Abstract Portable X-ray fluorescence (pXRF) spectrometry offers valuable information for prediction models of soil fertility attributes spatial variation, although this approach is yet scarce in tropical regions. This study aims to predict and build spatial variability maps of soil pH, remaining phosphorus (P-Rem), soil organic matter (SOM) and sum of bases (SB) using pXRF results through stepwise multiple linear regression (SMLR) and Random Forest (RF) in a highly variable tropical area. Composite samples from soil A horizon were collected at 90 points throughout the campus of the Federal University of Lavras, Minas Gerais, Brazil, for pH, P-Rem, SOM, SB and pXRF analyses. RF predictions showed the highest accuracies, especially for P-Rem and SB (R² values of 0.66 and 0.55, respectively). Attributes that showed higher R² in punctual predictions also exhibited higher R² in spatial predictions. Data obtained from pXRF in tandem with RF can be used to assist prediction models for soil fertility attributes, consequently enabling the digital mapping of such attributes and helping to improve the knowledge about the spatial variability of such attributes in soils of tropical climate. This technique can therefore assist in the identification and orientation of adequate management practices in tropical agricultural practices.

RESUMO Há uma crescente demanda por mapas de solo, já que informações detalhadas de solos estão diretamente relacionadas com agricultura, urbanização e conservação ambiental. Porém, há escassez de mapas de solo em grande escala em países tropicais em desenvolvimento como o Brasil. Apesar de existirem mapas para pequenas áreas, grandes regiões possuem mapas pouco detalhados. Considerando-se a importância de se buscarem alternativas para superar a falta de informações detalhadas de solo, o objetivo deste trabalho foi extrapolar mapas locais para áreas maiores semelhantes que necessitam de informações mais detalhadas. A bacia do rio Anhumas, no município de Itajubá, sudeste do Brasil, foi manualmente mapeada e este mapa foi utilizado para predizer a distribuição de solos para todo o município. Primeiro, o modelo de predição foi testado na mesma bacia e alcançou acurácia global de 67% e coeficiente Kappa de 0,62. Depois, os resultados foram usados conjuntamente com dados da bacia José Pereira para predizer as classes de solo de todo o município, alcançando acurácia global de 54% e coeficiente Kappa de 0,40. Dados de material de origem em baixa resolução confundiram os modelos; as predições obtiveram melhores resultados quando esta variável foi removida. O mapa de solos de Minas Gerais apresenta apenas a classe de solo Argissolo e suas associações com outros solos para a área. O mapa confeccionado por este trabalho, porém, identificou mais classes de solo. O mapeamento de áreas representativas e sua extrapolação para áreas maiores constitui alternativa promissora para superar a escassez de mapas detalhados de solo.

ABSTRACT There is an ever-growing need for soil maps, since detailed soil information is directly related to agricultural activities, urbanization and environmental protection. However, there is a lack of large-scale soil maps in developing tropical countries such as Brazil. Albeit there are soil maps for small areas, large regions usually have undetailed maps. Considering the importance of finding low-cost alternatives to overcome the lack of detailed soil information, the main objective of this work was to manually create a local soil map and extrapolate it to similar larger areas that lack detailed soil information. The Anhumas River Basin, in the municipality of Itajubá, southeast Brazil, was manually mapped and this map was used to predict soils distribution for the entire municipality. First, the prediction model was tested in the same basin and provided sufficient results, achieving 67% global accuracy and 0.62 Kappa coefficient. Second, the resulting map was used together with the soil map of the larger José Pereira Basin to map the entire municipality, achieving 54% global accuracy and 0.40 Kappa coefficient. Low resolution parent material information was found to confuse models; maps showed better results when this variable was removed. The Minas Gerais soil map presents general mapping units only for the Acrisol class and its associations with other soil classes in the area. The soil map predicted by this work identified more soil classes. Mapping representative areas and extrapolating these maps to larger similar areas constitute a promising alternative to overcome the lack of detailed soil maps.

RESUMO Latossolos são os principais solos do Brasil e classicamente ocorrem em superfícies geomórficas suavizadas e estáveis. No entanto, no Sul de Minas Gerais, Latossolos têm sido observados em relevo forte ondulado, uma condição rara para estes solos nesta região fisiográfica. Este trabalho teve como objetivo acessar a dinâmica elementar e o relevo com uso de espectrometria de fluorescência de raios-X portátil (pXRF), em associação à geomorfologia, para entender tal ocorrência. Os solos estudados estão localizados no município de Muzambinho, Estado de Minas Gerais, Brasil. Perfis de Latossolo foram caracterizados no terço superior (P1), terço médio (P2) e terço inferior (P3) da encosta. Após a descrição morfológica, amostras de solo foram coletadas nos horizontes A, AB e Bw dos perfis. Foram realizadas análises físicas, químicas e espectrométricas dos solos em laboratório. Os teores de Ti e Fe (pXRF) tiveram alta correlação com as frações texturais dos solos. Foram encontrados altos graus de intemperismo-lixiviação dos Latossolos, embora ocorram em encosta íngreme onde solos mais jovens (Cambissolos) seriam esperados. A concordância de altitude dos topos observada nas áreas circundantes mais elevadas indica um paleorrelevo plano, ajudando a explicar esta ocorrência anormal. Os valores dos índices de intemperismo dos solos diminuíram ao longo da encosta, indicando o enriquecimento de sílica por escoamento superficial e fluxo de água subsuperficial nas posições mais baixas da paisagem. As análises de pXRF ajudaram na caracterização destes solos velhos em topografia forte ondulada. O equipamento forneceu bases para confirmação dos seus altos graus de intemperismo, além de detectar evidências do pré-intemperismo do regolito dessa paisagem muito antiga.

