RESUMO O intemperismo de alguns minerais silicáticos em rochas moídas pode ocorrer em alguns dias de cultivo e gerar diferentes propriedades físico-químicas, com benefícios potenciais a solos tropicais. Objetivou-se investigar a infuência da rizosfera do milho (Zea mays L.) nos produtos do intemperismo e na capacidade de troca de cátions da biotita-Mg da biotita xisto e biotita-Fe da biotita sienito. Um experimento em vasos foi conduzido de forma que plantas e rochas moídas foram avaliadas por sete ciclos de cultivo sucessivos. Os nutrientes ferro e potássio foram adquiridos da biotita xisto e da biotita sienito durante o cultivo. O intemperismo das biotitas promovido pela rizosfera causou mudanças mineralógicas. A mudança mais expressiva nos padrões da difração de raios-X ocorreu na fração com partículas < 53 µm, mas as frações 53-300 µm também mudaram. A alteração na biotita-Mg, que possui menor relação Fe/Mg nos sítios octaedrais que a biotita-Fe, foi responsável pelo maior aumento na capacidade de troca de cátions nas frações < 300 µm. Entretanto, o processo de intemperismo da biotita-Fe, a qual apresenta alta relação Fe/Mg nos sítios octaedrais, não aumentou a capacidade de troca de cátions.

ABSTRACT The weathering of some silicate minerals in crushed rocks may occur in a few days of cropping and generate different physicochemical properties, with potential benefits to tropical soils. This study aimed to investigate the infuence of maize (Zea mays L.) rhizosphere on the weathering products and on the cation exchange capacity of Mg-biotite from biotite schist and Fe-biotite from biotite syenite. An experiment was carried out in pots, so that plants and crushed rock materials could be evaluated during seven successive growth cycles. The nutrients iron and potassium were taken up from biotite schist and biotite syenite during cropping. The weathering of both biotites promoted by the rhizosphere caused mineralogical changes. The most expressive change in the X-ray diffraction patterns occurred in the < 53 µm particle size fraction; however, the 53-300 µm fractions also changed. The alteration in the Mg-biotite, which has a lower Fe/Mg relation in octahedral sites than the Fe-biotite, was responsible for the most expressive cation exchange capacity increase in the fractions < 300 µm. However, the Fe-biotite weathering process, which presents a higher Fe/Mg relation in octahedral sites, did not increase the cation exchange capacity.

Abstract In the bentonite industry - exploration and beneficiation - ore quality control has been traditionally carried out using the swelling parameter, denominating those that swell as naturally sodium bentonites and those that do not as naturally non-sodium bentonites. However, the properties of the bentonites can vary due to the quantity and cationic type of montmorillonite. The variation in those properties cannot always be predicted, because there is still no consolidated and convenient method for clays mineralogical quantification. A quantification via PXRD using the Rietveld method is only reliable when all the crystalline structures of the mineral phases are known. This is not the case for bentonites, since the montmorillonite shows turbostratic disorder that leads to extremely wide and asymmetric non-basal reflections that are not considered in the available structural models. Thus, in this work, is generate a calibrated hkl model for a Brazilian montmorillonite applying the combined Rietveld-Le Bail-Internal Standard method developed by Paz et al. (2018). The study concluded that the combined method is a good choice for the mineralogical quantification of the bentonites, handling turbostratic disorder of montmorillonite, since the develop hkl phase model showed good results in mixtures with >50% montmorillonite content (greater precision and reproducibility).

The waste from the processing of kaolin in the Amazonian region of Brazil was subjected to a calcination process at 700°C for 2 h to obtain metakaolin, which, together with sodium hydroxide and sodium silicate, formed the reaction mixture. This mixture was subjected to an aging step (24 h at 60 rpm), and a subsequent hydrothermal process at 110°C for 10 h. By means of X-ray diffraction (XRD), differential thermal and thermogravimetric analysis (DTA/TG) and scanning electron microscopy (SEM) techniques, the crystallization of a single phase, faujasite (FAU) zeolite, was observed. In the postsynthesis process, it was verified by means of XRD that the thermal stability of this structure persists up to a temperature of 600°C. At 800°C, the structure of FAU collapses. Beginning at 850°C, new nepheline phases are formed, and at 1000°C, nepheline and mullite phases are formed.

