Use of mid‐infrared spectroscopy in the diffuse‐reflectance mode for the prediction of the composition of organic matter in soil and litter

Mid‐infrared spectroscopy (MIRS) is assumed to be superior to near‐infrared spectroscopy (NIRS) for the prediction of soil constituents, but its usefulness is still not sufficiently explored. The objective of this study was to evaluate the ability of MIRS to predict the chemical and biological properties of organic matter in soils and litter. Reflectance spectra of the mid‐infrared region including part of the near‐infrared region (7000–400 cm^–1) were recorded for 56 soil and litter samples from agricultural and forest sites. Spectra were used to predict general and biological characteristics of the samples as well as the C composition which was measured by ¹³C CPMAS‐NMR spectroscopy. A partial least‐square method and cross‐validation were used to develop equations for the different constituents over selected spectra ranges after several mathematical treatments of the spectra. Mid‐infrared spectroscopy predicted well the C : N ratio: the modeling efficiency EF was 0.95, the regression coefficient (a) of a linear regression (measured against predicted values) was 1.0, and the correlation coefficient (r) was 0.98. Satisfactorily (EF ≥ 0.70, 0.8 ≤ a ≤ 1.2, r ≥ 0.80) assessed were the contents of C, N, and lignin, the production of dissolved organic carbon, and the contents of carbonyl C, aromatic C, O‐alkyl C, and alkyl C. However, the N mineralization rate, the microbial biomass and the alkyl–to–aromatic C ratio were predicted less satisfactorily (EF < 0.70). Limiting the sample set to mineral soils did generally not result in improved predictions. The good and satisfactory predictions reported above indicate a marked usefulness of MIRS in the assessment of chemical characteristics of soils and litter, but the accuracies of the MIRS predictions in the diffuse‐reflectance mode were generally not superior to those of NIRS.     

Use of near‐ and mid‐infrared spectroscopy to distinguish carbon and nitrogen originating from char and forest‐floor material in soils

The presence of relatively inert organic materials such as char has to be considered in calibrations of soil C models or when calculating C‐turnover times in soils. Rapid and cheap spectroscopic techniques such as near‐infrared (NIRS) or mid‐infrared spectroscopy (MIRS) may be useful for the determination of the contents of char‐derived C in soils. To test the suitability of both spectroscopic techniques for this purpose, artificial mixtures of C‐free soil, char (lignite, anthracite, charcoal, or a mixture of the three coals) and forest‐floor Oa material were produced. The total C content of these mixtures (432 samples) ranged from 0.5% to 6% with a proportion of char‐derived C amounting to 0%, 20%, 40%, 50%, 60%, or 80%. All samples were scanned in the visible and near‐IR region (400–2500 nm). Cross‐validation equations for total C and N, C and N derived from char (C_char, N_char) and Oa material were developed using the whole spectrum (first and second derivative) and a modified partial least‐square regression method. Thirty‐six samples were additionally scanned in the middle‐IR and parts of the near‐IR region (7000–400 cm^–1 which is 1430–25,000 nm) in the diffuse‐reflectance mode. All properties investigated were successfully predicted by NIRS as reflected by RSC values (ratio of standard deviation of the laboratory results to standard error of cross‐validation) > 4.3 and modeling efficiencies (EF) ≥ 0.98. Near‐infrared spectroscopy was also able to differentiate between the different coals. This was probably due to structural differences as suggested by wavelength assignment. Mid‐IR spectroscopy in the diffuse‐reflectance mode was also capable to successfully predict the parameters investigated. The EF values were > 0.9 for all constituents. Our results indicated that both spectroscopic techniques applied, NIRS and MIRS, are able to predict C and N derived from different sources in soil, if closed populations are considered.     

