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Made available in DSpace on 2015-03-26T14:02:19Z (GMT). No. of bitstreams: 1 texto completo.pdf: 1285438 bytes, checksum: 9ee3885cc388e9abcdec1aac69248461 (MD5) Previous issue date: 2014-06-30 / The aim of this work was to verify the occurrence of bovine brucellosis in dairy cows in the municipalities of Unaí and Buritis using the milk ring test (TAL). 423 milk samples collected were analyzed for the period from February 5 to April 3, 2014, at the dairy receiving platform and in the milk producing communities. Of these 423 samples, 87 were derived from the municipality of Buritis and 336 from Unaí. Of the samples derived in Unaí, 200 were collected in the milk platform of different regions of the municipality; 92 of the community of Pico; and 44 in Associação do Funil. TAL was performed stratifying positive samples in crosses. Of total samples analyzed, 73 showed positive results, corresponding to 17.25% of total. In the samples of the municipalities of Buritis and Unaí, 18.30% and 16.96% of the results were positive, respectively. In the municipality of Unaí, Associação do Funil was the community with the highest occurrence of the disease, 38.64%, while in the community of Pico the incidence was of 16.30% and in the other regions of the municipality, 12.5% of the results were positive. The samples of Associação do Funil, with 38.64% of positive results, are from small farms producing up to 300 L of milk and storing the product in cans. It is likely, therefore, that the low volume of milk, acidification, the presence of milk with mastitis, and even with colostrum, have contributed to an increase in false-positive results in this Associação. The national program for prevention of brucellosis should be intensified in the associations of small milk producers and properties with a positive result with three crosses, since the program more safely reduces the occurrence of false-positive results; however, the AAT test should be performed as confirmatory. / O objetivo neste trabalho foi verificar a ocorrência de brucelose bovina em vacas leiteiras nos municípios de Unaí e Buritis utilizando-se teste do anel do leite (TAL). Foram analisadas 423 amostras de leite coletadas no período de 5 de fevereiro a 3 de abril de 2014,na plataforma de recepção do laticínio e nas comunidades produtoras de leite. Dessas 423 amostras, 87 foram oriundas do município de Buritis e 336, de Unaí. Das amostras obtidas em Unaí, 200 foram coletadas na plataforma de leite de diferentes regiões do município; 92, da comunidade do Pico; e 44, na Associação do Funil. O TAL foi realizado estratificando-se as amostras positivas em cruzes. Do total de amostras analisadas, 73 apresentaram resultados positivos, correspondendo a 17,25% do total. Nas amostras dos municípios de Buritis e Unaí, 18,30% e 16,96% dos resultados foram positivos, respectivamente. No município de Unaí, a Associação do Funil foi a comunidade com maior ocorrência da doença, 38,64%, enquanto na comunidade do Pico a incidência foi de 16,30% e nas outras regiões do município, 12,5% dos resultados foram positivos. As amostras da Associação do Funil, com 38,64% de resultados positivos, são oriundas de pequenas propriedades, produtoras de até 300 L de leite e que armazenam o produto em latões. É provável, portanto, que o baixo volume de leite, a acidificação, a presença de leite com mamite, e até com colostro, tenham contribuído para o aumento de resultados falso-positivos nessa associação. O programa nacional de prevenção à brucelose deve ser intensificado nas associações de pequenos produtores de leite e nas propriedades com resultado positivo com três cruzes, uma vez que o programa reduz com maior segurança a ocorrência de resultados falsos-positivos,no entanto, deve-se realizar o teste AAT como confirmatório.

Submitted by AMÉRICO BIANCALANA NETO null (abiancalana@confab.com.br) on 2016-09-21T15:55:15Z No. of bitstreams: 1 DISSERTAÇÃO_Américo Biancalana Neto.pdf: 6507235 bytes, checksum: 42c17d17ef5a510dd34876071a8ff043 (MD5) / Approved for entry into archive by Juliano Benedito Ferreira (julianoferreira@reitoria.unesp.br) on 2016-09-26T19:52:21Z (GMT) No. of bitstreams: 1 biancalananeto_a_me_guara.pdf: 6507235 bytes, checksum: 42c17d17ef5a510dd34876071a8ff043 (MD5) / Made available in DSpace on 2016-09-26T19:52:21Z (GMT). No. of bitstreams: 1 biancalananeto_a_me_guara.pdf: 6507235 bytes, checksum: 42c17d17ef5a510dd34876071a8ff043 (MD5) Previous issue date: 2016-07-22 / Os processos tradicionais de produção de tubos API 5CT N80Q envolvem processos de bobinamento e desbobinamento, conformação por dobramento, soldagem, etapas de usinagem e expansão dos diâmetros interno e externo, tratamentos térmicos de têmpera e revenimento e endireitamento. Essas etapas são responsáveis por introduzir tensões residuais no material constituinte do tubo. Estas tensões residuais podem alcançar valores próximos aos do limite de escoamento do material base do tubo, podendo produzir distorções geométricas, falhas prematuras, baixa resistência à corrosão, e diminuição na sua capacidade de absorção de cargas em trabalho. O método mais utilizado para alívio de tensões é o tratamento térmico. Porém, a aplicação