Resumo O muiraquitã é um artefato arqueológico raro e característico das sociedades pré-coloniais do baixo Amazonas e de área circum-caribenha. Foi confeccionado por meio de diversos tipos de minerais, sendo os mais conhecidos os de pedra verde, sobretudo a nefrita. Embora sua função ainda seja desconhecida, a literatura etnográfica e arqueológica sugere que estes objetos conotavam símbolos de poder, haja vista a ampla rede de circulação em que estavam inseridos. Este artigo descreve um muiraquitã encontrado na estearia da Boca do Rio, região das estearias maranhenses. As análises foram feitas por MicroRaman, com auxílio do equipamento de bancada BWTEK, da GemExpert, difração de raios X (DRX), evidenciando que o artefato foi confeccionado em tremolita/actinolita, um mineral inexistente no Maranhão. Propõe-se uma possibilidade acerca da cadeia operatória do artefato e analisam-se as possíveis redes regionais de interação comercial e simbólica nas quais este muiraquitã esteve envolvido.

Abstract The muiraquitã is a rare and characteristic archaeological artifact of the Lower Amazon and Circum-Caribbean precolonial societies. It used to be made of various types of minerals, of which the best known are green stones, especially nephrite. Although its function is still unknown, ethnographic and archaeological literature suggests that these objects represented symbols of power, given the wide circulation network in which these artifacts were inserted. This article describes a muiraquitã found in the dwelling at Boca do Rio. The methods used in this analysis were MicroRaman together with BWTEK GemExpert and X-ray diffraction (XRD), which showed that the artifact was made of tremolite/actinolite, a mineral lacking in Maranhão. A possible operational sequence in the manufacture of the muiraquitã is proposed, as well as the possible regional networks to which it belonged.

RESUMO As bauxitas metalúrgicas da região de Paragominas-PA (norte do Brasil) comumente apresentam uma alta quantidade de caulinita. Durante a lixiviação da bauxita nas condições de processo Bayer, este mineral reage com NaOH formando indesejavelmente sodalita, o qual é insolúvel e, portanto, descartada com o resíduo sólido, causando significativa perda do agente lixiviante. Neste trabalho foi dada a atenção a dois tipos principais de sodalita formadas em função de diferenças na concentração caustica e tempo de reação. Assim, o processo hidrotérmico foi conduzido em temperatura de 150 °C, concentração caustica variando de 2,5 à 5,0 M e tempo variando de 60 à 420 min. Os resultados mostraram que estas variáveis afetam tanto a velocidade da transformação da caulinita em sodalita como a cristaloquímica desta fase, resultando na formação de dois tipos de sodalita: 1) sodalita básica tetrahidratada, fase mais estável formada inicialmente e remanescente em todas as condições do processo; e 2) hidrosodalita, a qual é a fase secundária, menos estável e observada apenas nas condições intermediárias. Esta última fase é mais desejável no contexto Bayer devido a menor quantidade de NaOH consumida. Observou-se que o favorecimento da formação desta fase depende de maiores tempos, concentração caustica e quantidade de caulinita.

ABSTRACT Metallurgical bauxites from Paragominas-PA region (northern Brazil) commonly exhibit high amounts of kaolinite. During caustic leaching of bauxite in the Bayer process conditions, this mineral reacts with NaOH and undesirable sodalite is formed, which is insoluble and therefore discarded with the solid residue, causing significant losses of the leaching agent. In the present work, an attention was given to two main types of sodalite formed as function of differences in caustic concentration and residence time. Thus, the hydrothermal process was carried out at temperature of 150 °C, caustic concentration ranging from 2.5 to 5.0 M and time varying from 60 to 420 min. Results showed that these variables affect both the speed of kaolinite to sodalite transformation as the crystal chemistry of the two main types of sodalite phases formed: 1) tetrahydrate basic sodalite, which is the more stable phase initially formed and that remains during all process conditions; and 2) hydrosodalite, which is the secondary phase, less stable and observed only in intermediate conditions. This last phase is more desirable in the Bayer context due the less amount of NaOH consumed. The favoring of this phase formation depends on the long time, caustic concentration and the amount of kaolinite.

