Desenvolvimento de uma unidade laboratorial para quantificação de BTX como poluentes atmosféricos, usando microextração em fase sólida

This dissertation aims the development of an experimental device to determine quantitatively the content of benzene, toluene and xylenes (BTX) in the atmosphere. BTX are extremely volatile solvents, and therefore play an important role in atmospheric chemistry, being precursors in the tropospheric ozone formation. In this work a BTX new standard gas was produced in nitrogen for stagnant systems. The aim of this dissertation is to develop a new method, simple and cheaper, to quantify and monitor BTX in air using solid phase microextraction/ gas chromatography/mass spectrometry (SPME/CG/MS). The features of the calibration method proposed are presented in this dissertation. SPME sampling was carried out under non-equilibrium conditions using a Carboxen/PDMS fiber exposed for 10 min standard gas mixtures. It is observed that the main parameters that affect the extraction process are sampling time and concentration. The results of the BTX multicomponent system studied have shown a linear and a nonlinear range. In the non-linear range, it is remarkable the effect of competition by selective adsorption with the following affinity order p-xylene > toluene > benzene. This behavior represents a limitation of the method, however being in accordance with the literature. Furthermore, this behavior does not prevent the application of the technique out of the non-linear region to quantify the BTX contents in the atmosphere.

Análise gráfica de estruturas porosas sobre a ótica da estereologia

In this work we developed a computer simulation program for physics porous structures based on programming language C + + using a Geforce 9600 GT with the PhysX chip, originally developed for video games. With this tool, the ability of physical interaction between simulated objects is enlarged, allowing to simulate a porous structure, for example, reservoir rocks and structures with high density. The initial procedure for developing the simulation is the construction of porous cubic structure consisting of spheres with a single size and with varying sizes. In addition, structures can also be simulated with various volume fractions. The results presented are divided into two parts: first, the ball shall be deemed as solid grains, ie the matrix phase represents the porosity, the second, the spheres are considered as pores. In this case the matrix phase represents the solid phase. The simulations in both cases are the same, but the simulated structures are intrinsically different. To validate the results presented by the program, simulations were performed by varying the amount of grain, the grain size distribution and void fraction in the structure. All results showed statistically reliable and consistent with those presented in the literature. The mean values and distributions of stereological parameters measured, such as intercept linear section of perimeter area, sectional area and mean free path are in agreement with the results obtained in the literature for the structures simulated. The results may help the understanding of real structures.

Pirólise termoquímica de pós da fibra de coco seco em um reator de cilindro rotativo para produção de bio-óleo

This master thesis aims at developing a new methodology for thermochemical degradation of dry coconut fiber (dp = 0.25mm) using laboratory rotating cylinder reactor with the goal of producing bio-oil. The biomass was characterized by infrared spectroscopy with Fourier transform FTIR, thermogravimetric analysis TG, with evaluation of activation energy the in non-isothermal regime with heating rates of 5 and 10 °C/min, differential themogravimetric analysis DTG, sweeping electron microscopy SEM, higher heating value - HHV, immediate analysis such as evaluated all the amounts of its main constituents, i.e., lignin, cellulose and hemicelluloses. In the process, it was evaluated: reaction temperature (450, 500 and 550oC), carrier gas flow rate (50 and 100 cm³/min) and spin speed (20 and 25 Hz) to condensate the bio-oil. The feed rate of biomass (540 g/h), the rotation of the rotating cylinder (33.7 rpm) and reaction time (30 33 min) were constant. The phases obtained from the process of pyrolysis of dry coconut fiber were bio-oil, char and the gas phase non-condensed. A macroscopic mass balance was applied based on the weight of each phase to evaluate their yield. The highest yield of 20% was obtained from the following conditions: temperature of 500oC, inert gas flow of 100 cm³/min and spin speed of 20 Hz. In that condition, the yield in char was 24.3%, non-condensable gas phase was 37.6% and losses of approximately 22.6%. The following physicochemical properties: density, viscosity, pH, higher heating value, char content, FTIR and CHN analysis were evaluated. The sample obtained in the best operational condition was subjected to a qualitative chromatographic analysis aiming to know the constituents of the produced bio-oil, which were: phenol followed by sirigol, acetovanilona and vinyl guaiacol. The solid phase (char) was characterized through an immediate analysis (evaluation of moisture, volatiles, ashes and fixed carbon), higher heating value and FTIR. The non-condensing gas phase presented as main constituents CO2, CO and H2. The results were compared to the ones mentioned by the literature.