de vibrações mecânicas, (Vibratory Stress Rielif) para reduzir e redistribuir as tensões residuais em estruturas conformadas a frio e em estruturas soldadas, tem sido utilizada com sucesso em várias partes do mundo, principalmente nos Estados Unidos, China e Canada. Para verificar a viabilidade deste processo, como um método alternativo para o alivio de tensões, selecionamos um tubo API 5CT 80NQ, com diâmetro de 178 mm com 8,05 mm de espessura e 3000 mm de comprimento. Os ensaios de vibração foram executados na frequência de ressonância do tubo, através de um indutor de vibração montado no seu comprimento médio, dentro de um intervalo de tempo correspondente ao seu peso. Comparando os valores de tensões residuais existentes no tubo antes e após o tratamento de vibração conseguimos uma redução média de 16% no valor das mesmas. Para a caracterização mecânica do tubo, antes e depois do processo vibratório, foram realizados os seguintes ensaios conforme a norma API 5CT 2001: impacto Charpy “V”, ensaios de tração e dureza Rockwell C, tanto no metal base do tubo, como na região da solda. Foi realizada, também, a sua caracterização micro estrutural através, microscopia ótica, antes e depois dos ensaios de vibração. Para avaliação das tensões residuais, antes e após os ensaios de vibração, foi utilizado o método de secção longitudinal de um anel (splitting ring test) conforme a norma ASTM EN 1928-13. / The traditional production processes API 5CT N80Q pipes involve coiling and uncoiling processes the plate, conformation by bending, welding, machining steps and expansion of its internal and external diameters, heat treatment of quenching and tempering and straightening. These steps are responsible for introducing residual stresses in the material of the tube. These residual stresses can reach values close to the yield strength of the pipe`s base material and may produce geometric distortions, premature failure, low corrosion resistance and reduction its capacity of absorption loads in the work. The most widely used method for relieving stress is the heat treatment. The application of mechanical vibrations, Vibratory stress relief ( VSR), to reduce and redistribute the residual stresses in cold shaped structures and welded structures, has been used with success in various parts of the world, especially the United States, China and Canada. Thus, the mechanical vibration, Vibratory stress relief (VSR), can prove to be an interesting process to relieve stress in the tubes. To verify the feasibility of this process, as an alternative method for the relief of stresses, we selected an API 5CT 80NQ tube with a diameter of 178 mm, with 8.05 mm thickness and 3000 mm in length. Vibration tests were performed in pipe resonance frequency, via a vibration-inducing mounted at its mid-length, within a time corresponding to their weight. Comparing the values of residual stress existing in the tube before and after the vibration treatment achieved a mean reduction of 16 % in the amount thereof. For the mechanical characterization of the pipe, before and after the vibration process, the following tests were conducted according to API standard 5CT 2001: Charpy 'V', tensile tests and hardness Rockwell C, both in the metal base tube, and in the weld region. It was also carried out their microstructural characterization through optical microscopy before and after the vibration tests. To evaluate the residual stress before and after the vibration tests, we used the ring splitting test according to ASTM E1928-13.

Conselho Nacional de Desenvolvimento Científico e Tecnológico / The dissertation was divided in three studies. Our first study determined the correlation between high somatic cell counts and positive milk ring tests (MRT). The milk ring test was performed on 181 milk samples from expansion tanks located at various rural sites in the regions of Brazil. Somatic cell counts (SCC) via flow cytometry were also performed. MRT identified 11 positive samples (6%) where the majority were reactive and 5 (2.8%) were found in the 6x105 cel/mL range. The results showed that there was no statistical relationship between high somatic cell counts and positive milk ring tests. Our second study evaluated the efficiency of an enzyme linked immunosorbent assay kit (ELISA) in diagnosing brucellosis in collective milk samples. The indirect ELISA test was used on 181 samples of fresh milk and identified 42 positive, 11 suspect and 128 negative samples. These results were compared to the MR test, the only test approved for collective milk samples by the Brazilian Ministry of Agriculture, Livestock and Supply (Ministério da Agricultura Pecuária e Abastecimento). The ELISA test had sensitivity of 72.7%, specificity of 78.6% and a Kappa concordance index of 0.22. Subsequently, random samples from lactating animals in nine herds were tested individually by the rose Bengal test (RBT) and the 2-mercaptoethanol 2(ME) tests. Positive animals were found only in herds that tested positive in both ELISA and MRT. The ELISA test was neither as sensitive nor as specific as reported in other countries where the ELISA test is used and where brucellosis outbreaks have been confirmed in dairy herds. Our third study used the