BiOCl/KBiO3 p-n heterostructures with hierarchical mesoporous architectures were successfully synthesized via a facile in situ method. The X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and scanning electron microscope (SEM) results indicate the formation of heterojunctions between BiOCl and KBiO3. The photocatalytic performance of the as-prepared samples was investigated by the degradation of dye Rhodamine B (RhB) under visible light irradiation. BiOCl/KBiO3 composite has never been used to photodegrade the RhB which is a common dye and very difficult to degrade. The results demonstrated that KBiO3 combined with proper amount of BiOCl nanosheets exhibited high efficiency in the photocatalytic process, and BiOCl/KBiO3 with the molar ratio of 70/30 demonstrated the highest photocatalytic activity due to its large surface area, excellent charge separation characteristics and the suppressed recombination of electron-hole pairs. The results of active species detection reveal that the superoxide radical anions (O2-), hydroxyl free radicals (·OH), photogenerated holes (h+) and photogenerated electrons (e-) reactive species work together for the photocatalytic degradation of RhB. A possible and new mechanism of photocatalysis that differs from other teams was also explored and proposed. The present study will benefit the development of the new p-n heterojunction photocatalysts and would be of great importance to meet ever-increasing environmental demands in the future. BiOClKBiO3 BiOClKBiO KBiO BiOCl/KBiO pn p n method Xray X ray XRD, XRD , (XRD) XPS (XPS SEM (SEM asprepared as prepared (RhB irradiation degrade process 7030 70 30 70/3 area electronhole hole pairs O2, O2 O (O2-) ·OH, OH ·OH (·OH) h+ h (h+ e (e- proposed everincreasing ever increasing future (XRD 703 7 3 70/ (O2- (·OH (h (e (O2 (O

Efavirenz, an antiretroviral drug, is a class 2 according to the biopharmaceutics classification system. Many dissolution enhancement systems have been tried and our group had success using wet milling to decrease particle size and granules were obtained by spray and freeze drying. In this paper we present data related to the upgrade in the process, raising the solids concentration in the suspension from 10 to 50% (m/v) and changing the drying step for a fluid bed granulation. After that, tablets were obtained. Granules and tablets were fully evaluated and a pharmacokinetic study was also performed with the granules. By powder X-ray diffraction (PXRD) and Fourier transform infrared spectroscopy (FTIR) it was possible to prove that there was no phase transition in the sample after milling and drying. Dissolution efficiency of 4 from 5 granules was higher than 90%, considering 83% for the raw material. Tablets were technically approved but the dissolution was impacted and just 2 out of 11 showed results > 80%. A high enhancement in the bioavailability was also observed, around 172%. So, it is possible to conclude that efavirenz microcrystals with enhanced dissolution and bioavailability can be formulated into tablets and are a viable system to develop a new drug product. Efavirenz process 1 50 m/v mv m v (m/v granulation Xray X ray PXRD (PXRD FTIR (FTIR 90 90% 83 material 80 80% observed 172 172% So product 9 8 17

ABSTRACT In this study, the particle sizes distribution model that best characterizes the granulometric composition of saprolite ores fed to the Cuban Caron process was determined. Three samples of soft and hard streamers from the Punta Gorda, Camarioca Este and Yagrumaje Sur deposits were evaluated. The main mineralogical phases of the samples were identified by the X-ray powder diffraction method. The predominance of the mineralogical phases lizardite, clinochlore and chlorite-serpentine was observed in the different samples under study. The determination of the parameters of the granulometric models and the evaluation of the quality of their adjustment with statistical techniques, allowed us to identify that the Swebrec function is the one that best describes the distribution of the experimental particle sizes of the streamer samples, with determination coefficients higher than 0,91 and residual errors lower than 6,9 %.

RESUMEN En este estudio se determinó el modelo de distribución de tamaños de partícula que mejor caracteriza la composición granulométrica de las menas de saprolitas alimentadas al proceso Caron cubano. Se evaluaron tres muestras de serpentinas blandas y duras concernientes a los yacimientos de Punta Gorda, Camarioca Este y Yagrumaje Sur. Las principales fases mineralógicas de las muestras se identificaron por el método de difracción de rayos X en polvo. Se observó el predominio de las fases mineralógicas lizardita, clinocloro y clorita-serpentina en las diferentes muestras bajo estudio. La determinación de los parámetros de los modelos granulométricos y la evaluación de la calidad de su ajuste con técnicas estadísticas, permitió identificar que la función Swebrec es la que mejor describe la distribución de los tamaños de partículas experimentales de las muestras de serpentinas, con coeficientes de determinación superiores a 0,91 y errores residuales inferiores a 6,9 %.

