Avaliação de características de ácidos húmicos de resíduos de origem urbana: I. métodos espectroscópicos (UV-Vis, IV, RMN 13C-CP/MAS) e microscopia eletrônica de varredura

Foram caracterizados fisico-quimicamente ácidos húmicos, obtidos de composto de resíduos sólidos urbanos (AH-CRSU) e de lodo de estação de tratamento de esgoto (AH-LETE), ambos produzidos na cidade do Rio de Janeiro, por meio da análise da composição elementar, acidez total, de dados espectroscópicos (UV-Vis; IV, RMN de 13C-CP/MAS) e microscopia eletrônica de varredura (MEV). A análise das características estruturais revelou diferenças entre os AHs estudados. A presença de sistemas aromáticos foi observada por meio da espectroscopia de UV-Vis, indicando sistemas mais substituídos nos AH-LETE. A espectroscopia na região do infravermelho (IV) mostrou a presença de estruturas alifáticas nos AHs e maior complexidade nos sinais de absorção devida a polissacarídeos nos AH-CRSU. Além disso, foram observados grupos OH, COOH, COO-, CO2NH2, e confirmada a presença de sistemas aromáticos. Com a análise de RMN de 13C-CP/MAS, foi possível verificar as diferenças quantitativas nos diferentes tipos de carbono. Os AH-LETE apresentaram maior quantidade de grupos aromáticos e de COOH. A análise de RMN de 13C-CP/MAS também mostrou presença de polissacarídeos, N em aminoácidos e grupamentos OCH3. O conjunto de propriedades avaliadas permitiu indicar que a fração ácidos húmicos dos resíduos é "do tipo" ou "análoga" aos ácidos húmicos de origem pedogênica.

Discovery of an albite gneiss from the Ile de Groix (Armorican Massif, France): Geochemistry and LA-ICP-MS U-Pb geochronology of its Ordovician protolith

For the first time, an albite orthogneiss has been recognised and dated within the HP-LT blueschist facies metabasites and metapelites of the Ile de Groix. It is characterised by a peraluminous composition, high LILE, Th and U contents, MORB-like HREE abundances and moderate Nb and Y values. A U-Pb age of 480.8 +/- A 4.8 Ma was obtained by LA-ICP-MS dating of zircon and titanite. It is interpreted as the age of the magmatic emplacement during the Early Ordovician. Morphologically different zircon grains yield late Neoproterozoic ages of 546.6-647.4 Ma. Zircon and titanite U-Pb ages indicate that the felsic magmatism from the Ile de Groix is contemporaneous with the acid, pre-orogenic magmatism widely recognised in the internal zones of the Variscan belt, related to the Cambro-Ordovician continental rifting. The magmatic protolith probably inherited a specific chemical composition from a combination of orogenic, back-arc and anorogenic signatures because of partial melting of the Cadomian basement during magma emplacement. Besides, the late Devonian U-Pb age of 366 +/- A 33 Ma obtained for titanite from a blueschist facies metapelite corresponds to the age of the HP-LT peak metamorphism.

Características estruturais de ácidos húmicos isolados de solos com adição de resíduos orgânicos de origem urbana: composição elementar, análise de RMN 13C e Pi-CG/EM

Foram avaliadas as alterações nas características estruturais de ácidos húmicos (AH) decorrentes da adição de matéria orgânica de resíduos urbanos. Os AH foram extraídos da camada superficial (0-20 cm) de um Argissolo Vermelho-Amarelo (Seropédica, RJ) e de um Latossolo Vermelho Amarelo (Piraí, RJ), ambos tratados com o equivalente a 80 t ha-1 (em base seca) de composto de lixo urbano e lodo de estação de tratamento de esgotos. O tempo de incubação em laboratório foi de 24 semanas à temperatura ambiente e umidade mantida na capacidade de campo. Para caracterizar os AH, foram utilizadas a análise elementar, a ressonância magnética nuclear (RMN) de 13C e Pirólise acoplada à cromatografia gasosa e a espectrometria de massas (Pi-CG/EM). A análise de RMN 13C permitiu observar alterações na composição molecular dos AH de forma clara, principalmente, pelo aumento do teor de C mono e di oxigenados (δC 50-110) e pela diminuição dos teores de grupos CH2 e CH3 (δC 50-110). O aumento no teor de carboidratos evidencia a presença de estruturas mais lábeis nos AH com adição dos resíduos. Em adição, a técnica de Pi-CG/EM permitiu verificar diferenças qualitativas significativas nos compostos orgânicos, provenientes da fragmentação térmica dos AH com incorporação de novas estruturas, sobretudo da fração lipídica e de derivados de carboidratos (furanos), nas amostras de solos tratados com ambos os resíduos orgânicos. O uso em conjunto das técnicas analíticas de RMN 13C e de Pi-CG/EM foi eficiente para avaliar as mudanças na composição molecular de ácidos húmicos decorrentes da adição de resíduos orgânicos de origem urbana.

