Fractionation of soil organic carbon (SOC) is crucial for mechanistic understanding and modeling of soil organic matter decomposition and stabilization processes. It is often aimed at separating the bulk SOC into fractions with varying turnover rates, but a comprehensive comparison of methods to achieve this is lacking. In this study, a total of 20 different SOC fractionation methods were tested by participating laboratories for their suitability to isolate fractions with varying turnover rates, using agricultural soils from three experimental sites with vegetation from C3 to C4 22-36 years ago. Enrichment of C4-derived carbon was traced and used as a proxy for turnover rates in the fractions. Methods that apply a

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Summary The sequestration of carbon (C) in soil is not completely understood, and quantitative information about the amounts of organic carbon in the various fractions and their rates of turnover could improve understanding. We aimed (i) to quantify the amounts of C derived from maize at various depths in the soil in a long‐term field experiment with and without fertilization using 13C/12C analysis, (ii) to model changes in the organic C, and (iii) to compare measured and modelled pools of C. The organic C derived from the maize was measured in soil samples collected to a depth of 65 cm from four plots, two of which had been under continuous maize and two under continuous rye during long‐term field experiments with NPK and without fertilization. The fractionation procedures included particle‐size fractionation and extractions in water and in pyrophosphate solution. We used the Rothamsted Carbon Model to model the dynamics of the carbon from 13C data. The amounts of C derived from maize in the Ap horizon after 39 years of continuous maize cropping were 9.5% of the total organic C (where unfertilized) and 14.0% where NPK had been applied. Fertilization did not affect the residence time of carbon in the soil. The amounts of C derived from maize in water extracts were 21% of the total organic C (where unfertilized) and 22% where NPK had been applied. The extracts that were soluble in pyrophosphate and insoluble in acid were depleted in C from maize (the amounts were 5% and 7% of the total organic C, respectively). The results of the 13C natural abundance technique were used to model the dynamics of the organic C. Both the total organic C and the C derived from maize in the particle‐size fraction 0–63 μm agreed well with the total and maize‐derived sums of the model pools ‘inert organic matter’, ‘humified organic matter’ and ‘microbial biomass’. The model suggested that 64% (unfertilized) or 53% (NPK) of the organic C in the Ap horizon were inert. Only one of three published equations to determine the size of the inert pool agreed well with these model results.

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The cation exchange capacity (CEC) of soils depends on the amount and composition not only of clay minerals but also of soil organic matter (SOM). While the CEC of soil clay minerals has been intensively studied, little is known about the CEC of organic matter (OM) fractions, in particular those obtained with newly developed SOM extraction techniques. The objective of this study was to develop and test a method to quantitatively determine the CEC of extracted OM fractions and to relate CEC(OM) to OM functional groups possibly responsible for sorption of cations. Water‐ and pyrophosphate‐soluble OM fractions were sequentially extracted from differently managed arable soils of two well‐known long‐term field experiments. The CEC of a freeze‐dried pyrophosphate‐soluble OM fraction [OM(PY)] (0.03 g) mixed with quartz sand (4.97 g) was determined by applying the standard percolation method. The chemical composition of OM(PY) was analyzed by Fourier‐transform infrared (FTIR) spectroscopy. For all plots except those fertilized with farmyard manure, the sorption properties of the OM(PY) fraction were found to be site specific and to reflect soil and crop rotation effects. The relative contribution of the CEC of OM(PY) to the CEC of the soil (0.8–11.6%) is dependent on soil C content and extractability. For all plots, however, the relative contents of carboxylic functional groups in OM(PY) determined with FTIR spectroscopy was found to be linearly related to the CEC of the OM(PY), similar to pure organic substances. This relationship indicates the usefulness of CEC determination on OM(PY) fractions. The results suggest that the relative contents of carboxylic functional groups in OM(PY) reflect long‐term effects of fertilization and crop rotation on the sorption properties of the SOM.

Application of ultrasound to disperse soil aggregates has been critical in enabling researchers to separate and analyze aggregate building blocks that include organic and mineral particles as well as mineral associated organic matter. But the forces generated in the process may also alter the dispersion products and, thus, potentially interfere with the interpretation of experimental results. This review summarizes present knowledge on experimental conditions that may lead to physical damage and chemical modifications of aggregate building blocks. The energy level at which physical disintegration of organic particles could be detected was as low as 60 J mL -1 . Physical damage of sand-and silt-sized mineral particles was observed to commence at energy levels exceeding 700 J cm -3 . No evidence was found for the disintegration of particles within the clay-size fraction of soils even though studies analyzing pure minerals such as kaolinite revealed particle breakage after application of energy amounts > 12,000 J cm -3 . Here we outline a strategy to minimize artifacts such as physical damage of mineral or organic particles resulting from ultrasonication by adopting a stepwise dispersion protocol involving successively higher energy levels, accompanied by a sequential separation of organic and mineral compounds.