Os monumentos históricos de Belém, PA, têm alvenarias estruturais constituídas de pedras e tijolos maciços assentados com argamassa de cal e podem apresentar diversas patologias, entre as quais se destacam a eflorescência salina e a ação da umidade. Alguns autores explicam que esses dois agentes ocasionam destacamento de camadas, pulverização de argamassa, surgimento de fissuras e aparência esbranquiçada. A pesquisa teve como principal objetivo identificar o processo de degradação atuante na alvenaria do transepto direito da Igreja de Santo Alexandre por meio da aplicação de técnicas instrumentais analíticas. Foram realizadas análises laboratoriais com o intuito de entender as condicionantes favoráveis ao processo de eflorescência salina, os danos provocados aos materiais e os tipos de sais mais atuantes. Primeiramente foi realizado o mapeamento da alvenaria e o mapeamento de danos, verificando a situação atual e as áreas mais degradadas. Posteriormente, foi realizada a caracterização física por meio de análise granulométrica, análise de traço e análise do teor de umidade da alvenaria, a caracterização química - teste qualitativo e quantitativo de sais - e a caracterização mineralógica por difração de raios X. Verificou-se que as técnicas aplicadas se mostraram eficientes e auxiliaram no diagnóstico correto, norteando quais intervenções devem ser utilizadas para amenizar a problemática.

The structural masonry of the historical monuments of the city of Belém, Brazil, is made of stones and solid bricks fixed with lime mortar, which is affected by different pathologies, including salt efflorescence and moisture action. Some authors explain that these two agents cause layer detachment, mortar pulverization, cracks and a whitened appearance. This aim of this study was to identify the degradation process affecting the masonry of the right transept of the Church of Santo Alexandre, using instrumental analytical techniques. Laboratory analyses were used in order to understand the saline efflorescence process, the material damage it causes and the main kinds of salts. The first step in the study was to map out the masonry and the damage, showing the current situation and the most damaged areas. That was followed by a physical characterisation through an analysis of mortar particle sizes and proportions, analysis of masonry moisture contents, chemical characterisation -qualitative and quantitative chemical analysis of soluble salts, and mineralogical characterisation by X-ray diffraction. The techniques applied were effective and contributed to the achievement of a correct diagnosis, guiding the type of interventions required to solve the problem.

The synthesis of zeolite NaP using kaolin waste, from the Amazon region, as a predominant source of silicon and aluminum has been studied. The zeolitisation process occurred in hydrothermal conditions using static autoclaving and the effects of time, temperature, and the Si/Al ratio were investigated. The starting material and the phases formed as reaction products were characterized by XRD, SEM and FTIR. The results showed that pure zeolite NaP is hydrothermally synthesized, at 100 °C for 20 hours, using metakaolin waste material in alkaline medium in presence of additional silica. The XRD and SEM analyses indicate that the synthesized zeolite presents good crystallinity.

Ultramarine pigments were successful synthesized from zeolite A obtained from kaolin waste. This waste has been used as an excellent source of silicon and aluminum for zeolite synthesis because of its high kaolinite concentrations and low contents of other accessory minerals. The cost is naturally less than the industrialized product. Color additives (Sulfur and Sodium Carbonate) were mixed with different proportions of zeolite A and further calcined for 5 h at 500 °C. They were characterized by XRD and XRF in addition to visual classification by color and shade. These products show colors from blue to green at different shades, both influenced by the amount of additives and cooling rate after calcination. Thus, a different quantity of the same additives in the same zeolitic matrix provides an increase in the color intensity. Cooling rate after calcination induces the color change which is substantially important in the pigments production.