Preparação e carcterização de complexos multicomponentes contendo ciclodextrinas e benznidazol

The benznidazole (BNZ) is the only alternative for Chagas disease treatment in Brazil. This drug has low solubility, which restricts its dissolution rate. Thus, the present work aimed to study the BNZ interactions in binary systems with beta cyclodextrin (β-CD) and hydroxypropyl-beta cyclodextrin (HP-β-CD), in order to increase the apparent aqueous solubility of drug. The influence of seven hydrophilic polymers, triethanolamine (TEA) and 1-methyl-2- pyrrolidone (NMP) in benznidazole apparent aqueous solubility, as well as the formation of inclusion complexes was also investigated. The interactions in solution were predicted and investigated using phase solubility diagram methodology, nuclear magnetic resonance of protons (RMN) and molecular modeling. Complexes were obtained in solid phase by spray drying and physicochemical characterization included the UV-Vis spectrophotometric spectroscopy in the infrared region, scanning electron microscopy, X-ray diffraction and dissolution drug test from the different systems. The increment on apparent aqueous solubility of drug was achieved with a linear type (AL) in presence of both cyclodextrins at different pH values. The hydrophilic polymers and 1-methyl-2-pyrrolidone contributes to the formation of inclusion complexes, while the triethanolamine decreased the complex stability constant (Kc). The log-linear model applied for solubility diagrams revealed that both triethanolamine and 1-methyl-2-pyrrolidone showed an action cosolvent (both solvents) and complexing (1-methyl-2-pyrrolidone). The best results were obtained with complexes involving 1-methyl-2-pyrrolidone and hydroxypropylbeta- cyclodextrin, with an increased of benznidazole solubility in 27.9 and 9.4 times, respectively. The complexes effectiveness was proven by dissolution tests, in which the ternary complexes and physical mixtures involving 1-methyl- 2-pyrrolidone and both cyclodextrins investigated showed better results, showing the potential use as novel pharmaceutical ingredient, that leads to increased benznidazole bioavailability

Preparação e caracterização de complexos multicomponentes contendo ciclodextrinas com metotrexato

Conselho Nacional de Desenvolvimento Científico e Tecnológico

Avaliação de catalisadores a base de carbeto e nitreto de molibdênio na obtenção de lactitol via hidrogenação da lactose

Seeking a greater appreciation of cheese whey was developed to process the hydrogenation of lactose for the production of lactitol, a polyol with high added value, using the catalyst Ni / activated carbon (15% and 20% nickel), the nitride Mo2N, the bimetallic carbide Ni-Mo/ activated carbon and carbide Mo2C. After synthesis, the prepared catalysts were analyzed by MEV, XRD, laser granulometry and B.E.T. The reactor used in catalytic hydrogenation of lactose was the type of bed mud with a pressure (68 atm), temperature (120 oC) and stirring speed (500 rpm) remained constant during the experiments. The system operated in batch mode for the solid and liquid and semi-continuous to gas. Besides the nature of the catalyst, we studied the influence of pH of reaction medium for Mo2C carbide as well as evaluating the character of the protein inhibitor and chloride ions on the activity of catalysts Ni (20%)/Activated Carbon and bimetallic carbide Ni-Mo/Activated Carbon. The decrease in protein levels was performed by coagulation with chitosan and adsorption of chloride ions was performed by ion exchange resins. In the process of protein adsorption and chloride ions, the maximum percentage extracted was about 74% and 79% respectively. The micrographs of the powders of Mo2C and Mo2N presented in the form of homogeneous clusters, whereas for the catalysts supported on activated carbon, microporous structure proved impregnated with small particles indicating the presence of metal. The results showed high conversion of lactose to lactitol 90% for the catalyst Ni (20%)/Activated Carbon at pH 6 and 46% for the carbide Mo2C pH 8 (after addition of NH4OH) using the commercial lactose. Monitoring the evolution of the constituents present in the reaction medium was made by liquid chromatography. A kinetic model of heterogeneous Langmuir Hinshelwood type was developed which showed that the estimated constants based catalysts promoted carbide and nitride with a certain speed the adsorption, desorption and production of lactitol