ABSTRACT In this study, the particle sizes distribution model that best characterizes the granulometric composition of saprolite ores fed to the Cuban Caron process was determined. Three samples of soft and hard streamers from the Punta Gorda, Camarioca Este and Yagrumaje Sur deposits were evaluated. The main mineralogical phases of the samples were identified by the X-ray powder diffraction method. The predominance of the mineralogical phases lizardite, clinochlore and chlorite-serpentine was observed in the different samples under study. The determination of the parameters of the granulometric models and the evaluation of the quality of their adjustment with statistical techniques, allowed us to identify that the Swebrec function is the one that best describes the distribution of the experimental particle sizes of the streamer samples, with determination coefficients higher than 0,91 and residual errors lower than 6,9%.

RESUMEN En este estudio se determinó el modelo de distribución de tamaños de partícula que mejor caracteriza la composición granulométrica de las menas de saprolitas alimentadas al proceso Caron cubano. Se evaluaron tres muestras de serpentinas blandas y duras concernientes a los yacimientos de Punta Gorda, Camarioca Este y Yagrumaje Sur. Las principales fases mineralógicas de las muestras se identificaron por el método de difracción de rayos X en polvo. Se observó el predominio de las fases mineralógicas lizardita, clinocloro y clorita-serpentina en las diferentes muestras bajo estudio. La determinación de los parámetros de los modelos granulométricos y la evaluación de la calidad de su ajuste con técnicas estadísticas, permitió identificar que la función Swebrec es la que mejor describe la distribución de los tamaños de partículas experimentales de las muestras de serpentinas, con coeficientes de determinación superiores a 0,91 y errores residuales inferiores a 6,9%.

This work aims to synthesize the alloy Co64Nb30B6 through mechanical alloying using a planetary ball mill. A disc rotation per minute and a ball/powder weight ratio of 300 rpm and 10:1 were used, with a milled time of 10 h, respectively. The characterization of the Co64Nb30B6 alloy was performed by X-ray diffraction (XRD), examined by scanning electron microscope-energy dispersive X-ray spectroscopy (SEM-EDS), thermoanalytical techniques (TGA/DTA), vibrating sample magnetometer (VSM) and confirmed by Braunauer, Emmet e Teller (BET) method type IV isotherms with a hysteresis loop for mesoporous materials. The results indicated that the evolution of the amorphous phase in the Co64Nb30B6 composition through the mechanical alloying process exhibited good soft magnetic properties with the addition of the metalloid element B and its excellent unique ferromagnetic properties. Through thermoanalytical analysis (TGA/DTA), it was shown that at higher temperatures, Co and Nb ions are oxidized by the environment and, therefore, the mass can be slightly increased to 14.9% and a probable contribution of boron in evolution stability thermal and magnetic in the amorphous phase, respectively. This suggests that the newly developed high-performance amorphous alloy Co64Nb30B6 has great application potential. CoNbB Co64Nb30B mill ballpowder powder 30 101 1 10: used h respectively Xray X ray XRD, XRD , (XRD) microscopeenergy microscope energy SEMEDS, SEMEDS SEM EDS (SEM-EDS) TGA/DTA, TGADTA TGA/DTA TGA DTA (TGA/DTA) VSM (VSM Braunauer BET (BET materials temperatures therefore 149 14 9 14.9 highperformance high performance potential 3 (XRD (SEM-EDS (TGA/DTA 14.