Polymerase Chain Reaction (PCR) technique to detect Brucella abortus in samples of fresh milk. Ninety samples were preselected for the PCR test including 45 that tested positive in ELISA and/or MRT, 11 suspect in ELISA and 34 negative in both tests. Extraction was carried out by enzymatic lysis followed by amplification using BAB and IS 711 primers, which amplify fragments of 498 base pairs. Visualization was accomplished with 1% agarose gel and an Alpha Digidoc Photo Documentation system. Brucella abortus DNA was not amplified in any of the samples, demonstrating that PCR is not the best screening technique for brucellosis in milk samples at the herd level, given that these microorganisms do not always escape into the milk. / A dissertação foi dividida em três estudos. O primeiro objetivou verificar a existência de correlação entre altas contagens de células somáticas e reações positivas no Teste do anel em leite (TAL). Foram coletadas 181 amostras de leite oriundas de tanques de expansão provenientes de diferentes propriedades rurais e submetidas ao Teste de Anel em Leite (TAL). Também foi realizada a contagem de células somáticas (CCS) através do método de citometria de fluxo. O TAL resultou em 11 amostras positivas (6%), da quais, 5 (45,4%) encontravam-se na faixa de 6x105 cel/mL. Os resultados das análises demonstraram não haver associação estatística entre altas contagens de células somáticas e reações positivas no Teste de Anel em Leite. O segundo estudo teve como objetivo avaliar a eficiência de um kit de teste imunoenzimático indireto (ELISA) para diagnóstico de brucelose em amostras coletivas de leite. Amostras de leite in natura, totalizando 181, foram submetidas ao teste ELISA indireto. O teste ELISA identificou 42 (23,2%) amostras positivas, 11 (6%) suspeitas e 128 (70,7%) negativas. Para comparação foi utilizado o TAL. O ELISA apresentou sensibilidade de 72,7%, especificidade de 78,6% e um índice de concordância Kappa de 0,22. Posteriormente 9 rebanhos foram selecionados para realização de testes individuais de Antígeno Acidificado Tamponado (AAT) e 2-Mercaptoetanol 2(ME), por meio de amostragem aleatória dos animais em lactação. Foram encontrados animais reagentes apenas em rebanhos considerados positivos no TAL e no ELISA simultaneamente. Constatou-se que o teste ELISA apresentou valores de sensibilidade e especificidade inferiores aos relatados em outros países onde o teste ELISA já é utilizado, assim como foi confirmada a existência de focos de brucelose em rebanhos leiteiros. No terceiro estudo, a Reação em Cadeia de Polimerase (PCR) foi empregada para detecção de Brucella abortus em amostras de leite in natura. Foram selecionadas 90 amostras para realização da técnica de PCR, sendo 8 positivas no TAL, 37 positivas no ELISA, 11 suspeitas no ELISA e 34 negativas em ambos os testes. A extração foi realizada por meio de lise enzimática, seguida de amplificação utilizando primers BAB e IS 711, que amplificam fragmentos de 498 pares de bases. A visualização foi realizada utilizando gel de agarose 1% em fotodocumentador Alpha Digi Doc. Não foi amplificado DNA de Brucella abortus, demonstrando a PCR não se a melhor técnica para o diagnóstico de brucelose em amostras coletivas de leite. / Mestre em Ciências Veterinárias

The autogenous shrinkage due to self-desiccation of high- and ultra-high performance concretes with very low water-cement ratio in case of restraint leads to considerable stresses starting from very early age. The resultant risk of cracking presently cannot be adequately investigated. Parameters that are particularly difficult to capture experimentally are the concrete temperature and the viscoelasticity. The primary objective of this work was to assess as precise as possible the autogenous shrinkage cracking propensity of representative concretes at strong restraint and constant room temperature. Test methods needed to be chosen and enhanced in a way that preferably allowed for the efficient and precise investigation of all relevant factors in the future. Ideally, a method suitable for a complete empirical modeling was provided. First the methodological requirements and the advantages and disadvantages of existing test methods were discussed. Based on this, optimized test methods were proposed. Their suitability was verified using the example of ultra-high strength concrete. The choice of concrete compositions considered the essential measures for reducing shrinkage (internal curing, shrinkage-reducing admixtures, reduction of the fraction of Portland cement in the binder). The autogenous shrinkage was measured with the shrinkage cone method. This new test method was validated by investigations of the repeatability and reproducibility and proved efficient and precise. It allows for measurements under non-isothermal conditions; no established test method exists for that purpose to date. The autogenous shrinkage of the ultra-high strength concretes at the age of 24 h, investigated under quasi-isothermal conditions (20 °C), was between 0,25 mm/m and 0,70 mm/m. It was particularly low when a shrinkage-reducing admixture was added and when superabsorbent polymers were used. The stresses due to restraint were determined with the restrained ring