Recuperação e purificação de ramnolipídeos produzidos por pseudomonas aeruginosa P029-GVIIA utilizando melaço de cana como substrato

Biosurfactants are molecules produced by microorganisms mainly bacteria as Pseudomonas and Bacillus. Among the biosurfactants, rhamnolipids play an important role due to their tensoactive as well as emulsifying properties. Besides can be produced in a well consolidated way the production costs of biosurfactants are quite expansive mainly if downstream processing is goning to be considered. Actually, attention has been given to identification of biosurfactants as well as optimization of its fermentative processes including downstream ones. This work deals with the development of strategies to recovery and purification of rhamnolipids produced by Pseudomonas aeruginosa P029-GVIIA using sugar-cane molasses as substrate. Broth free of cells was used in order to investigate the best strategies to recovery and purification produced by this system. Between the studied acids (HCl and H2SO4) for the acid precipitation step, HCl was the best one as has been showed by the experimental design 24. Extraction has been carried out using petroleum ether and quantification has been done using the thioglycolic acid method. Adsorption studies were carried out with activated carbon in a batch mode using a 24 experimental design as well as combined with an hydrophobic resin Streamline Phenyl aiming to separate the produced biosurfactant. Biosurfactant partial identification was carried out using High Performance Liquid Chromatography (HPLC). Experiments in batch mode showed that adsorption has been controlled mainly by pH and temperature. It was observed a reduction of 41.4% for the liquid phase and the solid phase it was possible to adsorb up to 15 mg of rhamnolipd/g of activated carbon. The kinetics of adsorption has been well fitted to a pseudo-first order reaction with velocity constant (k1) of 1.93 x 10-2 min-1. Experiments in packed bed ranging concentration on eluent (acetone) has been shown the highest recovery factor of 98% when pure acetone has been used. The combined effect if using activated carbon with an hydrophobic resin Streamline Phenyl has been shown successful for the rhamnolipids purification. It has been possible to purify a fraction of the crude broth with 98% of purity when the eluted of activated carbon packed bed was used with pure acetone

Bio-óleo e biogás da degradação termoquímica de lodo de esgoto doméstico em cilindro rotativo

The objective of this study was to produce biofuels (bio-oil and gas) from the thermal treatment of sewage sludge in rotating cylinder, aiming industrial applications. The biomass was characterized by immediate and instrumental analysis (elemental analysis, scanning electron microscopy - SEM, X-ray diffraction, infrared spectroscopy and ICP-OES). A kinetic study on non-stationary regime was done to calculate the activation energy by Thermal Gravimetric Analysis evaluating thermochemical and thermocatalytic process of sludge, the latter being in the presence of USY zeolite. As expected, the activation energy evaluated by the mathematical model "Model-free kinetics" applying techniques isoconversionais was lowest for the catalytic tests (57.9 to 108.9 kJ/mol in the range of biomass conversion of 40 to 80%). The pyrolytic plant at a laboratory scale reactor consists of a rotating cylinder whose length is 100 cm with capable of processing up to 1 kg biomass/h. In the process of pyrolysis thermochemical were studied following parameters: temperature of reaction (500 to 600 ° C), flow rate of carrier gas (50 to 200 mL/min), frequency of rotation of centrifugation for condensation of bio-oil (20 to 30 Hz) and flow of biomass (4 and 22 g/min). Products obtained during the process (pyrolytic liquid, coal and gas) were characterized by classical and instrumental analytical techniques. The maximum yield of liquid pyrolytic was approximately 10.5% obtained in the conditions of temperature of 500 °C, centrifugation speed of 20 Hz, an inert gas flow of 200 mL/min and feeding of biomass 22 g/min. The highest yield obtained for the gas phase was 23.3% for the temperature of 600 °C, flow rate of 200 mL/min inert, frequency of rotation of the column of vapor condensation 30 Hz and flow of biomass of 22 g/min. The non-oxygenated aliphatic hydrocarbons were found in greater proportion in the bio-oil (55%) followed by aliphatic oxygenated (27%). The bio-oil had the following characteristics: pH 6.81, density between 1.05 and 1.09 g/mL, viscosity between 2.5 and 3.1 cSt and highest heating value between 16.91 and 17.85 MJ/ kg. The main components in the gas phase were: H2, CO, CO2 and CH4. Hydrogen was the main constituent of the gas mixture, with a yield of about 46.2% for a temperature of 600 ° C. Among the hydrocarbons formed, methane was found in higher yield (16.6%) for the temperature 520 oC. The solid phase obtained showed a high ash content (70%) due to the abundant presence of metals in coal, in particular iron, which was also present in bio-oil with a rate of 0.068% in the test performed at a temperature of 500 oC.

