Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-04-25T20:37:14Z No. of bitstreams: 1 RosimeireFilgueiraCosta_DISSERT.pdf: 1863855 bytes, checksum: 98da8847b8f23900b5d51e026eebbf2e (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-04-27T00:02:09Z (GMT) No. of bitstreams: 1 RosimeireFilgueiraCosta_DISSERT.pdf: 1863855 bytes, checksum: 98da8847b8f23900b5d51e026eebbf2e (MD5) / Made available in DSpace on 2016-04-27T00:02:09Z (GMT). No. of bitstreams: 1 RosimeireFilgueiraCosta_DISSERT.pdf: 1863855 bytes, checksum: 98da8847b8f23900b5d51e026eebbf2e (MD5) Previous issue date: 2015-07-24 / Neste trabalho, foi investigado o efeito da adi??o de poliacrilamida parcialmente hidrolisada (HPAM) e bentonita nas propriedades f?sico-qu?micas de fluidos de perfura??o aquosos. Duas formula??es foram avaliadas: a formula??o F1, que foi utilizada como refer?ncia, contendo carboximetilcelulose (CMC), ?xido de magn?sio (MgO), calcita (carbonato de c?lcio ? CaCO3 ), goma xantana, cloreto de s?dio (NaCl) e triazina (bactericida); e a formula??o F2, contendo HPAM em substitui??o a CMC e bentonita em substitui??o ? calcita. Os fluidos preparados foram caracterizados quanto ?s propriedades reol?gicas, a lubricidade e o volume de filtrado. A calcita foi caracterizada por granulometria e an?lise termogravim?trica (TGA). A formula??o F2 apresentou controle de filtra??o ? temperatura de 93 ?C 34 mL, enquanto a F1 apresentou filtra??o total. O coeficiente de lubricidade da formula??o F2 foi 0, 1623 e o da F1 0, 2542, acarretando uma redu??o de torque de 25% para F1 e de 52% para F2, comparado ? ?gua. Na temperatura de 49 ?C e taxa de cisalhamento 1022 s ?1 , as viscosidades aparentes foram 25, 5 e 48 cP para as formula??es F1 e F2, respectivamente, evidenciando maior resist?ncia t?rmica para F2. Com a comprova??o da maior estabilidade t?rmica de F2, um planejamento fatorial foi realizado, a fim de determinar as concentra??es de HPAM e de bentonita de melhor desempenho nos fluidos. O planejamento estat?stico gerou superf?cies de resposta indicando as melhores concentra??es de HPAM (4, 3 g/L) e de bentonita (28, 5 g/L) para se alcan?ar propriedades melhoradas dos fluidos (viscosidade aparente, viscosidade pl?stica, limite de escoamento e volume de filtrado) com 95% de confian?a, assim como as correla??es entre esses fatores (concentra??es de HPAM e bentonita). Os testes de envelhecimento t?rmico indicaram que as formula??es contendo HPAM e bentonita podem ser utilizadas ? temperatura m?xima de 150 ?C. A an?lise do reboco formado ap?s filtra??o dos fluidos por Difra??o de Raios X indicou intera??es espec?ficas entre a HPAM e a bentonita, justificando a maior estabilidade t?rmica do fluido F2 comparado ao F1, que suporta temperatura m?xima de 93 ?C. / In this study, we investigated the effect of addition of partially hydrolyzed polyacrylamide (HPAM) and bentonite in the physicochemical properties of acquous drilling fluids. Two formulations were evaluated: F1 formulation, which was used as reference, containing carboxymethylcellulose (CMC), magnesium oxide (MgO), calcite (calcium carbonate - CaCO3 ), xanthan gum, sodium chloride (NaCl) and triazine (bactericidal); and F2, containig HPAM steady of CMC and bentonite in substituition of calcite. The prepared fluids were characterized by rheological properties, lubricity and fluid loss. Calcite was characterized by granulometry and thermal gravimetric analysis (TGA). The formulation F2 presented filtration control at 93?C 34 mL while F1 had total filtration. The lubricity coefficient was 0.1623 for F2 and 0.2542 for F1, causing reduction in torque of 25% for F1 and 52 % for F2, compared to water. In the temperature of 49 ?C and shear rate of 1022 s ?1 , the apparent viscosities were 25, 5 and 48 cP for F1 and F2 formulation, respectively, showing greater thermal resistance to F2. With the confirmation of higher thermal stability of F2, factorial design was conducted in order to determine the HPAM and of bentonite concentrations that resulted in the better performance of the fluids. The statistical design response surfaces indicated the best concentrations of HPAM (4.3g/L) and bentonite (28.5 g/L) to achieve improved properties of the fluids (apparent viscosity, plastic viscosity, yield point and fluid loss) with 95% confidence, as well as the correlations between these factors (HPAM and bentonite concentrations). The thermal aging tests indicated that the formulations containing HPAM and bentonite may be used to the maximum temperature until 150 ?C. The analyze of the filter cake formed after filtration of fluids by X-ray diffraction showed specific interactions between the bentonite and HPAM, explaining the greater thermal stability of F2 compared to the fluid F1, that supports maximum temperature of 93 ?C.

Submitted by Sandra Pereira (srpereira@ufrrj.br) on 2016-09-28T13:47:04Z No. of bitstreams: 1 2011- Marcio Osvaldo Lima Magalhaes.pdf: 4632406 bytes, checksum: 8ccefc16f724417fcb426aaf9aac9f4a (MD5) / Made available in DSpace on 2016-09-28T13:47:04Z (GMT). No. of bitstreams: 1 2011- Marcio Osvaldo Lima Magalhaes.pdf: 4632406 bytes, checksum: 8ccefc16f724417fcb426aaf9aac9f4a (MD5) Previous issue date: 2011-12-19 / Coordena??o de Aperfei?oamento de Pessoal de N?vel Superior - CAPES / Despite the known problems caused by the by-products generated from the exploration of oil, this activity will be a part of our reality for the next 50 years. The oil drilling and exploration industry creates a substantial amount of waste that, if not adequately disposed of, could cause environmental problems. One of the main contaminates found in the waste related to oil drilling is the element barium. The purpose of this study was to evaluate the contamination of soil containing barium, its impact on the growth of rice plants (Orysa sativa) and potential risk of contaminating groundwater. This paper was divided into four chapters. The goal of the first chapter was to evaluate the spatial variability of barium levels found in former oil well drilling waste disposal sites. For this study, soil was collected from georeferenced points, analyzed in terms of its pseudo total levels, and