Otimização de metodologias para determinação de hidrocarbonetos policíclicos aromáticos:aplicação em água do Rio Potengi

This work aims to detect polycyclic aromatic hydrocarbons (PAHs) through optimized analytical techniques, such as gas chromatography with flame-ionisation detector (CGFID), gas chromatography coupled to mass spectrometry (CGMS), Fluorescence Spectroscopy of Molecular and Purpot of oils and greases (POG). Apply to chemometrics, Factorial Planning 23, in the preparation of samples by liquid-liquid extraction. The sample preparation was used for liquid-liquid extraction and factors in this sample was used for the application of factorial planning 23, such as the use of ultrasound, solvents (dichloromethane, hexane and chloroform) and ratio of solvent / synthetic sample. These factors were assigned two types of levels: positive and negative. It was used to form the cube to better analyze the answers. The responses of the eight combinations were obtained in reading the spectrofluorimetric. The optimization of equipment were used, and they served in the HPA's identification of the samples collected in Rio Potengi. The optimization of the equipment was observed every 16's and PAH in the samples was found that the HPA's came from contamination of the Rio Potengi. The contamination comes through organic household waste, hospital waste, and among other contamination that comes from industries that are installed around the River The factorial design of high validity, it was observed a more effective sample preparation. The factorial design of liquid-liquid extraction showed a way to spend less solvent in less time using an ideal solvent, but also a way to extract more analyte from the matrix itself is water. In planning a smaller form factor extraction was the use of ultrasound, the ratio 1:3 corresponding to a solvent and sample 3 and the best solvent was dichloromethane who presented a viable extraction, not discarding the possibility of using also the hexane. The chloroform and may be toxic not had a good extraction

Assinaturas antropogênicas de elementos maiores e traços em poeira urbana na cidade do Natal-RN

Although there are many studies on urban dust contamination by heavy metals in developed countries, little attention has been paid to this type of study in developing countries, including Brazil. Therefore, a series of investigations were performed to provide signatures of heavy metals in urban dust and assess the potential sources in the city of Natal - RN-Brazil. The fraction of these sediments was studied to pass through a sieve of 63 micrometers. For the study analyzed two groups of samples, one collected in September 2009 at the end of the rainy season (9 samples) and one collected in January 2010 in the dry season (21 samples). So in all, thirty sediment samples were collected from the street. Then, in Fluorescence Spectrometry X-rays were determined major elements SiO2, Na2O, K2O, Al2O3, MgO, P2O5, Fe2O3, MnO, TiO2 and CaO, and trace Rb, Cr, Ni, Cu, Zn, Sr and Pb by an ICPOES was determined Zn, V, Na, K, Ni, Mn, Mg, P, Fe, Cr, Cu, Pb, Ba, Ca and Al from leaching HCl 0.5 mol L-1 . The results of the concentrations of elements show that the greater presence of these occurs in the dry season, except for Si which is higher in the rainy season. Analyses by geoaccumulation Index (IGEO) Enrichment Factor (EF), Contamination Factor (CF), analysis correlation and Hierarchical Cluster, confirm that Zn, Cu and Pb is anthropogenic character. Zinc may be derived from various sources related to motor vehicles or the road signs and street grids. The elements Na, K, Mg and Ca may be related to droplets suspended in air containing cations and anions present in seawater (salty), common in Christmas throughout the year, brought by winds SE-NW. The elements Na, Mg, Ca and K are the most abundant in seawater and were analyzed in this study. This indicates that the source of these additional elements detected by analyzing the contamination factor may be the very sea. Moreover, Ni, Fe, Cr and Ba can be either as a source of anthropogenic geogênica. The source of Ca is different, because it comes in lime and paint (painting guides of buildings and streets) in construction materials, but may also be present in sediments in the fragments of shells or carbonate bioclasts common in the coastal area

Bioprospecção química da esponja callyspongia vaginalis (Callyspongiidae)