Near‐infrared spectroscopy can predict the composition of organic matter in soil and litter

The usefulness and limitations of near‐infrared reflectance spectroscopy (NIRS) for the assessment of several soil characteristics are still not sufficiently explored. The objective of this study was to evaluate the ability of visible and near‐infrared reflectance (VIS‐NIR) spectroscopy to predict the composition of organic matter in soils and litter. Reflectance spectra of the VIS‐NIR region (400–2500 nm) were recorded for 56 soil and litter samples from agricultural and forest sites. Spectra were used to predict general and biological characteristics of the samples as well as the C composition which was measured by ¹³C‐CPMAS‐NMR spectroscopy. A modified partial least‐square method and cross‐validation were used to develop equations for the different constituents over the whole spectrum (1st to 3rd derivation). Near‐infrared spectroscopy predicted well the C : N ratios, the percentages of O‐alkyl C and alkyl C, the ratio of alkyl C to O‐alkyl C, and the sum of phenolic oxidation products: the ratios of standard deviation of the laboratory results to standard error of cross‐validation (RSC) were greater than 2, the regression coefficients (a) of a linear regression (measured against predicted values) ranged from 0.9 to 1.1, and the correlation coefficients (r) were greater than 0.9. Satisfactorily (0.8 ≤ a ≤ 1.2, r ≥ 0.8, and 1.4 ≤ RSC ≤ 2.0) assessed were the contents of C, N, and production of DOC, the percentages of carbonyl C and aromatic C and the ratio of alkyl C to aromatic C. However, the N‐mineralization rate and the microbial biomass were predicted unsatisfactorily (RSC < 1.4). The good and satisfactory predictions reported above indicate a marked usefulness of NIRS in the assessment of biological and chemical characteristics of soils and litter.     

Thermal oxidation does not fractionate soil organic carbon with differing biological stabilities

Thermal analysis techniques have been used to differentiate soil organic carbon (SOC) pools with differing thermal stability. A correlation between thermal and biological stability has been indicated in some studies, while others reported inconsistent relationships. Despite these controversial findings and no standardized method, several recently published studies used thermal analysis techniques to determine the biological stability and quality of SOC in mineral soils. This study examined whether thermal oxidation at temperature levels between 200°C and 400°C, combined with evolving gas analysis and isotope ratio mass spectrometry, is capable of identifying SOC pools with differing biological stability in mineral soils. Soil samples from three sites being under Miscanthus (C₄‐plant) cultivation for more than 17 years following former agricultural cropland (only C₃‐plant) cultivation were used. Due to natural shifts in ¹³C content, young and labile Miscanthus‐derived SOC could be distinguished from stable and old C₃‐plant‐derived SOC. The proportion of Miscanthus‐derived SOC increased significantly with increasing temperatures up to 350°C in bulk soil samples, indicating increasing oxidation of labile and young SOC with increasing temperatures. Use of density fractions to validate the thermally oxidized SOC from bulk soil samples revealed that the thermal oxidation patterns did not reflect the biological stability of SOC. The suggested biologically labile particulate organic carbon (light fraction from density fractionation) was clearly enriched in Miscanthus‐derived young SOC. The thermal oxidation patterns, however, revealed preferential oxidation of these biologically labile fractions not at low temperatures, but rather at higher temperatures. The reverse was found for the biologically stable mineral‐associated density fraction (heavy fraction). Based on different soil types, it was concluded that the thermal stability of SOC between 200°C and 400°C is not a suitable indicator of the biological stability of SOC and, thus, thermal oxidation is not capable of fractionating SOC pools with differing biological stability.     

Authentication of Rice Using Near‐Infrared Reflectance Spectroscopy

The authentication of rice (Korean domestic rice vs. foreign rice) has been attempted using near‐infrared spectroscopy (NIRS). Two sample sets (n₁ = 280 and n₂ = 200) were used to obtain calibration equations and the spectral regions used for this study were 500–600 nm, 700–900nm, and 980–2,498 nm. Modified partial least square (MPLS) regression was used to develop the prediction model. The standard error of cross validation (SECV) and the r² were 0.165 and 0.91 respectively for 1st calibration set and 0.165 and 0.93 for 2nd calibration set respectively. The results of the independent validation (n₃ = 80) showed that all of 80 samples were identified correctly. Even though authentication of rice was performed successfully using NIRS, the calibration statistics in this study showed that further effort is needed for implementation of NIRS for authentication of rice for industry purposes.     