Biodiesel is obtained from the alcoholysis of triglycerides and has been used as a renewable alternative to diesel. Though the methanolysis of triglycerides in the presence of MeONa catalyst has been widely used, searching for alternatives that may improve the competitiveness of the production chain is still a challenge. The aim of this work was to evaluate sodium glyceroxide as a catalyst in the methanolysis of soy oil. Sodium glyceroxide was obtained from glycerol and NaOH in ethanol, and characterized by thermogravimetric analysis (TGA), X-ray powder diffraction (XRD) and, Fourier transform infrared (FTIR) spectroscopy. The transesterification reaction was optimized after two sets of experiments based on the Doehlert matrix experimental design. In the first one, the influence of the molar ratio of methanol/triglyceride, and the amount of catalyst (m/m with respect to the triglyceride) were studied. In the second set, the temperature, and the reaction time were studied. The best conditions were found as 12:1 molar ratio, 2% of catalyst, 50 ºC, and 60 min. The conditions were applied in the transesterification of canola and sunflower oils, and tallow. All the biodiesels were obtained with an ester content superior to 98%, free from methanol and triglycerides. Specific mass, viscosity, and pour point were determined and met the international specifications. diesel challenge oil ethanol TGA, TGA , (TGA) Xray X ray XRD (XRD FTIR (FTIR spectroscopy design one methanoltriglyceride triglyceride methanol/triglyceride m/m mm m studied set temperature 121 12 1 12: 2 5 ºC 6 min oils tallow 98 98% mass viscosity specifications (TGA 9

The reduction kinetics of hematite (Fe2O3) powders was studied using nonequilibrium hydrogen plasma as reducing agent. Reduction experiments were performed in a DC pulsed plasma reactor, hydrogen flow-rate of 300 cm3/min, at pressure of 400 Pa, reduction times in range 30-120 minutes and in temperatures range 320-380 °C. Fe2O3 powders after reduction experiments were characterized by X-ray diffraction, weight loss of oxygen (gravimetric analyses), optic microscope and scanning electron microscope. The results showing that the reduction temperature of 380 °C after 120 min allows obtaining α-iron with a reduction fraction of about 0.93. The powder particles are transformed into two steps: Fe2O3→Fe3O4→Fe-α. The activation energy experimentally established for the reduction of Fe2O3 was about 98.4 kJ/mol. FeO Fe O (Fe2O3 agent reactor flowrate flow rate 30 cm3min cmmin cm3 cm cm3/min 40 Pa 30120 30-12 320380 320 320-38 C Fe2O Xray X ray diffraction gravimetric analyses, analyses , analyses) 38 12 αiron α iron 093 0 93 0.93 steps Fe2O3→Fe3O4→Feα. Fe2O3Fe3O4Feα FeOFeOFeα Fe2O3→Fe3O4→Fe α. Fe3O4 Fe2O3→Fe3O4→Fe-α 984 98 4 98. kJmol kJ mol kJ/mol (Fe2O 3 3012 30-1 32038 32 320-3 1 09 9 0.9 Feα Fe2O3→Fe3O4→Feα Fe2O3Fe3O4Fe FeOFeOFe Fe3O 301 30- 3203 320- 0.

ABSTRACT In this work, the evolution and formation of the amorphous phase during the preparation of amorphous Co67Si23B10 (at.%) powder by mechanical alloying (MA) under an argon atmosphere were studied. The grinding time of 15 h had a profound effect on the phase transformation, microstructure, morphology development, and thermal and magnetic behavior of the powders. These effects were studied by X-ray diffraction (XRD), EDX scanning electron microscopy (SEM), thermal analysis (TGA/DTA), N2 texture analysis (BET/BJH) and, magnetic measurements (VSM). The results show that the evolution of the amorphous phase in the early stage of milling consists of nanocrystalline α-Co2B and β-Co2Si phases, which are diluted and coexist with the amorphous phase. After 15 hours of ball milling, the amorphous phase became the main phase with a proportion of 98.1%, which is relatively high compared to the 1.9% of the nanocrystalline phases α-Co2B and β-Co2Si. The results obtained indicate that amorphization develops with higher thermal stability than a small fraction of the nanocrystalline phase diluted in the amorphous phase. This behavior suggests the presence of the amorphous phase coexisting with the nanocrystalline phase in a small fraction with overlapping crystallization and recrystallization at a temperature of around 924.42°C. work CoSiB Co Si B Co67Si23B1 at.% (at.% MA (MA 1 transformation microstructure development powders Xray X ray XRD, XRD , (XRD) SEM, SEM (SEM) TGA/DTA, TGADTA TGA/DTA TGA DTA (TGA/DTA) N BET/BJH BETBJH BET BJH (BET/BJH VSM. VSM . (VSM) αCo2B αCoB α Co2B βCo2Si βCoSi β Co2Si 981 98 98.1% 19 9 1.9 βCo2Si. Co2Si. 92442C C 924 42 924.42°C Co67Si23B at. (at. (XRD (SEM (TGA/DTA (VSM αCo CoB βCo CoSi 98.1 1. 92 4 (at 98.