test. A large part of the stresses to be expected according to Hooke’s Law were eliminated by creep and relaxation. The relaxation capacity being very pronounced at very early age was the main reason that no visible cracking occurred, not even with the concretes with high autogenous shrinkage. The development of the autogenous shrinkage cracking propensity was described as ratio of restraint stress and splitting tensile strength. By means of modified ring tests, used to determine the maximum tensile stress, it could be shown that the ratio of stress to strength is an appropriate failure criterion. However, the cracking propensity can be calculated correctly only if the strongly age-dependent ratio of uniaxial to splitting tensile strength is accounted for. Besides, it needs to be considered that at very early age a plastic stress redistribution may occur in restrained ring tests. The reference concrete showed a high cracking propensity of up to 0.68. The fact that shrinkage-reducing measures led to significantly lower values reveals their relevance for the safe application of ultra-high strength concrete. However, the investigations carried out here at 20 °C do not allow for a final assessment of the cracking propensity under typical on-site conditions. To empirically model the autogenous shrinkage cracking propensity as a function of temperature and stress level in the future, an analytical stress solution for non-isothermal restrained ring tests and a new approach for investigating the residual stress and relaxation capacity by means of non-passive restrained ring tests was suggested. / Das durch Selbstaustrocknung verursachte autogene Schwinden von besonders leistungsfähigen Betonen mit sehr niedrigem Wasserzementwert führt bei Dehnungsbehinderung bereits in sehr frühem Alter zu erheblichen Zwangsspannungen. Die Gefahr der Rissbildung, die sich daraus ergibt, lässt sich bislang nur unzureichend untersuchen. Experimentell besonders schwer zu erfassende Faktoren sind die Betontemperatur und die Viskoelastizität. Das vorrangige Ziel der Arbeit war die möglichst genaue Ermittlung der autogenen Schwindrissneigung repräsentativer Betone bei starker Dehnungsbehinderung und konstanter Raumtemperatur. Dabei waren die Prüfverfahren möglichst so zu wählen und weiterzuentwickeln, dass sich zukünftig alle relevanten Faktoren effizient und genau untersuchen lassen. Im Idealfall sollte eine Methode entstehen, die eine vollständige empirische Modellierung erlaubt. Zunächst wurden die methodischen Anforderungen und die Vor- und Nachteile existierender Prüfverfahren diskutiert. Darauf aufbauend wurden optimierte Verfahren vorgeschlagen. Ihre Eignung wurde an ultrahochfestem Beton überprüft. Bei der Auswahl der Betone wurden die wesentlichen Maßnahmen zur Schwindreduzierung berücksichtigt (innere Nachbehandlung, schwindreduzierende Zusatzmittel, Verringerung des Portlandzementanteils am Bindemittel). Das autogene Schwinden wurde mit dem Schwindkegelverfahren gemessen. Das neue Verfahren wurde durch Untersuchungen zur Wiederhol- und Vergleichsgenauigkeit validiert und erwies sich als effizient und genau. Es ermöglicht Messungen unter nicht-isothermen Bedingungen; hierfür existiert bisher kein etabliertes Verfahren. Das autogene Schwinden der untersuchten ultrahochfesten Betone unter quasi-isothermen Bedingungen (20 °C) betrug im Alter von 24 h zwischen 0,25 mm/m und 0,70 mm/m. Besonders gering war es bei Zugabe eines schwindreduzierenden Zusatzmittels bzw. Verwendung superabsorbierender Polymere. Mit dem Ring-Test wurden die bei Dehnungsbehinderung entstehenden Spannungen ermittelt. Ein großer Teil der gemäß Hooke’schem Gesetz zu erwartenden Spannungen wurde durch Kriechen und Relaxation abgebaut. Die im sehr frühen Alter stark ausgeprägte Relaxationsfähigkeit war der wesentliche Grund dafür, dass es selbst bei Betonen mit hohem autogenen Schwinden zu keiner erkennbaren Rissbildung kam. Die Entwicklung der autogenen Schwindrissneigung wurde als Verhältnis von Zwangsspannung und Spaltzugfestigkeit beschrieben. Durch modifizierte Ring-Tests, mit deren Hilfe die maximale Zugspannung ermittelt wurde, konnte gezeigt werden, dass das Verhältnis von Spannung und Festigkeit als Versagenskriterium geeignet ist. Die Rissneigung lässt sich aber nur dann korrekt berechnen, wenn das stark altersabhängige Verhältnis von einaxialer Zugfestigkeit und Spaltzugfestigkeit berücksichtigt wird. Außerdem ist zu beachten, dass es im sehr frühen Alter zu einer plastischen Spannungsumlagerung in Ring-Tests kommen kann. Der Referenzbeton wies eine hohe Rissneigung von bis zu 0,68 auf. Dass die schwindreduzierenden Maßnahmen zu deutlich geringeren Werten führten, zeigt deren Bedeutung für den sicheren Einsatz von ultrahochfestem Beton. Die hier bei 20 °C durchgeführten Untersuchungen erlauben allerdings keine abschließende Bewertung der Rissneigung unter baustellentypischen Bedingungen. Um die autogene Schwindrissneigung zukünftig als Funktion der Temperatur und des Lastniveaus empirisch modellieren zu können, wurden eine analytische Spannungslösung für nicht-isotherme Ring-Tests und ein neuer Ansatz zur Untersuchung der Resttrag- und Relaxationsfähigkeit mit Hilfe nicht-passiver Ring-Tests vorgeschlagen.