Modelagem Matemática e Computacional de fenômenos eletrocinéticos em meios porosos carregados eletricamente

In this work we present a mathematical and computational modeling of electrokinetic phenomena in electrically charged porous medium. We consider the porous medium composed of three different scales (nanoscopic, microscopic and macroscopic). On the microscopic scale the domain is composed by a porous matrix and a solid phase. The pores are filled with an aqueous phase consisting of ionic solutes fully diluted, and the solid matrix consists of electrically charged particles. Initially we present the mathematical model that governs the electrical double layer in order to quantify the electric potential, electric charge density, ion adsorption and chemical adsorption in nanoscopic scale. Then, we derive the microscopic model, where the adsorption of ions due to the electric double layer and the reactions of protonation/ deprotanaç~ao and zeta potential obtained in modeling nanoscopic arise in microscopic scale through interface conditions in the problem of Stokes and Nerst-Planck equations respectively governing the movement of the aqueous solution and transport of ions. We developed the process of upscaling the problem nano/microscopic using the homogenization technique of periodic structures by deducing the macroscopic model with their respectives cell problems for effective parameters of the macroscopic equations. Considering a clayey porous medium consisting of kaolinite clay plates distributed parallel, we rewrite the macroscopic model in a one-dimensional version. Finally, using a sequential algorithm, we discretize the macroscopic model via the finite element method, along with the interactive method of Picard for the nonlinear terms. Numerical simulations on transient regime with variable pH in one-dimensional case are obtained, aiming computational modeling of the electroremediation process of clay soils contaminated

Estudo do comportamento da sinterização de compactos de cavacos de um aço SAE 1050 obtidos sob alta pressão

From an economic standpoint, the powder metallurgy (P/M) is a technique widely used for the production of small parts. It is possible, through the P/M and prior comminution of solid waste such as ferrous chips, produce highly dense sintered parts and of interest to the automotive, electronics and aerospace industries. However, without prior comminution the chip, the production of bodies with a density equal to theoretical density by conventional sintering techniques require the use of additives or significantly higher temperatures than 1250ºC. An alternative route to the production of sintered bodies with high density compaction from ferrous chips (≤ 850 microns) and solid phase sintering is a compression technique under high pressure (HP). In this work, different compaction pressures to produce a sintered chip of SAE 1050 carbon steel were used. Specifically, the objective was to investigate them, the effect of high pressure compression in the behavior of densification of the sintered samples. Therefore, samples of the chips from the SAE 1050 carbon steel were uniaxially cold compacted at 500 and 2000 MPa, respectively. The green compacts obtained were sintered under carbon atmosphere at 1100 and 1200°C for 90 minutes. The heating rate used was 20°C/min. The starting materials and the sintered bodies were characterized by optical microscopy, SEM, XRD, density measurements (geometric: mass/volume, and pycnometry) and microhardness measurements Vickers and Rockwell hardness. The results showed that the compact produced under 2000 MPa presented relative density values between 93% and 100% of theoretical density and microhardness between 150 HV and 180 HV, respectively. In contrast, compressed under 500 MPa showed a very heterogeneous microstructure, density value below 80% of theoretical density and structural conditions of inadequate specimens for carrying out the hardness and microhardness measurements. The results indicate that use of the high pressure of ferrous chips compression is a promising route to improve the sinterability conditions of this type of material, because in addition to promoting greater compression of the starting material, the external tension acts together with surface tension, functioning as the motive power for sintering process. Additionally, extremely high pressures allow plastic deformation of the material, providing an intimate and extended contact of the particles and eliminating cracks and pores. This tends to reduce the time and / or temperature required for good sintering, avoiding excessive grain growth without the use of additives. Moreover, higher pressures lead to fracture the grains in fragile or ductile materials highly hardened, which provides a starting powder for sintering, thinner, without the risk of contamination present when previous methods are used comminution of the powder.