prepared for the geochemical fractionation of barium, classifying the material in accordance with resolution 420 of CONAMA [Brazilian National Counsel on the Environment] (2009). In the second chapter, the effect of redox potential in soil on the mobility and absorption of barium by rice, having barium sulfate P.A. as the element?s source, was assessed. The effect was evaluated by performing rice culture pot and column leaching tests. The aim of the third chapter was the characterization and traceability of heavy metals in waste generated during the recovery of oil well drilling fluids. The waste was collected during the drilling of well 7-MGP-98D-BA, where the material was separated by composite sample, based on depth and equipment. In the fourth chapter, the effects of redox potential in soil interaction and heavy metals coming from the waste generated from onshore oil well drilling were analyzed. This chapter was similar to chapter two, with the main difference being the waste generated from well 7-MGP-98D-BA, which supplied the source of barium. The waste materials selected were those that displayed the lowest levels of arsenic, cadmium, barium, lead, and sodium. The obtained results showed that waste generated from oil well drilling contains high levels of barium, and that when disposed of in soil can significantly contribute to site contamination, having used the guiding values of CONAMA (2009) as a reference. As such, the barium present in this area was in the form of low solubility, as evidenced by the geochemical fractionation of the element. It was also observed that the conditions of low values of redox potential (-200 mV) promoted an increase of barium in fractions of greater mobility, causing major losses of the element by leaching, and increased absorption by plants. Among the studied waste materials, the waste from the dehydrator and the centrifuge 1 presented high levels of sodium as its greatest limitation, which affected the development of plants. / Apesar da verifica??o de problemas ocasionados pelo uso de produtos gerados a partir da explora??o do petr?leo, essa atividade ? uma realidade nos pr?ximos 50 anos. A industria de perfura??o e explora??o de petr?leo ? uma atividade que gera muitos residuos que, caso dispostos de forma inadequada, podem ocasionar problemas ambientais. Um dos principais contaminantes relacionados aos res?duos de perfura??o de po?os de petr?leo ? o elemento b?rio. A proposta desse estudo foi de avaliar a contamina??o dos solos com b?rio e seu impacto no desenvolvimento de plantas de arroz (Orysa sativa) e o risco de contamina??o do len?ol fre?tico. Para isso o trabalho foi dividido em quatro cap?tulos. O primeiro cap?tulo teve como objetivo avaliar a variabilidade espacial dos teores de b?rio em antiga ?rea de disposi??o de res?duo de perfura??o de po?os de petr?leo. Nesse estudo foram coletados solos em pontos georreferenciados e analisados quanto aos teores pseudototais e feito o fracionamento geoqu?mico do b?rio, classificando o material de acordo com a resolu??o 420 do Conama (2009). No segunto cap?tulo foi avaliado o efeito do potencial redox do solo na mobilidade e absor??o de b?rio por arroz, tendo como fonte do elelmento o sulfato de b?rio P.A. Esse efeito foi avaliado atrav?s de ensaios em vasos com cultivo de arroz e em colunas de lixivia??o. O terceiro cap?tulo teve como objetivo a caracteriza??o e rastreabilidade de metais pesados em res?duos gerados na recupera??o do fluido de perfura??o de po?os de petr?leo. O res?duo foi coletado durante a perfura??o do po?o 7-MGP-98D-BA, onde os materiais foram separados em amostras compostas em fun??o da profundidade e do equipamento. No quarto cap?tulo foi analisado o efeito do potencial redox na intera??o solo e metais pesados provenientes de res?duos oriundos da perfura??o de po?os de petr?leo ?onshore?. Esse cap?tulo foi semelhante ao cap?tulo 2, diferindo principalmente na fonte de b?rio que foi o res?duo gerado no po?o 7-MGP-98D-BA. Os res?duos selecionados foram os que apresentaram como os mais restrit?vos com rela??o aos teores de ars?nio, c?dmio, b?rio, chumbo e s?dio. Os resultados obtidos evidenciaram que os res?duos oriundos da perfura??o de po?os de petr?leo possuem altos teores de b?rio, que quando dispostos nos solos podem contribuir significativamente para a contamina??o das ?reas, tendo como refer?ncia os valores orientadores do Conama (2009). Entretanto, o b?rio presente nessa ?rea estava sob forma de baixa solubilidade, evidenciada pelo fracionamento geoqu?mico do elemento. Tamb?m foi observado que a condi??o de baixos valores de potencial redox (-200 mV) promoveu o aumento do b?rio nas fra??es de maior mobilidade, ocasionando maiores perdas do elemento por lixivia??o e maior absor??o pelas plantas. Dentre os res?duos estudados, os res?duos do secador e da centr?fuga 1 apresentaram como maior limita??o os altos teores de s?dio, o que afetou o desenvolvimento das plantas.

Submitted by Jorge Silva (jorgelmsilva@ufrrj.br) on 2017-10-04T17:50:04Z No. of bitstreams: 1 2013 - Leilane da SIlva Lima.pdf: 2571314 bytes, checksum: 6a887a80293fe4214d8df0859a55db54 (MD5) / Made available in DSpace on 2017-10-04T17:50:04Z (GMT). No. of bitstreams: 1 2013 - Leilane da SIlva Lima.pdf: 2571314 bytes, checksum: 6a887a80293fe4214d8df0859a55db54 (MD5) Previous issue date: 2013-03-04 / CNPq / A major environmental issue is the impact caused by the extraction of primary materials and the waste disposal. The industry tries to change that with adjustments in the production chain to reduce impacts to the environment. However, this is a subject that has few studies. This study aimed to evaluate the development of rice plants (Oryza sativa) in soils incubated with waste from drilling oil wells, treated by washing to eliminate the influence of sodium and under two moisture conditions. Two residues generated during the drilling of the well 7-SMC- 50D AL were selected. Subsequently, the residue washing was done in water with the 1:5 proportions, to reduce the effects of sodium. Thus, the washing treatment defined two conditions: washed and unwashed residues. The amount of residue added to the soil was set