A comparison of two methods for the isolation of free and occluded participate organic matter

Various methods exist for the isolation of particulate organic matter (POM), one of the soil-organic-matter (SOM) fractions reacting most sensitive on land-use or soil-management changes. A combination of density separation and ultrasonic treatment allows to isolate two types of POM: (1) free POM and (2) POM occluded in soil aggregates. POM fractions are closely linked to their biochemical function for the formation and stabilization of aggregates, therefore methods using different aggregate sizes may result in different POM fractions isolated. We evaluated two physical fractionation procedures to reveal whether they yield different POM fractions with respect to amount and composition, using grassland and arable soils with sandy-loam to sandy-clay-loam texture and thus low macroaggregate stability. Method I used air-dried aggregates of <2.0 mm size and a low-energy sonication for aggregate disruption, method II used field-moist aggregates <6.3 mm and a high-energy-sonication procedure for aggregate disruption. POM fractions were analyzed by elemental analysis (C, N) and CPMAS ¹³C-NMR spectroscopy. With both methods, about similar proportions of the SOM are isolated as free or occluded POM, respectively. The free- and occluded-POM fractions obtained with method I are also rather similar in C and N concentration and composition as shown by ¹³C-NMR spectroscopy. Method II isolates a free-and occluded-POM fraction with significantly different C and N concentrations. NMR spectra revealed significant differences in the chemical composition of both fractions from method II, with the occluded POM having lower amounts of O-alkyl C and higher amounts of aryl C and alkyl C than the free POM. Due to the use of larger, field-moist aggregates with minimized sample pretreatment, two distinctly different POM fractions are isolated with method II, likely to be more closely linked to their biochemical function for the formation and stabilization of aggregates. High-energy sonication as in method II also disrupts small microaggregates <63 μm and releases fine intraaggregate POM. This fraction seems to be a significant component of occluded POM, that allows a differentiation between free and occluded POM in sandy soils with significant microaggregation. It can be concluded, that microaggregation in arable soils with sandy texture is responsible for the storage of a more degraded occluded POM, that conversely supports the stabilization of fine microaggregates.