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Abstract:
Soils and sediments contain only small amounts of organic matter, and large concentrations of paramagnetic metals can give poor solid-state nuclear magnetic resonance (NMR) spectra of organic matter. Pretreatment of samples with hydrofluoric acid (HF) dissolves significant proportions of the mineral matrix and extracts paramagnetic elements. We investigated the effects of 10% HF treatment on the stable isotope content of carbon (C) and nitrogen (N) of organic matter from soils, composts and shales. Additionally we inferred molecular and isotopic characteristics of lost materials from calculations of isotope mass balances. Treatment with HF enriched C and N in mineral samples substantially (factors 2.5–42.4), except for Podzol B horizons (1.1–1.7) and organic material (1.0–1.3). After treatment most of the C (59.7–91.7%) and N (53.7–86.6%) was recovered, although changing C/N ratios often indicated a preferential loss of N-rich material. Isotope ratios of C and N in the remaining material became more negative when net alterations exceeded 0.3‰. The isotope ratios of the lost material contained more 13C (1–2‰) and 15N (1–4‰) than the initial organic matter. Acid hydrolysis typically removes proteins, amino acids and polysaccharides, all of which are enriched in 13C, and in the case of proteins and amino acids, enriched in 15N as well. We conclude that HF treatment released fresh, soluble, probably microbial, biomass in addition to carbohydrates. Net changes of the bulk chemical composition of organic matter were small for most soils, size fractions and plant material, but not for samples containing little organic matter, or those rich in easily soluble organic matter associated with iron oxides, such as Podzol B horizons.