The autogenous shrinkage due to self-desiccation of high- and ultra-high performance concretes with very low water-cement ratio in case of restraint leads to considerable stresses starting from very early age. The resultant risk of cracking presently cannot be adequately investigated. Parameters that are particularly difficult to capture experimentally are the concrete temperature and the viscoelasticity. The primary objective of this work was to assess as precise as possible the autogenous shrinkage cracking propensity of representative concretes at strong restraint and constant room temperature. Test methods needed to be chosen and enhanced in a way that preferably allowed for the efficient and precise investigation of all relevant factors in the future. Ideally, a method suitable for a complete empirical modeling was provided. First the methodological requirements and the advantages and disadvantages of existing test methods were discussed. Based on this, optimized test methods were proposed. Their suitability was verified using the example of ultra-high strength concrete. The choice of concrete compositions considered the essential measures for reducing shrinkage (internal curing, shrinkage-reducing admixtures, reduction of the fraction of Portland cement in the binder). The autogenous shrinkage was measured with the shrinkage cone method. This new test method was validated by investigations of the repeatability and reproducibility and proved efficient and precise. It allows for measurements under non-isothermal conditions; no established test method exists for that purpose to date. The autogenous shrinkage of the ultra-high strength concretes at the age of 24 h, investigated under quasi-isothermal conditions (20 °C), was between 0,25 mm/m and 0,70 mm/m. It was particularly low when a shrinkage-reducing admixture was added and when superabsorbent polymers were used. The stresses due to restraint were determined with the restrained ring test. A large part of the stresses to be expected according to Hooke’s Law were eliminated by creep and relaxation. The relaxation capacity being very pronounced at very early age was the main reason that no visible cracking occurred, not even with the concretes with high autogenous shrinkage. The development of the autogenous shrinkage cracking propensity was described as ratio of restraint stress and splitting tensile strength. By means of modified ring tests, used to determine the maximum tensile stress, it could be shown that the ratio of stress to strength is an appropriate failure criterion. However, the cracking propensity can be calculated correctly only if the strongly age-dependent ratio of uniaxial to splitting tensile strength is accounted for. Besides, it needs to be considered that at very early age a plastic stress redistribution may occur in restrained ring tests. The reference concrete showed a high cracking propensity of up to 0.68. The fact that shrinkage-reducing measures led to significantly lower values reveals their relevance for the safe application of ultra-high strength concrete. However, the investigations carried out here at 20 °C do not allow for a final assessment of the cracking propensity under typical on-site conditions. To empirically model the autogenous shrinkage cracking propensity as a function of temperature and stress level in the future, an analytical stress solution for non-isothermal restrained ring tests and a new approach for investigating the residual stress and relaxation capacity by means of non-passive restrained ring tests was suggested.:1 Introduction 2 Autogenous shrinkage 5 2.1 Shrinkage and hydration 5 2.2 Definitions and research approaches 10 2.3 Metrological issues 14 2.3.1 Multitude of test methods 14 2.3.2 Time-zero 16 2.3.3 Other metrological issues 18 2.4 Corrugated tube method 19 2.5 Influencing parameters 21 2.5.1 Concrete composition 21 2.5.2 Temperature 23 2.5.3 Specific countermeasures 25 2.6 Summary and conclusions with respect to the own work 25 3 Concretes used in the own investigations 27 3.1 Preliminary remarks 27 3.2 Concrete compositions 27 3.3 Constituents 28 3.3.1 Cement 28 3.3.2 Ground-granulated blast furnace slag 28 3.3.3 Silica fume 28 3.3.4 Admixtures 29 3.3.5 Aggregates 29 3.4 Mixing 29 3.5 Basic properties 30 3.5.1 Compressive strength 30 3.5.2 Splitting tensile strength 31 3.5.3 Modulus of elasticity 33 3.5.4 Analysis of mechanical properties 35 3.5.5 Coefficient of thermal expansion 38 3.5.6 Isothermal calorimetry 39 3.6 Summary 39 4 Shrinkage cone method for measuring autogenous shrinkage 41 4.1 Introduction 41 4.2 Setup and measurement procedure 41 4.3 Temperature control 44 4.4 Precision under quasi-isothermal conditions 47 4.4.1 Repeatability 47 4.4.2 Reproducibility 49 4.4.3 Shrinkage cone method vs. corrugated tube method 49 4.5 Autogenous shrinkage of the investigated concretes at 20 °C 54 4.6 Tests under non-isothermal conditions 55 4.7 Summary 56 5 Stress and cracks due to restrained autogenous shrinkage 58 5.1 Introduction 58 5.2 Degree of restraint 58 5.3 Formation of cracks 60 5.4 Very early age and importance of stress relaxation 63 5.5 Creep and cracking - further methodological aspects 65 5.6 Autogenous shrinkage cracking propensity 69 5.7 Role of temperature history 70 5.8 Further state of knowledge 72 5.8.1 Preliminary remarks on test methods 72 5.8.2 Quantitative investigations under restraint conditions 73 5.8.3 A full-scale model for assessing the cracking risk at very early age 