizer N. Ammonium nitrate, urea and ammonium sulphate gave 59.3%, 42.8% and 26.3% more added N interaction, respectively, when applied by the broadcast/worked-in method than with band placement. A highly significant correlation between soil N and grain yield, dry matter and added N interaction showed that soil N was more important than fertilizer N in wheat production. A values were not significantly correlated with added N interaction (r=0.719). The observed added N interaction may have been the result of pool substitution, whereby added labelled fertilizer N stood proxy for unlabelled soil N.     

Use of NMR spectroscopy to study transformations of nitrogenous substances during incubation of peat

Abstract. Samples of peat were incubated with ¹⁵N-labelled ammonium sulphate, urea, wheat straw and glycine and divided into six size fractions of solid components and a water-soluble fraction. The fractions were analysed by NMR spectroscopy to study the formation of humic substances and rind how fertilizer nitrogen is immobilized in peaty soils. After six months' incubation about half of the ammonium sulphate nitrogen was still present as ammonium in the soluble fraction, the urea had been entirely metabolized to ammonium and various organic compounds, about half the straw had been decomposed to ammonium and amino acid or peptide materials, and most of the glycine had been transformed to ammonium, amide and aliphatic amine.     

Incorporation studies of NH+4 during incubation of organic residues by l5N-CPMAS-NMR-spectroscopy

This study focuses on the processes occurring during incorporation of inorganic nitrogen into humic substances. Therefore rye grass, wheat straw, beech saw dust, sulphonated lignin and organosolve lignin were incubated together with highly ¹⁵N-enriched ammonium sulphate in the laboratory for 600 days. Samples from the incubates were periodically analysed for weight loss, and carbon and nitrogen contents. The samples were also analysed by solid-state ¹³C- and ¹⁵N-CPMAS-NMR-spectroscopy to follow the turnover of the materials during incubation. Most of the detectable N-signals was assigned to amide - peptide structures. The remaining intensities could be ascribed to free and alkylated amino groups, and those on the low field side of the broad amide-peptide signal to indole, pyrrole and nucleotide derivatives. Abiotic reactions of ammonia with suitable precursors and the formation of pyridine, pyrazine or phenyloxazone derivatives were not observed. Signals from ammonia and nitrate occurred only at the end of the incubation.     

Leaching and plant offtake of N in field pea/cereal cropping sequences with incorporation of 15N-labelled pea harvest residues

Abstract. Field peas (Pisum sativum L.) were grown in sequence with winter wheat (Triticum aestivum L.) or spring barley (Hordeum vulgare L.) in large outdoor lysimeters. The pea crop was harvested either in a green immature state or at physiological maturity and residues returned to the lysimeters after pea harvest. After harvest of the pea crop in 1993, pea crop residues (pods and straw) were replaced with corresponding amounts of ¹⁵N‐labelled pea residues grown in an adjacent field plot. Reference lysimeters grew sequences of cereals (spring barley/spring barley and spring barley/winter wheat) with the straw removed. Leaching and crop offtake of ¹⁵N and total N were measured for the following two years. These treatments were tested on two soils: a coarse sand and a sandy loam. Nitrate concentrations were greatest in percolate from lysimeters with immature peas. Peas harvested at maturity also raised the nitrate concentrations above those recorded for continuous cereal growing. The cumulative nitrate loss was 9–12 g NO₃‐N m^–2 after immature peas and 5–7 g NO₃‐N m^–2 after mature peas. Autumn sown winter wheat did not significantly reduce leaching losses after field peas compared with spring sown barley. ¹⁵N derived from above‐ground pea residues accounted for 18–25% of the total nitrate leaching losses after immature peas and 12–17% after mature peas. When compared with leaching losses from the cereals, the extra leaching loss of N from roots and rhizodeposits of mature peas were estimated to be similar to losses of ¹⁵N from the above‐ground pea residues. Only winter wheat yield on the coarse sand was increased by a previous crop of peas compared to wheat following barley. Differences between barley grown after peas and after barley were not statistically significant. ¹⁵N lost by leaching in the first winter after incorporation accounted for 11–19% of ¹⁵N applied in immature pea residues and 10–15% of ¹⁵N in mature residues. Another 2–5% were lost in the second winter. The ¹⁵N recovery in the two crops succeeding the peas was 3–6% in the first crop and 1–3% in the second crop. The winter wheat did not significantly improve the utilization of ¹⁵N from the pea residues compared with spring barley.     