to achieve concentrations of barium of 300 mg kg-1, 600 mg kg -1 and 900 mg kg-1. The soils were kept in two moisture conditions (70% of field capacity and waterlogged to get a reduced condition). During the incubation of vessels the redox potential (Eh) was monitored until values close to -200 mV was reached, in the reduction condition. After reaching these values, we waited up to 30 days before transplanting the rice seedlings and the test starting. Samples were collected from each experimental unit, and the elements barium, iron, manganese, calcium, sodium and potassium were analyzed. The rice was planted, and went throughout the vegetative cycle (approximately 3 months) until the plants were harvested for analysis. The results showed that the residues from the dryer and the centrifuge, with and without washing, in the oxidized condition, did not affect the dry matter yield of the rice plants. However, the soil reduction condition promoted increasing concentrations of barium absorbed by plants, and reduced the iron level. In the treatments with the residue and reduction condition, the solubilization of barium combined with a moderate iron deficiency possible interfered on dry matter production. / Uma grande quest?o ambiental ? o impacto causado pela extra??o de materiais prim?rios e pela deposi??o de res?duos. A ind?stria tenta mudar esse cen?rio com adequa??es ao longo da cadeia produtiva para diminuir os impactos ao meio ambiente. Entretanto, essa ? uma ?rea ainda pouco estudada.Este trabalho teve como objetivo avaliar o desenvolvimento de plantas de arroz (Oryza sativa) em solos incubados comres?duos de perfura??o de po?o de petr?leo tratados com lavagem para eliminar a influ?ncia do s?dio e sob duas condi??es de umidade. Foram selecionados dois res?duos gerados durante a perfura??o do Po?o7-SMC-50D-AL. Posteriormente, foi feita a sua lavagem em ?gua, na propor??o 1:5, visando diminuir os efeitos do s?dio. Dessa forma, o tratamento de lavagem definiu duas condi??es: res?duo lavado e res?duo n?o lavado. A quantidade de res?duo adicionada ao solo foi definida de modo a atingir as concentra??es de b?rio de 300 mg kg-1, 600 mg kg-1 e 900 mg kg-1. Os solos foram mantidos em duas condi??es de umidade (70% da capacidade de campo e reduzido com presen?a de l?mina de ?gua). Durante a incuba??o dos vasos foi monitorado o potencial redox (Eh) at? que, na condi??o de redu??o, fossem atingidos valores pr?ximos de -200mV. Ap?s atingir esses valores, aguardou-se 30 dias para o transplantio das mudas de arroz e in?cio da realiza??o do ensaio. Foram coletadas amostras de cada unidade experimental, onde foram feitas an?lises dos elementos b?rio, ferro, mangan?s, c?lcio, s?dio e pot?ssio. Foi realizado o plantio do arroz, permanecendo durante todo ciclo vegetativo (aproximadamente 3 meses) at? serem colhidas as plantaspara an?lise. Os resultados obtidos demonstraram que os res?duos do secador e da centr?fuga, com e sem lavagem, na condi??o de oxida??o, n?o interferiram na produ??o de mat?ria seca das plantas de arroz. Entretanto, a condi??o de redu??o do solo promoveu o aumento dos teores de b?rio absorvidos pelas plantas e redu??o nos de ferro. Nos tratamentos com res?duo e na condi??o de redu??o, a solubiliza??o de b?rio combinada a uma defici?ncia moderada para ferro levou a uma poss?vel interfer?ncia na produ??o de mat?ria seca.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-01-26T17:52:56Z No. of bitstreams: 1 AngeloAraujoSoares_DISSERT.pdf: 3657002 bytes, checksum: 1a693a97ecee47bfb0e92f21e2c60179 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-01-28T18:59:11Z (GMT) No. of bitstreams: 1 AngeloAraujoSoares_DISSERT.pdf: 3657002 bytes, checksum: 1a693a97ecee47bfb0e92f21e2c60179 (MD5) / Made available in DSpace on 2016-01-28T18:59:11Z (GMT). No. of bitstreams: 1 AngeloAraujoSoares_DISSERT.pdf: 3657002 bytes, checksum: 1a693a97ecee47bfb0e92f21e2c60179 (MD5) Previous issue date: 2014-12-29 / O teste de compatibilidade entre um fluido de perfura??o e uma pasta de cimento ? uma das etapas que antecedem uma opera??o de cimenta??o de po?os de petr?leo. Este teste permite avaliar os principais efeitos que uma contamina??o destes dois fluidos pode ocasionar as propriedades tecnol?gicas de uma pasta de cimento. As intera??es entre uma pasta de cimento e um fluido de perfura??o, devido suas diferentes composi??es qu?micas, podem comprometer as rea??es de hidrata??o do cimento, prejudicando a opera??o de cimenta??o. Desta forma, realizou-se o estudo da compatibilidade de um fluido de perfura??o n?o-aquoso e uma pasta de cimento aditivada. Os procedimentos de prepara??o do fluido de perfura??o n?o-aquoso, da pasta de cimento e de realiza??o do teste de compatibilidade foram realizados conforme estabelecido por normas da ind?stria do petr?leo. Neste teste de compatibilidade avaliou-se as propriedades reol?gicas, o tempo de espessamento, a estabilidade e a resist?ncia ? compress?o das pastas de cimento. Realizou-se tamb?m an?lises de microscopia eletr?nica de varredura e difra??o de raios X das misturas obtidas pelo teste de compatibilidade para se determinar as modifica??es microestruturais nas pastas de cimento. O teste de compatibilidade n?o apresentou mudan?as visuais nas propriedades da pasta de cimento, como a separa??o de fases. Entretanto, ap?s a adi??o de fluido de perfura??o n?o-aquoso ? pasta de cimento houve um aumento do valor da viscosidade pl?stica, do limite de escoamento e da for?a gel. Dentre os principais fatores causadores pode-se citar: a rea??o qu?mica dos componentes presentes no fluido de perfura??o n?o-aquoso, como o emulsificante prim?rio, o agente ?leo molhante e a parafina, com os constituintes qu?micos do cimento. Houve uma redu??o da resist?ncia mec?nica ? compress?o da pasta de cimento ap?s a mistura com este fluido de perfura??o. O teste de espessamento demonstrou que o agente ?leo molhante e a alta salinidade do fluido n?oaquoso possuem a??o aceleradora do tempo de pega da pasta de cimento. A estabilidade da pasta de cimento ? prejudicada ? medida que ocorre o aumento da contamina??o da pasta de cimento com o fluido n?o-aquoso. A difra??o de raios X identificou a forma??o