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  • 1
    Electronic Resource
    Electronic Resource
    Oxford, UK; Malden, USA : Blackwell Science Ltd
    ISSN: 1365-2389
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Analysis of soil lipids may contribute to an improved understanding of atmosphere to soil carbon fluxes, soil organic matter source differentiation and pollutant accumulation. Soil lipids, mostly originating from plants and microorganisms, have traditionally been analysed by non-automated extraction and separation methods, which produce several lipid fractions, operationally defined by polarity. Here we present a combination of fast, automated and reproducible techniques, adopted from organic geochemical studies, for preparative separation of individual soil lipid fractions with increasing polarity. These techniques involve commercially available instruments, including accelerated solvent extraction and a two-step automated medium-pressure liquid chromatography procedure. The method yields eight lipid fractions consisting of five fractions fully amenable to gas chromatography/mass spectrometry (GC/MS) (aliphatic hydrocarbons, aromatic hydrocarbons, ketones, alcohols, carboxylic acids), and three fractions of highly polar or high molecular weight compounds (bases, very long-chain wax esters (C40+), high polarity compounds) that were not measurable with GC/MS under standard conditions. We tested the method on five agricultural soils. Results show that (i) mass recoveries for the individual fractions are reproducible, (ii) within individual fractions compound distribution patterns are reproducible, as demonstrated for alkanes and carboxylic acids, and (iii) individual fractions represent distinct and clean compound classes, free of interfering substances detectable by GC/MS. Thus, automated separation can be a fast, effective and reproducible procedure for fractionation of complex mixtures of soil lipids into clean compound classes, directly suitable for a variety of molecular (e.g. GC/MS) and isotopic characterizations (e.g. gas chromatography coupled with isotope ratio monitoring mass spectrometry or accelerator mass spectrometry).
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  • 2
    ISSN: 1365-2389
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Burning vegetation produces partly charred plant material which subsequently could contribute to the highly refractory proportion of soil organic matter. The presence of charred organic carbon (COC) was investigated in 17 horizons originating from nine soils from Germany and the Netherlands using a suite of complementary methods (high-energy ultraviolet photo-oxidation, scanning electron microscopy, solid-state 13C nuclear magnetic resonance, lignin analysis by CuO oxidation). Charred organic carbon could not be detected in the A horizons of an Alisol and a Gleysol, but it contributed up to 45% of the organic carbon and up to about 8 g kg–1 of the soil in a range of grey to black soils (Cambisol, Luvisol, Phaeozem, Chernozem and Greyzem). All these soils have chernozemic soil properties (dark colour, A–C profile, high base saturation, bioturbation). A 10-km colour sequence of four chernozemic soils, which were very similar in chemical and physical properties, showed a strong relation between colour and the content of COC. This suggests that the COC affects mainly soil colour in the sequence studied. Finely divided COC seems to be a major constituent of many chernozemic soils in Germany. These results suggest that besides climate, vegetation and bioturbation, fire has played an important role in the pedogenesis of chernozemic soils.
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  • 3
    ISSN: 1365-2389
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: 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.
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  • 4
    ISSN: 1365-2389
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: The organic matter in soils may be stabilized by its interactions with minerals. We have studied such interactions in a Haplic Alisol under forest in which clay and organic matter have migrated from an eluvial A horizon to accumulate in an illuvial B horizon. We have tried to trace the fate of organic matter in these horizons (Ah and Bvt) by determining clay mineralogy, carbon and nitrogen content, hydrolysable amino acids, lignin signature by alkaline CuO oxidation and carbon species by 13C CPMAS NMR of bulk soils and particle-size fractions. In both horizons, most of the organic matter was present in O–alkyl and methylene structures, each contributing one-third to the bulk organic matter. In the Ah horizon the ratios of carbon-to-nitrogen, and yields for lignin and hydrolysable amino acids decreased as the particle-size class decreased, but side-chain oxidation of lignin compounds increased with decreasing particle size. In contrast to previous observations, the proportions of O–alkyl carbon increased as particle size decreased, constituting a major proportion of the organic carbon in the clay-size fractions from both the Ah and Bvt horizons (≥ 38%), while proportions of methylene carbon decreased. Illite was the dominant mineral in the fraction ≤ 6 μm, whereas the mobile fine clay fraction (〈0.2 μm) was rich in smectites – minerals with large surface areas. Our results support the hypothesis that potentially labile organic matter, such as O–alkyl carbon typically present in polysaccharides, may be stabilized against further degradation in organomineral complexes.