Soil carbon pools and fluxes after land conversion in a semiarid shrub-steppe ecosystem

Worldwide soil carbon (C) losses associated with agricultural expansion and intensification have contributed significantly to increased atmospheric CO₂. Soil disturbances resulting from land use changes were shown to modify the turnover of C and the formation of soil organic matter. A native semiarid shrub-steppe ecosystem recently converted into an irrigated agricultural development in the Columbia Basin of Washington State was evaluated for several abiotic indicators that might signal changes in an ecosystem during the initial stages of conversion and disturbance. Soil samples were collected in March of 2003 and 2004 from nine sites that included native shrub-steppe and agricultural fields converted in 2001 and 2002. Disturbance from conversion to irrigated crop production influenced total organic C and nitrogen (N) storage, C and N mineralization, and C turnover. Cultivated fields had greater concentrations of total organic C and N and higher cumulative C and N mineralization than native sites after 3 years of cultivation. Soil organic C was divided into three pools: an active pool (C _a) consisting of labile C (simple sugars, organic acids, the microbial biomass, and metabolic compounds of incorporated plant residues) with a mean residence time of days, an intermediate or slow pool (C _s) consisting of structural plant residues and physically stabilized C, and a resistant fraction (C _r) consisting of lignin and chemically stabilized C. Extended laboratory incubations of soil with measurements of CO₂ were used to differentiate the size and turnover of the C _a and C _s functional C pools. The active pools were determined to be 4.5 and 6.5% and slow pools averaged 44 and 47% of the total C in native and cultivated fields, respectively. Cultivation, crop residue incorporation, and dairy manure compost amendments contributed to the increase in total soil C.     

Can Near or Mid‐Infrared Diffuse Reflectance Spectroscopy Be Used to Determine Soil Carbon Pools?

Abstract

The objective of this study was to compare mid‐infrared (MIR) an near‐infrared (NIR) spectroscopy (MIRS and NIRS, respectively) not only to measure soil carbon content, but also to measure key soil organic C (SOC) fractions and the δ¹³C in a highly diverse set of soils while also assessing the feasibility of establishing regional diffuse reflectance calibrations for these fractions. Two hundred and thirty‐seven soil samples were collected from 14 sites in 10 western states (CO, IA, MN, MO, MT, ND, NE, NM, OK, TX). Two subsets of these were examined for a variety of C measures by conventional assays and NIRS and MIRS. Biomass C and N, soil inorganic C (SIC), SOC, total C, identifiable plant material (IPM) (20× magnifying glass), the ratio of SOC to the silt+clay content, and total N were available for 185 samples. Mineral‐associated C fraction, δ¹³C of the mineral associated C, δ¹³C of SOC, percentage C in the mineral‐associated C fraction, particulate organic matter, and percentage C in the particulate organic matter were available for 114 samples. NIR spectra (64 co‐added scans) from 400 to 2498 nm (10‐nm resolution with data collected every 2 nm) were obtained using a rotating sample cup and an NIRSystems model 6500 scanning monochromator. MIR diffuse reflectance spectra from 4000 to 400 cm^?1 (2500 to 25,000 nm) were obtained on non‐KBr diluted samples using a custom‐made sample transport and a Digilab FTS‐60 Fourier transform spectrometer (4‐cm^?1 resolution with 64 co‐added scans). Partial least squares regression was used with a one‐out cross validation to develop calibrations for the various analytes using NIR and MIR spectra. Results demonstrated that accurate calibrations for a wide variety of soil C measures, including measures of δ¹³C, are feasible using MIR spectra. Similar efforts using NIR spectra indicated that although NIR spectrometers may be capable of scanning larger amounts of samples, the results are generally not as good as achieved using MIR spectra.     