Recently, marine organisms have attracted attention because of the complexity and potent biological activity from your secondary metabolites. Our planet has 80% it surface covered by oceans and seas, therefore, housing a wide number of different forms of life, among them, the sponges. These sessile and filtrating animals, according to numerous researches, come showing like true chemistry factories. The substances from these animals, sometimes show as news targets to therapeutics agents, and some countries has already use them for treatment of some diseases. Further of the secondary metabolites, the polysaccharides of marine origin also have been target of studies, because the presence of the sulfates groups in its molecules. Polysaccharides with differents biological activities have been related in a large number of researches. Actually, many studies show the sponges as source of promising medicine. These studies inspire new researches, because the few number of sponges species studied until now. Because of that, the present work shows the chemistry prospection of the sponge Callyspongia vaginalis. Chromatographic methods in silica gel allowed the isolations of two secondary metabolites: the known β- sitosterol and a ceramide, no reported in the genus Callyspongia, previously. The analysis of the their lipid extracts show different kinds of fatty acids with a variety of chain length (saponifiable fraction), and others metabolites like Lupenone and stigmasterol, also unprecedented in the genus. The Polysaccharide characterization and the elucidation of the secondary metabolites acquired through of chromatography analysis (CC, molecular exclusion) and spectrometric (NMR 1H and 13C, mass, IR), respectively and comparison with literature data

Caracterização e aplicação de vermicultura natural e quimicamente modificada na adsorção de azul de metileno

Chemical modification of clays has been extremely studied in the search for improvements of their properties for use in various areas, such as in combating pollution by industrial effluents and dyes. In this work, the vermiculite was chemically modified in two ways, characterized and evaluated the adsorption of methylene blue dye. First was changed with the addition of a surfactant (hexadecyltrimethylammonium bromide, BHTA) making it an organophilic clay and then by adding an acid (HCl) by acid activation. Some analyzes were performed as X-ray fluorescence (FRX), X-ray diffraction (DRX), adsorption isotherms of methylene blue dye, infrared (FTIR) , scanning electron microscopy (SEM), thermal gravimetric analysis and spectroscopy energy dispersive (EDS). Analysis by FRX of natural vermiculite indicates that addition of silicon and aluminum, clay presents in its structure the magnesium, calcium and potassium with 16 % organic matter cations. The DRX analyzes indicated that the organic vermiculite was an insertion of the surfactant in the space between the lamellae, vermiculite and acid partial destruction of the structure with loss of crystallinity. The adsorption isotherms of methylene blue showed that there was a significant improvement in the removal of dye to the vermiculite with the addition of cationic surfactant hexadecyltrimethylammonium bromide and treatment with acid using HCl 2 mol/L. In acid vermiculites subsequently treated with surfactant, the adsorption capacity increased with respect to natural vermiculite, however was much lower compared vermiculite modified with acid and surfactant separately. Only the acidic vermiculite treated with surfactant adjusted to the Langmuir model. As in the infrared spectrometry proved the characteristics of natural vermiculite. In the organic vermiculite was observed the appearance of characteristic bands of CH3, CH2, and (CH3)4N. Already on acid vermiculite, it was realized a partial destruction with decreasing intensity of the characteristic band of vermiculite that is between 1074 and 952 cm-1. In the SEM analysis, it was observed that there was partial destruction to the acid treatment and a cluster is noted between the blades caused by the presence of the surfactant. The TG shows that the higher mass loss occurs at the beginning of the heating caused by the elimination of water absorbed on the surface between layers. In the organic vermiculite also observed a loss of mass between 150 and 300 °C caused decomposition of the alkylammonium molecules (surfactants)

Eficiência de extração de cobre e níquel utilizando sistemas microemulsionados bifásicos e trifásicos