da portlandita e silicato de c?lcio nas amostras contaminadas. A microscopia eletr?nica de varredura confirmou o desenvolvimento das estruturas identificadas na difra??o de raios X e constatou tamb?m a presen?a de microcavidades na pasta de cimento curada. Estas ?ltimas, formadas pela estabiliza??o da emuls?o do fluido de perfura??o na pasta de cimento, corroboram com ? redu??o da resist?ncia mec?nica. O agente ?leo molhante, componente do fluido de perfura??o n?o-aquoso, modificou os processos de hidrata??o do cimento, afetando principalmente o tempo de pega / Compatibility testing between a drilling fluid and a cement slurry is one of the steps before an operation of cementing oil wells. This test allows us to evaluate the main effects that contamination of these two fluids may cause the technological properties of a cement paste. The interactions between cement paste and drilling fluid, because its different chemical compositions, may affect the cement hydration reactions, damaging the cementing operation. Thus, we carried out the study of the compatibility of non-aqueous drilling fluid and a cement slurry additives. The preparation procedures of the non-aqueous drilling fluid, the cement paste and completion of compatibility testing were performed as set out by the oil industry standards. In the compatibility test is evaluated rheological properties, thickening time, stability and compressive strength of cement pastes. We also conducted analyzes of scanning electron microscopy and X-ray diffraction of the mixture obtained by the compatibility test to determine the microstructural changes in cement pastes. The compatibility test showed no visual changes in the properties of the cement paste, as phase separation. However, after the addition of nonaqueous drilling fluid to cement slurry there was an increased amount of plastic viscosity, the yield point and gel strength. Among the major causative factors can include: chemical reaction of the components present in the non-aqueous drilling fluid as the primary emulsifier, wetting agent and paraffin oil, with the chemical constituents of the cement. There was a reduction in the compressive strength of the cement paste after mixing with this drilling fluid. Thickening test showed that the oil wetting agent and high salinity of the non-aqueous fluid have accelerating action of the handle of the cement paste time. The stability of the cement paste is impaired to the extent that there is increased contamination of the cement slurry with the nonaqueous fluid. The X-ray diffraction identified the formation of portlandite and calcium silicate in contaminated samples. The scanning electron microscopy confirmed the development of the identified structures in the X-ray diffraction and also found the presence of wells in the cured cement paste. The latter, formed by the emulsion stability of the drilling fluid in the cement paste, corroborate the reduction of mechanical strength. The oil wetting agent component of the non-aqueous drilling fluid, the modified cement hydration processes, mainly affecting the setting time.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-02-05T22:26:11Z No. of bitstreams: 1 LaisSibaldoRibeiro_DISSERT.pdf: 1705871 bytes, checksum: 948e4beb72da1823f2fb24c8464e7377 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-02-16T19:20:45Z (GMT) No. of bitstreams: 1 LaisSibaldoRibeiro_DISSERT.pdf: 1705871 bytes, checksum: 948e4beb72da1823f2fb24c8464e7377 (MD5) / Made available in DSpace on 2016-02-16T19:20:45Z (GMT). No. of bitstreams: 1 LaisSibaldoRibeiro_DISSERT.pdf: 1705871 bytes, checksum: 948e4beb72da1823f2fb24c8464e7377 (MD5) Previous issue date: 2015-02-03 / Ag?ncia Nacional do Petr?leo - ANP / Os fluidos de perfura??o t?m import?ncia fundamental nas atividades petrol?feras, uma vez que, s?o respons?veis por permitir a retirada dos cascalhos provenientes da perfura??o, a manuten??o da press?o e a estabilidade do po?o, evitando desmoronamentos e influxo de fluido na forma??o rochosa, al?m da lubrifica??o e resfriamento da broca. Existem basicamente tr?s tipos de fluidos de perfura??o, s?o eles: de base aquosa, de base n?o aquosa e aerado. O fluido de perfura??o de base aquosa ? amplamente usado por ser menos agressivo ao meio ambiente e apresentar excelente estabilidade e inibi??o (em fluidos aquosos inibidos), entre outras qualidades. A ?gua produzida ? gerada simultaneamente com o petr?leo durante a produ??o e possui grandes concentra??es de metais e contaminantes, sendo necess?rio trat?-la para descart?-la. A ?gua produzida dos campos de Urucu-AM e do Riacho da Forquilha-RN possuem elevadas concentra??es de contaminantes, metais e sais, como de c?lcio e magn?sio, dificultando o seu tratamento e descarte. Com isso, o objetivo desse trabalho foi analisar o uso da ?gua produzida sint?tica com caracter?sticas semelhantes ?s ?guas produzidas de UrucuAM e de Riacho da Forquilha-RN na formula??o de um fluido de perfura??o aquoso, observando nas ?guas sint?ticas de Urucu-AM e de Riacho da forquilha-RN a influ?ncia da varia??o da concentra??o de c?lcio e de magn?sio nos testes de reologia e filtrado. Realizouse um planejamento experimental fatorial simples 32 para modelagem estat?stica dos dados. Os resultados mostraram que a varia??o das concentra??es de c?lcio e magn?sio n?o influencia na reologia do fluido, onde a viscosidade pl?stica, viscosidade aparente e os g?is inicial e final n?o oscilaram significativamente. Para o filtrado, a concentra??o de c?lcio influenciou de forma linear na concentra??o de cloreto, onde quanto maior a concentra??o de c?lcio, maior a concentra??o de cloreto no filtrado. Para o volume de filtrado foi observado nos fluidos formulados com ?gua sint?tica de Urucu-AM que a concentra??o de c?lcio influencia de forma quadr?tica, isso significa que elevadas concentra??es de c?lcio interferem no poder de reten??o dos inibidores de filtrado utilizados na formula??o do fluido, j? nos fluidos formulados a partir de ?gua produzida sint?tica de Riacho da Forquilha-RN, a concentra??o de c?lcio influencia de forma linear. A concentra??o de magn?sio influenciou apenas na concentra??o de cloreto de forma