Analysis of dry matter and protein contents in fresh yam bean tubers by near‐infrared reflectance spectroscopy

Abstract

Fast screening methods are needed for plant breeding. The objective of this research was to evaluate the potential of near‐infrared reflectance spectroscopy (NIRS) for the simultaneous analysis of dry matter and protein contents in intact discs of fresh yam bean (Pachyrhizus spp.) tubers. Discs from 210 tubers were extracted with a punch few hours after harvesting and scanned by NIRS using a specially designed adapter. External validation revealed a close relationship between NIRS and reference methods for dry matter content (r²=0.94; standard error of performance, SEP=1.2%) and protein content (r²=0.87; SEP=1.94%). The calibration for protein content was compared with another one developed using dried‐ground tuber samples (r²=0.97; SEP=0.97%). These results suggested that NIRS can be used to determine dry matter and protein contents in fresh tuber samples of yam beans with acceptable accuracy. Further research will have to determine if additional traits can be incorporated into this scheme.     

Soil‐carbon turnover under different crop management: Evaluation of RothC‐model predictions under Pannonian climate conditions

Despite the importance of soil organic matter (SOM), very few long‐term data concerning soil organic‐C dynamics are available for calibrating and evaluating C models. The long‐term ¹⁴C‐turnover field experiment, established in 1967 in Fuchsenbigl, Lower Austria, offers the unique opportunity to follow the fate of labeled C under different crop‐management systems (bare fallow, spring wheat, crop rotation) over a period of more than 35 y. Compared with the crop‐rotation and spring‐wheat treatments, the decline of total organic C was largest in the bare‐fallow treatments, because no significant C input has occurred since 1967. Nonetheless, the decline was not as fast as predicted with the original RothC‐26.3‐model decomposition rate constants. In this work, we therefore calibrated the Roth‐C‐26.3 model for the Pannonian climatic region based on the field‐experiment results. The main adjustment was in the decomposition rate constant for the humified soil C pool (HUM), which was set to 0.009 instead of 0.02 y^–1 as determined in the original Rothamsted field trial. This resulted in a higher HUM pool in the calibrated model because of a longer turnover period (111 vs. 50 y). The modeled output based on the calibrated model fitted better to measured values than output obtained with the original Roth‐C‐26.3‐model parameters. Additionally, the original decomposition rate constant for resistant plant material (RPM) was changed from 0.3 to 0.6 y^–1 to describe the decomposition of ¹⁴C‐labeled straw more accurately. Application of the calibrated model (modified HUM decomposition rate) to simulate removal of crop residues showed that this can entail a long‐term decline of SOM. However, these impacts are strongly dependent on the crop types and on environmental conditions at a given location.     

Use of near infrared spectroscopy to determine biological and chemical characteristics of organic layers under spruce and beech stands

The chemical composition of organic layers of forest soils shows a high spatial variability and fast methods may be required for its study at a landscape level. The objective was to assess the applicability of near infrared spectroscopy (NIRS) to measure several chemical and biological properties of organic layers in spruce, beech, and mixed spruce‐beech stands. Spectra in the VIS‐NIR region (400—2500 nm) were recorded for 406 samples representing Oi, Oe, and Oa layers of forest soils from Solling (Germany), 195 of them were used for calibration and 211 for validation. The calibration equations for each constituent were developed using the whole spectrum (0^th to 3^rd derivative). Humus samples were analyzed for contents of C and N and contents of P, S, Na, K, Ca, Mg, Mn, Fe, and Al after pressure digestion in HNO₃. Additionally, basal respiration and microbial C (C_mic) were measured. NIRS predicted well the contents of C, N, P, S, Ca, Na, K, Fe, and Al and C/N and C/P ratios: the regression coefficients (a) of a linear regression (measured against predicted values) ranged from 0.9 to 1.1, and the correlation coefficients (r) were greater or equal 0.9. C_mic (a = 0.87, r = 0.83) was predicted satisfactorily, whereas the prediction of the basal respiration (a = 0.74, r = 0.87) was less satisfactory. Due to liming of some of the plots NIRS failed to predict contents of Mg (a = 1.27, r = 0.68). For all chemical and biological characteristics the best prediction performances were achieved using the whole sample population. Splitting the samples into smaller groups according to a dominant tree species or an organic layer did not improve the predictions.<?show $6#>     