Improvement of 13C and 15N CPMAS NMR spectra of bulk soils, particle size fractions and organic material by treatment with 10% hydrofluoric acid

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.     

Short-term kinetics of residual wheat straw C and N under field conditions: characterization by 13C15N tracing and soil particle size fractionation

Summary A clear understanding of the short-term decomposition and fate of crop residues is necessary to predict the availability of mineral N in soil. The fate of ¹³ C¹⁵N-labelled wheat straw in a silty soil (Typic Hapludalf) was studied using particle size fractionation and in situ incubation in which the equivalent of 8 t dry matter per ha of straw was incorporated into the soil over 574 days. Soil samples were separated into five particle-size fractions by wet sieving after disruption of aggregates. The weight, C and N contents, and ¹³C and ¹⁵N atom excess of each fraction were determined. Straw-derived C disappeared rapidly from the > 2000-μm fraction with an estimated half-life of 53 'normalized' days (equivalent of 10°C and −0−01 MPA water potential). Straw-derived C appeared to be only temporarily stored in the intermediate fractions (1000–2000 and 200–1000 pm). The maximum net ¹³C accumulation in the 50–200-μm fraction was 4·4% of added ¹³C. Straw-derived C accumulated most rapidly and preferentially in the 50-μm fraction, which stabilized after 265 days and accounted for 70% of the residual ¹³C on day 574. Although there was more residual ¹⁵N than ¹³C, the distributions and kinetics of the two isotopes in the fractions were similar.     

TRANSFORMATION OF 15N-LABELLED AMMONIUM IN TWO SOILS DIFFERING IN NH+4-FIXING CAPACITY

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.     

13C and 15N natural abundances of urban soils and herbaceous vegetation in Karlsruhe, Germany

We undertook what we believe to be a unique survey of the natural abundances of ¹³C and ¹⁵N in urban soils and plants in Karlsruhe (Germany), a European city of average size. We found broad patterns of these abundances in both soils and plants, which reflected geology and land use. In contrast with studies on smaller areas (showing the direct effect of human activities), our study first determined the extent to which the abundances correlated with land use or underlying geology and then assessed how we could further test such relationships. The spatial pattern of δ¹³C in surface soil correlated with that of the underlying parent material; construction activities superimposed a secondary signal. Maize cultivation was a source of less negative soil δ¹³C, whereas the C₃ vegetation is a source of more negative soil δ¹³C. There was a footprint of less negative plant δ¹³C in the industrial and port areas; plant δ¹³C downwind of the city was less negative than upwind, which might relate to atmospheric pollution from the port area or to differences in soil properties. There was no significant effect of wind direction or geology on soil or plant δ¹⁵N, which was correlated mainly with land use. The largest soil δ¹⁵N was under agriculture and the smallest under woodland. The abundance of ¹⁵N in inner-urban soil and plants was intermediate between those of agriculture and forests. This study represents a major advance in the use of stable isotope geochemistry in understanding urban environments.     

Amino acid 15N in long-term bare fallow soils: influence of annual N fertilizer and manure applications

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.     

Immobilization of 15N in forest litter studied by 15N CPMAS NMR spectroscopy

Solutions labelled with ¹⁵N were applied as (¹⁵NH₄)₂SO₄ or K¹⁵NO₃ to isolated microplots in the floor of mountain beech forest (Nothofagus solandri var. cliffortioides) and incubated for 135 days under field conditions of moisture and temperature. Solid state ¹⁵N CPMAS NMR spectra of the forest litter layer showed that more than 80% of the total signal intensity was attributable to the secondary amide-peptide peak. The degree of ¹⁵N enrichment or form of N did not alter the relative intensity of signals attributable to ¹⁵N in peptides, nucleic acids and aliphatic amine groups (amino sugars and free NH₂ on amino acids). Combinations of ¹³C and ¹⁵N-NMR spectra, edited by a process that exploited differences in proton spin properties between distinct categories of organic matter, indicated incorporation of ¹⁵N in humified organic matter rather than partly degraded plant material. This application demonstrated that solid state ¹⁵N CPMAS NMR has potential for use in studies of N immobilization under field conditions and with materials containing little N and small ¹⁵N enrichment.     