77 5.9 Summary 78 6 Investigation of the autogenous shrinkage cracking propensity 80 6.1 Introduction 80 6.2 Suitability of temperature-stress testing machines 80 6.2.1 Development, setup and use 80 6.2.2 Results of round robin tests 83 6.3 Restrained ring test - methodological foundations 86 6.3.1 Setup and use 86 6.3.2 Evaluation of restrained ring tests 90 6.3.3 Use of temperature changes for the investigation of creep and relaxation 96 6.4 Own investigations with the restrained ring test 97 6.4.1 Setup 97 6.4.2 Compensation of disturbing temperature effects 99 6.4.3 Repeatability 100 6.4.4 Measured steel ring strains 101 6.4.5 Simple stress analysis 102 6.4.6 Autogenous shrinkage cracking propensity - further analysis 106 6.4.7 Thermal stress component 116 6.4.8 Period of maximum cracking propensity 118 6.4.9 Restraint stress versus autogenous shrinkage 119 6.4.10 Cracking propensity versus autogenous shrinkage 120 6.4.11 Further considerations on creep 121 6.5 Summary 126 7 Summary, conclusions and outlook 128 7.1 Summary and conclusions 128 7.2 Outlook 130 8 Literature 131 9 Annex 159 / Das durch Selbstaustrocknung verursachte autogene Schwinden von besonders leistungsfähigen Betonen mit sehr niedrigem Wasserzementwert führt bei Dehnungsbehinderung bereits in sehr frühem Alter zu erheblichen Zwangsspannungen. Die Gefahr der Rissbildung, die sich daraus ergibt, lässt sich bislang nur unzureichend untersuchen. Experimentell besonders schwer zu erfassende Faktoren sind die Betontemperatur und die Viskoelastizität. Das vorrangige Ziel der Arbeit war die möglichst genaue Ermittlung der autogenen Schwindrissneigung repräsentativer Betone bei starker Dehnungsbehinderung und konstanter Raumtemperatur. Dabei waren die Prüfverfahren möglichst so zu wählen und weiterzuentwickeln, dass sich zukünftig alle relevanten Faktoren effizient und genau untersuchen lassen. Im Idealfall sollte eine Methode entstehen, die eine vollständige empirische Modellierung erlaubt. Zunächst wurden die methodischen Anforderungen und die Vor- und Nachteile existierender Prüfverfahren diskutiert. Darauf aufbauend wurden optimierte Verfahren vorgeschlagen. Ihre Eignung wurde an ultrahochfestem Beton überprüft. Bei der Auswahl der Betone wurden die wesentlichen Maßnahmen zur Schwindreduzierung berücksichtigt (innere Nachbehandlung, schwindreduzierende Zusatzmittel, Verringerung des Portlandzementanteils am Bindemittel). Das autogene Schwinden wurde mit dem Schwindkegelverfahren gemessen. Das neue Verfahren wurde durch Untersuchungen zur Wiederhol- und Vergleichsgenauigkeit validiert und erwies sich als effizient und genau. Es ermöglicht Messungen unter nicht-isothermen Bedingungen; hierfür existiert bisher kein etabliertes Verfahren. Das autogene Schwinden der untersuchten ultrahochfesten Betone unter quasi-isothermen Bedingungen (20 °C) betrug im Alter von 24 h zwischen 0,25 mm/m und 0,70 mm/m. Besonders gering war es bei Zugabe eines schwindreduzierenden Zusatzmittels bzw. Verwendung superabsorbierender Polymere. Mit dem Ring-Test wurden die bei Dehnungsbehinderung entstehenden Spannungen ermittelt. Ein großer Teil der gemäß Hooke’schem Gesetz zu erwartenden Spannungen wurde durch Kriechen und Relaxation abgebaut. Die im sehr frühen Alter stark ausgeprägte Relaxationsfähigkeit war der wesentliche Grund dafür, dass es selbst bei Betonen mit hohem autogenen Schwinden zu keiner erkennbaren Rissbildung kam. Die Entwicklung der autogenen Schwindrissneigung wurde als Verhältnis von Zwangsspannung und Spaltzugfestigkeit beschrieben. Durch modifizierte Ring-Tests, mit deren Hilfe die maximale Zugspannung ermittelt wurde, konnte gezeigt werden, dass das Verhältnis von Spannung und Festigkeit als Versagenskriterium geeignet ist. Die Rissneigung lässt sich aber nur dann korrekt berechnen, wenn das stark altersabhängige Verhältnis von einaxialer Zugfestigkeit und Spaltzugfestigkeit berücksichtigt wird. Außerdem ist zu beachten, dass es im sehr frühen Alter zu einer plastischen Spannungsumlagerung in Ring-Tests kommen kann. Der Referenzbeton wies eine hohe Rissneigung von bis zu 0,68 auf. Dass die schwindreduzierenden Maßnahmen zu deutlich geringeren Werten führten, zeigt deren Bedeutung für den sicheren Einsatz von ultrahochfestem Beton. Die hier bei 20 °C durchgeführten Untersuchungen erlauben allerdings keine abschließende Bewertung der Rissneigung unter baustellentypischen Bedingungen. Um die autogene Schwindrissneigung zukünftig als Funktion der Temperatur und des Lastniveaus empirisch modellieren zu können, wurden eine analytische Spannungslösung für nicht-isotherme Ring-Tests und ein neuer Ansatz zur Untersuchung der Resttrag- und Relaxationsfähigkeit mit Hilfe nicht-passiver Ring-Tests vorgeschlagen.:1 Introduction 2 Autogenous shrinkage 5 2.1 Shrinkage and hydration 5 2.2 Definitions and research approaches 10 2.3 Metrological issues 14 2.3.1 Multitude of test methods 14 2.3.2 Time-zero 16 2.3.3 Other metrological issues 18 2.4 Corrugated tube method 19 2.5 Influencing parameters 21 2.5.1 Concrete composition 21 2.5.2 Temperature 23 2.5.3 Specific countermeasures 25 2.6 Summary and conclusions with respect to the own work 25 3 Concretes used in the own investigations 27 3.1 Preliminary remarks 27 3.2 Concrete compositions 27 3.3 Constituents 28 3.3.1 Cement 28 3.3.2 Ground-granulated blast furnace slag 28 3.3.3 Silica fume 28 3.3.4 Admixtures 29 3.3.5 Aggregates 29 3.4 Mixing 29 3.5 Basic properties 30 3.5.1 Compressive strength 30 3.5.2 Splitting tensile