Ocorrência de compostos de interesse emergente no aquífero Dunas-Barreiras e nos esgotos de Natal/RN

The detection of emerging interest microcontaminants in environmental samples of surface water, groundwater, drinking water, wastewater and effluents from water and sewage treatment plants (WTP and STP), in many countries, suggests these pollutants are widespread in the environment, mainly in urban areas. This is a reason for great concern, since many of these compounds are potentially harmful for humans other living beings, and they are not efficiently removed in the majority of WTP and STP, which is exacerbated by precariousness of water supply and sanitation services. In Natal, like other Brazilian cities, the sewage system serves only part of the urban area (about 30%), so that the rest of the wastewater is infiltrated in the sandy soil of the region in cesspool-dry well systems. This has resulted in contamination of groundwater in the area (sand-dune barrier aquifer, which supplies more than 50% of the city population), which has been observed by the increase in nitrate concentration in supply wells. The vulnerability of the sanddune barrier aquifer, combined with reports of the presence of emerging interest microcontaminants in Brazil and worldwide, led to this research, which investigated the occurrence of fifteen microcontaminants in Natal groundwater and sewage. Samples were collected at five wells used for water supply, the raw sewage and the effluents from biological reactors from STP (UASB and activated sludge reactors). Two samples of each sample were taken, with one week apart between the samples. To determine the contaminants, extraction of aquifer water, and raw and treated sewage samples were performed, through the technique of using SPE Strata X cartridge (Phenomenex®) to the aquifer water, and Strata SAX and Strata X (Phenomenex® ) for samples of raw and treated sewage. Subsequently the extracts were analyzed using GC-MS technique. Much of the analyzed microcontaminants were detected in groundwater and sewage. The concentrations in groundwater are generally lower than those found in the sewers. Some of the compounds (estrone, estradiol, bisphenol A, caffeine, diclofenac, naproxen, paracetamol and ibuprofen) are partially removed at STP.

Estudo de duas pseudoligas de Nb-Cu obtidas pela rota da metalurgia do pó

The Nb-Cu pseudoalloys present themselves as potential substitutes for the alloys from a well known system and already commercially applied, as the W-Cu alloys, used in applications such as heat sinks, electrical contacts and coils for the generation of high magnetic fields. Because it is an immiscible system, where there is mutual insolubility and low wettability of the liquid Cu on the Nb surface, the processing route used in this work was the Powder Metallurgy. Two Nb alloys were used, with additions of 10% and 20% in weight of Cu, and times of 20, 30 and 40 hours for the high energy milling of the starting powders. The milling evolution of the powders is presented through the characterization techniques, such as the LASER diffraction for particle size, XRD, SEM, EDS, DSC, dilatometry, TEM and chemical analysis. After the milling, portions of the loads were submitted to the annealing heat treatment. The process used for the samples consolidation was the hot pressing, which has been applied both on some milled powders samples, as on the annealed powders. Subsequent heat treatments were performed in the samples at temperatures of 1000ºC (solid phase) and 1100ºC (in the Cu liquid phase). All sets of consolidated samples, and also the two sets of the heat treated, were analyzed by XRD, SEM, EDS, density and Vickers microhardness. Moreover, other Nb powder samples with 10% and 20% in weight of Cu obtained by simple mechanical mixing, were consolidated, thermally treated and characterized with the same techniques applied to the others, and the results were compared among themselves. Despite the difficulty of consolidation and densification of the two pseudoalloys of the Nb-Cu system of this study, on the route that passes through the HEM, samples were obtained with densities around 90% of the theoretical density. And, on the processing route of which were only mixed, the values reached up to 97%. Therefore, in this work are also emphasized the processes that made possible these results.