The environmental impact due to the improper disposal of metal-bearing industrial effluents imposes the need of wastewater treatment, since heavy metals are nonbiodegradable and hazardous substances that may cause undesirable effects to humans and the environment. The use of microemulsion systems for the extraction of metal ions from wastewaters is effective when it occurs in a Winsor II (WII) domain, where a microemulsion phase is in equilibrium with an aqueous phase in excess. However, the microemulsion phase formed in this system has a higher amount of active matter when compared to a WIII system (microemulsion in equilibrium with aqueous and oil phases both in excess). This was the reason to develop a comparative study to evaluate the efficiency of two-phases and three-phases microemulsion systems (WII and WIII) in the extraction of Cu+2 and Ni+2 from aqueous solutions. The systems were composed by: saponified coconut oil (SCO) as surfactant, n-Butanol as cosurfactant, kerosene as oil phase, and synthetic solutions of CuSO4.5H2O and NiSO4.6H2O, with 2 wt.% NaCl, as aqueous phase. Pseudoternary phase diagrams were obtained and the systems were characterized by using surface tension measurements, particle size determination and scanning electron microscopy (SEM). The concentrations of metal ions before and after extraction were determined by atomic absorption spectrometry. The extraction study of Cu+2 and Ni+2 in the WIII domain contributed to a better understanding of microemulsion extraction, elucidating the various behaviors presented in the literature for these systems. Furthermore, since WIII systems presented high extraction efficiencies, similar to the ones presented by Winsor II systems, they represented an economic and technological advantage in heavy metal extraction due to a small amount of surfactant and cosurfactant used in the process and also due to the formation of a reduced volume of aqueous phase, with high concentration of metal. Considering the reextraction process, it was observed that WIII system is more effective because it is performed in the oil phase, unlike reextraction in WII, which is performed in the aqueous phase. The presence of the metalsurfactant complex in the oil phase makes possible to regenerate only the surfactant present in the organic phase, and not all the surfactant in the process, as in WII system. This fact allows the reuse of the microemulsion phase in a new extraction process, reducing the costs with surfactant regeneration

Síntese de catalisadores nanoporosos na ausência total e parcial de direcionadores orgânicos para pirólise catalítica de óleos pesados e intermediários

The processing of heavy oil produced in Brazil is an emergency action and a strategic plan to obtain self-sufficiency and economic surpluses. Seen in these terms, it is indispensable to invest in research to obtain new catalysts for obtaining light fraction of hydrocarbons from heavy fractions of petroleum. This dissertation for the degree of Doctor of Philosophy reports the materials preparation that combine the high catalytic activity of zeolites with the greater accessibility of the mesoporosity, more particularly the HZSM-5/MCM-41 hybrid, done by synthesis processes with less environmental impact than conventional ones. Innovative methodologies were developed for the synthesis of micro-mesoporous hybrid material by dual templating mechanism and from crystalline zeolitic aluminosilicate in the absence of organic template. The synthesis of hybrid with pore bimodal distribution took place from one-single organic directing agent aimed to eliminate the use of organic templates, acids of any kind or organic solvents like templating agent of crystalline zeolitic aluminosilicate together with temperature-programmed microwave-assisted, making the experimental procedures of preparation most practical and easy, with good reproducibility and low cost. The study about crystalline zeolitic aluminosilicate in the absence of organic template, especially MFI type, is based on use of H2O and Na+ cation playing a structural directing role in place of an organic template. Advanced characterization techniques such as X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Highresolution Transmission Electron Microscopy (HRTEM), Adsorption of N2 and CO2, kinetic studies by Thermogravimetric Analysis (TGA) and Pyrolysis coupled to Gas Chromatography/Mass Spectrometry (Pyrolysis-GC/MS) were employed in order to evaluate the synthesized materials. Achieve the proposed objectives, has made available a set of new methodologies for the synthesis of zeolite and hybrid micro-mesoporous material, these suitable for catalytic pyrolysis of heavy oils aimed at producing light fraction