strength 31 3.5.3 Modulus of elasticity 33 3.5.4 Analysis of mechanical properties 35 3.5.5 Coefficient of thermal expansion 38 3.5.6 Isothermal calorimetry 39 3.6 Summary 39 4 Shrinkage cone method for measuring autogenous shrinkage 41 4.1 Introduction 41 4.2 Setup and measurement procedure 41 4.3 Temperature control 44 4.4 Precision under quasi-isothermal conditions 47 4.4.1 Repeatability 47 4.4.2 Reproducibility 49 4.4.3 Shrinkage cone method vs. corrugated tube method 49 4.5 Autogenous shrinkage of the investigated concretes at 20 °C 54 4.6 Tests under non-isothermal conditions 55 4.7 Summary 56 5 Stress and cracks due to restrained autogenous shrinkage 58 5.1 Introduction 58 5.2 Degree of restraint 58 5.3 Formation of cracks 60 5.4 Very early age and importance of stress relaxation 63 5.5 Creep and cracking - further methodological aspects 65 5.6 Autogenous shrinkage cracking propensity 69 5.7 Role of temperature history 70 5.8 Further state of knowledge 72 5.8.1 Preliminary remarks on test methods 72 5.8.2 Quantitative investigations under restraint conditions 73 5.8.3 A full-scale model for assessing the cracking risk at very early age 77 5.9 Summary 78 6 Investigation of the autogenous shrinkage cracking propensity 80 6.1 Introduction 80 6.2 Suitability of temperature-stress testing machines 80 6.2.1 Development, setup and use 80 6.2.2 Results of round robin tests 83 6.3 Restrained ring test - methodological foundations 86 6.3.1 Setup and use 86 6.3.2 Evaluation of restrained ring tests 90 6.3.3 Use of temperature changes for the investigation of creep and relaxation 96 6.4 Own investigations with the restrained ring test 97 6.4.1 Setup 97 6.4.2 Compensation of disturbing temperature effects 99 6.4.3 Repeatability 100 6.4.4 Measured steel ring strains 101 6.4.5 Simple stress analysis 102 6.4.6 Autogenous shrinkage cracking propensity - further analysis 106 6.4.7 Thermal stress component 116 6.4.8 Period of maximum cracking propensity 118 6.4.9 Restraint stress versus autogenous shrinkage 119 6.4.10 Cracking propensity versus autogenous shrinkage 120 6.4.11 Further considerations on creep 121 6.5 Summary 126 7 Summary, conclusions and outlook 128 7.1 Summary and conclusions 128 7.2 Outlook 130 8 Literature 131 9 Annex 159

Esta tese apresenta o estudo sobre microconformação, no caso microextrusão de quatro materiais diferentes, um aço SAE 1020, um aço inoxidável AISI 304, um alumínio AA6531 e um latão ASTM C34000. Para avaliar o efeito do tamanho da peça sobre o processo de microextrusão, dois tamanhos de corpos de prova foram utilizados, um com ∅ 4 mm e outro com ∅ 1 mm. Para cada tamanho de corpo de prova, três ângulos de extrusão foram utilizados, 30°, 45° e 60°. A primeira parte do trabalho se resume a caracterização dos materiais, com analise química e metalográfica. Após a caracterização dos materiais, as curvas de escoamento através do ensaio de compressão utilizando dois tamanhos de corpos de prova foram feitos em todos os materiais. O atrito foi determinado utilizando o ensaio de anel de atrito com três tamanhos diferentes de corpos de prova. As curvas de calibração foram feitas utilizando o software SIMUFACT. Os ensaios de extrusão foram feitos em uma máquina de ensaio universal com capacidade de captura de dados como força e deslocamento. Um modelo matemático foi utilizado para comparar a força de extrusão calculada com o medido no processo. Os resultados indicam que as curvas de escoamento de tamanho macro podem ser aplicadas a peças de tamanho meso. O atrito medido pelo ensaio de anel de atrito mostrou que os valores de atrito de tamanho micro tem um pequeno valor maior que para tamanho macro. Os valores de força de extrusão calculada e medido no ensaio para peças de tamanho meso tem boa aproximação com diferença de 3,2% para o aço inoxidável. Para peça de tamanho micro, a diferença entre o valor medido e o calculado aumenta chegando a diferença de 995% para o corpos de prova de aço comum. / This thesis presents the study about microforming, in this case microextrusion of the four different materials, an SAE 1020 steel, an AISI 304 stainless steel, an AA6531 aluminum and a C34000 brass. To evaluate the size effect about microextrusion process, two sizes of specimens were used, with a ∅ 4 mm and another with ∅ 1 mm. For each size of specimen, three extrusion angles were used, 30 °, 45 ° and 60 °. The first part of the work was to materials characterizations with chemical and metallographic analysis. Following the materials characterization, the flow stress curves was made using the compression test with two sizes of specimens. The friction was determined using the friction ring test with the three different size. Calibration curves were performed using the software SIMUFACT . The extrusion tests were performed in a universal testing machine capable of capturing such as force and displacement data. A mathematical model was used to compare the extrusion force it was calculated and the force measured in microextrusion. The results indicate that the flow stress curves of macro size can be applied to meso sizes. The ring friction test indicate that the friction values of the micro size has a small value greater than macro size. The extrusion force calculated and measured in the test to meso size has good approximation with a difference of 3.2% in the stainless steel. To pieces of the micro size, the difference between the measured and calculated force increases 995% for the samples of SAE 1020 steel.