Turnover and availability of soil organic carbon under different Mediterranean land‐uses as estimated by 13C natural abundance

Soil organic matter (SOM) is an important factor in ecosystem stability and productivity. This is especially the case for Mediterranean soils suffering from the impact of human degradation as well as harsh climatic conditions. We used the carbon (C) exchange resulting from C₃‐C₄ and C₄‐C₃ vegetation change under field conditions combined with incubations under controlled conditions to evaluate the turnover and availability of soil organic C under different land‐uses. The 40‐year succession of Hyparrenia hirta L. (C₄ photosynthesis) after more than 85 years of olive tree (Olea europaea L.; C₃ photosynthesis) growth led to the exchange of 54% of soil organic C from C₃ to C₄ forms. In contrast, 21 years of vine (Vitis vinifera L.) growing after H. hirta decreased the organic C content to 57%. Considering this exchange and decrease as well as the periods after the land‐use changes, we calculated the mean residence time (MRT) of soil C of different ages. The MRT of C under grassland dominated by H. hirta was about 19 years, but was 180 years under the vineyard. The rates of C accumulation under the H. hirta grassland were about 0.36 Mg C ha^?1 year^?1. In contrast, the rates of C losses after conversion from natural grassland to a vineyard were 1.8 times greater and amounted to 0.65 Mg C ha^?1 year^?1. We conclude that changes of land use from natural Mediterranean grassland to a vineyard lead to very large C losses that cannot be compensated for over the same periods.     

The use of visible and near‐infrared spectroscopy for the analysis of soil water repellency

This study investigated the potential of visible/near‐infrared reflectance spectroscopy (Vis‐NIRS) to predict soil water repellency (SWR). The top 40 mm of soils (n = 288) across 48 sites under pastoral land‐use in the North Island of New Zealand, which represented 10 soil orders and covered five classes of drought proneness, were analysed by standard laboratory methods and Vis‐NIRS. Soil WR was measured by using the molarity of ethanol droplet (MED) and the water drop penetration time (WDPT) tests. Soil organic carbon content (%C) was also measured to examine a possible relationship with SWR. A partial least squares regression (PLSR) model was developed by using Vis‐NIRS spectral data and the reference laboratory data. In addition, we explored the power of discrimination based on WDPT classes using partial least squares discriminant analysis (PLS‐DA). The PLSR of the processed spectra produced moderately accurate prediction for MED (R²_val = 0.61, RPD_val = 1.60, RMSE_val = 0.59) and good prediction for %C (R²_val = 0.82, RPD_val = 2.30, RMSE_val = 2.72). When the data from the 10 soil orders were considered separately and based on soil order rather than being grouped, the prediction of MED was further improved except for the Allophanic, Brown, Organic and Ultic soil orders. The PLS‐DA was successful in classifying 60% of soil samples into the correct WDPT classes. Our results indicate clearly that Vis‐NIRS has the potential to predict SWR. Further improvement in the prediction accuracy of SWR is envisaged by increasing the understanding of the relationship between Vis‐NIRS and the SWR of all New Zealand soil orders as a function of their physical properties and chemical constituents such as hydrophobic compounds.     