quadr?tica nos fluidos formulados a partir da ?gua sint?tica de Urucu-AM. O fluido com concentra??o m?xima de magn?sio (9,411g/L), e concentra??o m?nima de c?lcio (0,733g/L) apresentou bons resultados. Portanto, uma ?gua produzida com concentra??o m?xima de magn?sio de 9,411g/L e m?xima de c?lcio de 0,733g/L pode ser utilizada para formula??o de fluidos de perfura??o de base aquosa, conferindo propriedades adequadas a esse tipo de fluido. / Drilling fluids have fundamental importance in the petroleum activities, since they are responsible for remove the cuttings, maintain pressure and well stability, preventing collapse and inflow of fluid into the rock formation and maintain lubrication and cooling the drill. There are basically three types of drilling fluids: water-based, non-aqueous and aerated based. The water-based drilling fluid is widely used because it is less aggressive to the environment and provide excellent stability and inhibition (when the water based drilling fluid is a inhibition fluid), among other qualities. Produced water is generated simultaneously with oil during production and has high concentrations of metals and contaminants, so it?s necessary to treat for disposal this water. The produced water from the fields of Urucu-AM and Riacho da forquilha-RN have high concentrations of contaminants, metals and salts such as calcium and magnesium, complicating their treatment and disposal. Thus, the objective was to analyze the use of synthetic produced water with similar characteristics of produced water from Urucu-AM and Riacho da Forquilha-RN for formulate a water-based drilling mud, noting the influence of varying the concentration of calcium and magnesium into filtered and rheology tests. We conducted a simple 32 factorial experimental design for statistical modeling of data. The results showed that the varying concentrations of calcium and magnesium did not influence the rheology of the fluid, where in the plastic viscosity, apparent viscosity and the initial and final gels does not varied significantly. For the filtrate tests, calcium concentration in a linear fashion influenced chloride concentration, where when we have a higher concentration of calcium we have a higher the concentration of chloride in the filtrate. For the Urucu?s produced water based fluids, volume of filtrate was observed that the calcium concentration influences quadratically, this means that high calcium concentrations interfere with the power of the inhibitors used in the formulation of the filtered fluid. For Riacho?s produced water based fluid, Calcium?s influences is linear for volume of filtrate. The magnesium concentration was significant only for chloride concentration in a quadratic way just for Urucu?s produced water based fluids. The mud with maximum concentration of magnesium (9,411g/L), but minimal concentration of calcium (0,733g/L) showed good results. Therefore, a maximum water produced by magnesium concentration of 9,411g/L and the maximum calcium concentration of 0,733g/L can be used for formulating water-based drilling fluids, providing appropriate properties for this kind of fluid.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-04-01T00:12:18Z No. of bitstreams: 1 RavennaMariaMonteiroBarros_DISSERT.pdf: 14068389 bytes, checksum: 8ee91e6f3ca8a944dc4350382caa62de (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-04-06T00:06:40Z (GMT) No. of bitstreams: 1 RavennaMariaMonteiroBarros_DISSERT.pdf: 14068389 bytes, checksum: 8ee91e6f3ca8a944dc4350382caa62de (MD5) / Made available in DSpace on 2016-04-06T00:06:40Z (GMT). No. of bitstreams: 1 RavennaMariaMonteiroBarros_DISSERT.pdf: 14068389 bytes, checksum: 8ee91e6f3ca8a944dc4350382caa62de (MD5) Previous issue date: 2015-04-20 / Durante suas opera??es, a ind?stria petrol?fera gera uma grande quantidade de res?duos, dentre eles, o cascalho de perfura??o. O controle dos impactos ambientais causados devido a esses res?duos representa um grande desafio. Tais impactos podem ser minimizados quando ? dado um gerenciamento adequado, sendo convenientemente tratados e corretamente dispostos ou quando reciclados. As propriedades dos materiais cer?micos podem ser fortemente influenciadas quando adicionado um res?duo ? sua composi??o. Este trabalho tem como objetivo estudar a incorpora??o do res?duo de cascalho de perfura??o de po?os de petr?leo na massa padr?o para fabrica??o de cer?mica vermelha proveniente de uma ind?stria cer?mica do munic?pio de S?o Gon?alo do Amarante/RN. O sucesso da incorpora??o pode minimizar custos na produ??o das pe?as cer?micas e diminuir os impactos ambientais gerados pelo res?duo. As mat?rias-primas utilizadas foram coletadas e caracterizadas, sendo formuladas com os percentuais de 0, 20 e 40% em substitui??o de massa por res?duo, foram sinterizadas nas temperaturas de 900, 1.010 e 1.120 ?C utilizando patamares de queima de 30min, 1h30min e 2h30min com base em um planejamento fatorial 2?. Em seguida amostras foram submetidas aos ensaios de Absor??o de ?gua, Retra??o Linear de Queima, Tens?o de Ruptura ? Flex?o, Porosidade Aparente, Massa Especifica Aparente e Microscopia Eletr?nica de Varredura (MEV) da se??o de ruptura. Os resultados mostraram que ? poss?vel a utiliza??o do res?duo para a fabrica??o de produtos da cer?mica vermelha (telhas, tijolos maci?os e tijolos furados) substituindo-se a argila em at? 40%, atendendo aos requisitos exigidos pela norma e pela literatura para as propriedades tecnol?gicas do produto final. / During its operations, the oil industry generates a lot of waste, including gravel from drilling. Control of environmental impacts caused by this waste represents a major challenge. Such impacts can be minimized when it is given an appropriate management by being properly treated and properly disposed or recycled. The properties of these materials can be greatly influenced when a waste is added to its composition. This work aims to study the incorporation of gravel waste oil-well drilling in the standard body for production of red ceramic from a ceramic industry in S?o Gon?alo do Amarante / RN. The success of the incorporation can minimize costs in the production of ceramic pieces and reduce the environmental impacts caused by waste. The raw materials used were collected, characterized, and formulated with the percentages of 0%, 20% and 40% by weight of substitution of residue were synthesized at temperatures of 900, 1.010 and 1.120 ?C using 30 minute firing intervals, 1 hour and 30min and 2 hours and 30 minutes, based on a factorial design 2?. Samples were then subjected to the tests of Water Absorption, Linear Retraction Firing, Flexural Rupture Strength, Apparent Porosity and Apparent Specific mass and Scanning Electron Microscopy (SEM) of break section. The results showed that the use of the residue for the manufacture of the ceramic products is possible (tiles, bricks and massive hollow bricks) replacing the clay to 40%, meeting the requirements of the standard and the literature for the technological properties of the final product.