Esta tese apresenta o estudo sobre microconformação, no caso microextrusão de quatro materiais diferentes, um aço SAE 1020, um aço inoxidável AISI 304, um alumínio AA6531 e um latão ASTM C34000. Para avaliar o efeito do tamanho da peça sobre o processo de microextrusão, dois tamanhos de corpos de prova foram utilizados, um com ∅ 4 mm e outro com ∅ 1 mm. Para cada tamanho de corpo de prova, três ângulos de extrusão foram utilizados, 30°, 45° e 60°. A primeira parte do trabalho se resume a caracterização dos materiais, com analise química e metalográfica. Após a caracterização dos materiais, as curvas de escoamento através do ensaio de compressão utilizando dois tamanhos de corpos de prova foram feitos em todos os materiais. O atrito foi determinado utilizando o ensaio de anel de atrito com três tamanhos diferentes de corpos de prova. As curvas de calibração foram feitas utilizando o software SIMUFACT. Os ensaios de extrusão foram feitos em uma máquina de ensaio universal com capacidade de captura de dados como força e deslocamento. Um modelo matemático foi utilizado para comparar a força de extrusão calculada com o medido no processo. Os resultados indicam que as curvas de escoamento de tamanho macro podem ser aplicadas a peças de tamanho meso. O atrito medido pelo ensaio de anel de atrito mostrou que os valores de atrito de tamanho micro tem um pequeno valor maior que para tamanho macro. Os valores de força de extrusão calculada e medido no ensaio para peças de tamanho meso tem boa aproximação com diferença de 3,2% para o aço inoxidável. Para peça de tamanho micro, a diferença entre o valor medido e o calculado aumenta chegando a diferença de 995% para o corpos de prova de aço comum. / This thesis presents the study about microforming, in this case microextrusion of the four different materials, an SAE 1020 steel, an AISI 304 stainless steel, an AA6531 aluminum and a C34000 brass. To evaluate the size effect about microextrusion process, two sizes of specimens were used, with a ∅ 4 mm and another with ∅ 1 mm. For each size of specimen, three extrusion angles were used, 30 °, 45 ° and 60 °. The first part of the work was to materials characterizations with chemical and metallographic analysis. Following the materials characterization, the flow stress curves was made using the compression test with two sizes of specimens. The friction was determined using the friction ring test with the three different size. Calibration curves were performed using the software SIMUFACT . The extrusion tests were performed in a universal testing machine capable of capturing such as force and displacement data. A mathematical model was used to compare the extrusion force it was calculated and the force measured in microextrusion. The results indicate that the flow stress curves of macro size can be applied to meso sizes. The ring friction test indicate that the friction values of the micro size has a small value greater than macro size. The extrusion force calculated and measured in the test to meso size has good approximation with a difference of 3.2% in the stainless steel. To pieces of the micro size, the difference between the measured and calculated force increases 995% for the samples of SAE 1020 steel.

Esta tese apresenta o estudo sobre microconformação, no caso microextrusão de quatro materiais diferentes, um aço SAE 1020, um aço inoxidável AISI 304, um alumínio AA6531 e um latão ASTM C34000. Para avaliar o efeito do tamanho da peça sobre o processo de microextrusão, dois tamanhos de corpos de prova foram utilizados, um com ∅ 4 mm e outro com ∅ 1 mm. Para cada tamanho de corpo de prova, três ângulos de extrusão foram utilizados, 30°, 45° e 60°. A primeira parte do trabalho se resume a caracterização dos materiais, com analise química e metalográfica. Após a caracterização dos materiais, as curvas de escoamento através do ensaio de compressão utilizando dois tamanhos de corpos de prova foram feitos em todos os materiais. O atrito foi determinado utilizando o ensaio de anel de atrito com três tamanhos diferentes de corpos de prova. As curvas de calibração foram feitas utilizando o software SIMUFACT. Os ensaios de extrusão foram feitos em uma máquina de ensaio universal com capacidade de captura de dados como força e deslocamento. Um modelo matemático foi utilizado para comparar a força de extrusão calculada com o medido no processo. Os resultados indicam que as curvas de escoamento de tamanho macro podem ser aplicadas a peças de tamanho meso. O atrito medido pelo ensaio de anel de atrito mostrou que os valores de atrito de tamanho micro tem um pequeno valor maior que para tamanho macro. Os valores de força de extrusão calculada e medido no ensaio para peças de tamanho meso tem boa aproximação com diferença de 3,2% para o aço inoxidável. Para peça de tamanho micro, a diferença entre o valor medido e o calculado aumenta chegando a diferença de 995% para o corpos de prova de aço comum. / This thesis presents the study about microforming, in this case microextrusion of the four different materials, an SAE 1020 steel, an AISI 304 stainless steel, an AA6531 aluminum and a C34000 brass. To evaluate the size effect about microextrusion process, two sizes of specimens were used, with a ∅ 4 mm and another with ∅ 1 mm. For each size of specimen, three extrusion angles were used, 30 °, 45 ° and 60 °. The first part of the work was to materials characterizations with chemical and metallographic analysis. Following the materials characterization, the flow stress curves was made using the compression test with two sizes of specimens. The friction was determined using the friction ring test with the three different size. Calibration curves were performed using the software SIMUFACT . The extrusion tests were performed in a universal testing machine capable of capturing such as force and displacement data. A mathematical model was used to compare the extrusion force it was calculated and the force measured in microextrusion. The results indicate that the flow stress curves of macro size can be applied to meso sizes. The ring friction test indicate that the friction values of the micro size has a small value greater than macro size. The extrusion force calculated and measured in the test to meso size has good approximation with a difference of 3.2% in the stainless steel. To pieces of the micro size, the difference between the measured and calculated force increases 995% for the samples of SAE 1020 steel.

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