O uso adequado de pozolanas possibilita a produção de cimentos especiais, de menor custo de fabricação e de maior durabilidade que os correspondentes sem adição. O emprego dessas adições minerais possibilita ganhos significativos em termos de produtividade e uma extensão da vida útil dos equipamentos de produção e da própria jazida de calcário, também ajudando na diminuição de CO2 lançado na atmosfera.As zeólitas têm sido utilizadas como material pozolânico em misturas com "terras vulcânicas" e água nas construções desde o tempo do antigo Império Romano. Nos dias atuais, existem muitas discussões envolvendo reatividade pozolânica das zeólitas naturais na incorporação dos cimentos Portland.Na Região nordeste do Brasil, zeólitas sedimentares relacionadas a arenitos da Bacia do Parnaíba foram descobertas pelo Serviço Geológico do Brasil nos anos 2000. Estes arenitos são constituídos em sua maioria de quartzo, zeólitas naturais (estilbita) e argilominerais (esmectita). Estudos preliminares constataram que este arenito pode ser empregado como material pozolânico em sistemas a base de cimento Portland, desde que o material seja peneirado para remoção do quartzo e ativado termicamente, uma vez que a estilbita é uma zeólita de baixa atividade pozolânica.O objetivo geral desse trabalho foi determinar qual proporção de arenito zeolítico ativado termicamente proporciona melhores propriedades mineralógicas e mecânicas ao cimento Portland.No programa experimental empregou-se o arenito zeolítico passante na peneira 200# e calcinado à temperatura de 500ºC. A análise química das amostras foi realizada por espectroscopia de fluorescência de raios-x e a caracterização mineralógica por difração de raios-x e análise termogravimétrica e termodiferencial. O comportamento da hidratação dos cimentos foi avaliado através de calorimetria de condução, difratometria de raio-X e análises termodiferencial e termogravimétricas. Para avaliação da atividade pozolânica foi adotado um ensaio mecânico de resistência à compressão em argamassas cimento Portland (CP I -S) e areia, com percentuais de substituição de cimento por arenito de 10, 20 e 30%.Os resultados mostraram que o arenito zeolítico calcinado com a percentual de substituição de 10% proporcionou às argamassas melhor resultado tem termos de resistência à compressão simples, contudo estudos mais aprofundados de durabilidade e a idades mais avançadas podem indicar que teores mais elevados do arenito zeolítico podem também ser apropriados para a produção de concretos, principalmente em obras de infraestrutura como barragens, canais, entre outras.

The proper use of pozzolans enables the production of special cements with lower manufacturing cost and higher durability in comparison with cements without mineral additions. It also enables significant gains in productivity and in equipment service life in the factory as well as reduce the CO2 emission into the atmosphere.Zeolites have been used as pozzolanic material in mixtures with Fuller's Earth and water in buildings from the ancient Roman Empire. Nowadays, there are many discussions involving pozzolanic reactivity of natural zeolites in the incorporation to Portland cement.In the Northeastern region of Brazil, sedimentary zeolites related to sandstones of the Parnaiba Basin were discovered by the Geological Survey of Brazil in the 2000s. These sandstones are mainly composed by quartz, natural zeolites (estilbity) and clay (smectite). Preliminary studies have pointed that this sandstone may be used as pozzolanic material in Portland cements. The material must be previously grinded to remove quartz and thermally activated, since stilbite is a zeolite with low pozzolanic activity.The aim of this study was to evaluate the ideal amount of thermally activated zeolitic sandstone to be incorporated in the Portland cement in order to improve its mechanical and mineralogical properties.In the laboratory, the < # 200 fraction of the zeolitic sandstone was calcined at 500 º C. Chemical and miner-alogical analysis were carried out by X-ray fluorescence spectroscopy (XRF) and X-ray Diffractometry (XRD), respectively. The hydration behavior of the cements was evaluated using heat-flow calorimetry, besides thermal analysis and XRD. To evaluate the physical properties, mechanical testing of compressive strength in cement mortar Portland with different proportions of sandstone was carried out.The results showed that the AZ2-3 zeolitic sandstone with the proportion of 10% incorporated in Portland cement type CPI-S, showed the best result of compressive strength and mineralogical properties of the samples suitable for the production of CPII-Z type commercial cement.