Microbial C,N, and P relationships in moisture‐stressed soils of Potohar,Pakistan

In 11 rain‐fed arable soils of the Potohar plateau, Pakistan, the amounts of microbial‐biomass C (C_mic), biomass N (N_mic), and biomass P (P_mic) were analyzed in relation to the element‐specific total storage compartment, i.e., soil C_org, N_t, and P_t. The effects of climatic conditions and soil physico‐chemical properties on these relationships were highlighted with special respect to crop yield levels. Average contents of soil C_org, N_t, and P_t were 3.9, 0.32, and 0.61 mg (g soil)^–1, respectively. Less than 1% of P_t was extractable with 0.5 M NaHCO₃. Mean contents of C_mic, N_mic, and P_mic were 118.4, 12.0, and 3.9 µg (g soil)^–1. Values of C_mic, N_mic, P_mic, soil C_org, and N_t were all highly significantly interrelated. The mean crop yield level was closely connected with all soil organic matter– and microbial biomass–related properties, but showed also some influence by the amount of precipitation from September to June. Also the fraction of NaHCO₃‐extractable P was closely related to soil organic matter, soil microbial biomass, and crop yield level. This reveals the overwhelming importance of biological processes for P turnover in alkaline soils.     

Three‐source partitioning of CO2 efflux from maize field soil by 13C natural abundance

A natural‐¹³C‐labeling approach—formerly observed under controlled conditions—was tested in the field to partition total soil CO₂ efflux into root respiration, rhizomicrobial respiration, and soil organic matter (SOM) decomposition. Different results were expected in the field due to different climate, site, and microbial properties in contrast to the laboratory. Within this isotopic method, maize was planted on soil with C₃‐vegetation history and the total CO₂ efflux from soil was subdivided by isotopic mass balance. The C₄‐derived C in soil microbial biomass was also determined. Additionally, in a root‐exclusion approach, root‐ and SOM‐derived CO₂ were determined by the total CO₂ effluxes from maize (Zea mays L.) and bare‐fallow plots. In both approaches, maize‐derived CO₂ contributed 22% to 35% to the total CO₂ efflux during the growth period, which was comparable to other field studies. In our laboratory study, this CO₂ fraction was tripled due to different climate, soil, and sampling conditions. In the natural‐¹³C‐labeling approach, rhizomicrobial respiration was low compared to other studies, which was related to a low amount of C₄‐derived microbial biomass. At the end of the growth period, however, 64% root respiration and 36% rhizomicrobial respiration in relation to total root‐derived CO₂ were calculated when considering high isotopic fractionations between SOM, microbial biomass, and CO₂. This relationship was closer to the 50% : 50% partitioning described in the literature than without fractionation (23% root respiration, 77% rhizomicrobial respiration). Fractionation processes of ¹³C must be taken into account when calculating CO₂ partitioning in soil. Both methods—natural ¹³C labeling and root exclusion—showed the same partitioning results when ¹³C isotopic fractionation during microbial respiration was considered and may therefore be used to separate plant‐ and SOM‐derived CO₂ sources.     

Rapid Prediction of Rice Quality Characteristics by Near‐Infrared Reflectance Spectroscopy for Breeding Programs

Breeding of high‐quality rice requires quick methods to evaluate the quality characteristics such as milling, grain appearance, nutritional, eating, and cooking qualities. Because routine measurements of these quality traits are time consuming and expensive, a rapid predictive method based on near‐infrared spectroscopy (NIRS) can be applied to measure these quality parameters. In this study, calibration models for measurement of grain quality were developed using a total of 570 brown and milled rice samples. The results indicated that the models developed from the spectra of brown rice for all the quality traits had the coefficient of determination for external validation (R²) larger than 0.64 except for gel consistency. The best model was developed for the protein content, with R² of 0.94 for external validation. The model for the total score of physicochemical characteristics (TSPC), a comprehensive index reflecting all other traits, had R² of 0.70 and SD/SEP of 1.70, which indicates that high or low TSPC for a given rice could be discriminated by NIRS. The models developed from brown rice were as accurate as those from milled rice. Results suggest that NIRS‐based predictions for rice quality traits may be used as indicator traits to improve rice quality in breeding programs.     