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-04-25T20:37:14Z No. of bitstreams: 1 GisellePereiraMoreira_DISSERT.pdf: 2433742 bytes, checksum: d2cf05db4d69f9db9774ee92c4f96457 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-04-26T23:11:44Z (GMT) No. of bitstreams: 1 GisellePereiraMoreira_DISSERT.pdf: 2433742 bytes, checksum: d2cf05db4d69f9db9774ee92c4f96457 (MD5) / Made available in DSpace on 2016-04-26T23:11:44Z (GMT). No. of bitstreams: 1 GisellePereiraMoreira_DISSERT.pdf: 2433742 bytes, checksum: d2cf05db4d69f9db9774ee92c4f96457 (MD5) Previous issue date: 2010-02-12 / Ag?ncia Nacional do Petr?leo - ANP / Este trabalho descreve a s?ntese e o estudo da aplica??o em fluido de perfura??o de um novo tensoativo (Tri-?ster Lipof?lico - TEL) obtido a partir de ?cido c?trico com octanol. A rea??o foi acompanhada por cromatografia em camada delgada (CCD) e o produto, ap?s a purifica??o, foi caracterizado por resson?ncia magn?tica nuclear de pr?ton e carbono (RMN H1 e C 13), an?lise termogravim?trica e de tens?o superficial em ?leo e ?gua. Atrav?s de testes comparativos com dois produtos comerciais usados em campo, avaliou-se o desempenho, como emulsificante, do TEL em fluidos ? base de ?ster, n-parafina e biodiesel de mamona nas raz?es ?leo/?gua (ROA) 70/30 e 60/40. Posteriormente, esses fluidos foram envelhecidos em estufa rotativa a 200 ?F durante 16 h, sendo ent?o realizadas medidas reol?gicas e de estabilidade el?trica a 135 ?F, separa??o de fase ap?s sete (7) dias em repouso e volume de filtrado em alta press?o e alta temperatura. O comportamento reol?gico foi avaliado a partir das curvas de fluxos. Observou-se, tamb?m, que estes apresentaram comportamento similares aos dos fluidos usados em campo (Binghamiano e pseudopl?stico com limite de escoamento). Os testes laboratoriais mostraram que o TEL reduziu o volume de filtrado e promoveu um aumento de estabilidade mec?nica e t?rmica. / This work describes the synthesis and study of the application of a new surfactant (Triester Lipophilic ? TEL) obtained by citric acid with octanol. It is reaction was followed by thin layer chromatography (TLC) and after purification the product was characterized by proton and 13 ? carbon nuclear magnetic resonance spectroscopy ( H and 13C NMR), thermogravimetric analysis (TGA) and surface tension analysis of oil-in-water emulsions. The TEL performance as surfactant in ester, n-paraffin and biodiesel based drilling fluids on the 70/30 and 60/40 water- oil rations (WOR) was evaluated by comparative tests of two commercial products used in the fields. These drilling fluids were aged in roller oven at 200 0 F during 16 h. The rheological and electric stability measurements were carried out at 135 ?F, the phase separation was evaluated after seven days at rest and the filtrate volume of drilling fluids was determined at high temperature and high pressure. The rheological behavior of the drilling fluids was evaluated by the flow curves. The results showed that the drilling fluids studied here presented Binghamian behavior as well as the used in the oil fields. The laboratory tests showed that the TEL reduced the filtrate volume and promoted the enhance of the thermal and mechanical stabilities.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-07-08T20:49:48Z No. of bitstreams: 1 LisztYeltsinCoutinhoMadruga_DISSERT.pdf: 2271075 bytes, checksum: b618178f5d7788b3f44ca35a53e1646c (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-07-11T21:22:52Z (GMT) No. of bitstreams: 1 LisztYeltsinCoutinhoMadruga_DISSERT.pdf: 2271075 bytes, checksum: b618178f5d7788b3f44ca35a53e1646c (MD5) / Made available in DSpace on 2016-07-11T21:22:52Z (GMT). No. of bitstreams: 1 LisztYeltsinCoutinhoMadruga_DISSERT.pdf: 2271075 bytes, checksum: b618178f5d7788b3f44ca35a53e1646c (MD5) Previous issue date: 2016-01-14 / Nas opera??es de perfura??o de po?os, s?o frequentes os problemas provocados pela contamina??o do fluido de perfura??o. A dissolu??o de ?ons provenientes das forma??es geol?gicas prejudica as propriedades reol?gicas e de filtra??o dos fluidos. Esses ?ons blindam as cargas dos pol?meros i?nicos, podendo levar a sua precipita??o. Neste trabalho foi realizado um estudo criterioso sobre a estabilidade das propriedades de solu??es aquosas e de fluidos de perfura??o aquosos na presen?a de pol?meros carboxilados e sulfatados, empregando a carboximetilcelulose e a kappa-carragenana como compostos modelo de pol?mero carboxilado e sulfatado, respectivamente. Os efeitos da for?a i?nica do meio aquoso contendo ?ons Na+, Mg2+ e Ca2+ sobre as propriedades reol?gicas das solu??es polim?ricas e dos fluidos de perfura??o foram avaliados variando a concentra??o dos sais, pH e temperatura. Foi observado que os fluidos com ?