ABSTRACT Currently in Brazil, large grain cultivation projects on Plinthosols are a reality, however, there is little or no knowledge of the real mechanism of formation of the plinthite feature, in addition to what is reported in the literature as being a product of oxidation-reduction processes of iron element. This study evaluates iron redoximorphic features and investigates their chemical and mineralogical composition in two profiles of Plinthosols from the Araguaia River plain (P1 and P2). The study strengthens the understanding of the pedogenetic processes involved in the formation of mottles and plinthite. In this sense, it assesses whether the formation mechanisms corroborate the literature. Soil features were sampled in the upper right and left position at the initial plinthic horizon, upper right and left position at the main plinthic horizon, and lower right position at the base horizon of the plinthite zone in the profile. Separated samples comprising the soil matrix, mottles, and plinthite under natural moisture conditions were ground into powder form for chemical determinations by X-ray fluorescence (XRF), sulfuric acid attack (H2SO4), sodium dithionite-citrate-bicarbonate (DCB), and ammonium acid oxalate; and mineralogical determinations by X-ray diffraction. Iron contents in all determined forms were always higher in the plinthite feature, intermediate in the mottle feature, and lower in the soil matrix feature. Most of the Fe in all redoximorphic features is included in the structure of primary minerals and their derivatives (vermiculite, illite, and VHEs). Only part of the iron present (about 35.40 % in P1 and 41.98 % in P2) is detected in the form of oxides such as goethite and hematite, which could be formed in redox processes. The mottle and plinthite features under study are not the product of the classic process of segregation, mobilization, and accumulation of iron as a consequence of redox processes. These features were formed or emerged as a result of a relatively slow and constant weathering process of their source material, which is gradually decomposed in an aqueous medium, releasing most of its components. These components include iron and more mobile elements such as bases and silicon, which leave the system through drainage water, and of which a small part may eventually recombine to form new less complex minerals such as kaolinite and oxides. Brazil reality however feature oxidationreduction oxidation reduction element P (P P2. P2 . sense profile Xray X ray XRF, XRF , (XRF) H2SO4, H2SO4 HSO H SO (H2SO4) dithionitecitratebicarbonate dithionite citrate bicarbonate DCB, DCB (DCB) oxalate diffraction vermiculite, vermiculite (vermiculite illite VHEs. VHEs VHEs) about 3540 35 40 35.4 4198 41 98 41.9 hematite segregation mobilization material medium silicon water (XRF H2SO (H2SO4 (DCB 354 3 4 35. 419 9 41. (H2SO

ABSTRACT The wet beneficiation process of ornamental stone generates waste in the form of sludge that, after drying, becomes a non-biodegradable fine powder. Its improper disposal can lead to various negative environmental impacts. Therefore, new destinations for waste should be evaluated in search of innovation and sustainability. In Brazil, this issue is of particular interest since the country stands out globally as one of the largest producers of ornamental stone, generating significant quantities of waste annually. Thus, mortars with replacement percentages (5, 10, 15, and 20 wt.%) of Portland cement (PC) by ornamental stone waste (OSW) were analyzed as supplementary cementitious material (SCM). The analysis included compressive strength tests, ultrasonic pulse velocity (UPV) at 7- and 28-day curing, X-ray diffraction, and a simplified carbon dioxide (CO2) emissions analysis. The results indicated that the partial replacement of PC by OSW up to 20% resulted in compressive strengths at 28 days statistically equal to the control sample, which can be attributed to the formation of AFm phases. When analyzing the CO2 emissions of the samples, higher substitution percentages were associated with lower reported emissions, reaching a reduction of 61.4% when comparing the 20% replacement with the reference. drying nonbiodegradable non biodegradable powder impacts Therefore sustainability Brazil annually Thus 5, 5 (5 10 15 2 wt.% wt (PC (OSW SCM. SCM . (SCM) tests UPV (UPV 7 28day day curing Xray X ray diffraction CO (CO2 sample phases samples 614 61 4 61.4 reference ( 1 wt. (SCM (CO 6 61.