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  • 5
    ISSN: 1365-2389
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Soil organic matter can be intimately associated with mineral particles of various sizes. For structural studies, soil organic matter can be isolated in particle size fractions after complete dispersion of the aggregates by ultrasonication. The ultrasonic dispersion energy necessary for complete dispersion was investigated in three A and two B horizons originating from four soils differing in pedogenesis (Gleysol, Phaeozem, Podzol, Alisol), organic C (4.2–34.5 g kg–1) and clay content (24–294 g kg–1). Calorimetric calibration of five probe-type ultrasonifiers revealed that the actual energy output from an instrument can depart widely from its nominal output, and that this discrepancy varies from instrument to instrument. Calorimetric calibration is therefore essential for consistency and comparisons between laboratories. Between 450 and 500 J ml–1 of ultrasonic dispersion energy was enough to disperse completely all samples investigated. The particle size distributions obtained were close to those from standard analysis, except for smaller yields (–20 to –80 g kg–1) of sand size fractions, which suggests that dispersion by ultrasound is more effective. Based on total C, C:N ratio and distribution of dissolved C, no detachment of soil organic matter from primary organomineral complexes and no redistribution between particle size fractions could be detected in the range 30–590 J ml–1 of dispersion energy.
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  • 6
    ISSN: 1365-2389
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Fires in boreal forests frequently convert organic matter in the organic layer to black carbon, but we know little of how changing fire frequency alters the amount, composition and distribution of black carbon and organic matter within soils, or affects podzolization. We compared black carbon and organic matter (organic carbon and nitrogen) in soils of three Siberian Scots pine forests with frequent, moderately frequent and infrequent fires.Black carbon did not significantly contribute to the storage of organic matter, most likely because it is consumed by intense fires. We found 99% of black carbon in the organic layer; maximum stocks were 72 g m−2. Less intense fires consumed only parts of the organic layer and converted some organic matter to black carbon (〉 5 g m−2), whereas more intense fires consumed almost the entire organic layer. In the upper 0.25 m of the mineral soil, black carbon stocks were 0.1 g m−2 in the infrequent fire regime.After fire, organic carbon and nitrogen in the organic layer accumulated with an estimated rate of 14.4 g C m−2 year−1 or 0.241 g N m−2 year−1. Maximum stocks 140 years after fire were 2190 g organic C m−2 and 40 g N m−2, with no differences among fire regimes. With increasing fire frequency, stocks of organic carbon increased from 600 to 1100 g m−2 (0–0.25 m). Stocks of nitrogen in the mineral soil were similar among the regimes (0.04 g m−2). We found that greater intensities of fire reduce amounts of organic matter in the organic layer but that the greater frequencies may slightly increase amounts in the mineral soil.
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  • 7
    ISSN: 1365-2389
    Source: Blackwell Publishing Journal Backfiles 1879-2005
    Topics: Geosciences , Agriculture, Forestry, Horticulture, Fishery, Domestic Science, Nutrition
    Notes: Standard procedure for dispersing natural soils for particle size fractionation can be too aggressive for soil containing coal and other organic particles from coal industries. We have investigated ultrasonic dispersion for the latter in four soils differing in pedogenesis (Phaeozem, Podzol, reclaimed mine soils), carbon content (27.5–138.6 g kg–1), clay content (80–153 g kg–1) and sources of particles (airborne coal dust, combustion residues, lignite particles). As we found previously for natural soils, the ultrasonic energy needed for complete dispersion varies between 450 and 500 J ml–1, but the resulting particle size distributions differ from those obtained by standard textural analysis. This is probably related to the different properties of native soil organic matter and coal and combusted particles. Coal and soot particles may partly resist oxidation with hydrogen peroxide, depending on material and particle size. The diameter of lignite particles, remaining after oxidation, is overestimated in sedimentation analysis by a factor of 1.66. Sand-sized lignite particles can be disrupted by ultrasonication and redistributed to finer particle size fractions. The ultrasonic dispersion and particle size fractionation procedure can be applied to soils containing coal and combusted particles, but caution is needed in interpreting the results if they contain large proportions of coal particles.