-carragenana sofreram menor influ?ncia frente ? contamina??o pelos ?ons em pH 9 a 10, mesmo em maiores concentra??es, por?m maior influ?ncia em pH >11. Os fluidos contendo carboximetilcelulose se mostraram mais sens?veis ? contamina??o, com redu??o brusca da viscosidade e aumento significativo do volume de filtrado, enquanto que os fluidos ? base do pol?mero sulfatado kappa-carragenana apresentaram evid?ncias de intera??o com c?tions com preserva??o das propriedades reol?gicas e maior estabilidade no volume de filtrado. / In the well drilling operations problems caused by contamination of the drilling fluid are common. The dissolution of ions from the geological formations affects the rheological and filtration properties of the fluids. These ions shield the charges of ionic polymers, leading to its precipitation. In this work was performed a detailed study on the stability of the properties of aqueous solutions and aqueous drilling fluids in the presence of sulphated and carboxylated polymers, using carboxymethylcellulose and kappa-carrageenan as polymer compounds carboxylated and sulfated model, respectively. The effects of ionic strength of the aqueous medium containing Na+, Mg2+ and Ca2+ on rheological properties of the polymer and drilling fluids solutions were evaluated by varying the concentration of salts, pH and temperature. It was observed that the fluids with ?-carrageenan suffered less influence against the contamination by the ions at pH 9 to 10, even at higher concentrations, but higher influence on pH> 11. The fluids containing carboxymethylcellulose were more sensitive to contamination, with rapid reduction in viscosity and significant increase of the filtrate volume, while the fluid based polymer sulfated kappa-carrageenan showed evidence of interaction with cations and preserve the rheological properties and improved stability the volume of filtrate.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2016-07-22T15:10:02Z No. of bitstreams: 1 PauloCesarFrancaDaCamara_DISSERT.pdf: 1632237 bytes, checksum: 8e0cfc36c6d0195008822612bbadae28 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2016-07-27T19:54:25Z (GMT) No. of bitstreams: 1 PauloCesarFrancaDaCamara_DISSERT.pdf: 1632237 bytes, checksum: 8e0cfc36c6d0195008822612bbadae28 (MD5) / Made available in DSpace on 2016-07-27T19:54:25Z (GMT). No. of bitstreams: 1 PauloCesarFrancaDaCamara_DISSERT.pdf: 1632237 bytes, checksum: 8e0cfc36c6d0195008822612bbadae28 (MD5) Previous issue date: 2016-01-13 / O avan?o das perfura??es em po?os mais profundos tem requerido materiais cada vez mais termoest?veis que v?o ao encontro ?s condi??es de po?o. A utiliza??o de fluidos sint?ticos, que costumam apresentar uma boa estabilidade qu?mica, esbarra nas limita??es ambientais, al?m de gerarem mais descarte e requererem um tratamento oneroso dos cascalhos perfurados, que s?o por vezes n?o eficientes e exigem componentes mec?nicos que dificultam a opera??o. A ado??o de fluidos aquosos, geralmente, implica na utiliza??o do lignossulfonato de cromo, empregado como dispersante, que confere estabilidade nas propriedades reol?gicas e controle de filtrado de fluidos submetidos a altas temperaturas e press?es. Por?m, devido ao impacto ambiental associado ? utiliza??o de compostos cromados, o setor de perfura??o necessita de alternativas que mantenham ?ntegras as propriedades e garantam sucesso da opera??o tendo em vista a forte influencia da temperatura sob a viscosidade de fluidos aquosos e nos pol?meros empregados nesse tipo de fluido, frequentemente de origem natural, passivos de hidr?lise e degrada??o biol?gica. Pol?meros vin?licos, por possu?rem cadeia predominantemente carb?nica, resistem a maiores temperaturas. Al?m disso, a aus?ncia de liga??es acetal diminui a sensibilidade a ataques por bact?rias. Medidas reol?gicas dos fluidos de perfura??o utilizando polivinilpirrolidona (PVP), poliacrilamidas parcialmente hidrolisada e argila, como principais constituintes, foram determinadas atrav?s do viscos?metro rotativo da Fann, modelo 35A, e o volume de filtrado obtido atrav?s de filtra??o ATAP, seguindo a norma API 13B-2. Observou-se que o novo sistema de fluido em que o PVP de alta massa molar foi utilizado apresentou maiores valores de viscosidade, g?is e limite de escoamento, por efeito da flocula??o argilosa. Por sua vez, o PVP de baixa massa molar contribuiu para a forma??o de sistemas dispersos com menores valores nas propriedades reol?gicas e de filtrado. Ambos os sistemas apresentaram ganho de estabilidade t?rmica, mantendo os par?metros reol?gicos est?veis. Os resultados foram ainda corroborados atrav?s de ensaios de inchamento linear de argila.O avan?o das perfura??es em po?os mais profundos tem requerido materiais cada vez mais termoest?veis que v?o ao encontro ?s condi??es de po?o. A utiliza??o de fluidos sint?ticos, que costumam apresentar uma boa estabilidade qu?mica, esbarra nas limita??es ambientais, al?m de gerarem mais descarte e requererem um tratamento oneroso dos cascalhos perfurados, que s?o por vezes n?o eficientes e exigem componentes mec?nicos que dificultam a opera??o. A ado??o de fluidos aquosos, geralmente, implica na utiliza??o do lignossulfonato de cromo, empregado como dispersante, que confere estabilidade nas propriedades reol?gicas e controle de filtrado de fluidos submetidos a altas temperaturas e press?es. Por?m, devido ao impacto ambiental associado ? utiliza??o de compostos cromados, o setor de perfura??o necessita de alternativas que mantenham ?ntegras as propriedades e garantam sucesso da opera??o tendo em vista a forte influencia da temperatura sob a viscosidade de fluidos aquosos e nos pol?meros empregados nesse tipo de fluido, frequentemente de origem natural, passivos de hidr?lise e degrada??o biol?gica. Pol?meros vin?licos, por possu?rem cadeia predominantemente carb?nica, resistem a maiores temperaturas. Al?m disso, a aus?ncia de liga??es acetal diminui a sensibilidade a ataques por bact?rias. Medidas reol?gicas dos fluidos de perfura??o utilizando polivinilpirrolidona (PVP), poliacrilamidas parcialmente hidrolisada e argila, como principais constituintes, foram determinadas atrav?s do viscos?metro rotativo da Fann, modelo 35A, e o volume de filtrado obtido atrav?s de filtra??o ATAP, seguindo a norma API 13B-2. Observou-se que o novo sistema de fluido em que o PVP de alta massa molar foi utilizado apresentou maiores valores de viscosidade, g?is e limite de escoamento, por efeito da flocula??o argilosa. Por sua vez, o PVP de baixa massa molar contribuiu para a forma??o de sistemas dispersos com menores valores nas propriedades reol?gicas e de filtrado. Ambos os sistemas apresentaram ganho de estabilidade t?rmica, mantendo os par?metros reol?gicos est?veis. Os