Incrustação em poço produtor de petróleo e gás natural: um estudo de caso

Water and gas is a common by - product of the oil production process. Production may be compromised by the precipitation of inorganic salts in both the reservoir and producing well, through scale formation. This precipitation is likely the cause of the formation damage. High temperatures and h igh pressures (HTHP) may favor the precipitation of insoluble salts. The most common types of scale in oil fields are calcium carbonate and calcium sulphate, strontium and barium sulphate. New types of scale formation have attracted special attention such as zinc sulphide and lead. This precipitation may occur in the pores of reservoir rocks, in the production string and in equipment, causing obstructions and consequent production losses. In this study, the influence of well depth on incrustation compositio n was investigated to design removal treatments and assess the behavior of these deposits along the string, through the analysis of pressure and temperature. Scale residues were recovered from the inside of the production string of an oil and gas well duri ng the string removal operation. A total of 10 samples from different depths (15.4 m to 4061.5 m) were obtained. Initially a dissolution test was conducted in weak acid, similar to that used in removal operations with this type of scale formation. Majority composition was defined and confirmed by dissolution tests using X - Ray Fluorescence Spectroscopy (XRF), X - Ray Diffraction (XRD) and Scanning Electron Microscope (SEM) techniques. Residues with distinct characteristics were observed in different proportion s, showing a tendency toward increased and/or decreased mass with depth. In the samples closest to the surface, typical sandstone residues were found, with calcium (45% Ca) as the metal of highest concentration. The obtained results indicate correlations o f the scale types studied with the depth and, consequently, with the thermodynamic conditions of pressure and temperature.

Determinação da concentração de metais no material particulado (PM10 e PM2,5) do ar atmosférico em uma área urbana da cidade do Natal – RN

This study aimed to assess ambient air quality in a urban area of Natal, capital of Rio Grande do Norte (latitude 5º49'29 '' S and longitude 35º13'34'' W), aiming to determine the metals concentration in particulate matter (PM10 and PM2,5) of atmospheric air in the urban area o the Natal city. The sampling period for the study consisted of data acquisition from January to December 2012. Samples were collected on glass fiber filters by means of two large volumes samplers, one for PM2,5 (AGV PM 2,5) and another for PM10 (PM10 AGV). Monthly averages ranged from 8.92 to 19.80 g.m-3 , where the annual average was 16,21 g.m-3 for PM10 and PM2,5 monthly averages ranged from 2,84 to 7,89 g.m -3 , with an annual average of 5,61 g.m-3 . The results of PM2,5 and PM10 concentrations were related meteorological variables and for information on the effects of these variables on the concentration of PM, an exploratory analysis of the data using Principal Component Analysis (PCA) was performed. The results of the PCA showed that with increasing barometric pressure, the direction of the winds, the rainfall and relative humidity decreases the concentration of PM and the variable weekday little influence compared the meteorological variables. Filters containing particulate matter were selected in six days and subjected to microwave digestion. After digestion samples were analyzed by with Inductively Coupled Plasma Mass Spectrometry (ICP-MS). The concentrations for heavy metals Vanadium, Chromium, Manganese, Nickel, Copper, Arsenic and lead were determined. The highest concentrations of metals were for Pb and Cu, whose average PM10 values were, respectively, 5,34 and 2,34 ng.m-3 and PM2,5 4,68 and 2,95 ng.m-3 . Concentrations for metals V, Cr, Mn, Ni, and Cd were respectively 0,13, 0,39, 0,48, 0,45 and 0,03 ng.m-3 for PM10 fraction and PM2,5 fraction, 0,05, 0,10, 0,10, 0,34 and 0,01 ng.m-3. The concentration for As was null for the two fractions

Determinação de CD, PB, e TL em água produzida por HR-CS GF AAS após extração em ponto nuvem