Long‐Term Changes in Soil Carbon Stocks in the Brazilian Cerrado Under Commercial Soybean

The net effect of agriculture on soil carbon is not yet fully understood. While a number of studies on shallow profiles have been published, evidence suggests that carbon stock changes occur in deeper layers. In this study we analyzed the effect of agriculture in the Cerrado soil C looking at changes in seven different profile depths from 0 to 100 cm in a commercial grain farm. We also used isotopic techniques to distinguish between the original Cerrado C₃ carbon and the C₄ carbon derived from the grasses used in agriculture. At 0–5 cm depth C stocks significantly decreased with cultivation time. The C stock did not change significantly when it was calculated using the 0–10, 0–20, 0–30, 0–50 or 0–75 cm profile (p > 0·05) but increased with cultivation time when the profile considered was 0–100 cm (p < 0·05). A two‐source isotope model revealed that there was a significant increase in carbon derived from C₄ grasses for all depths with cultivation time. Annual carbon sequestration rates for the upper 100 cm of soil were 1·1 Mg C ha⁻¹ year⁻¹ for total carbon and 0·8 Mg C₄ C ha⁻¹ year⁻¹ for C₄ carbon. The oldest area, with 23 years of cultivation, had a soil C stock increase compared to the native Cerrado soil of 17·6%. These findings suggest that commercial grain farms practices may increase soil C stock compared to native Cerrado soil, if a more complete soil profile down to 100 cm is used to assess C stocks. Copyright © 2015 John Wiley & Sons, Ltd.     

Soil‐organic‐matter stability in sandy cropland soils is related to land‐use history

Sandy cropland soils in NW Europe were found to contain unusually high organic‐carbon (OC) levels, and a link with their land‐use history has been suggested. This study's aim was to assess the discriminating power of physical and chemical fractionation procedures to yield information on soil‐organic‐matter (OM) stability for these soils. In relict‐ and cultivated‐heathland soils, much higher proportions of 6% NaOCl treatment–resistant but 10% HF–soluble OC (MOC) and N (32.2% and 29.9%) were measured compared to a set of “permanent"‐cropland soils without a history of heathland land use (11.9% and 8.5%). Also, the proportions of 6% NaOCl– and 10% HF treatment–resistant OC and N in the relict and cultivated heathlands (19.2% and 12.0%) were higher than in the permanent‐cropland soils (17.7% and 5.7%). Stepwise multiple linear‐regression yielded a significant relationship between the annual mineralization (g C [100 g OC]^–1), soil OC (g C kg^–1) content, and %MOC: Annual mineralization = 4.347 – 0.087 soil OC – 0.032 %MOC (R² = 0.65). Combinations of incubation experiments for quantification of the labile soil OM pool with chemical fractionation may thus yield meaningful data for development of soil‐organic‐matter models with measurable pools, but their applicability will be limited to specific combinations of former land use with soil, climate, and current management.     

Organic‐carbon and nitrogen stocks and organic‐carbon fractions in soil under mixed pine and oak forest stands of different ages in NE Germany

The objective of this work was to evaluate the C and N stocks and organic‐C fractions in soil under mixed forest stands of Scots pine (Pinus sylvestris L.) and Sessile oak (Quercus petraea [Matt.] Liebl.) of different ages in NE Germany. Treatments consisted of pure pine (age 102 y), and pine (age 90–102 y) mixed with 10‐, 35‐, 106‐, and 124‐y‐old oak trees. After sampling O layers, soils in the mineral layer were taken at two different depths (0–10 and 10–20 cm). Oak admixture did not affect total organic‐C (TOC) and N stocks considering the different layers separately. However, when the sum of TOC stocks in the organic and mineral layers was considered, TOC stocks decreased with increasing in oak age (r² = 0.58, p < 0.10). The microbial C (C_MB) was not directly correlated with increase of oak age, however, it was positively related with presence of oak species. There was an increase in the percentage of the C_MB‐to‐TOC ratio with increase of oak‐tree ages. On average, light‐fraction C (C_LF) comprised 68% of the soil TOC in upper layer corresponding to the highest C pool in the upper layer. C_LF and heavy‐fraction C (C_HF) were not directly affected by the admixture of oak trees in both layers. The C_HF accounted on average for 30% and 59% of the TOC at 0–10 and 10–20 cm depths, respectively. Despite low clay contents in the studied soils, the differences in the DCB‐extractable Fe and Al affected the concentrations of the C_HF and TOC in the 10–20 cm layers (p < 0.05). Admixture of oak in pine stands contributed to reduce topsoil C stocks, probably due to higher soil organic matter turnover promoted by higher quality of oak litter.     