resultados foram ainda corroborados atrav?s de ensaios de inchamento linear de argila. / The advance of drilling in deeper wells has required more thermostable materials. The use of synthetic fluids, which usually have a good chemical stability, faces the environmental constraints, besides it usually generate more discharge and require a costly disposal treatment of drilled cuttings, which are often not efficient and require mechanical components that hinder the operation. The adoption of aqueous fluids generally involves the use of chrome lignosulfonate, used as dispersant, which provides stability on rheological properties and fluid loss under high temperatures and pressures (HTHP). However, due to the environmental impact associated with the use of chrome compounds, the drilling industry needs alternatives that maintain the integrity of the property and ensure success of the operation in view of the strong influence of temperature on the viscosity of aqueous fluids and polymers used in these type fluids, often polysaccharides, passives of hydrolysis and biological degradation. Therefore, vinyl polymers were selected for this study because they have predominantly carbon chain and, in particular, polyvinylpyrrolidone (PVP) for resisting higher temperatures and partially hydrolyzed polyacrylamide (PHPA) and clay by increasing the system's viscosity. Moreover, the absence of acetal bonds reduces the sensitivity to attacks by bacteria. In order to develop an aqueous drilling fluid system for HTHP applications using PVP, HPAM and clay, as main constituents, fluid formulations were prepared and determined its rheological properties using rotary viscometer of the Fann, and volume filtrate obtained by filtration HTHP following the standard API 13B-2. The new fluid system using polyvinylpyrrolidone (PVP) with high molar weight had higher viscosities, gels and yield strength, due to the effect of flocculating clay. On the other hand, the low molecular weight PVP contributed to the formation of disperse systems with lower values in the rheological properties and fluid loss. Both systems are characterized by thermal stability gain up to around 120 ? C, keeping stable rheological parameters. The results were further corroborated through linear clay swelling tests.

Submitted by Automa??o e Estat?stica (sst@bczm.ufrn.br) on 2017-08-01T13:13:46Z No. of bitstreams: 1 NarioCezarCamaraAlves_DISSERT.pdf: 3724020 bytes, checksum: 7d9bb0f760270e1cb1c18ea011288bb0 (MD5) / Approved for entry into archive by Arlan Eloi Leite Silva (eloihistoriador@yahoo.com.br) on 2017-08-03T23:20:45Z (GMT) No. of bitstreams: 1 NarioCezarCamaraAlves_DISSERT.pdf: 3724020 bytes, checksum: 7d9bb0f760270e1cb1c18ea011288bb0 (MD5) / Made available in DSpace on 2017-08-03T23:20:46Z (GMT). No. of bitstreams: 1 NarioCezarCamaraAlves_DISSERT.pdf: 3724020 bytes, checksum: 7d9bb0f760270e1cb1c18ea011288bb0 (MD5) Previous issue date: 2016-12-20 / Dois campos de pesquisas s?o essenciais para o mercado do petr?leo nos dias atuais: otimiza??o de custos e quest?es ambientais. Nas opera??es de perfura??o de po?os o sistema de fluido se mostra como sendo essencial, e assim requer uma otimiza??o cont?nua. Fluidos de perfura??o ? base org?nica s?o largamente utilizados nestas opera??es, onde, ap?s a sua utiliza??o, se tornam um passivo caro e poluente. Atualmente o tratamento realizado neste tipo de fluido ? somente de corre??o, o que requer, geralmente, grandes quantidades de insumos, elevando ainda mais o custo do Sistema de Fluidos para a opera??o de perfura??o. Com isso, o objetivo deste trabalho foi desenvolver um m?todo de recupera??o de fluidos de perfura??o n?o aquosos atrav?s da quebra da emuls?o de ?gua em ?leo, utilizando como agente desemulsificante sistemas microemulsionados. Para a obten??o desta microemuls?o estudou-se qualitativamente a influ?ncia de diferentes tensoativos na separa??o de fases do fluido e definiu-se o de melhor efici?ncia (ULX 95). Para mapeamento do fluido utilizado nos ensaios foram feitas an?lises de reologia, raz?o de ?gua/?leo/s?lidos, salinidade e Estabilidade El?trica. Para o estudo da quebra de emuls?o variou-se: a composi??o do sistema microemulsionado para o tensoativo ULX 95, a fase aquosa da microemuls?o atrav?s da utiliza??o ou n?o de sal (CaCl2), a propor??o sistema microemulsionado/fluido e a temperatura no momento da mistura. Tamb?m foram feitos testes para a caracteriza??o das fases obtidas ap?s o ensaio de quebra, assim como a possibilidade de reutiliza??o do fluido n?o-aquoso recuperado. Os testes de reutiliza??o do fluido n?o aquoso recuperado obtiveram resultados satisfat?rios. / There are two research fields essential for the oil market: cost optimization and environmental issues. In the well drilling operations the fluid system is shown to be essential, and thus requires a continuous optimization. Organic based drilling fluids are widely used in these operations, which, after use, become expensive and polluting liabilities. Currently the treatment performed in this type of fluid is only correction, which usually requires large quantities of inputs, further increasing the cost of Fluid System for the drilling operation. Thus, the aim of this study was to develop a method of recovery of non-aqueous drilling fluids through the breaking of the water in oil emulsion using as demulsifying agent microemulsions systems. To obtain the microemulsion system qualitative studies were performed where the influence of different surfactants in the phase separation of the fluid were studied and defined the best efficiency (RNX 95). For mapping of the fluid used in the tests were made rheology analysis, ratio of water / oil / solids, salinity, and electrical stability to study the emulsion breaking was varied: the composition of microemulsion system for the surfactant (RNX 95), the aqueous phase of the microemulsion by using or not salt (CaCl2), the rate microemulsion / fluid system and the temperature at mixture. Test have also been made to the characterization of phases obtained after breaking test, as well as the possibility of reusing the non-aqueous fluid recovered. The tests had a satisfactory result.