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  • 8
    ISSN: 1432-0967
    Source: Springer Online Journal Archives 1860-2000
    Topics: Geosciences
    Notes: Abstract The fluid-absent reaction 12 zoisite = 3 lawsonite + 7 grossular + 8 kyanite + 1 coesite was experimentally reversed in the model system CaO-Al2O3-SiO2-H2O (CASH) using a multi-anvil apparatus. The upper pressure stability limit for zoisite was found to extend to 5.0 GPa at 700 °C and to 6.6 GPa at 950 °C. Additional experiments both in the H2O-SiO2-saturated and in the H2O-Al2O3-saturated portions of CASH provide further constraints on high pressure phase relationships of lawsonite, zoisite, grossular, kyanite, coesite, and an aqueous fluid. Consistency of the present experiments with the H2O-saturated breakdown of lawsonite is demonstrated by thermodynamic analysis using linear programming techniques. Two sets of data consistent with databases of Berman (1988) and Holland and Powell (1990) were retrieved combining experimental phase relationships, calorimetric constraints, and recently measured elastic properties of solid phases. The best fits result in G f ,1,298 ∘,zoisite=−6,499,400 J and S 1,298 ∘,zoisite=302 J/K, and G f ,1,298 ∘,lawsonite=−4,514,600 J and S 1,298 ∘,lawsonite=220 J/K for the dataset of Holland and Powell, and G f ,1,298 ∘,zoisite=−6,492,120 J and S 1,298 ∘,zoisite=304 J/K, and G f ,1,298 ∘,lawsonite=−4,513,000 J and S 1,298 ∘,lawsonite= 218 J/K for the dataset of Berman. Examples of the usage of zoisite as a geohygrometer and as a geobarometer in rocks metamorphosed at eclogite facies conditions are worked, profiting from the thermodynamic properties retrieved here.
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  • 9
    Source: ACS Legacy Archives
    Topics: Chemistry and Pharmacology , Physics
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  • 10
    ISSN: 1432-2021
    Keywords: Key words Lawsonite ; Equation of state ; X-ray diffraction ; High-pressure ; High-temperature
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: Abstract  A pressure-volume-temperature data set has been obtained for lawsonite [CaAl2Si2O7(OH)2.H2O], using synchrotron X-ray diffraction and an externally heated diamond anvil cell. Unit-cell volumes were measured to 9.4 GPa and 767 K by angle dispersive X-ray diffraction using imaging plates. Phase changes were not observed within this pressure-temperature range, and lawsonite compressed almost isotropically at constant temperature. The P-V-T data have been analyzed using a Birch- Murnaghan equation of state and a linear equation of state expressed as β=–1/V0 (∂V/∂P) T . At room temperature, the derived equation of state parameters are: K 0=124.1 (18) GPa K'0 set to 4) and β–1=142.0(24) GPa, respectively. Our results are intermediate between previously reported measurements. The high-temperature data show that the incompressibility of lawsonite decreases with increasing temperature to ∼500 K and then increases above. Hence, the second order temperature derivative of the bulk modulus is taken into account in the equation of state; a fit of the volume data yields K 0=123.9(18) GPa, (∂K/∂T)P=–0.111(3) GPa K–1, (∂2 K/∂T 2)P=0.28(6) 10–3 GPa K–2, α0=3.1(2) 10–5 K–1, assuming K'0=4.
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