Decomposition of 15N-labelled catch-crop residues in soil: evaluation of N mineralization and plant-N uptake potentials under controlled conditions

The decomposition of ¹⁵N-labelled catch-crop materials (rape, radish and rye), obtained from field experiments, was studied in a chalky Champagne soil during a 60-week incubation at 28°C. Mineralized N was assumed to come from either labile or recalcitrant fractions of plant residues. The labile fraction represented about one-third of the catch-crop N; its mineralization rate constant varied from 0.06 to 0.12 d^?1. The decomposition rate of the recalcitrant N fraction ranged from 0.03 × 10^?2 to 0.06 × 10^?2 d^?1. Catch-crop species and rate of incorporation had no effect on N residue mineralized at the end of incubation. The decomposition of labelled rye was monitored in the same soil during a 5-month pot experiment to determine the N availability to an Italian ryegrass crop and the effect of plants on the decomposition processes. The ¹⁵N-rye decomposed rapidly both in the presence or absence of Italian ryegrass, but the amounts of N mineralized were influenced by the presence of living roots: 42% of the ¹⁵N in labelled rye was present as inorganic N in the pots without plants after 5 months, compared with only 32% in the ryegrass crop. Comparison of microbial-biomass dynamics in both treatments suggested that there had been preferential utilization by soil micro-organisms of materials released from the living roots than the labelled plant residues.     

Untersuchungen zur gezielten 15N-Substitution und -Akkumulation in der organischen Substanz ausgewählter Dauerversuchsböden

Investigation of specific ¹⁵N-substitution and accumulation in organic matter of soil from continuous fertilizer experiments Ray grass was grown in pots with upper layer substrates of longterm fertilizer experiments and fertilized with ¹⁵N labelled ammonium sulphate for three years. The ¹⁵N-labelled harvested mass was returned into the soil at the end of each year. Using the ¹⁵N tracer technique the accumulation of N in humic and nitrogen fractions was studied. After the first year, all fractions contained ¹⁵N. In sandy soil especially easily soluble compounds were formed and accumulated with ¹⁵N. On the contrary in loamy-soils more resistant fractions marked with the isotop were increased.     

Near infrared reflectance spectroscopy for determination of organic matter fractions including microbial biomass in coniferous forest soils

The objective of this work was to investigate the usefulness of near infrared reflectance spectroscopy (NIRS) in determining some C and N fractions of soils: labile compounds, microbial biomass, compounds derived from added ¹³C- and ¹⁵N-labelled straw. Soil samples were obtained from a previous experiment where soils were labelled by addition of ¹³C- and ¹⁵N-labelled wheat straw and incubated in coniferous forests in northern Sweden (64-60°N) and south France (43°N). The incubation lasted three years with 7-9 samplings at regular time steps and four replicates at each sampling (204 samples). Samples were scanned using a near infrared reflectance spectrophotometer (NIRSystem 6500). Calibrations were obtained by using a modified partial least squares regression technique with reference data on total C and N, ¹³C, ¹⁵N, control extract-C, -N, -¹³C and -¹⁵N, fumigated extract-C, -N, -¹³C and -¹⁵N, biomass-C, -N, -¹³C and -¹⁵N contents. Mathematical treatments of the absorbance data were first or second derivative with a gap from 4 to 10 nm. The standard error of calibration (SEC)-to-standard deviation of the reference measurements ratio was ≤0.2 for 10 models, namely total C and N, ¹³C, ¹⁵N, control extract-C, fumigated extract-C and -N, biomass-C and -N and biomass-¹⁵N models and therefore considered as very good. With an R²=0.955, the fumigated extract-¹⁵N model is also good. The standard error of performance calculated on the independent set of data and SEC were within 20% of each other for all the best equations except for the biomass-¹⁵N model. The ability of NIRS to detect ¹³C and ¹⁵N in total C and N and in the extracts is noteworthy, not because of its predictive function that is not really of interest in this case, but because it indicates that the spectra kept the signature of the properties of the organic matter derived from the straw even after two- or three-year decomposition. The incorporation of the ¹³C in the biomass was less well predicted than that of the ¹⁵N. This could indicate that the biomass derived from the straw was characterised by a particular protein or amino acid composition compared to the total biomass that includes a large proportion of dormant micro-organisms. The predictive ability of NIRS for microbial biomass-C and -N is particularly interesting because the conventional analyses are time consuming. In addition, NIRS allows detecting analytical errors.