Produced water is a major problem associated with the crude oil extraction activity. The monitoring of the levels of metals in the waste is constant and requires the use of sensitive analytical techniques. However, the determination of trace elements can often require a pre-concentration step. The objective of this study was to develop a simple and rapid analytical method for the extraction and pre-concentration based on extraction phenomenon cloud point for the determination of Cd, Pb and Tl in produced water samples by spectrometry of high resolution Absorption source continues and atomization graphite furnace. The Box Behnken design was used to obtain the optimal condition of extraction of analytes. The factors were evaluated: concentration of complexing agent (o,o-dietilditilfosfato ammonium, DDTP), the concentration of hydrochloric acid and concentration of surfactant (Triton X -114). The optimal condition obtained through extraction was: 0,6% m v-1 DDTP, HCl 0,3 mol L-1 and 0,2% m v-1 of Triton X - 114 for Pb; 0,7% m v-1 DDTP, HCl 0,8 mol L-1 and 0,2% m v-1 Triton X-114 for Cd. For Tl was evidenced that best extraction condition occurs with no DDTP, the extraction conditions were HCl 1,0 mol L-1 e 1,0% m v-1 de Triton X - 114. The limits of detection for the proposed method were 0,005 µg L-1 , 0,03 µg L-1 and 0,09 µg L-1 to Cd, Pb and Tl, Respectively. Enrichment factors Were greater than 10 times. The method was applied to the water produced in the Potiguar basin, and addition and recovery tests were performed, and values were between 81% and 120%. The precision was expressed with relative standard deviation (RSD) is less than 5%

Desenvolvimento de metodologia de extração e pré-concentração utilizando sistema microemulsionado para determinação de Cd, Co, Cu, Ni, Pb e Tl em águas naturais e produzidas por HR-CS AAS

The determination and monitoring of metallic contaminants in water is a task that must be continuous, leading to the importance of the development, modification and optimization of analytical methodologies capab le of determining the various metal contaminants in natural environments, because, in many cases, the ava ilable instrumentation does not provide enough sensibility for the determination of trace values . In this study, a method of extraction and pre- concentration using a microemulsion system with in the Winsor II equilibrium was tested and optimized for the determination of Co, Cd, P b, Tl, Cu and Ni through the technique of high- resolution atomic absorption spectrometry using a continuum source (HR-CS AAS). The optimization of the temperature program for the graphite furnace (HR-CS AAS GF) was performed through the pyrolysis and atomization curves for the analytes Cd, Pb, Co and Tl with and without the use of different chemical modifiers. Cu and Ni we re analyzed by flame atomization (HR-CS F AAS) after pre-concentr ation, having the sample introduction system optimized for the realization of discrete sampling. Salinity and pH levels were also analyzed as influencing factors in the efficiency of the extraction. As final numbers, 6 g L -1 of Na (as NaCl) and 1% of HNO 3 (v/v) were defined. For the determination of the optimum extraction point, a centroid-simplex statistical plan was a pplied, having chosen as the optimum points of extraction for all of the analytes, the follo wing proportions: 70% aqueous phase, 10% oil phase and 20% co-surfactant/surfactant (C/S = 4). After extraction, the metals were determined and the merit figures obtained for the proposed method were: LOD 0,09, 0,01, 0,06, 0,05, 0,6 and 1,5 μg L -1 for Pb, Cd, Tl, Co, Cu and Ni, re spectively. Line ar ranges of ,1- 2,0 μg L -1 for Pb, 0,01-2,0 μg L -1 for Cd, 1,0 - 20 μg L -1 for Tl, 0,1-5,0 μg L -1 for Co, 2-200 μg L -1 and for Cu e Ni 5-200 μg L -1 were obtained. The enrichment factors obtained ranged between 6 and 19. Recovery testing with the certified sample show ed recovery values (n = 3, certified values) after extraction of 105 and 101, 100 and 104% for Pb, Cd, Cu and Ni respectively. Samples of sweet waters of lake Jiqui, saline water from Potengi river and water produced from the oil industry (PETROBRAS) were spiked and the recovery (n = 3) for the analytes were between 80 and 112% confirming th at the proposed method can be used in the extraction. The proposed method enabled the sepa ration of metals from complex matrices, and with good pre-concentration factor, consistent with the MPV (allowed limits) compared to CONAMA Resolution No. 357/2005 which regulat es the quality of fresh surface water, brackish and saline water in Brazil.

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.