In this work, a method was developed for the application of red mud, an alkaline leaching waste, from a bauxite processing plant located in northern Brazil (Amazon region) as starting material for heavy clay products. Samples were prepared by pressing blends of red mud and clay, which were then fired at temperatures from 900 ºC to 1190 ºC. Characterization was carried out by chemical analysis, differential thermal analysis (DTA) and X-ray diffraction (XRD), and the following ceramic properties were evaluated: water absorption, linear shrinkage and flexural strength. In order to evaluate the Na+ stability in the dense ceramic, leaching tests were also carried out on the specimens after sintering process. Results indicated that samples with 50 and 70 wt% of red mud are proper for being used in the production of ceramic bodies, due to its excellent properties, mainly high mechanical resistance and low water absorption, showing thus, an option to minimizing the environmental impacts caused by the aluminum industry.

Calcium aluminate cements (CAC) were prepared using the sonochemical process, followed by heat treatment. A study was made of the action of ultrasonic waves and the influence of thermal treatment conditions on two initial molar compositions of 1:1 and 1:2 of calcia:alumina. The aqueous suspension containing the raw materials (A-50 alumina and CaO) was subjected to an ultrasonic bath, followed by drying and burning at 1000, 1200 and 1300 ºC. These cements were characterized by SEM, XRD and the mechanical strength was evaluated by splitting tensile tests, using commercial cement as a reference. Furthermore, the phases were semi-quantified using the Rietveld method. The results show that hydration and sonochemical action increased the reactivity of the raw materials during firing and that phase formation is dependent on the thermal treatment conditions. The CAC cements were obtained at temperatures at least 200 ºC lower than those used in conventional methods, indicating the potential of this route of synthesis.

Trace element concentrations were measured in atmospheric particulate matter collected in 2009 and 2010, in a Brazilian region influenced by pre-harvest burning of sugar cane crops. For coarse particles, high concentrations of Al, Fe, K and Ca suggested that re-suspended soil dust was the main source of aerosol trace elements, subsequently confirmed by XRD analysis. High levels of K, Zn, As, Cd and Pb were found in fine particles, confirming the contribution of biomass burning and vehicle emissions, whereas Na, Al, K, Fe and Zn were the representative elements in ultrafine particles, influenced by a diversity of sources.

Nesse trabalho, foram caracterizadas algumas argilas coletadas nos municípios de São Luís, Rosário, Pinheiro e Mirinzal. A caracterização foi realizada através dos ensaios de difração de raios X, massa específica real, capacidade de troca de cátions (CTC), área superficial, distribuição granulométrica, análise química, análise térmica (TG-DTA) e limites de Atterberg. Ensaios tecnológicos de retração linear, antes e após a queima, absorção de água e tensão de ruptura a flexão, em três pontos, foram realizados em corpos de prova prensados uniaxialmente a 20 MPa e tratados termicamente em 850, 950, 1050, 1150 e 1250ºC. Os resultados obtidos permitiram identificar duas argilas de queima branca, constituídas de quartzo, caolim, feldspato e anatásio, com excelentes propriedades para uso em cerâmica branca. As restantes são queima vermelha e possuem composição mineralógica de quartzo, caolim, feldspato, montmorilonita, hematita e goetita. Estas últimas apresentaram valores moderados de plasticidade e são adequadas para aplicações em cerâmica vermelha.

This work involved the characterization of clays collected in the municipalities of São Luis, Rosário, Pinheiro and Mirinzal (state of Maranhão, Brazil), based on specific mass, specific surface area, cation exchange capacity (CEC), particle size distribution, X-ray diffraction (XRD), differential thermal analysis (DTA), thermogravimetric analysis (TG-DTA) and Atterberg limits. Technological tests for ceramic applications were also carried out on compacts pressed under 20 MPa and heat-treated at 850, 950, 1050, 1150 and 1250ºC. Our results indicated that two of the clays composed of kaolinite, quartz, and anatase with high plasticity limits, have excellent properties and can be used in the whiteware industry. The other ones are red-firing clays and have a mineralogical composition of quartz, kaolin, feldspar, montmorillonite, hematite and goethite. The latter showed low and moderate values of plasticity, which makes them suitable for the production of heavy clay products.