Transformations in occluded light fraction organic matter in a clayey oxisol: evidence from 13C-CPMAS-NMR and delta13C Signature

We hypothesised that, during occlusion inside granular aggregates of oxide-rich soils, the light fraction organic matter would undergo a strong process of decomposition, either due to the slow process of aggregate formation and stabilisation or due to digestion in the macro- and meso-fauna guts. This process would favour the accumulation of recalcitrant materials inside aggregates. The aim of this study was to compare the dynamics and the chemical composition of free and occluded light fraction organic matter in a natural cerrado vegetation (woodland savannah) and a nearby pasture (Brachiaria spp.) to elucidate the transformations during occlusion of light fraction in aggregates of a clayey Oxisol. Nuclear Magnetic Resonance of the 13C, with Cross Polarisation and Magic Angle Spinning (13C-CPMAS-NMR), and 13C/12C isotopic ratio were combined to study organic matter composition and changes in carbon dynamics, respectively. The occluded light fraction had a slower turnover than the free light fraction and the heavy fraction. Organic matter in the occluded fraction also showed a higher degree of decomposition. The results confirm that processes of soil organic matter occlusion in the typical "very fine strong granular" structure of the studied oxide-rich soil led to an intense transformation, selectively preserving stable organic matter. The small amount of organic material stored as occluded light faction, as well as its stability, suggests that this is not an important or manageable sink for sequestration of atmospheric CO2.

Suomen ja viron u- ja ne-verbijohdosten käytön vertailua

Summary: Comparison of the use of verb derivatives with the suffixes -u- and -ne- in Finnish and Estonian

Quantification of brain glycogen concentration and turnover through localized 13C NMR of both the C1 and C6 resonances.

We have recently shown that at isotopic steady state (13)C NMR can provide a direct measurement of glycogen concentration changes, but that the turnover of glycogen was not accessible with this protocol. The aim of the present study was to design, implement and apply a novel dual-tracer infusion protocol to simultaneously measure glycogen concentration and turnover. After reaching isotopic steady state for glycogen C1 using [1-(13)C] glucose administration, [1,6-(13)C(2)] glucose was infused such that isotopic steady state was maintained at the C1 position, but the C6 position reflected (13)C label incorporation. To overcome the large chemical shift displacement error between the C1 and C6 resonances of glycogen, we implemented 2D gradient based localization using the Fourier series window approach, in conjunction with time-domain analysis of the resulting FIDs using jMRUI. The glycogen concentration of 5.1 +/- 1.6 mM measured from the C1 position was in excellent agreement with concomitant biochemical determinations. Glycogen turnover measured from the rate of label incorporation into the C6 position of glycogen in the alpha-chloralose anesthetized rat was 0.7 micromol/g/h.

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Geoecological drivers of cerrado heterogeneity and 13C natural abundance in oxisols after land-use change

The 13C natural abundance technique was applied to study C dynamics after land-use change from native savanna to Brachiaria, Pinus, and Eucalyptus in differently textured Cerrado Oxisols. But due to differences in the d13C signatures of subsoils under native savanna and under introduced species, C substitution could only be calculated based on results of cultivated soils nearby. It was estimated that after 20 years, Pinus C had replaced only 5 % of the native C in the 0-1.2 m layer, in which substitution was restricted to the top 0.4 m. Conversely, after 12 years, Brachiaria had replaced 21 % of Cerrado C to a depth of 1.2 m, where substitution decreased only slightly throughout the entire profile. The high d13C values in the subsoils of the cultivated sites led to the hypothesis that the natural vegetation there had been grassland rather than Cerrado sensu stricto, in spite of the comparable soil and site characteristics and the proximity of the studied sites. The hypothesis was tested using aerial photographs of 1964, which showed that the cultivated sites were located on a desiccated runoff head. The vegetation shift to a grass-dominated savanna formation might therefore have occurred in response to waterlogging and reduced soil aeration. A simple model was developed thereof, which ascribes the different Cerrado formations mainly to the plant-available water content and soil aeration. Soil fertility is considered of minor significance only, since at the studied native savanna sites tree density was independent of soil texture or nutrient status.

1H-[13C] NMR spectroscopy of the rat brain during infusion of [2-13C] acetate at 14.1 T.

Full signal intensity (1)H-[(13)C] NMR spectroscopy, combining a preceding (13)C-editing block based on an inversion BISEP (B(1)-insensitive spectral editing pulse) with a spin-echo coherence-based localization, was developed and implemented at 14.1 T. (13)C editing of the proposed scheme was achieved by turning on and off the (13)C adiabatic full passage in the (13)C-editing block to prepare inverted and noninverted (13)C-coupled (1)H coherences along the longitudinal axis prior to localization. The novel (1)H-[(13)C] NMR approach was applied in vivo under infusion of the glia-specific substrate [2-(13)C] acetate. Besides a approximately 50% improvement in sensitivity, spectral dispersion was enhanced at 14.1 T, especially for J-coupled metabolites such as glutamate and glutamine. A more distinct spectral structure at 1.9-2.2 ppm(parts per million) was observed, e.g., glutamate C3 showed a doublet pattern in both simulated (1)H spectrum and in vivo (13)C-edited (1)H NMR spectra. Besides (13)C time courses of glutamate C4 and glutamine C4, the time courses of glutamate C3 and glutamine C3 obtained by (1)H-[(13)C] NMR spectroscopy were reported for the first time. Such capability should greatly improve the ability to study neuron-glial metabolism using (1)H-observed (13)C-edited NMR spectroscopy.