Interações da trancinolona com ciclodextrinas em sistemas multicomponentes

Triamcinolone is a relevant anti-inflammatory costicosteroid drug, used mainly by injectable suspensions due its poor water solubility. The association of triamcinolone with cyclodextrins and co-solvents (triethanolamine TEA and N-methylpirrolidone NMP) was held to solubilize the drug and explain the involved interactions. Phase-solubility diagrams showed that triamcinolone was solubilized forming incredible stable complexes with cyclodextrins, in which bests results were observed applying randomyl-methylated-beta-cyclodextrin (RMβCD) (161 fold on increased solubility). The co-solvents TEA and NMP also enhanced drug solubility 1.4 and 6.7 fold, respectively. The association of both co-solvents with CDs seems decreased complexation stability, but enables higher amount of uncomplexed drug. Experimental magnetic resonance 2D-ROESY and theoretical molecular modeling studies demonstrated TRI-CDs interactions and elucidated the structure of formed complex, which occurred due to the inclusion of ring A of TRI on CDs cavity. Physicochemical aspects of solid binary and ternary complexes prepared by spray drying were assessed by using FTIR, X-ray diffraction and SEM photographs. Dissolution studies showed that binary and ternary associations presented higher dissolution efficacy in detrimental to pure drug system. In addition, the ternary complex containing TEA and RMβCD allowed drug dissolution faster than binary complex with RMβCD. Therefore, given the higher solubility and drug dissolution rate, binary and ternary complexes are new raw materials with great potential for pharmaceuticals containing triamcinolone.

Efeito da adição de WC e Co na sinterização e propriedades mecânicas da alumina

Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.

Efeito da adição de WC e Co na sinterização e propriedades mecânicas da alumina

Composites based on alumina (Al2O3), tungsten carbide (WC) and cobalt (Co) exhibit specific properties such as low density, high oxidation resistance, high melting point and high chemical inertia. That composite shows to be a promising material for application in various fields of engineering. In this work, the mechanical properties of the composite (Al2O3 – WC – Co), particularly density and hardness, were evaluated according to the effects of the variables of powder processing parameters, green compact and sintered. Powder composites with the composition of 80 wt% Al2O3, 18 wt% WC and 2 wt% Co were processed by high energy ball milling in a planetary mill for 50 hours as well as mixed by manual mixing in a glass vessel with the same proportion. Samples were collected (2, 10, 20, 30, 40 and 50 hours) during the milling process. Then, the powders were compacted in a cylindrical die with 5 mm in diameter in a uniaxial press with pressures of 200 and 400 MPa. The sintering was in two stages: first, the solid phase sintering was performed at 1126 and 1300 °C for 1 hour with a heating rate of 10 °C/min in a resistive furnace under argon atmosphere for green samples compacted in 200 and 400 MPa; the second sintering was performed on dilatometer in solid phase at 1300 °C for green sample compacted in 200 MPa, another sintering also was performed on dilatometer, this time in liquid phase at 1550 °C for green samples compacted in 200 and 400 MPa, with the same parameters used in resistive furnace. The raw materials were characterized by X – ray diffraction (XRD), X – ray fluorescence (XRF), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and laser particlemeter. The sintered samples were subjected to microhardness testing. The results showed that high energy milling achieved to the objectives regarding the particle size and the dispersion of composite phases. However, the hardness did not achieve to significant results, this is an indication that the composite has low fracture toughness.