ABSTRACT Oxisols are the main soils in Brazil and they classically occur in stable and gentle geomorphic surfaces. However, in the south of Minas Gerais State, Oxisols have been observed under strongly undulated relief, a very rare condition for these soils in this physiographic region. Therefore, this work aimed to assess the elemental dynamics and relief enhanced with portable X-ray fluorescence (pXRF) spectrometry, associated to geomorphology, to understand such occurrence. The studied soils are located in Muzambinho municipality, Minas Gerais State, Brazil. Oxisol profiles were characterized in the upper third (P1), middle third (P2) and lower third (P3) of the hillslope. After morphological description, soil samples were collected in the A, AB and Bo horizons of the profiles. Physical, chemical and pXRF analyses of the soils were carried out in the laboratory. Ti and Fe content (pXRF) had a high correlation with the soil textural fractions. High weathering-leaching degrees were determined, although they occur on a steep slope where younger soils (Inceptisols) would be expected in this region. The altitudinal concordance of summits observed in the more elevated surrounding areas indicates a flat paleorelief, helping to explain this unusual occurrence. The soils’ weathering degree values decreased down the hillslope, indicating silica enrichment through runoff and subsuperficial water flux in the lower landscape positions. The pXRF analyses assisted the characterization of these old soils occurring in steep relief. It provided bases for confirming their high weathering degree indexes and detected evidences of the pre-weathering of the regolith of this very old landscape.

Summary: The synthesis of like-hydrotalcites materials (layered double hydroxides - LDHs) with molecular formula MgxM3+y(CO3)(OH)16·4H2O in different ratios Mg2+/M3+ where M3+ is Al3+, Ga3+ or both was carried out by the coprecipitation method to be applied in the transesterification reactions for synthesis of ethyl biodiesel from soybean oil and ethanol. The reactions were processed for 12 hours at 120 ºC at a molar ratio oil/ethanol (1/20) with 20% (m/m) of the catalyst in relation to the oil mass, and the products were quantified by GC-FID. With the introduction of Ga3+ in the solid, some physicochemical characteristics of LDHs were kept based in the data from X-ray pattern diffraction (XRD), vibrational spectrometry (ATR-FTIR), and scanning electron microscopy (SEM), but changes from thermogravimetric analysis (TGA), superficial area (BET), and the acidity/basicity properties were observed. Typical hydrotalcite with Mg2+/M3+ = 3 was used as reference material and reach 45.1% of biodiesel conversion. Although the best conversion result (77.6%) was reached from the solid without Ga3+ and with Mg2+/M3+ ratio 4/1, there is an interesting correlation between the catalytic activities and the physicochemical properties of the solids with Ga3+ and their respective homologous materials as discussed in this work.

Hydrolysis of albumin (BSA), as a model protein, in 6N HCl inside a PFA screw capped sample vial, was analysed at diferent times by heating in a household microwave oven. The protein hydrolisis reaction times were followed through molecular filtration chromatography, by measuring in a UV monitor at 254 nm, the decreasing in protein and increasing in free amino acids (tyrosine) peak´s absorbances, of the samples eluted from a Sephadex G-25 column. The total hydrolysis of the protein was achieved after 30 minutes and at a half of the nominal power of the microwave oven (approx. 300 W). The method was succesfully applied to the hydrolysis of the protein present in fish meal, as previous preparation of the sample, for later determination of basic amino acids and biogenic amines, by ion exchange chromatography, followed by HPLC

La hidrólisis de albúmina (BSA), utilizada como una proteína modelo, en HCl 6N en el interior de una cápsula de teflón PFA con tapa atornillada, fue analizada a diferentes tiempos de calentamiento en un horno de microondas doméstico. Los tiempos de la reacción de hidrólisis de la proteína fueron seguidos, por cromatografía de filtración molecular, a través de la disminución de la absorbancia, medida en un monitor UV a 254 nm, del peak proteico y aumento de la correspondiente a aminoácidos libres (tirosina), en las muestras eluídas de una columna de Sephadex G-25. La hidrólisis completa de la proteína fue obtenida después de 30 minutos, cuando se utilizó la mitad de la potencia nominal del horno de microondas (aproximadamente 300W). El método fue aplicado satisfactoriamente a la hidrólisis de la proteína presente en harinas de pescado, como preparación previa de la muestra, para determinar posteriormente los aminoácidos básicos y aminas biógenas, por cromatografía de intercambio iónico, seguida de HPLC