ABSTRACT The application of rock dust (RD) in agricultural soils has shown the capacity to improve soil conditions for plant growth. However, the successful use of RD requires understanding its effects on weathering in soil surfaces and its possible products. In this study, we present the results of an exploratory test in which a RD had its weathering intensified in a soil column by temperature (45 °C) and intense leaching (1,339.2 mm in 24 weeks), in the absence of plants. There was a significant increase in amorphous phases of iron (Fe) and particularly of aluminum (Al) to the amount of 0.13 g kg –1 for Fe and 0.16 g kg –1 for Al in the 0-0.05 m layer of the column and 0.22 g kg –1 for Al in the 0.05-0.10 m layer. These values account for 6 % of the total Fe, and 27 % of the total Al added as RD in the column. Spectral features in the visible-near infrared-short wave infrared (VIS-NIR-SWIR) and mid-infrared (MIR) range, as well as X-ray diffraction (XRD) scans, were inconclusive because of the small signal-noise ratio of the newly precipitated phases. Selective chemical methods targeted to specific soil pools (precipitated, adsorbed, and leached) were more sensitive to capture the new amorphous phases resulting from the RD dissolution. This study contributes to understanding the effects of RD on the availability of ions and the possibility of amorphous oxides precipitating in the soil. In addition, it helps identify other effects associated with using RD, such as changes in the pH, cation exchange capacity (CEC), and nutrient availability. (RD growth However products 45 (4 °C C 1,339.2 13392 1 339 2 (1,339. weeks, weeks , weeks) plants (Fe (Al 013 0 13 0.1 – 016 16 00.05 0005 0.05 05 0-0.0 022 22 0.2 0.050.10 005010 0.10 10 0.05-0.1 visiblenear visible near infraredshort short VISNIRSWIR VIS NIR SWIR (VIS-NIR-SWIR midinfrared mid MIR (MIR range Xray X ray XRD (XRD scans signalnoise signal noise precipitated, (precipitated adsorbed leached dissolution addition pH CEC, CEC (CEC) 4 ( 1,339. 1339 33 (1,339 01 0. 00 00.0 000 005 0.0 0-0. 02 050 0.050.1 00501 010 0.05-0. (CEC 1,339 133 3 (1,33 00. 0-0 0.050. 0050 0.05-0 1,33 (1,3 0- 0.050 0.05- 1,3 (1, 1, (1

Abstract The pharmaceutical industry is mostly dedicated to the production of drugs in solid forms such as tablets and capsules with active ingredients and excipients in the same physical state. Regarding the regulatory requirements for the analytical development and implementation of solid-state analyses, internationally recognized pharmaceutical compendia play an important role. However, the information contained in the various general chapters and monographs differs from each other, especially in countries that have national pharmacopeias, such as Brazil. Thus, the main objective of this work is to critically evaluate, based on the technical-scientific literature, the harmonization of the United States, European, British, Japanese and Brazilian pharmacopeias with respect to the following analytical techniques used for solid-state characterization: X-ray powder diffraction, differential scanning calorimetry, thermogravimetric analysis, and infrared and Raman spectroscopies. The working principle of each analytical technique, as well as the methodological parameters that impact the implementation of the analyses, are detailed. The results indicate that, in terms of solid-state characterization analysis, the adoption of unified scientific standards and principles is not yet a reality for all compendia. Additionally, the lack of harmonization between BrazP and the other compendia is especially significant, considering that ANVISA is an ICH member, the main entity responsible for promoting harmonization. state solidstate analyses role However Brazil Thus evaluate technicalscientific technical literature States European British Xray X ray diffraction calorimetry analysis spectroscopies technique detailed Additionally significant member