Medium‐ and short‐term available organic matter,microbial biomass,and enzyme activities in soils under Pinus sylvestris L. and Robinia pseudoacacia L. in a sandy soil in NE Saxony,Germany

Total, mobile, and easily available C and N fractions, microbial biomass, and enzyme activities in a sandy soil under pine (Pinus sylvestris L.) and black locust (Robinia pseudoacacia L.) stands were investigated in a field study near Riesa, NE Germany. Samples of the organic layers (Oi and Oe‐Oa) and the mineral soil (0–5, 5–10, 10–20, and 10–30 cm) were taken in fall 1999 and analyzed for their contents of organic C and total N, hot‐water‐extractable organic C and N (HWC and HWN), KCl‐extractable organic C and N (C_org(KCl) and N_org(KCl)), NH ‐N and NO ‐N, microbial‐biomass C and N, and activities of β‐glucosidase and L‐asparaginase. With exception of the HWC, all investigated C and N pools showed a clear response to tilling, which was most pronounced in the Oi horizon. Compared to soils under pine, those under black locust had higher contents of medium‐ and short‐term available C (HWC, C_org(KCl)) and N (HWN, N_org(KCl)), mineral N (NH ‐N, NO ‐N), microbial‐biomass C and N, and enzyme activities in the uppermost horizons of the soil. The strong depth gradient found for all studied parameters was most pronounced in soils under black locust. Microbial‐biomass C and N and enzyme activities were closely related to the amounts of readily mineralizable organic C (HWC and C_org(KCl)). However, the presented results implicate a faster C and N turnover in the top‐soil layers under black locust caused by higher N‐input rates by symbiotic N₂ fixation.     

Quantification of long‐chain fatty acids in dissolved organic matter and soils

The objective was to develop and adapt a versatile analytical method for the quantification of solvent extractable, saturated long‐chain fatty acids in aquatic and terrestrial environments. Fulvic (FA) and humic (HA) acids, dissolved organic matter (DOM) in water, as well as organic matter in whole soils (SOM) of different horizons were investigated. The proposed methodology comprised extraction by dichloromethane/acetone and derivatization with tetramethylammonium hydroxide (TMAH) followed by gas chromatography/mass spectrometry (GC/MS) and library searches. The C_10:0 to C_34:0 methyl esters of n‐alkyl fatty acids were used as external standards for calibration. The total concentrations of C_14:0 to C_28:0 n‐alkyl fatty acids were determined in DOM obtained by reverse‐osmosis of Suwannee river water (309.3 μg g^—1), in freeze‐dried brown lake water (180.6 μg g^—1), its DOM concentrate (93.0 μg g^—1), humic acid (43.1 μg g^—1), and fulvic acid (42.5 μg g^—1). The concentrations of the methylated fatty acids (n‐C_16:0 to n‐C_28:0) were significantly (r² = 0.9999) correlated with the proportions of marker signals (% total ion intensity (TII), m/z 256 to m/z 508) in the corresponding pyrolysis‐field ionization (FI) mass spectra. The concentrations of terrestrial C_10:0 to C_34:0 n‐alkyl fatty acids from four soil samples ranged from 0.02 μg g^—1 to 11 μg g^—1. The total concentrations of the extractable fatty acids were quantified from a Podzol Bh horizon (26.2 μg g^—1), Phaeozem Ap unfertilized (48.1 μg g^—1), Phaeozem Ap fertilized (57.7 μg g^—1), and Gleysol Ap (66.7 μg g^—1). Our results demonstrate that the method is well suited to investigate the role of long‐chain fatty acids in humic fractions, whole soils and their particle‐size fractions and can be serve for the differentiation of plant growth and soil management.