No nordeste do Brasil, existe a ocorrência de zeolitas sedimentares relacionadas a arenitos, descoberta nos anos 2000. Esses arenitos são constituídos de quartzo, zeolitas naturais (estilbita) e argilominerais (esmectita). Estudos preliminares constataram que esse arenito pode ser empregado como material pozolânico em sistemas à base de cimento Portland, desde que o material seja peneirado para remoção do quartzo e ativado termicamente, uma vez que a estilbita é zeolita de baixa atividade pozolânica. O objetivo geral desse trabalho foi determinar qual a fração granulométrica que proporciona a maior concentração de zeolita e esmectita e a temperatura de calcinação que acarreta a maior atividade pozolânica. No programa experimental, empregou-se o arenito zeolítico passante nas peneiras #200 e #325 e calcinado às temperaturas de 150ºC, 300ºC e 500ºC. A análise da caracterização mineralógica das amostras peneiradas foi realizada por difração de raios X, por análises termogravimétrica e termodiferencial. Para avaliação da reatividade, foram realizados ensaios mecânicos de atividade pozolânica em argamassas de cal hidratada e cimento Porltand. Os resultados mostraram que a amostra peneirada na peneira #200 foi a mais adequada porque apresentou elevada concentração de estilbita e um percentual maior de material passante em comparação a amostra da peneira #325, 15% e 2% respectivamente. A temperatura de calcinação de 500ºC foi a que proporcionou a maior atividade pozolânica, em razão da modificação mais efetiva da estrutura cristalina, tanto da estilbita, como da esmectita. As temperaturas mais moderadas a 150ºC e 300ºC não foram suficientes para a obtenção dos mesmos resultados. As argamassas com o arenito passante na peneira #200 e calcinado a 500ºC atingiram os valores limites mínimos exigidos para que um material seja considerado pozolânico, no caso, 6 MPa para argamassas de cal hidratada e 75% para o índice de atividade pozolânica (IAP).

In northeastern Brazil, sedimentary zeolites occur associated with sandstones of the Corda Formation (Parnaiba Paleozoic Basin), discovered in the 2000s. These sandstones are composed of quartz, natural zeolites (estilbite) and clay minerals (smectite). Preliminary studies have shown that this sandstone can be used as a pozzolanic material in Portland-cement-based systems after the material has been sieved to remove the quartz and after thermal activation because the estilbite has low pozzolanic activity. The main objective of this study was to determine the best particle size distribution that yields the highest smectite and zeolite concentration, besides the best temperature for higher pozzolanic activity. The experimental program employed the zeolitic sandstone passing through a #200 and #325 mesh sieve and calcination at the following temperatures: 150°C, 300°C and 500°C. Chemical analysis of the sieved samples was carried out by X-ray fluorescence spectroscopy and X-ray diffractometry, while mineralogical characterization was done by X-ray and thermogravimetric analysis and thermogravimetry..To assess reactivity, calorimetry driving and mechanical tests for pozzolanic activity in hydrated lime and cement Porltand were performed. The results showed that the sample sieved through at #200 mesh was the most suitable because it had a higher concentration of estilbite and a higher percentage of material seived compared to the sample sieved at #325 mesh, 15% and 2% respectively. The 500°C calcination temperature was accompanied by increased pozzolanic activity due to changes in estilbite and smectite cristalinity; the more moderate temperatures of 150°C and 300°C were not sufficient to achieve similar results. The mortars with sandstone sieved at #200 mesh and calcinated at 500°C reached the minimum limits required for a material to be considered as pozzolanic, i.e, 6 MPa for hydrated lime mortars and 75% for the pozzolanic index activity (PAI).

Basic sodalite was successfully synthesized by hydrothermal method using kaolin waste as source of Aluminum and Silicon. This waste is mainly composed by kaolinite and is produced in large amount by kaolin processing industries for paper coating from the Amazon region. Initially, the waste has been calcined at 700 ºC for 2 h and then reacted with the following solutions: Na2CO3 and mixture of Na2CO3 + NaOH to 150 ºC with autogenous pressure for 24 h. The raw materials and transformed materials were characterized by XRD, FTIR and SEM. In both studied media, well-crystallized, basic sodalite was the only phase synthesized, while in the literature usually a mixture of zeolites is obtained.