ABSTRACT Autoclaved Aerated Concrete (AAC) developed with Coconut Shell Charcoal (CSC) powder is a newly developed concrete with reasonable compressive strength and durability properties. The main idea of this study is to find out the applicability of CSC powder as partial replacement for fine aggregate in AAC, and the role of CSC in obtaining the strength and durability of AAC are discussed. In this study, material selection is done with reference to ASTM C1693-11 and CSC was used as a replacement material for river sand. CSC is an agricultural waste. Since the SiO2 content of CSC is very low, Silica Fume (SF) is also used as fine aggregate replacement in addition to CSC to enhance the SiO2 content. The specimens were made combining CSC and SF powders; CSC at 0%, 5%, 10%, 15% and 20% and SF at 0%, 1%, 2%, 3% and 4% by weight, and are coded as B0, B5, B10, B15 and B20 respectively. The developed AAC was analysed by conducting compressive strength, bulk density, thermal conductivity, scanning electron microscope (SEM) and X-ray diffraction (XRD) analyses. Additionally, water absorption, porosity, ultrasonic pulse velocity and acid attack tests were performed to determine the durability. XRD analysis showed the traces of C-S-H (Calcium Silicate Hydrate) gel and tobermorite peaks in B5 specimen, which produced enhanced compressive strength of 3.12 N/mm2. Thermal conductivity of the specimen with CSC replacement was between 0.218 to 0.186 W/m-K; it could be remarked from the results that the developed AAC is good in thermal insulation. Even though the porosity level reduced to 2% in B20 replacement, the specimens were light in weight, compared to B0. From the results obtained, it could be drawn the inference that CSC is a potential replacement for fine aggregate in AAC. (AAC (CSC properties discussed C169311 C C1693 11 C1693-1 sand waste SiO low (SF powders 0 0% 5 5% 10 10% 15 20 1 1% 2 3 4 weight B0 B B10 B1 B2 respectively density SEM (SEM Xray X ray (XRD analyses Additionally absorption CSH S H Calcium Hydrate 312 12 3.1 Nmm2 Nmm N mm2 mm N/mm2 0218 218 0.21 0186 186 0.18 W/mK WmK W/m K W m W/m-K insulation obtained C16931 C169 C1693- 31 3. N/mm 021 21 0.2 018 18 0.1 mK Wm C16 02 0. 01 C1

The extraction and processing of ornamental rocks generate a very significant amount of waste, representing an environmental and public health problem. The residue is a fine-grained compound by rock powder and inputs used in the processing process have a potential economic value. The present study was carried out to evaluate the efficiency of the waste generated in the discoloration of an aqueous solution containing methylene blue dye, such as alternative for treating textile effluents. The samples were characterized by X-ray diffraction, inductively coupled plasma optical emission spectroscopy, scanning electron microscopy, transmission electron microscopy and energy dispersive X-ray spectroscopy. The catalytic properties of the samples were evaluated in the Fenton and photo Fenton reactions at pH 3 and natural pH. The best decolorization efficiency (≈ 95%) was achieved using the GRM catalyst at pH 3, after 5 min of photo Fenton reaction. Importantly, owing to its excellent structural and chemical stability, the samples showed a decolorization efficiency above 95% after 5 consecutive cycles of 30 min of reaction. This innovative strategy not only offers a new prospect for the rational disposal of abrasive mud waste, but also contributes to minimizing environmental impacts, promoting sustainable development in the stone industry. problem finegrained fine grained value dye effluents Xray X ray diffraction spectroscopy ≈ ( 95 reaction Importantly stability impacts industry 9

Abstract In Brazil, a significant amount of tilapia carcass waste is produced every year. The aim of this study is to evaluate the recycling of tilapia carcass waste as an alternative calcium precursor to produce biphasic calcium phosphate (BCP) powder via a wet chemical precipitation method in different HNO3 concentrations. The synthesized powders were characterized by X-ray diffraction, scanning electron microscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy, average crystallite size, and refinement by the Rietveld method for the quantification of crystalline phases. The experimental results indicated the formation of a BCP bioceramic with different amounts of β-calcium pyrophosphate (β-CPP) and β-tricalcium phosphate (β-TCP), depending on the HNO3 concentration. The new BCP powders showed an average crystallite size between 57.7 and 59.2 nm. Such a result suggests a possibility of friendly recycling of tilapia carcass waste for biomedical applications. Brazil year (BCP HNO concentrations Xray X ray diffraction microscopy analysis spectroscopy phases βcalcium β βCPP CPP (β-CPP βtricalcium tricalcium βTCP, βTCP TCP , (β-TCP) concentration 577 57 7 57. 592 59 2 59. nm applications (β-TCP 5