Desenvolvimento biotecnológico de uma emulsão de uso tópico a base de óleo de rã-touro Rana catesbeiana Shaw

The skin is one of the largest organs of the human body and accounts for about 16% of body weight. The body protection against the external environment microorganisms is one of its most important functions, however is necessary that the skin remain intact for this function be exercised, so that when there is an injury on the skin, the process of restructuring needs to be starts, however this restructuration may also be compromised due to some diseases, justifying even more the need for the development of topical products that promote or accelerate the skin healing. Thus the aim of this study was to extract bullfrog oil and to develop a suitable topical emulsion. Two different oil samples were extracted by hot or organic solvent process. Titration techniques and gas chromatography- mass spectrometry were used to characterize the bullfrog oil. The required hydrophile-lipophile balance (HLBr) of bullfrog oil was determined and a pseudo-ternary phase diagram was constructed. The stability of the topical emulsion was evaluated. Then, cellular viability was determined by MTT assay using normal fibroblasts (3T3) and melanoma (B16F10) cells lines. The hot extraction yield was 60.6%. The major polyunsaturated compounds found were Eicosapentaenoic acid (17.6%) and Arachidonic acid (8.4%). HLBr study demonstrated the presence of stable systems with HLB ranging from 12.1 to 13.5 and the pseudo-ternary phase diagram showed mainly emulsion systems (62%). Topical emulsion showed 390 nm, polydispersity 0.05, zeta potential -25 mV and remained stable for ninety days. The bullfrog oil and topical emulsion did not showed citotoxicity in normal fibroblasts cells. However, these systems showed significantly inhibition of melanoma cells growth. In conclusion, the bullfrog oil presented desirable chemical characteristics required to be used for the development of a pharmaceutical and cosmetic products.

Um novo inibidor de tripsina multifuncional de sementes de Erythrina velutina: caracterizacao e propriedades farmacologicas

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior

Desenvolvimento de filtros cerâmicos impregnados com nanopartículas de prata para desinfecção de água potável

Brazil has vast amounts of hydric resources, whose quality has been deteriorating due to pollutant dumping. Household waste disposal is one of the main sources of water pollution, stimulating bacteria proliferation and introducing microorganisms, including those from fecal matter. Conventional water disinfection methods are a solution, but on the downside, they lead to the formation byproducts hazardous to human health. In this study, aiming to develop bactericidal filters for the disinfection of drinking water; silver nanoparticles were deposited on alumina foams through three routes: sputtering DC, dip coating and in situ chemical reduction of silver nitrate. The depositions were characterized through X-ray diffraction, scanning electron microscopy and EDS element mapping. The influence of the depositions on permeability and mechanical properties of the ceramic foams was assessed and, in sequence, a preliminary antibacterial efficiency analysis was carried out. Characterization results indicate that the chemical reduction routes were efficient in depositing homogeneously distributed silver particles and that the concentration of the metallic precursor salt affects size and morphology of the particles. The antibacterial efficiency analysis indicates that the chemical reduction filters have potential for water disinfection

Quantificação de Fases Cristalinas de Incrustações em Colunas de Produção de Petróleo pelo Método Rietveld

The scale is defined as chemical compounds from inorganic nature, initially soluble in salt solutions, which may precipitate accumulate in columns of production and surface equipment. This work aimd to quantify the crystalline phases of scale through the Rietveld method. The study was conducted in scale derived from columns production wells in development and recipients of pigs. After collecting samples of scale were performed the procedure for separations of inorganic and organic phase and preparation to be analyzed at the X-ray Laboratory. The XRD and XRF techniques were used to monitor whether identifying and quantifying crystalline phases present in the deposits. The SEM technique was used to visualize the morphology of the scales and assess their homogeneity after the milling process. XRD measurements were performed with and without milling and with or without the accessory spinner. For quantify crystalline phases the program DBWStools was used. The procedure for conducting the first refinement was instrumental in setting parameters, then the structural parameters of the phases in the sample and finally the parameters of the function profile used. In the diffraction patterns of samples of scale observed that the best measures were those that passed through the mill and used the accessory spinner. Through the results, it was noted that the quantitative analysis for samples of scale is feasible when need to monitor a particular crystalline phase in a well, pipeline or oil field. Routinely, the quantification of phases by the Rietveld method is hardwork because in many scale was very difficult to identify the crystalline phases present